WO2021075508A1 - Absorbent article and auxiliary sheet - Google Patents
Absorbent article and auxiliary sheet Download PDFInfo
- Publication number
- WO2021075508A1 WO2021075508A1 PCT/JP2020/038951 JP2020038951W WO2021075508A1 WO 2021075508 A1 WO2021075508 A1 WO 2021075508A1 JP 2020038951 W JP2020038951 W JP 2020038951W WO 2021075508 A1 WO2021075508 A1 WO 2021075508A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- water
- sheet
- resin particles
- absorbent resin
- swelling
- Prior art date
Links
- 239000002250 absorbent Substances 0.000 title claims abstract description 279
- 230000002745 absorbent Effects 0.000 title claims abstract description 108
- 239000002245 particle Substances 0.000 claims abstract description 231
- 239000011347 resin Substances 0.000 claims abstract description 169
- 229920005989 resin Polymers 0.000 claims abstract description 169
- 238000010521 absorption reaction Methods 0.000 claims abstract description 128
- 230000008961 swelling Effects 0.000 claims abstract description 121
- 239000007788 liquid Substances 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 171
- 238000012360 testing method Methods 0.000 claims description 78
- 239000002504 physiological saline solution Substances 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 15
- 239000010410 layer Substances 0.000 description 113
- 239000000178 monomer Substances 0.000 description 93
- 229920000642 polymer Polymers 0.000 description 82
- -1 N, N-diethylaminoethyl Chemical group 0.000 description 81
- 239000004745 nonwoven fabric Substances 0.000 description 66
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 63
- 239000000835 fiber Substances 0.000 description 59
- 238000006116 polymerization reaction Methods 0.000 description 58
- 238000000034 method Methods 0.000 description 46
- 239000000853 adhesive Substances 0.000 description 45
- 230000001070 adhesive effect Effects 0.000 description 45
- 239000000463 material Substances 0.000 description 45
- 239000007864 aqueous solution Substances 0.000 description 44
- 239000002585 base Substances 0.000 description 40
- 239000003431 cross linking reagent Substances 0.000 description 40
- 238000004132 cross linking Methods 0.000 description 33
- 238000003756 stirring Methods 0.000 description 30
- 229930195733 hydrocarbon Natural products 0.000 description 23
- 239000004094 surface-active agent Substances 0.000 description 23
- 238000004519 manufacturing process Methods 0.000 description 22
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 21
- 150000002430 hydrocarbons Chemical class 0.000 description 21
- 239000012071 phase Substances 0.000 description 21
- 239000004215 Carbon black (E152) Substances 0.000 description 20
- 150000001875 compounds Chemical class 0.000 description 20
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- 239000000017 hydrogel Substances 0.000 description 19
- 239000007870 radical polymerization initiator Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 235000014113 dietary fatty acids Nutrition 0.000 description 18
- 239000000194 fatty acid Substances 0.000 description 18
- 229930195729 fatty acid Natural products 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 17
- 239000010954 inorganic particle Substances 0.000 description 17
- 239000000203 mixture Substances 0.000 description 17
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 15
- 239000002609 medium Substances 0.000 description 15
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 14
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 14
- 239000002270 dispersing agent Substances 0.000 description 14
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 13
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 12
- 210000002700 urine Anatomy 0.000 description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 11
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- 238000001035 drying Methods 0.000 description 8
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- 239000002657 fibrous material Substances 0.000 description 7
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 7
- IVIDDMGBRCPGLJ-UHFFFAOYSA-N 2,3-bis(oxiran-2-ylmethoxy)propan-1-ol Chemical compound C1OC1COC(CO)COCC1CO1 IVIDDMGBRCPGLJ-UHFFFAOYSA-N 0.000 description 6
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- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 5
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- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
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- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 239000003945 anionic surfactant Substances 0.000 description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 4
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- HDPLHDGYGLENEI-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COC(C)COCC1CO1 HDPLHDGYGLENEI-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- 230000003187 abdominal effect Effects 0.000 description 3
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- GKIPXFAANLTWBM-UHFFFAOYSA-N epibromohydrin Chemical compound BrCC1CO1 GKIPXFAANLTWBM-UHFFFAOYSA-N 0.000 description 3
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Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
- A61F13/534—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having an inhomogeneous composition through the thickness of the pad
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
- A61F13/534—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having an inhomogeneous composition through the thickness of the pad
- A61F13/537—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having an inhomogeneous composition through the thickness of the pad characterised by a layer facilitating or inhibiting flow in one direction or plane, e.g. a wicking layer
Definitions
- the present invention relates to an absorbent article and an auxiliary sheet.
- an absorber having an absorbing layer capable of absorbing a liquid is used as an absorbent article for absorbing a liquid containing water as a main component such as urine.
- Patent Document 1 describes an absorbent article having a width direction and a front-rear direction, and having a top sheet, a back sheet, and a first absorbent body provided between them; a plurality of first absorbent bodies are provided. It contains a layer of sheet members, is configured to have a water-absorbent resin between the sheet members and no pulp fibers, and has end regions and a central region located between them on both sides in the width direction; An absorbent article in which a water-absorbent resin having a water absorption rate of 20 seconds or less by the vortex method is arranged in a partial region; and a water-absorbent resin having a water absorption rate of 40 seconds or more by the vortex method is arranged in a central region is disclosed. Has been done.
- absorbent articles such as diapers can absorb more liquid when worn, and that liquid leakage to the outside of the absorbent articles is suppressed.
- An object of the present invention is to provide an absorbent article having a high liquid absorption amount when worn by a user and in which liquid leakage is suppressed. It is also an object of the present invention to provide an auxiliary sheet which has a high liquid absorption amount when worn by a user and can provide an absorbent article in which liquid leakage is suppressed.
- One aspect of the present invention includes a strip-shaped water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet and a liquid permeable sheet, and includes a liquid impermeable sheet, a water absorbing core and a liquid permeable sheet.
- the sheets are arranged in this order, and the auxiliary sheet relates to an absorbent article which is arranged between the impermeable sheet and the water absorbing core and / or between the water absorbing core and the liquid permeable sheet.
- the auxiliary sheet has a swelling layer containing water-absorbing resin particles, and the swelling layers are provided on both ends of the water-absorbing core in the lateral direction along the longitudinal direction of the water-absorbing core.
- the 10-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer is 5 N or more.
- the 10-second value of the swelling power is measured by the swelling power test performed in the following order of i), ii), iii), iv) and v).
- i) Prepare a cylinder with an inner diameter of 20 mm, which has openings at both ends and has a mesh mounted on one of the openings, with the cylinder standing vertically with the side on which the mesh is mounted facing down.
- 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
- a glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
- An impermeable sheet is placed on the upper surface of a glass filter permeated with physiological saline, and a cylinder containing water-absorbent resin particles is erected vertically on the impermeable sheet with the mesh facing down.
- iv) Remove the impermeable sheet and start water absorption by the water-absorbent resin particles.
- the force for pushing up the cylindrical jig generated by the swelling of the water-absorbent resin particles at 10 seconds after the impermeable sheet is removed is measured by the load cell and recorded as a 10-second value of the swelling force.
- Another aspect of the present invention is an auxiliary sheet used to assist the absorption of liquid in the water-absorbing core in an absorbent article provided with a water-absorbing core, which includes a swelling layer containing water-absorbing resin particles and is included in the swelling layer.
- the present invention relates to an auxiliary sheet in which the 10-second value of the swelling force of the water-absorbent resin particles is 5 N or more.
- an absorbent article having a high liquid absorption amount in a wearing state of a user and suppressing liquid leakage.
- the auxiliary sheet of the present invention for example, by arranging the absorbent article at a predetermined position, the absorbent article having a high liquid absorption amount in the wearing state of the user and the liquid leakage is suppressed is provided. be able to.
- test absorbent article having a swelling layer provided along the outer circumference (edge) of the absorption core on the water absorption core on the user side is shown, (A) is a top view, and (B) is from the longitudinal direction.
- the side view is shown.
- An example of a test absorbent article having swelling layers provided along the longitudinal direction on both ends of the water absorption core in the lateral direction on the side opposite to the user side on the water absorption core is shown, and (A) shows an upper surface.
- FIG. 3B shows a side view seen from the longitudinal direction.
- An example of a test absorbent article having no swelling layer on the water absorption core is shown, (A) is a top view, and (B) is a side view seen from the longitudinal direction.
- test absorbent article having swelling layers provided along the longitudinal direction on both ends of the water absorption core in the lateral direction on the user side on the water absorption core is shown, (A) is a top view, (B). ) Indicates a side view seen from the longitudinal direction. It is a schematic diagram which shows the measuring apparatus of a swelling force test. It is a schematic diagram which shows the measuring apparatus of a crotch leakage test. It is a schematic diagram which shows the measuring apparatus of abdominal leakage and back leakage test.
- each component in the composition means the total amount of the plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified.
- the absorbent article includes a water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet, and a liquid permeable sheet.
- the liquid impermeable sheet, the water absorbing core and the liquid permeable sheet are arranged in this order.
- the auxiliary sheet is arranged between the impermeable sheet and the water absorbing core and / or between the water absorbing core and the liquid permeable sheet.
- the auxiliary sheet includes a swelling layer containing water-absorbent resin particles.
- the auxiliary sheet is used in an absorbent article provided with a water-absorbing core to assist the liquid absorption of the water-absorbing core.
- the 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer which is measured in the swelling force test performed in the order of i), ii), iii), iv) and v) below, is 5 N or more. ..
- 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
- a glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
- the 10-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer may be 5N or more, 6N or more, 7N or more, 8N or more, 9N or more, 10N or more, or 11N or more, 20N or less, 18N or more. Hereinafter, it may be 16N or less, 14N or less, or 13N or less.
- the 10-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer may be 5N or more and 20N or less, 5N or more and 18N or less, 5N or more and 16N or less, 5N or more and 14N or less, or 5N or more and 13N or less.
- the 10-second value of the swelling force can be determined by, for example, changing the shape of the water-absorbent resin particles to adjust the specific surface area, performing surface treatment to make the surface of the water-absorbent resin hydrophilic, internal cross-linking and surface cross-linking. It can be controlled by adjusting the balance of the light and shade of the cross-linking density in one particle by the above.
- the absorbent article first, when a liquid to be absorbed invades, the liquid is absorbed by the water absorption core and the auxiliary sheet.
- the water-absorbent resin particles having a swelling force of 10 seconds or more tend to swell more easily in the initial stage of liquid absorption, and the swelling layer containing such water-absorbent resin particles is formed in the lateral direction of the water-absorbing core.
- the water-absorbent resin particles swollen in the initial stage of liquid absorption suppress the generation of liquid flow to the outside in the lateral direction due to the liquid that has subsequently invaded.
- the 60-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer is 30 N or less, 20 N or less, 18 N or less, 15 N or less, 13 N or less, 10 N or less, or from the viewpoint of being more excellent in the liquid leakage suppressing effect in the used state. It may be 8N or less, 6N or more, or 7N or more.
- the 60-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer is 6N or more and 30N or less, 6N or more and 20N or less, 6N or more and 18N or less, and 6N or more and 15N or less from the viewpoint of being more excellent in the liquid leakage suppressing effect in the used state. , 7N or more and 30N or less, 7N or more and 20N or less, 7N or more and 18N or less, or 7N or more and 15N or less.
- the 60-second value of the swelling force is measured by the swelling force test performed in the order of i), ii), iii) and iv) described above and vi) below. vi) The force to push up the cylindrical jig generated by the swelling of the water-absorbent resin particles 60 seconds after removing the impermeable sheet is measured by the load cell, and the measured value at 60 seconds later is the swelling force. Record as a 60-second value of. The 60-second value of the swelling force is specifically measured by the method described in Examples described later.
- the 60-second value of the swelling force can be controlled, for example, by adjusting the balance of the density of the cross-linking in each particle due to the internal cross-linking and the surface cross-linking.
- the water absorption amount of the physiological saline of the water-absorbent resin particles may be, for example, 20 to 80 g / g, 30 to 70 g / g, or 40 to 65 g / g.
- the water absorption rate (Vortex method) of the water-absorbent resin particles may be, for example, 1 to 70 seconds, 2 to 50 seconds, 2 to 25 seconds, or 2 to 10 seconds.
- the water absorption amount and the water absorption rate of the physiological saline can be measured by the method described in Examples described later.
- the shape of the water-absorbent resin particles according to the present embodiment is not particularly limited, and may be, for example, substantially spherical, crushed, or granular, and even if primary particles having these shapes are aggregated to form particles. Good.
- the medium particle size of the water-absorbent resin particles may be 100 to 800 ⁇ m, 150 to 700 ⁇ m, 200 to 600 ⁇ m, or 250 to 500 ⁇ m.
- the medium particle size can be measured by the following method. From the top, JIS standard sieves have a mesh size of 600 ⁇ m, a mesh size of 500 ⁇ m, a mesh size of 425 ⁇ m, a mesh size of 300 ⁇ m, a mesh size of 250 ⁇ m, a mesh size of 180 ⁇ m, a mesh size of 150 ⁇ m, and a sieve. , Combine in the order of the saucer.
- the mass of the particles remaining on each sieve is calculated as a mass percentage with respect to the total amount to obtain the particle size distribution.
- the relationship between the mesh size of the sieve and the integrated value of the mass percentage of the particles remaining on the sieve is plotted on the logarithmic probability paper by integrating the particles on the sieve in order from the one having the largest particle size with respect to this particle size distribution. By connecting the plots on the probability paper with a straight line, the particle size corresponding to the cumulative mass percentage of 50% by mass is obtained as the medium particle size.
- the water-absorbent resin particles 61a can include, for example, polymer particles formed by polymerizing a monomer containing an ethylenically unsaturated monomer.
- the polymer particles may be water-absorbent particles containing a polymer contained as a monomer unit derived from an ethylenically unsaturated monomer.
- the ethylenically unsaturated monomer may be a water-soluble monomer, and examples thereof include (meth) acrylic acid and salts thereof, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts.
- the amino group may be quaternized.
- the ethylenically unsaturated monomer may be used alone or in combination of two or more.
- Functional groups such as the carboxyl group and amino group of the above-mentioned monomers can function as functional groups capable of cross-linking in the surface cross-linking step described later.
- the ethylenically unsaturated monomer may be used alone or in combination of two or more.
- the proportion of the polymer containing the ethylenically unsaturated monomer as a monomer unit in the polymer particles is 50 to 100% by mass, 60 to 100% by mass, and 70 to 100% by mass based on the mass of the polymer particles. , Or 80 to 100% by mass.
- the polymer particles may be particles containing a (meth) acrylic acid-based polymer containing at least one of (meth) acrylic acid or (meth) acrylate as a monomer unit.
- the total ratio of the monomer units derived from (meth) acrylic acid or (meth) acrylate in the (meth) acrylic acid-based polymer may be 70 to 100% by mass based on the mass of the polymer. , 90-100% by mass.
- the water-absorbent resin particles 61a can be produced by a method including a step of polymerizing a monomer containing an ethylenically unsaturated monomer.
- the polymerization method include a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method. From the viewpoint of ensuring good water absorption characteristics of the obtained water-absorbent resin particles and facilitating control of the polymerization reaction, a reverse phase suspension polymerization method or an aqueous solution polymerization method may be applied.
- a reverse phase suspension polymerization method will be described as an example.
- the ethylenically unsaturated monomer is at least one selected from the group consisting of (meth) acrylic acid and salts thereof, acrylamide, methacrylamide, and N, N-dimethylacrylamide. It may contain a compound of the species.
- the ethylenically unsaturated monomer may contain (meth) acrylic acid and a salt thereof, and at least one compound selected from the group consisting of acrylamide.
- the ethylenically unsaturated monomer may contain at least one compound selected from the group consisting of (meth) acrylic acid and salts thereof.
- the ethylenically unsaturated monomer can be used in the polymerization reaction as an aqueous solution.
- concentration of the ethylenically unsaturated monomer in the aqueous solution containing the ethylenically unsaturated monomer (hereinafter, simply referred to as "monomeric aqueous solution”) is 20% by mass or more and the saturation concentration or less, 25 to 70% by mass, or 30. It may be up to 55% by mass.
- Examples of the water used in the aqueous solution include tap water, distilled water, ion-exchanged water and the like.
- a monomer other than the above-mentioned ethylenically unsaturated monomer may be used.
- Such a monomer can be used, for example, by mixing with an aqueous solution containing the above-mentioned ethylenically unsaturated monomer.
- the amount of the ethylenically unsaturated monomer used may be 70 to 100 mol% with respect to the total amount of the monomer.
- the ratio of (meth) acrylic acid and a salt thereof may be 70 to 100 mol% with respect to the total amount of the monomer.
- the acidic group may be neutralized with an alkaline neutralizer and then the monomer solution may be used in the polymerization reaction.
- the degree of neutralization of an ethylenically unsaturated monomer by an alkaline neutralizing agent increases the osmotic pressure of the obtained water-absorbent resin particles and further enhances the water absorption characteristics (water absorption amount, etc.). It may be 10-100 mol%, 50-90 mol%, or 60-80 mol% of the acidic group in the body.
- alkaline neutralizing agent examples include alkali metal salts such as sodium hydroxide, sodium carbonate, sodium hydrogen carbonate, potassium hydroxide and potassium carbonate; ammonia and the like.
- the alkaline neutralizer may be used alone or in combination of two or more.
- the alkaline neutralizer may be used in the form of an aqueous solution to simplify the neutralization operation. Neutralization of the acidic group of the ethylenically unsaturated monomer can be performed, for example, by dropping an aqueous solution of sodium hydroxide, potassium hydroxide or the like into the above-mentioned monomer aqueous solution and mixing them.
- an aqueous monomer solution is dispersed in a hydrocarbon dispersion medium in the presence of a surfactant, and an ethylenically unsaturated monomer is polymerized using a radical polymerization initiator or the like.
- a radical polymerization initiator a water-soluble radical polymerization initiator can be used.
- surfactant examples include nonionic surfactants, anionic surfactants and the like.
- nonionic surfactant sorbitan fatty acid ester and (poly) glycerin fatty acid ester (“(poly)” means both with and without the prefix of “poly”. The same shall apply hereinafter.
- Sucrose fatty acid ester polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, sorbitol fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene himashi
- oil polyoxyethylene hydrogenated castor oil, alkylallyl formaldehyde condensed polyoxyethylene ether, polyoxyethylene polyoxypropylene block copolymer, polyoxyethylene polyoxypropyl alkyl ether, polyethylene glycol fatty acid ester and the like.
- Anionic surfactants include fatty acid salts, alkylbenzene sulfonates, alkylmethyl taurates, polyoxyethylene alkylphenyl ether sulfates, polyoxyethylene alkyl ether sulfonates, and polyoxyethylene alkyl ether phosphates. , And the phosphate ester of polyoxyethylene alkyl allyl ether and the like.
- the surfactant may be used alone or in combination of two or more.
- the surfactant is a sorbitan fatty acid ester. It may contain at least one compound selected from the group consisting of polyglycerin fatty acid ester and sucrose fatty acid ester. From the viewpoint of easily improving the water absorption characteristics of the obtained water-absorbent resin particles, sorbitan fatty acid ester (for example, sorbitan monolaurate) and / or sucrose fatty acid ester (for example, sucrose stearic acid ester) are used as the surfactant. Good. These surfactants may be used alone or in combination of two or more.
- the amount of the surfactant may be 0.05 to 10 parts by mass, 0.08 to 5 parts by mass, or 0.1 to 3 parts by mass with respect to 100 parts by mass of the aqueous monomer solution.
- a polymer-based dispersant may be used in combination with the above-mentioned surfactant.
- the polymer dispersant include maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, maleic anhydride-modified ethylene / propylene copolymer, maleic anhydride-modified EPDM (ethylene / propylene / diene / terpolymer), and maleic anhydride.
- the polymer-based dispersant may be used alone or in combination of two or more.
- the polymer-based dispersant includes maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, maleic anhydride-modified ethylene / propylene copolymer, and maleic anhydride / ethylene copolymer.
- Maleic anhydride / propylene copolymer, maleic anhydride / ethylene / propylene copolymer, polyethylene, polypropylene, ethylene / propylene copolymer, oxidized polyethylene, oxidized polypropylene, and oxidized ethylene / propylene copolymer It may be at least one selected from the group consisting of.
- the amount of the polymer-based dispersant may be 0.05 to 10 parts by mass, 0.08 to 5 parts by mass, or 0.1 to 3 parts by mass with respect to 100 parts by mass of the aqueous monomer solution.
- the hydrocarbon dispersion medium may contain at least one compound selected from the group consisting of chain aliphatic hydrocarbons having 6 to 8 carbon atoms and alicyclic hydrocarbons having 6 to 8 carbon atoms.
- Hydrocarbon dispersion media include chain aliphatic hydrocarbons such as n-hexane, n-heptane, 2-methylhexane, 3-methylhexane, 2,3-dimethylpentane, 3-ethylpentane, and n-octane; cyclohexane.
- the hydrocarbon dispersion medium may be used alone or in combination of two or more.
- the hydrocarbon dispersion medium may contain at least one selected from the group consisting of n-heptane and cyclohexane.
- the mixture of the above-mentioned hydrocarbon dispersion medium for example, commercially available ExxonHeptane (manufactured by ExxonMobil: containing 75 to 85% of n-heptane and isomeric hydrocarbons) is used. You may.
- the amount of the hydrocarbon dispersion medium is 30 to 1000 parts by mass, 40 to 500 parts by mass, or 50 parts by mass with respect to 100 parts by mass of the monomer aqueous solution from the viewpoint of appropriately removing the heat of polymerization and easily controlling the polymerization temperature. It may be up to 300 parts by mass. When the amount of the hydrocarbon dispersion medium is 30 parts by mass or more, the polymerization temperature tends to be easily controlled. When the amount of the hydrocarbon dispersion medium is 1000 parts by mass or less, the productivity of polymerization tends to be improved, which is economical.
- the radical polymerization initiator may be water-soluble.
- water-soluble radical polymerization initiators include persulfates such as potassium persulfate, ammonium persulfate, and sodium persulfate; methyl ethyl ketone peroxide, methyl isobutyl ketone peroxide, di-t-butyl peroxide, and t-butyl cumylper.
- Peroxides such as oxides, t-butylperoxyacetate, t-butylperoxyisobutyrate, t-butylperoxypivalate, hydrogen peroxide; 2,2'-azobis (2-amidinopropane) dihydrochloride , 2,2'-azobis [2- (N-phenylamidino) propane] dihydrochloride, 2,2'-azobis [2- (N-allylamidino) propane] dihydrochloride, 2,2'-azobis [ 2- (2-imidazolin-2-yl) propane] 2 hydrochloride, 2,2'-azobis ⁇ 2- [1- (2-hydroxyethyl) -2-imidazolin-2-yl] propane ⁇ 2 hydrochloride, 2,2'-azobis ⁇ 2-methyl-N- [1,1-bis (hydroxymethyl) -2-hydroxyethyl] propionamide ⁇ , 2,2'-azobis [2-methyl-N- (2-hydroxy) Ethyl) -propion
- the radical polymerization initiator may be used alone or in combination of two or more. Radical polymerization initiators are potassium persulfate, ammonium persulfate, sodium persulfate, 2,2'-azobis (2-amidinopropane) dihydrochloride, 2,2'-azobis [2- (2-imidazolin-2-yl). ) Propane] 2 hydrochloride and 2,2'-azobis ⁇ 2- [1- (2-hydroxyethyl) -2-imidazolin-2-yl] propane ⁇ 2 hydrochloride, at least one selected from the group. There may be.
- the amount of the radical polymerization initiator may be 0.00005 to 0.01 mol per 1 mol of the ethylenically unsaturated monomer.
- the amount of the radical polymerization initiator used is 0.00005 mol or more, the polymerization reaction does not require a long time and is efficient.
- the amount of the radical polymerization initiator is 0.01 mol or less, it is easy to suppress the occurrence of a rapid polymerization reaction.
- the exemplified radical polymerization initiator can also be used as a redox polymerization initiator in combination with a reducing agent such as sodium sulfite, sodium hydrogen sulfite, ferrous sulfate, and L-ascorbic acid.
- a reducing agent such as sodium sulfite, sodium hydrogen sulfite, ferrous sulfate, and L-ascorbic acid.
- the aqueous monomer solution may contain a chain transfer agent.
- chain transfer agent include hypophosphates, thiols, thiolic acids, secondary alcohols, amines and the like.
- the monomer aqueous solution used for polymerization may contain a thickener in order to control the particle size of the water-absorbent resin particles.
- a thickener examples include hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, carboxymethyl cellulose, polyacrylic acid, polyethylene glycol, polyacrylamide, polyethyleneimine, dextrin, sodium alginate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide and the like. If the stirring speed at the time of polymerization is the same, the higher the viscosity of the aqueous monomer solution, the larger the medium particle size of the obtained particles tends to be.
- Cross-linking by self-cross-linking may occur during polymerization, but cross-linking may be further performed by using an internal cross-linking agent.
- an internal cross-linking agent When an internal cross-linking agent is used, it is easy to control the water absorption characteristics of the water-absorbent resin particles.
- the internal cross-linking agent is usually added to the reaction solution during the polymerization reaction.
- the internal cross-linking agent examples include di or tri (meth) acrylic acid esters of polyols such as ethylene glycol, propylene glycol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; Unsaturated polyesters obtained by reacting polyols with unsaturated acids (maleic acid, fumaric acid, etc.); bis (meth) acrylamides such as N, N'-methylenebis (meth) acrylamide; polyepoxides and (meth) Di or tri (meth) acrylic acid esters obtained by reacting with acrylic acid; di (meth) obtained by reacting polyisocyanate (tolylene diisocyanate, hexamethylene diisocyanate, etc.) with hydroxyethyl (meth) acrylate.
- polyols such as ethylene glycol, propylene glycol, trimethylolpropane, glycerin, polyoxyethylene glycol,
- Acrylic acid carbamil esters compounds having two or more polymerizable unsaturated groups such as allylated starch, allylated cellulose, diallyl phthalate, N, N', N "-triallyl isocyanurate, divinylbenzene; Poly such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, polyglycerol polyglycidyl ether, etc.
- Poly such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene
- Glyceridyl compound such as epichlorohydrin, epibromhydrin, ⁇ -methylepichlorohydrin; 2 reactive functional groups such as isocyanate compound (2,4-tolylene diisocyanate, hexamethylene diisocyanate, etc.) Examples thereof include compounds having more than one.
- the internal cross-linking agent may be used alone or in combination of two or more.
- the internal cross-linking agent may be a polyglycidyl compound or diglycidyl. It may be an ether compound.
- the internal cross-linking agent comprises at least one selected from the group consisting of (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, and (poly) glycerin diglycidyl ether. It may be.
- the amount of the internal cross-linking agent is not ethylenically from the viewpoint that the water-soluble property is suppressed by appropriately cross-linking the polymer obtained by the polymerization of the above-mentioned monomer aqueous solution, and a sufficient water absorption amount can be easily obtained. It may be 0 mmol or more, 0.01 mmol or more, 0.015 mmol or more, 0.020 mmol or more, or 0.1 mol or less, per 1 mol of saturated monomer.
- Reversed phase suspension polymerization can be carried out in an aqueous system in oil by heating with stirring in a state where the phases are mixed.
- a monomer aqueous solution containing an ethylenically unsaturated monomer is used as a hydrocarbon dispersion medium in the presence of a surfactant (and, if necessary, a polymer-based dispersant). Disperse in.
- the timing of adding the surfactant, the polymer-based dispersant, or the like may be either before or after the addition of the aqueous monomer solution, as long as it is before the start of the polymerization reaction.
- a surfactant is added after dispersing the monomer aqueous solution in the hydrocarbon dispersion medium in which the polymer-based dispersant is dispersed.
- the polymer may be further dispersed and then polymerized.
- Reverse phase suspension polymerization can be carried out in one stage or in multiple stages of two or more stages. Reversed phase suspension polymerization may be carried out in two or three stages from the viewpoint of increasing productivity.
- an ethylenically unsaturated monomer is added to the reaction mixture obtained in the first step polymerization reaction after the first step reverse phase suspension polymerization is carried out. It may be added and mixed, and the reverse phase suspension polymerization of the second and subsequent steps may be carried out in the same manner as in the first step.
- the above-mentioned radical polymerization initiator is used in the reverse phase suspension polymerization in each stage of the second and subsequent stages.
- the ethylenically unsaturated monomer to be added Based on the amount of the ethylenically unsaturated monomer to be added, it may be added within the range of the molar ratio of each component to the above-mentioned ethylenically unsaturated monomer to carry out reverse phase suspension polymerization.
- an internal cross-linking agent In the reverse phase suspension polymerization in each stage after the second stage, an internal cross-linking agent may be used if necessary.
- an internal cross-linking agent When an internal cross-linking agent is used, it is added within the range of the molar ratio of each component to the above-mentioned ethylenically unsaturated monomer based on the amount of the ethylenically unsaturated monomer provided in each stage, and the suspension is reversed. Muddy polymerization may be carried out.
- the temperature of the polymerization reaction varies depending on the radical polymerization initiator used, but by rapidly advancing the polymerization and shortening the polymerization time, the efficiency is improved and the heat of polymerization is easily removed to carry out the reaction smoothly. From the viewpoint, it may be 20 to 150 ° C. or 40 to 120 ° C.
- the reaction time is usually 0.5-4 hours.
- the completion of the polymerization reaction can be confirmed, for example, by stopping the temperature rise in the reaction system. As a result, the polymer of the ethylenically unsaturated monomer is usually obtained in the state of a hydrogel-like polymer.
- cross-linking may be performed after polymerization by adding a cross-linking agent to the obtained hydrogel polymer and heating it.
- a cross-linking agent to the obtained hydrogel polymer and heating it.
- cross-linking agent for performing post-polymerization cross-linking examples include polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; Compounds having two or more epoxy groups such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, and (poly) glycerin diglycidyl ether; epichlorohydrin, epibromhydrin, ⁇ -methylepicrolhydrin and the like.
- polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane
- glycerin polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin
- Compounds having two or more epoxy groups such as (poly) ethylene glyco
- Haloepoxy compounds compounds having two or more isocyanate groups such as 2,4-tolylene diisocyanate and hexamethylene diisocyanate; oxazoline compounds such as 1,2-ethylene bisoxazoline; carbonate compounds such as ethylene carbonate; bis [N , N-di ( ⁇ -hydroxyethyl)] hydroxyalkylamide compounds such as adipamide can be mentioned.
- Cross-linking agents for post-polymerization cross-linking are (poly) ethylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, and polyglycerol polyglycidyl ether. It may be a polyglycidyl compound such as. These cross-linking agents may be used alone or in combination of two or more.
- the amount of the cross-linking agent used for post-polymerization cross-linking is 1 mol of the water-soluble ethylenically unsaturated monomer from the viewpoint of appropriately cross-linking the obtained hydrogel-like polymer to exhibit suitable water absorption characteristics. It may be 0 to 0.03 mol, 0 to 0.01 mol, or 0.00001 to 0.005 mol.
- the cross-linking agent for post-polymerization cross-linking is added to the reaction solution after the polymerization reaction of the ethylenically unsaturated monomer.
- a cross-linking agent for post-polymerization cross-linking may be added after the multi-stage polymerization.
- the cross-linking agent for post-polymerization cross-linking is , From the viewpoint of water content (described later), it may be added in the region of [water content immediately after polymerization ⁇ 3% by mass].
- drying to remove water gives polymer particles containing a polymer of ethylenically unsaturated monomers.
- the drying method include (a) a method of removing water by azeotropic distillation in a state where the hydrogel polymer is dispersed in a hydrocarbon dispersion medium, and (b) a method of taking out the hydrogel polymer by decantation and reducing the pressure. Examples thereof include a method of drying, and (c) a method of filtering the hydrogel polymer by a filter and drying under reduced pressure.
- the particle size of the water-absorbent resin particles can be adjusted by adjusting the rotation speed of the stirrer during the polymerization reaction, or by adding a flocculant into the system after the polymerization reaction or in the early stage of drying. By adding a flocculant, the particle size of the obtained water-absorbent resin particles can be increased.
- an inorganic flocculant can be used as the flocculant.
- the inorganic flocculant for example, powdered inorganic flocculant
- the aggregating agent may be at least one selected from the group consisting of silica, aluminum oxide, talc and kaolin.
- a coagulant is previously dispersed in a hydrocarbon dispersion medium of the same type as that used in the polymerization or water, and then this is placed in a hydrocarbon dispersion medium containing a hydrogel polymer under stirring. May be mixed with.
- the amount of the flocculant is 0.001 to 1 part by mass, 0.005 to 0.5 part by mass, or 0.01 to 0.2 with respect to 100 parts by mass of the ethylenically unsaturated monomer used for the polymerization. It may be a mass part. When the amount of the flocculant is within these ranges, it is easy to obtain water-absorbent resin particles having a desired particle size distribution.
- the polymerization reaction can be carried out using various stirrers having stirring blades.
- a flat plate blade a lattice blade, a paddle blade, a propeller blade, an anchor blade, a turbine blade, a Faudler blade, a ribbon blade, a full zone blade, a max blend blade and the like can be used.
- the flat plate blade has a shaft (stirring shaft) and a flat plate portion (stirring portion) arranged around the shaft. Further, the flat plate portion may have a slit or the like.
- cross-linking of the surface portion of the hydrogel polymer may be carried out using a cross-linking agent in any of the drying step and subsequent steps.
- a cross-linking agent By performing surface cross-linking, it is easy to control the water absorption characteristics of the water-absorbent resin particles.
- the water content of the surface-crosslinked hydrogel polymer may be 5 to 50% by mass, 10 to 40% by mass, or 15 to 35% by mass.
- the water content (mass%) of the water-containing gel polymer is calculated by the following formula.
- Moisture content [Ww / (Ww + Ws)] x 100 Ww: Necessary when mixing a flocculant, a surface cross-linking agent, etc. to the amount obtained by subtracting the amount of water discharged to the outside of the system by the drying step from the amount of water contained in the monomer aqueous solution before polymerization in the entire polymerization step. The amount of water in the hydrogel polymer calculated by adding the amount of water used according to.
- Ws The amount of solid content calculated from the amount of materials such as ethylenically unsaturated monomers, cross-linking agents, and initiators that make up the hydrogel polymer.
- surface cross-linking agents include, for example, polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; (poly) ethylene.
- Polyglycidyl compounds such as glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, trimethylpropan triglycidyl ether (poly) propylene glycol polyglycidyl ether, (poly) glycerol polyglycidyl ether; Haloepoxy compounds such as chlorohydrin, epibromhydrin, ⁇ -methylepichlorohydrin; isocyanate compounds such as 2,4-tolylene diisocyanate, hexamethylene diisocyanate; 3-methyl-3-oxetane methanol, 3-ethyl- Oxetane compounds such as 3-oxetane methanol, 3-butyl-3-oxetane methanol, 3-methyl-3-oxetaneethanol, 3-ethyl-3-oxetaneethanol, 3-butyl-3-o
- the surface cross-linking agent may be used alone or in combination of two or more.
- the surface cross-linking agent may be a polyglycidyl compound, and may be (poly) ethylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, and poly. It may be at least one selected from the group consisting of glycerol polyglycidyl ether.
- the amount of the surface cross-linking agent used is 0.01 to 20 mmol, 0.05 to 10 mmol, based on 1 mol of the ethylenically unsaturated monomer used for the polymerization, from the viewpoint that suitable water absorption characteristics can be easily obtained. It may be 0.1-5 mmol, 0.15-3 mmol, or 0.2-1 mmol.
- the surface portion of the hydrogel polymer is treated (surface modification) with a surface modifier in either the drying step (moisture removal step) or a subsequent step. You may.
- the surface modification may be carried out, for example, before, during or after the surface cross-linking step. Surface modification may be carried out after surface cross-linking.
- the surface modifier may be, for example, a surfactant such as a nonionic surfactant, an anionic surfactant, a cationic surfactant, or an amphoteric surfactant.
- a surfactant such as a nonionic surfactant, an anionic surfactant, a cationic surfactant, or an amphoteric surfactant.
- the HLB value of the nonionic surfactant used as the surface modifier may be, for example, 3 to 12, or 6 to 10.
- the nonionic surfactant include sorbitan fatty acid esters such as sorbitan monolaurate. The HLB value is measured by the Griffin method.
- the amount of the surface modifier is 0.01 to 0.50 parts by mass, 0.02 to 0.40 parts by mass, or 0.04 with respect to 100 parts by mass of the ethylenically unsaturated monomer used for the polymerization. It may be ⁇ 0.30 parts by mass.
- water and a hydrocarbon dispersion medium can be distilled off from the hydrogel polymer to obtain polymer particles which are dry products. it can.
- the water-absorbent resin particles 61a may be composed of only polymer particles, but further contain various additional components selected from, for example, a gel stabilizer, a metal chelating agent, a fluidity improver (lubricant), and the like. be able to. Additional components may be placed inside the polymer particles, on the surface of the polymer particles, or both. The additional component may be a fluidity improver (lubricant).
- the fluidity improver may contain inorganic particles. Examples of the inorganic particles include silica particles such as amorphous silica.
- the water-absorbent resin particles 61a may contain a plurality of inorganic particles arranged on the surface of the polymer particles. For example, by mixing the polymer particles and the inorganic particles, the inorganic particles can be arranged on the surface of the polymer particles.
- the inorganic particles may be silica particles such as amorphous silica.
- the ratio of the amount of the inorganic particles to the mass of the polymer particles is 0.2% by mass or more, 0.5% by mass or more, It may be 1.0% by mass or more, 1.5% by mass or more, 5.0% by mass or less, or 3.5% by mass or less.
- the inorganic particles here usually have a minute size as compared with the size of the polymer particles.
- the average particle size of the inorganic particles may be 0.1 to 50 ⁇ m, 0.5 to 30 ⁇ m, or 1 to 20 ⁇ m.
- the average particle size here can be a value measured by a dynamic light scattering method or a laser diffraction / scattering method.
- FIG. 1 is a cross-sectional view showing a strip-shaped auxiliary sheet according to an embodiment.
- the auxiliary sheet 60 shown in FIG. 1 has a swelling layer 61 and two sheet base materials 62a and 62b.
- the sheet base materials 62a and 62b are arranged on both sides of the swelling layer 61.
- the swelling layer 61 is arranged inside the sheet base materials 62a and 62b.
- the swelling layer 61 is held in shape by being sandwiched between the two sheet base materials 62a and 62b.
- the sheet base materials 62a and 62b may be two sheets, one folded sheet, or one bag.
- the auxiliary sheet 60 may further have an adhesive 63a interposed between the sheet base material 62a and the swelling layer 61, and further has an adhesive 63b interposed between the sheet base material 62b and the swelling layer 61. You may have.
- the adhesives 63a and 63b may be, for example, a water-based adhesive, a solvent-based adhesive, an elastic adhesive, an aerosol adhesive, a hot melt adhesive, or the like.
- the length of the auxiliary sheet 60 in the longitudinal direction may be, for example, 20 cm or more, 22 cm or more, 24 cm or more, or 26 cm or more in a dry state, and is 60 cm or less, 50 cm or less, 40 cm or less, 38 cm or less, 36 cm or less, 34 cm or less. , Or 32 cm or less.
- the length of the auxiliary sheet 60 in the longitudinal direction may be 0.8 to 1.2 times the length of the water absorbing core included in the absorbent article in the dry state. , May be the same length.
- the length of the auxiliary sheet 60 in the lateral direction may be, for example, 0.5 cm or more, 1 cm or more, 1.5 cm or more, or 2 cm or more in a dry state, and may be 6.5 cm or less, 5.5 cm or less, 4. It may be 5 cm or less, 3.5 cm or less, 3.0 cm or less, or 2.5 cm or less.
- the length of the region where the swelling layer 61 exists in the auxiliary sheet 60 in the lateral direction is less than 1 / 2W with respect to the width W of the water absorption core included in the absorbent article in the dry state, and the water absorption core. Even if it is placed at both ends in the lateral direction, it does not cover the entire water absorption core.
- the thickness of the auxiliary sheet 60 may be, for example, 3.0 mm or less, 2.5 mm or less, 2.0 mm or less, or 1.8 mm or less in a dry state, and is 0.1 mm or more, 0.3 mm or more, or 0. It may be 5.5 mm or more.
- the thickness can be measured using, for example, a dial thickness gauge JB manufactured by Ozaki Seisakusho Co., Ltd. (the stylus is made of aluminum having a diameter of 50 mm).
- the amount of water-absorbent resin particles (mass of water-absorbent resin particles per unit area) is 10 to 100 g / m 2 , 15 to 60 g / m 2 , or 18 to 45 g / m 2. Good.
- the swelling layer 61 has the water-absorbent resin particles 61a according to the above-described embodiment and the fiber layer 61b containing a fibrous material.
- the swelling layer 61 does not have to have the fiber layer 61b.
- the content of the water-absorbent resin particles in the swelling layer may be 70 to 100% by mass, 80 to 100% by mass, or 90 to 100% by mass based on the mass of the swelling layer 61.
- the thickness of the swelling layer 61 may be, for example, 2.0 mm or less, 1.5 mm or less, 1.0 mm or less, or 0.8 mm or less in a dry state, and is 0.1 mm or more, or 0.3 mm or more. You may.
- the mass per unit area of the swelling layer 61 may be 100 g / m 2 or less, 80 g / m 2 or less, 60 g / m 2 or less, or 40 g / m 2 or less, 10 g / m 2 or more, 20 g / m. It may be 2 or more, or 25 g / m 2 or more.
- the fibrous material constituting the fiber layer 61b can be, for example, a cellulosic fiber, a synthetic fiber, or a combination thereof.
- cellulosic fibers include crushed wood pulp, cotton, cotton linters, rayon and cellulosic acetate.
- synthetic fibers include polyamide fibers, polyester fibers, and polyolefin fibers.
- the fibrous material may be hydrophilic fibers (for example, pulp).
- the swelling layer 61 may further contain inorganic particles (for example, amorphous silica), a deodorant, an antibacterial agent, a fragrance, and the like.
- the sheet base materials 62a and 62b may be, for example, a non-woven fabric, a tissue, or the like.
- the two sheet base materials 62a and 62b can be the same or different non-woven fabrics.
- the non-woven fabric may be a non-woven fabric composed of short fibers (that is, staples) (short-fiber non-woven fabric) or a non-woven fabric composed of long fibers (that is, filaments) (long-fiber non-woven fabric).
- the staples may generally have a fiber length of several hundred mm or less.
- the non-woven fabrics used as the sheet base materials 62a and 62b are thermal-bonded non-woven fabrics, air-through non-woven fabrics, resin-bonded non-woven fabrics, spunbonded non-woven fabrics, melt-blown non-woven fabrics, air-laid non-woven fabrics, spunlaced non-woven fabrics, point-bonded non-woven fabrics, or two or more kinds selected from these. It may be a laminate containing a non-woven fabric.
- the non-woven fabric used as the sheet base materials 62a and 62b can be a non-woven fabric formed of synthetic fibers, natural fibers, or a combination thereof.
- synthetic fibers include polyolefins such as polyethylene (PE) and polypropylene (PP), polyesters such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN), polyamides such as nylon, and Examples thereof include fibers containing a synthetic resin selected from rayon.
- Examples of natural fibers include fibers containing cotton, silk, hemp, or pulp (cellulose).
- the fibers forming the non-woven fabric may be polyolefin fibers, polyester fibers or a combination thereof.
- the sheet base materials 62a and 62b may be tissues.
- the tissues used as the sheet base materials 62a and 62b may be natural fibers or natural fibers mixed with synthetic fibers.
- the mass per unit area of the tissue may be 16 ⁇ 2 g / m 2.
- the thickness of the tissue may be 0.12 ⁇ 0.02 mm.
- the sheet base materials 62a and 62b may have a main surface wider than the main surface of the swelling layer 61. That is, the outer edges of the sheet base materials 62a and 62b may extend around the swelling layer 61.
- the sheet base materials 62a and 62b may be adhered to each other at the outer edge portion extending around the swelling layer 61.
- the auxiliary sheet 60 can be obtained, for example, by sandwiching the swelling layer 61 between the sheet base materials 62a and 62b and pressurizing the formed structure while heating it as necessary. If necessary, the adhesives 63a and 63b are arranged between the sheet base materials 62a and 62b and the swelling layer 61.
- the auxiliary sheet 60 is used, for example, for producing various absorbent articles.
- absorbent articles include diapers (eg paper diapers), toilet training pants, incontinence pads, sanitary materials (sanitary napkins, tampons, etc.), sweat pads, pet sheets, toilet components, and animal waste treatment materials. Can be mentioned.
- FIG. 2 is a cross-sectional view of the absorbent article according to the embodiment in the lateral direction.
- the absorbent article 100 shown in FIG. 2 includes a strip-shaped water absorbing core 50, an auxiliary sheet 60, a liquid permeable sheet 30, and a liquid permeable sheet 40.
- the auxiliary sheet 60 provided with the swelling layer 61 is arranged between the water absorbing core 50 and the liquid permeable sheet 30.
- the auxiliary sheet 60 may be arranged between the impermeable sheet 40 and the water absorbing core 50 instead of being arranged between the water absorbing core 50 and the liquid permeable sheet 30.
- the auxiliary sheet 60 may be arranged between the water absorption core 50 and the liquid permeable sheet 30, and between the water absorption core 50 and the liquid permeable sheet 30.
- the auxiliary sheet may be arranged between the water absorption core and the liquid permeable sheet from the viewpoint of being more excellent in the liquid leakage suppressing effect in the use state.
- the auxiliary sheet 60 shown in FIG. 2 is arranged on the main surface of the user side when the water absorption core 50 is worn by the user, but is opposite to the user side (outside) when the water absorption core 50 is worn by the user. ), And may be arranged on both the user side and the outer side.
- the auxiliary sheet 60 has a swelling layer 61 containing water-absorbent resin particles 61a.
- the swelling layer 61 is provided on both ends of the water absorption core 50 in the lateral direction along the longitudinal direction of the water absorption core 50.
- the swelling layer on one end of the water absorption core and the swelling layer on the other end are provided on separate sheet base materials. It may be provided on one sheet base material.
- the swelling layer 61 in the auxiliary sheet 60 may be further provided on both ends of the water absorption core 50 in the longitudinal direction along the lateral direction of the water absorption core 50.
- one auxiliary sheet having a swelling layer 61 provided along the outer circumference (edge) on the end of the water absorption core 50 can be used.
- the absorbent article 100 has water-absorbent resin particles having a 10-second value of the above-mentioned swelling force of 5 N or more between the swelling layers provided along the longitudinal direction on both ends of the water-absorbing core 50 in the lateral direction. It has an area that does not include it. In other words, the absorbent article 100 has a region on the central portion of the water absorbing core 50 that does not contain the water absorbing resin particles having the above-mentioned 10-second value of the swelling force of 5 N or more. For example, a substance other than the water-absorbent resin particles having a 10-second value of the swelling force of 5 N or more may be arranged in the region, if necessary, and the region may be a void.
- the water absorption core 50 has an absorption layer 10 and two core wrap sheets 20a and 20b.
- the core wrap sheets 20a and 20b are arranged on both sides of the absorption layer 10.
- the absorbent layer 10 is arranged inside the core wrap sheets 20a and 20b, and is held in shape by being sandwiched between the two core wrap sheets.
- the core wrap sheets 20a and 20b may be separate sheets, one folded sheet, or one bag body.
- the water absorption core 50 does not have to have one or both of the two core wrap sheets 20a and 20b.
- the core wrap sheet 20a may not be arranged between the absorption layer 10 and the auxiliary sheet 60.
- the absorption layer 10 is sandwiched between one core wrap sheet 20b and the auxiliary sheet 60. It is kept in shape.
- the water absorption core 50 may further have an adhesive interposed between the core wrap sheet 20a and the absorption layer 10, and further has an adhesive interposed between the core wrap sheet 20b and the absorption layer 10. May be.
- An adhesive layer may be interposed between the core wrap sheets 20a and 20b on both sides and the absorption layer 10.
- FIG. 3 is a plan view showing an example of an adhesive application pattern formed on the core wrap sheet.
- the adhesive 21 shown in FIG. 3 forms a coating pattern composed of a plurality of linear portions arranged at intervals on the core wrap sheet 20a.
- the coating pattern of the adhesive 21 may be linear, curved, dot-shaped, or a combination thereof.
- the adhesive may be, for example, a water-based adhesive, a solvent-based adhesive, or a hot-melt adhesive.
- the absorption layer 10 has water-absorbent resin particles 10a and a fiber layer 10b containing a fibrous material.
- the absorption layer 10 does not have to have the fiber layer 10b.
- the content of the water-absorbent resin particles in the absorption layer may be 70 to 100% by mass, 80 to 100% by mass, or 90 to 100% by mass based on the mass of the absorption layer 10.
- the water-absorbent resin particles 10a may be particles containing a polymer containing an ethylenically unsaturated monomer as a monomer unit.
- the ethylenically unsaturated monomer may be a water-soluble monomer, and examples thereof include (meth) acrylic acid and salts thereof, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts.
- the ethylenically unsaturated monomer may be used alone or in combination of two or more.
- the water-absorbent resin particles may be particles containing a polymer containing at least one of (meth) acrylic acid or a salt of (meth) acrylic acid as a monomer unit.
- the water-absorbent resin particles 10a can be produced, for example, by a method including polymerizing a monomer containing an ethylenically unsaturated monomer.
- the polymerization method of the monomer can be selected from, for example, a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method. From the viewpoint of ensuring good water absorption characteristics of the water-absorbent resin particles and easily controlling the polymerization reaction, a reverse phase suspension polymerization method or an aqueous solution polymerization method may be adopted.
- the polymer constituting the water-absorbent resin particles 10a may be a crosslinked polymer.
- the polymer may be crosslinked by self-crosslinking, cross-linking by reaction with a cross-linking agent, or both.
- the water-absorbent resin particles may be surface-crosslinked by cross-linking at least the polymer of the surface layer portion with a cross-linking agent.
- the water-absorbent resin particles 10a may contain various additional components in addition to the polymer of the ethylenically unsaturated monomer.
- additional ingredients include gel stabilizers, metal chelating agents, and fluidity improvers (lubricants).
- Additional components may be placed inside the polymer particles, including the polymer, on the surface of the polymer particles, or both.
- the additional component may be a fluidity improver (lubricant).
- the fluidity improver may contain inorganic particles. Examples of the inorganic particles include silica particles such as amorphous silica.
- the shape of the water-absorbent resin particles 10a may be, for example, substantially spherical, crushed or granular, and particles having these shapes may be aggregated.
- the medium particle size of the water-absorbent resin particles may be 250 to 850 ⁇ m, 300 to 700 ⁇ m, or 300 to 600 ⁇ m.
- the water absorption amount of the physiological saline may be 20 to 80 g / g, 30 to 70 g / g, or 40 to 65 g / g.
- the 10-second value of the gel swelling force of the water-absorbent resin particles 10a may be less than 5N, may be 4N or less, and may be 0N or more from the viewpoint of further enhancing the liquid leakage suppressing effect in the wearing state of the user. You can.
- the 60-second value of the gel swelling force of the water-absorbent resin particles 10a is 20 N or less, 16 N or less, 12 N or less, 8 N or less, less than 7 N, or 5 N or less from the viewpoint of further enhancing the liquid leakage suppressing effect in the wearing state of the user. It may be 0N or more, or 2N or more.
- the method for measuring the 10-second value and the 60-second value of the gel swelling force is as described above.
- the thickness of the absorption layer 10 may be, for example, 20 mm or less, 15 mm or less, 10 mm or less, 5 mm or less, 4 mm or less, or 3 mm or less, even if it is 0.1 mm or more, or 0.3 mm or more in a dry state. Good.
- the mass per unit area of the absorption layer 10 may be 1000 g / m 2 or less, 800 g / m 2 or less, or 600 g / m 2 or less, 100 g / m 2 or more, or 200 g / m 2 or more. May be good.
- the fibrous material constituting the fiber layer 10b can be, for example, a cellulosic fiber, a synthetic fiber, or a combination thereof.
- cellulosic fibers include crushed wood pulp, cotton, cotton linters, rayon and cellulosic acetate.
- synthetic fibers include polyamide fibers, polyester fibers, and polyolefin fibers.
- the fibrous material may be hydrophilic fibers (for example, pulp).
- the absorption layer 10 may further contain inorganic particles (for example, amorphous silica), a deodorant, an antibacterial agent, a fragrance, and the like.
- inorganic particles for example, amorphous silica
- the absorption layer 10 may contain inorganic particles in addition to the inorganic particles in the water-absorbent resin particles 10a.
- the core wrap sheets 20a and 20b may be, for example, a non-woven fabric.
- the two core wrap sheets 20a and 20b can be the same or different non-woven fabrics.
- the non-woven fabric may be a non-woven fabric composed of short fibers (that is, staples) (short-fiber non-woven fabric) or a non-woven fabric composed of long fibers (that is, filaments) (long-fiber non-woven fabric).
- the staples may generally have a fiber length of several hundred mm or less.
- the core wrap sheets 20a and 20b are laminated including a thermal bond non-woven fabric, an air-through non-woven fabric, a resin bond non-woven fabric, a spunbond non-woven fabric, a melt blow non-woven fabric, an air-laid non-woven fabric, a spunlace non-woven fabric, a point bond non-woven fabric, or two or more kinds of non-woven fabrics selected from these. It can be a body.
- the non-woven fabric used as the core wrap sheets 20a and 20b can be a non-woven fabric formed of synthetic fibers, natural fibers, or a combination thereof.
- synthetic fibers include polyolefins such as polyethylene (PE) and polypropylene (PP), polyesters such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN), polyamides such as nylon, and Examples thereof include fibers containing a synthetic resin selected from rayon.
- Examples of natural fibers include fibers containing cotton, silk, hemp, or pulp (cellulose).
- the fibers forming the non-woven fabric may be polyolefin fibers, polyester fibers or a combination thereof.
- the core wrap sheets 20a and 20b may be tissues.
- the water-absorbing core 50 is sandwiched between, for example, the water-absorbent resin particles 10a or a mixture containing the water-absorbent resin particles 10a and the fibrous material and the core wrap sheets 20a and 20b, and the formed structure is heated as necessary. It can be obtained by the method of pressurizing. If necessary, an adhesive is placed between the core wrap sheets 20a and 20b and the water-absorbent resin particles 10a or a mixture containing the same.
- the water-absorbing core 50 includes a water-absorbing core in which the core wrap sheet 20a, the water-absorbent resin particles 10a, the absorbent layer 10 composed of the fiber layer 10b, and the core wrap sheet 20b are arranged in this order, and substantially the entire fiber layer. It may be in the form of a sheet that does not include it.
- the water absorption core may include a plurality of (for example, two) absorption layers. When the water absorption core includes a plurality of absorption layers, a core wrap sheet may be arranged between the absorption layers.
- the water-absorbent resin particles contained in the plurality of absorption layers may be of the same type or different types.
- the mass and thickness per unit area of each of the plurality of absorption layers may be the same or different.
- the liquid permeable sheet 30 is arranged at the position of the outermost layer on the side where the liquid to be absorbed enters.
- the liquid permeable sheet 30 is arranged on the outside of the core wrap sheet 20b in contact with the core wrap sheet 20b.
- the liquid permeable sheet 40 is arranged at the position of the outermost layer on the side opposite to the liquid permeable sheet 30 in the absorbent article 100.
- the liquid impermeable sheet 40 is arranged on the outside of the core wrap sheet 20a in a state of being in contact with the core wrap sheet 20a.
- the liquid permeable sheet 30 and the liquid permeable sheet 40 have a main surface wider than the main surface of the water absorbing core 50, and the outer edges of the liquid permeable sheet 30 and the liquid permeable sheet 40 are an absorbing layer. It extends around 10 and the core wrap sheets 20a and 20b. However, the magnitude relationship of the absorbent layer 10, the core wrap sheets 20a and 20b, the auxiliary sheet 60, the liquid permeable sheet 30, and the liquid permeable sheet 40 is appropriately adjusted according to the use of the absorbent article and the like.
- the liquid permeable sheet 30 may be a non-woven fabric.
- the non-woven fabric used as the liquid permeable sheet 30 may have appropriate hydrophilicity from the viewpoint of the liquid absorption performance of the absorbent article. From this point of view, the liquid permeable sheet 30 is obtained from the pulp and paper test method No. 1 by the Paper and Pulp Technology Association. A non-woven fabric having a hydrophilicity of 5 to 200 measured according to the measuring method of 68 (2000) may be used. The hydrophilicity of the non-woven fabric may be 10 to 150. Pulp and paper test method No. For details of 68, for example, WO2011 / 086843 can be referred to.
- the non-woven fabric having hydrophilicity may be formed of fibers showing appropriate hydrophilicity such as rayon fiber, or obtained by hydrophilizing a hydrophobic chemical fiber such as polyolefin fiber or polyester fiber. It may be formed of rayon fibers.
- Examples of a method for obtaining a non-woven fabric containing hydrophobic chemical fibers that have been hydrophilized include a method for obtaining a non-woven fabric by a spunbond method using a mixture of hydrophobic chemical fibers and a hydrophilic agent, and hydrophobic chemistry.
- Hydrophilic agents include anionic surfactants such as aliphatic sulfonates and higher alcohol sulfates, cationic surfactants such as quaternary ammonium salts, polyethylene glycol fatty acid esters, polyglycerin fatty acid esters, and sorbitan fatty acids.
- Nonionic surfactants such as esters, silicone-based surfactants such as polyoxyalkylene-modified silicones, and stain-releasing agents made of polyester-based, polyamide-based, acrylic-based, and urethane-based resins are used.
- the amount of texture (mass per unit area) of the non-woven fabric used as the liquid permeable sheet 30 is from the viewpoint of imparting good liquid permeability, flexibility, strength and cushioning property to the absorbent article, and the liquid of the absorbent article. From the viewpoint of increasing the permeation rate, it may be 5 to 200 g / m 2 , 8 to 150 g / m 2 , or 10 to 100 g / m 2 .
- the thickness of the liquid permeable sheet 30 may be 20 to 1400 ⁇ m, 50 to 1200 ⁇ m, or 80 to 1000 ⁇ m.
- the liquid impermeable sheet 40 prevents the liquid absorbed by the absorption layer 10 or the swelling layer 61 from leaking to the outside from the liquid impermeable sheet 40 side.
- the liquid impermeable sheet 40 may be a resin sheet or a non-woven fabric.
- the resin sheet may be a sheet made of a synthetic resin such as polyethylene, polypropylene, or polyvinyl chloride.
- the non-woven fabric may be a spunbond / meltblow / spunbond (SMS) non-woven fabric in which a water-resistant melt-blow non-woven fabric is sandwiched between high-strength spunbond non-woven fabrics.
- SMS spunbond / meltblow / spunbond
- the liquid permeable sheet 40 may be a composite sheet of a resin sheet and a non-woven fabric (for example, a spunbonded non-woven fabric or a spunlaced non-woven fabric).
- the liquid impermeable sheet 40 may have breathability from the viewpoint that stuffiness at the time of wearing is reduced and discomfort given to the wearer can be reduced.
- a sheet of low density polyethylene (LDPE) resin can be used as the liquid impermeable sheet 40 having breathability.
- the basis weight (mass per unit area) of the liquid impermeable sheet 40 is 5 to 100 g / m 2 or 10 to 50 g / m 2. It may be.
- the absorbent article 100 is, for example, in an absorbent article including a strip-shaped water absorbing core 50, a liquid permeable sheet 30, and a liquid impermeable sheet 40, and the auxiliary sheet 60 is a liquid impermeable sheet 40 and a water absorbing core 50. It can be manufactured by a method including placing between and / or between the water absorbing core 50 and the liquid permeable sheet 30.
- the liquid permeable sheet 40, the water absorbing core 50 and the liquid permeable sheet 30 are provided in this order, and the auxiliary sheet 60 is provided between the liquid permeable sheet 40 and the water absorbing core 50 and / or between the water absorbing core and the liquid permeable sheet 30.
- the structural units may be bonded with an adhesive.
- the present embodiment it is possible to provide a method for suppressing liquid leakage using the auxiliary sheet according to the present embodiment.
- the method for suppressing liquid leakage according to the present embodiment is to use an auxiliary sheet having the swelling layer in an absorbent article provided with a strip-shaped water absorbing core, a liquid impermeable sheet and a liquid permeable sheet in the lateral direction of the water absorbing core.
- the swelling layer is arranged along the longitudinal direction on both ends of the swelling layer.
- Production Example 1 Water-absorbent resin particles a Inner diameter 11 cm, contents equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirrer (a stirrer blade having two stages of four inclined paddle blades (surface treated with fluororesin) with a blade diameter of 5 cm).
- n-heptane as a hydrocarbon dispersion medium
- sorbitan monolaurate Naonion LP-20R, HLB value: 8.6, manufactured by NOF CORPORATION
- the mixture was obtained by addition.
- the sorbitan monolaurate was dissolved in n-heptane by heating the mixture to 50 ° C. while stirring at a stirring speed of 300 rpm, and then the mixture was cooled to 40 ° C.
- the inside of the system was sufficiently replaced with nitrogen. Then, the flask was immersed in a water bath at 70 ° C. and held for 60 minutes to complete the polymerization while stirring at a rotation speed of 700 rpm of the stirrer to obtain a hydrogel polymer.
- amorphous silica (Oriental Silicas Corporation, oriental silicas corporation, etc.) was added to the polymer solution containing the produced hydrogel polymer, n-heptane and a surfactant as a powdery inorganic flocculant.
- the flask containing the reaction solution was immersed in an oil bath at 125 ° C., and 98.0 g of water was extracted from the system while refluxing n-heptane by azeotropic distillation of n-heptane and water. Then, 4.14 g (ethylene glycol diglycidyl ether: 0.475 mmol) of 2% by mass of an ethylene glycol diglycidyl ether aqueous solution was added as a surface cross-linking agent, and the mixture was maintained at an internal temperature of 83 ⁇ 2 ° C. for 2 hours.
- ethylene glycol diglycidyl ether 0.475 mmol
- sorbitan monolaurate trade name: Nonion LP-20R, HLB value 8.6, manufactured by Nichiyu Co., Ltd.
- water and n-heptane were heated in an oil bath at 125 ° C. to evaporate, and dried until almost no evaporation from the system was distilled off to obtain a dried product of polymer particles.
- the polymer particles were passed through a sieve having an opening of 850 ⁇ m to obtain 90.1 g of water-absorbent resin particles a.
- the medium particle size of the water-absorbent resin particles a was 352 ⁇ m.
- Water-absorbent resin particles b 104.0 g of water was extracted from the system by azeotropic distillation, and the surface cross-linking agent was changed to 8.28 g of a 2 mass% ethylene glycol diglycidyl ether aqueous solution (ethylene glycol diglycidyl ether: 0.951 mmol).
- 90.3 g of water-absorbent resin particles b were obtained in the same manner as in Production Example 1 except for the above.
- the medium particle size of the water-absorbent resin particles b was 420 ⁇ m.
- the first-stage monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, 6.62 g of n-heptane was added as a surfactant to the sucrose stearic acid ester of HLB3. Mitsubishi Chemical Foods Co., Ltd., Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution dissolved by heating is further added, and the inside of the system is sufficiently filled with nitrogen while stirring at a stirring speed of 500 rpm. After the replacement, the flask was immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization was carried out for 60 minutes to obtain a first-stage polymerized slurry solution.
- the entire amount of the monomer aqueous solution in the second stage is added to the polymerized slurry liquid in the first stage.
- the flask was again immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization reaction was carried out for 60 minutes to obtain a hydrogel polymer.
- n-heptane and water were heated in an oil bath at 125 ° C. to evaporate and dry to obtain a dried product of polymer particles.
- the polymer particles are passed through a sieve having an opening of 850 ⁇ m, and 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) with respect to the mass of the polymer particles is mixed with the polymer particles.
- amorphous silica Oriental Silicas Corporation, Toxile NP-S
- 231.2 g of water-absorbent resin particles c containing amorphous silica were obtained.
- the medium particle size of the water-absorbent resin particles c was 359 ⁇ m.
- Production Example 4 Water-absorbent resin particles d
- the rotation speed of the stirrer adjusted after the addition of the surfactant solution was set to 550 rpm, and in the hydrogel polymer after the second-stage polymerization, 256.8 g by co-boiling distillation.
- the water was extracted from the system and the amount of amorphous silica mixed with the polymer particles was changed to 0.5% by mass with respect to the mass of the polymer particles. 230.2 g of water-absorbent resin particles d were obtained.
- the medium particle size of the water-absorbent resin particles d was 358 ⁇ m.
- the first-stage monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, 6.62 g of n-heptane was added as a surfactant to the sucrose stearic acid ester of HLB3. Mitsubishi Chemical Foods Co., Ltd., Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution dissolved by heating is further added, and the inside of the system is sufficiently filled with nitrogen while stirring at a stirring speed of 550 rpm. After the replacement, the flask was immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization was carried out for 60 minutes to obtain a first-stage polymerized slurry solution.
- the entire amount of the monomer aqueous solution in the second stage is added to the polymerized slurry liquid in the first stage.
- the flask was again immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization reaction was carried out for 60 minutes to obtain a hydrogel polymer.
- n-heptane and water were heated in an oil bath at 125 ° C. to evaporate and dry to obtain a dried product of polymer particles.
- the polymer particles are passed through a sieve having an opening of 850 ⁇ m, and 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) with respect to the mass of the polymer particles is mixed with the polymer particles.
- amorphous silica Oriental Silicas Corporation, Toxile NP-S
- 233.0 g of water-absorbent resin particles e containing amorphous silica were obtained.
- the medium particle size of the water-absorbent resin particles e was 128 ⁇ m.
- Test Water Absorption Core The following materials were prepared for manufacturing the test water absorption core.
- the air-laid non-woven fabric was cut into two pieces to a size of 10 cm ⁇ 30 cm to obtain air-laid non-woven fabric-1 and 2.
- An air-through non-woven fabric cut to a size of 10 cm x 30 cm is placed on the air-laid non-woven fabric-1, and 1.5 g of water-absorbent resin particles (Sumitomo Seika Chemical Co., Ltd.) are used using an airflow type mixer (Padformer manufactured by Otec Co., Ltd.).
- Aquakeep SA60S manufactured by Co., Ltd., water absorption of physiological saline 60 g / g, medium particle size 342 ⁇ m) were uniformly sprayed.
- Air-laid non-woven fabric-2 with hot melt coating machine (Henkel Co., Ltd., pump: Marshal150, table: XA-DT, tank set temperature: 150 ° C, hose set temperature: 165 ° C, gun head set temperature: 170 ° C)
- Ten 0.2 g of hot melt adhesive (Henkel Japan Ltd., ME-765E) was applied to the base material along the length direction as shown in FIG. 3 at 10 mm intervals.
- the adhesive application pattern was a spiral stripe.
- the surface of the air-laid non-woven fabric-2 to which the hot melt was attached was aligned with the surface on which the water-absorbent resin particles of the air-through non-woven fabric were sprayed, sandwiched between release papers, and turned upside down. Then, the release paper and the air-laid non-woven fabric-1 were removed.
- test water-absorbing core is in the order of air-laid non-woven fabric-1, hot melt adhesive, absorbent layer made of water-absorbent resin particles, air-through non-woven fabric, absorbent layer made of water-absorbent resin particles, hot-melt adhesive, and air-laid non-woven fabric-2. It is arranged in.
- Example 1 (Preparation of auxiliary sheet) Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 10 cm ⁇ 30 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (3M Spray Glue 77, manufactured by 3M Japan Ltd.) to the inner surface of the roll of the lower sheet base material, a flow-type mixer (pad former, manufactured by Otec Co., Ltd.) was promptly applied. Was used to uniformly spray 1.1 g of the water-absorbent resin particles a1 prepared in Production Example 1.
- adhesive 3M Spray Glue 77, manufactured by 3M Japan Ltd.
- an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to the upper sheet base material.
- the surface coated with the adhesive of the upper sheet base material was overlapped with the surface on which the water-absorbent resin particles of the lower sheet base material were sprayed so that both ends were aligned, and the entire surface was adhered to obtain a water-absorbent sheet for an auxiliary sheet.
- the obtained water-absorbing sheet for auxiliary sheet was cut into two pieces having a size of 3 cm ⁇ 30 cm to obtain an auxiliary sheet.
- 0.1 g of an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to one side of the auxiliary sheet. With the adhesive-coated side of the auxiliary sheet facing down, the auxiliary sheet is placed on the surface of the air-laid non-woven fabric-1 of the test water-absorbing core produced in Production Example 6 at both ends in the lateral direction of the main surface of the water-absorbing core. Was glued together along the longitudinal direction of the water absorption core. As a result, a test absorbent article of Example 1 was obtained.
- auxiliary sheet of Example 1 a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order.
- the swollen layers in Example 1 are provided on both ends of the water absorbing core in the lateral direction along the longitudinal direction of the water absorbing core.
- the auxiliary sheet is arranged on the user side (the side where the liquid invades) when it is attached.
- the test absorbent article of Example 1 has the same configuration as shown in FIGS. 4A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
- Example 2 The test-absorbent article of Example 2 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles b produced in Production Example 2.
- Example 3 The test-absorbent article of Example 3 was obtained in the same manner as in Example 1 except that the amount of the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet was changed to 0.6 g.
- Example 4 The test absorbent article of Example 4 was obtained in the same manner as in Example 1 except that the size to be cut as an auxiliary sheet was changed to 4 cm ⁇ 30 cm.
- Example 5 The test absorbent article of Example 5 was obtained in the same manner as in Example 1 except that the size to be cut as an auxiliary sheet was changed to 1 cm ⁇ 30 cm.
- Example 6 An absorbent article for testing in Example 6 was obtained in the same manner as in Example 1 except that the installation location of the auxiliary sheet was changed to the surface of the air-laid nonwoven fabric-2.
- the test absorbent article of Example 6 comprises a water absorption core and an auxiliary sheet.
- auxiliary sheet of Example 6 a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order.
- the swollen layers in Example 6 are provided on both ends of the water absorbing core in the lateral direction along the longitudinal direction of the water absorbing core.
- the auxiliary sheet is arranged on the side opposite to the user side (the side where the liquid invades) when it is attached.
- the test absorbent article of Example 6 has the same configuration as shown in FIGS. 7A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
- Example 7 Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 10 cm ⁇ 30 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) to the inner surface of the roll of the lower sheet base material, a rectangular shape with a short side of 4 cm and a long side of 30 cm in the center of the lower sheet base material. 0.7 g of the water-absorbent resin particles a produced in Production Example 1 was uniformly sprayed on a region other than the region.
- adhesive 3M spray glue 77 manufactured by 3M Japan Ltd.
- An adhesive is applied to the upper sheet base material, and the surface to which the adhesive is applied is overlapped with the surface on which the water-absorbent resin particles of the lower sheet base material are sprayed so that both ends are aligned, and the entire surface is adhered to form an auxiliary sheet. Obtained.
- the auxiliary sheet is made of tissue as a sheet base material, has a size of 10 cm ⁇ 30 cm, and swelling layers are provided in a range of 3 cm ⁇ 30 cm at both ends in the lateral direction thereof. ing. Only the tissue and the adhesive as the sheet base material are arranged in the range of 4 cm ⁇ 30 cm in the center of the auxiliary sheet in Example 7.
- auxiliary sheet of Example 7 a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order.
- the swollen layers in Example 7 are provided on both ends of the water absorbing core in the lateral direction along the longitudinal direction of the water absorbing core.
- the auxiliary sheet is arranged on the side opposite to the user side (the side where the liquid invades) when it is attached.
- the test absorbent article of Example 7 has the same configuration as shown in FIGS. 5A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
- Example 8 The same as in Example 1 except that the base material for the auxiliary sheet was changed to a spunlace non-woven fabric (Kuraray Co., Ltd., 70% ration; 20% PET; 10% PP / PE, basis weight 35 g / m 2). A test absorbent article of Example 8 was obtained.
- a spunlace non-woven fabric Karl Fischer Co., Ltd., 70% ration; 20% PET; 10% PP / PE, basis weight 35 g / m 2).
- Example 9 in the same manner as in Example 1 except that the base material for the auxiliary sheet was changed to a spunbonded non-woven fabric (Toray Polytech (Nantong) Co., Ltd., LIVESEN hydrophilic SSSS, basis weight 17 g / m 2). A test absorbent article was obtained.
- a spunbonded non-woven fabric Toray Polytech (Nantong) Co., Ltd., LIVESEN hydrophilic SSSS, basis weight 17 g / m 2).
- Example 10 A water absorption sheet for an auxiliary sheet (having a size of 10 cm on the short side and 30 cm on the long side) was prepared by the same method as that described in Example 1. A rectangular region having a short side of 4 cm and a long side of 24 cm, located at the center of the water absorption sheet, was cut. The water-absorbing sheet from which the predetermined region in the central portion was removed was used as an auxiliary sheet for producing an absorbent article of Example 10. The test absorbent article of Example 10 was obtained in the same manner as in Example 1 except that the auxiliary sheet was changed so as to adhere to the entire surface of the air-laid nonwoven fabric-1.
- auxiliary sheet of Example 10 a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order.
- the swollen layer in Example 10 is provided along the outer circumference (edge) on the water absorption core.
- the auxiliary sheet is arranged on the user side (the side where the liquid invades) when it is attached.
- the test absorbent article of Example 10 has the same configuration as shown in FIGS. 6A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
- the test-absorbent article of Comparative Example 1 includes only a water-absorbing core, and has the same configuration as that shown in FIGS. 8A (top view) and B (side view from one side in the longitudinal direction of the test-absorbent article). It has a structure.
- Comparative Example 2 The test-absorbent article of Comparative Example 2 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles c produced in Production Example 3. Got
- Comparative Example 3 The test-absorbent article of Comparative Example 3 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles d produced in Production Example 4.
- Comparative Example 4 The test-absorbent article of Comparative Example 4 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles e produced in Production Example 5.
- Comparative Example 5 The water-absorbent resin particles used to prepare the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles f collected from the sanitary napkin "Eris Morning Super Safe CLIINS" (purchased in 2017) of Daio Paper Corporation sold in Japan. Except for the above, a test absorbent article of Comparative Example 5 was obtained in the same manner as in Example 1.
- Comparative Example 6 Example 1 except that the size to be cut as an auxiliary sheet is set to 3 cm ⁇ 10 cm, and the long side of the auxiliary sheet is changed so as to be adhered to the surface of the air-laid non-woven fabric-1 along the short side of the water absorption core. In the same manner as above, a test absorbent article of Comparative Example 6 was obtained.
- auxiliary sheet in Comparative Example 6 a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order.
- the swollen layers in Comparative Example 6 are provided at both ends in the longitudinal direction of the water absorption core along the lateral direction of the water absorption core.
- the auxiliary sheet is arranged on the user side (the side where the liquid invades) when it is attached.
- the test absorbent article of Comparative Example 6 has a configuration similar to that shown in FIGS. 9A (top view) and B (side view seen from one side in the longitudinal direction).
- the above-mentioned medium particle size of the water-absorbent resin particles was measured by the following procedure. That is, from the top of the JIS standard sieve, a sieve with a mesh size of 600 ⁇ m, a sieve with a mesh size of 500 ⁇ m, a sieve with a mesh size of 425 ⁇ m, a sieve with a mesh size of 300 ⁇ m, a sieve with a mesh size of 250 ⁇ m, a sieve with a mesh size of 180 ⁇ m, and a sieve with a mesh size of 150 ⁇ m. , And the saucer in that order.
- the water absorption rate of the water-absorbent resin particles with respect to physiological saline was measured by the following procedure based on the Vortex method. First, 50 ⁇ 0.1 g of physiological saline adjusted to a temperature of 25 ⁇ 0.2 ° C. in a constant temperature water tank was weighed in a beaker having a capacity of 100 mL. Next, a vortex was generated by stirring at 600 rpm using a magnetic stirrer bar (8 mm ⁇ ⁇ 30 mm, without ring). 2.0 ⁇ 0.002 g of water-absorbent resin particles were added to physiological saline at one time. The time [seconds] from the addition of the water-absorbent resin particles to the time when the vortex on the liquid surface converged was measured, and the time was recorded as the water absorption rate of the water-absorbent resin particles.
- the swelling power test of the water-absorbent resin particles was performed using the apparatus shown in FIG.
- the swelling power test was carried out according to the procedure shown below.
- a small tabletop tester EZ-Test manufactured by Shimadzu Corporation was used to measure the swelling power of the water-absorbent resin particles.
- a cylindrical jig 74 (cylindrical weight) made of acrylic resin having a diameter of 19.5 mm and a height of 59 mm and a mass of 20.5 g is inserted into the cylinder 72, and the cylindrical jig 74 is placed on the water-absorbent resin particles 73.
- a dry glass filter 76 (filter hole diameter G1) having a diameter of 50 mm and a thickness of 5 mm was placed in the central portion of the petri dish 75, and physiological saline 77 was injected to a position slightly below the upper surface of the glass filter 76 ( About 20 ml).
- a 50 mm ⁇ 50 mm impermeable liquid sheet 78 is placed near the center of the upper surface of the glass filter 76 in which the physiological saline 77 has permeated, and the impermeable resin sheet 78 contains the water-absorbent resin particles 73.
- the cylinder 72 was placed vertically with the nylon (registered trademark) mesh 71 facing down.
- the load cell 79 was arranged so that the pressure-sensitive portion having a diameter of 20 mm connected to the load cell 79 of the EZ-Test was located immediately above the cylindrical jig 74 in the cylinder 72.
- Table 1 shows the measurement results of water absorption, water absorption rate, and swelling power for 10 seconds and 60 seconds.
- FIG. 11 A crotch leak test was performed using the device shown in FIG.
- the device shown in FIG. 11 is a device that imitates a standing position and a sitting position.
- a test absorbent article is placed on the device, and artificial urine is injected from vertically above the center of the test absorbent article with a dropping funnel. Thereby, the amount of artificial urine leaked from the short side of the test absorbent article is evaluated.
- the aluminum formwork 54 was assembled by assembling aluminum parts 54a and 54b (the width of the aluminum frame is 3 cm) so that the horizontal distance between the insides of the aluminum parts was 15 cm.
- the most slack portion of the impermeable sheet 53 was set at a position 9 cm vertically above the surface (horizontal plane) on which the measuring device was installed.
- test absorbent article 200 was placed on the impermeable sheet 53 imitating the back sheet of the measuring device, and the center of the test absorbent article 200 was placed on the most slack portion of the impermeable sheet 53. At this time, the test absorbent article 200 was placed in a state where the absorbent article 200 was exposed, and no top sheet or the like was used.
- Dropping funnel 52 (dropping funnel 52) whose dropping speed was adjusted to 8 ml / sec, with the position 1 cm above the center of the test absorbent article 200 in the vertical direction (10 cm above the surface on which the device was installed) as the loading point.
- Table 2 shows the composition of the auxiliary sheet and the evaluation results.
- the "user side” means that the auxiliary sheet is placed on the user side (the side where the liquid invades) when the user wears the auxiliary sheet on the main surface of the water absorption core
- the "outside” means that the auxiliary sheet is placed. It means that it is placed on the side opposite to the user side when it is worn by the user on the main surface of the water absorption core.
- the “longitudinal ends” in Table 2 mean that the swelling layer is provided on both ends of the water absorption core in the lateral direction along the longitudinal direction of the water absorption core.
- the user By providing a swelling layer containing the water-absorbent resin particles at a predetermined position on the auxiliary sheet and controlling the 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer to a specific value, the user is in a wearing state. It was shown that liquid leakage (crotch leakage) was suppressed.
- the device shown in FIG. 12 is a device that imitates lying on the back and lying down, and by placing the test absorbent article 200 on the device and injecting artificial urine toward the center of the test absorbent article 200 with a liquid feed pump. , The amount of artificial urine leaked is evaluated.
- Table 3 shows the composition of the auxiliary sheet and the evaluation results.
- “User side” and “longitudinal end” in Table 3 have the same meaning as in Table 2.
- swelling layers are provided on both ends of the water absorption core in the longitudinal direction along the short direction of the water absorption core, and on both ends in the short direction.
- the swelling layer is provided on both ends of the water absorption core in the longitudinal direction along the longitudinal direction of the water absorption core.
- the user By providing a swelling layer containing the water-absorbent resin particles at a predetermined position on the auxiliary sheet and controlling the 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer to a specific value, the user is in a wearing state. It was shown that liquid leakage (abdominal leakage and back leakage) was suppressed.
- 10 Absorbent layer, 10a ... Water-absorbent resin particles, 10b ... Fiber layer, 20a, 20b ... Core wrap sheet, 21 ... Adhesive, 30 ... Liquid permeable sheet, 40 ... Liquid impermeable sheet, 50 ... Water-absorbing core, 60 ... Auxiliary sheet, 61 ... Swelling layer, 61a ... Water-absorbent resin particles, 61b ... Fiber layer, 62a, 62b ... Sheet base material, 63a, 63b ... Adhesive, 100 ... Absorbent article.
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Abstract
Disclosed is an absorbent article equipped with a strip-shaped water-absorbing core, an auxiliary sheet that assists with liquid absorption by the water-absorbing core, a liquid-impermeable sheet, and a liquid-permeable sheet. The liquid-impermeable sheet, water-absorbing core, and liquid-permeable sheet are disposed in that order. The auxiliary sheet is disposed between the impermeable sheet and the water-absorbing core and/or between the water-absorbing core and the liquid-permeable sheet. The auxiliary sheet has a swelling layer including water-absorbing resin particles. The swelling layer is provided along the longitudinal direction of the water-absorbing core on both ends of the lateral direction of the water-absorbing core, and the 10-second value of the swelling power of the water-absorbing resin particles contained in the swelling layer is 5 N or higher.
Description
本発明は、吸収性物品及び補助シートに関する。
The present invention relates to an absorbent article and an auxiliary sheet.
尿等の水を主成分とする液体を吸収するための吸収性物品には、昨今では、液体を吸収可能な吸収層を備える吸収体が用いられている。
Recently, an absorber having an absorbing layer capable of absorbing a liquid is used as an absorbent article for absorbing a liquid containing water as a main component such as urine.
例えば、特許文献1には、幅方向と前後方向を有し、トップシートとバックシートとこれらの間に設けられた第1吸収体を有する吸収性物品であって;第1吸収体は、複数層のシート部材を含み、シート部材の間に吸水性樹脂を有しパルプ繊維を有しないように構成され、幅方向の両側に端部領域とこれらの間に位置する中央領域を有し;端部領域に、ボルテックス法による吸水速度が20秒以下である吸水性樹脂が配され;中央領域に、ボルテックス法による吸水速度が40秒以上である吸水性樹脂が配されている吸収性物品が開示されている。
For example, Patent Document 1 describes an absorbent article having a width direction and a front-rear direction, and having a top sheet, a back sheet, and a first absorbent body provided between them; a plurality of first absorbent bodies are provided. It contains a layer of sheet members, is configured to have a water-absorbent resin between the sheet members and no pulp fibers, and has end regions and a central region located between them on both sides in the width direction; An absorbent article in which a water-absorbent resin having a water absorption rate of 20 seconds or less by the vortex method is arranged in a partial region; and a water-absorbent resin having a water absorption rate of 40 seconds or more by the vortex method is arranged in a central region is disclosed. Has been done.
おむつ等の吸収性物品は、装着した状態においてより多くの液体を吸収することができ、吸収性物品の外部への液体漏れが抑制されていることが望ましい。
It is desirable that absorbent articles such as diapers can absorb more liquid when worn, and that liquid leakage to the outside of the absorbent articles is suppressed.
本発明は、使用者の装着状態において高い吸液量を有し、液体漏れが抑制された吸収性物品を提供することを目的とする。本発明は、使用者の装着状態において高い吸液量を有し、液体漏れが抑制された吸収性物品を与え得る補助シートを提供することも目的とする。
An object of the present invention is to provide an absorbent article having a high liquid absorption amount when worn by a user and in which liquid leakage is suppressed. It is also an object of the present invention to provide an auxiliary sheet which has a high liquid absorption amount when worn by a user and can provide an absorbent article in which liquid leakage is suppressed.
本発明の一側面は、短冊状の吸水コア、該吸水コアによる吸液を補助する補助シート、液体不透過性シート及び液体透過性シートを備え、液体不透過性シート、吸水コア及び液体透過性シートがこの順に配置され、補助シートは、不透過性シートと吸水コアとの間、及び/又は、吸水コアと液体透過性シートとの間に配置されている、吸収性物品に関する。当該吸収性物品において、補助シートは、吸水性樹脂粒子を含む膨潤層を有し、膨潤層は、吸水コアの短手方向の両端部上に吸水コアの長手方向に沿って設けられており、膨潤層に含まれる吸水性樹脂粒子の膨潤力の10秒値は5N以上である。
One aspect of the present invention includes a strip-shaped water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet and a liquid permeable sheet, and includes a liquid impermeable sheet, a water absorbing core and a liquid permeable sheet. The sheets are arranged in this order, and the auxiliary sheet relates to an absorbent article which is arranged between the impermeable sheet and the water absorbing core and / or between the water absorbing core and the liquid permeable sheet. In the absorbent article, the auxiliary sheet has a swelling layer containing water-absorbing resin particles, and the swelling layers are provided on both ends of the water-absorbing core in the lateral direction along the longitudinal direction of the water-absorbing core. The 10-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer is 5 N or more.
上記膨潤力の10秒値は、以下のi)、ii)、iii)、iv)及びv)の順で行われる膨潤力試験で測定される。
i)両端に開口部を有し、その一方の開口部にメッシュが装着された内径20mmのシリンダーを用意し、メッシュが装着された側を下になる向きでシリンダーを垂直に立てた状態で、シリンダー内でメッシュ上に0.1gの吸水性樹脂粒子を均一に散布し、その上に直径19.5mmの円筒形治具を置く。
ii)厚み5mmのガラスフィルターを、水平に設置されたシャーレ内に載置し、ガラスフィルターにその上面より僅かに下の位置まで生理食塩水を浸透させる。
iii)生理食塩水が浸透したガラスフィルターの上面に不透液シートを置き、該不透液シートの上に、吸水性樹脂粒子を含むシリンダーを、メッシュが下になる向きで垂直に立てる。
iv)不透液シートを取り除いて、吸水性樹脂粒子による吸水を開始させる。
v)不透液シートを取り除いてから10秒後の時点の、吸水性樹脂粒子の膨潤によって生じた円筒形治具を押し上げる力をロードセルによって測定し、膨潤力の10秒値として記録する。 The 10-second value of the swelling power is measured by the swelling power test performed in the following order of i), ii), iii), iv) and v).
i) Prepare a cylinder with an inner diameter of 20 mm, which has openings at both ends and has a mesh mounted on one of the openings, with the cylinder standing vertically with the side on which the mesh is mounted facing down. 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
ii) A glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
iii) An impermeable sheet is placed on the upper surface of a glass filter permeated with physiological saline, and a cylinder containing water-absorbent resin particles is erected vertically on the impermeable sheet with the mesh facing down.
iv) Remove the impermeable sheet and start water absorption by the water-absorbent resin particles.
v) The force for pushing up the cylindrical jig generated by the swelling of the water-absorbent resin particles at 10 seconds after the impermeable sheet is removed is measured by the load cell and recorded as a 10-second value of the swelling force.
i)両端に開口部を有し、その一方の開口部にメッシュが装着された内径20mmのシリンダーを用意し、メッシュが装着された側を下になる向きでシリンダーを垂直に立てた状態で、シリンダー内でメッシュ上に0.1gの吸水性樹脂粒子を均一に散布し、その上に直径19.5mmの円筒形治具を置く。
ii)厚み5mmのガラスフィルターを、水平に設置されたシャーレ内に載置し、ガラスフィルターにその上面より僅かに下の位置まで生理食塩水を浸透させる。
iii)生理食塩水が浸透したガラスフィルターの上面に不透液シートを置き、該不透液シートの上に、吸水性樹脂粒子を含むシリンダーを、メッシュが下になる向きで垂直に立てる。
iv)不透液シートを取り除いて、吸水性樹脂粒子による吸水を開始させる。
v)不透液シートを取り除いてから10秒後の時点の、吸水性樹脂粒子の膨潤によって生じた円筒形治具を押し上げる力をロードセルによって測定し、膨潤力の10秒値として記録する。 The 10-second value of the swelling power is measured by the swelling power test performed in the following order of i), ii), iii), iv) and v).
i) Prepare a cylinder with an inner diameter of 20 mm, which has openings at both ends and has a mesh mounted on one of the openings, with the cylinder standing vertically with the side on which the mesh is mounted facing down. 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
ii) A glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
iii) An impermeable sheet is placed on the upper surface of a glass filter permeated with physiological saline, and a cylinder containing water-absorbent resin particles is erected vertically on the impermeable sheet with the mesh facing down.
iv) Remove the impermeable sheet and start water absorption by the water-absorbent resin particles.
v) The force for pushing up the cylindrical jig generated by the swelling of the water-absorbent resin particles at 10 seconds after the impermeable sheet is removed is measured by the load cell and recorded as a 10-second value of the swelling force.
本発明の他の側面は、吸水コアを備える吸収性物品において、吸水コアの吸液を補助するために用いられる補助シートであって、吸水性樹脂粒子を含む膨潤層を備え、膨潤層に含まれる吸水性樹脂粒子の上記膨潤力の10秒値が5N以上である、補助シートに関する。
Another aspect of the present invention is an auxiliary sheet used to assist the absorption of liquid in the water-absorbing core in an absorbent article provided with a water-absorbing core, which includes a swelling layer containing water-absorbing resin particles and is included in the swelling layer. The present invention relates to an auxiliary sheet in which the 10-second value of the swelling force of the water-absorbent resin particles is 5 N or more.
本発明によれば、使用者の装着状態において高い吸液量を有し、液体漏れが抑制された吸収性物品を提供することができる。
According to the present invention, it is possible to provide an absorbent article having a high liquid absorption amount in a wearing state of a user and suppressing liquid leakage.
また、本発明の補助シートによれば、例えば、吸収性物品の所定位置に配置することによって、使用者の装着状態において高い吸液量を有し、液体漏れが抑制された吸収性物品を与えることができる。
Further, according to the auxiliary sheet of the present invention, for example, by arranging the absorbent article at a predetermined position, the absorbent article having a high liquid absorption amount in the wearing state of the user and the liquid leakage is suppressed is provided. be able to.
以下、本発明のいくつかの実施形態について詳細に説明する。ただし、本発明は以下の実施形態に限定されるものではない。
Hereinafter, some embodiments of the present invention will be described in detail. However, the present invention is not limited to the following embodiments.
本明細書において、「アクリル」及び「メタクリル」を合わせて「(メタ)アクリル」と表記する。「アクリレート」及び「メタクリレート」も同様に「(メタ)アクリレート」と表記する。本明細書に段階的に記載されている数値範囲において、ある段階の数値範囲の上限値又は下限値は、他の段階の数値範囲の上限値又は下限値と任意に組み合わせることができる。本明細書に記載されている数値範囲において、その数値範囲の上限値又は下限値は、実施例に示されている値に置き換えてもよい。「A又はB」とは、A及びBのどちらか一方を含んでいればよく、両方とも含んでいてもよい。「水溶性」とは、25℃において水に5質量%以上の溶解性を示すことをいう。本明細書に例示する材料は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。組成物中の各成分の含有量は、組成物中に各成分に該当する物質が複数存在する場合、特に断らない限り、組成物中に存在する当該複数の物質の合計量を意味する。
In this specification, "acrylic" and "methacryl" are collectively referred to as "(meth) acrylic". Similarly, "acrylate" and "methacrylate" are also referred to as "(meth) acrylate". In the numerical range described stepwise in the present specification, the upper limit value or the lower limit value of the numerical range of one step can be arbitrarily combined with the upper limit value or the lower limit value of the numerical range of another step. In the numerical range described in the present specification, the upper limit value or the lower limit value of the numerical range may be replaced with the value shown in the examples. "A or B" may include either A or B, or both. "Water-soluble" means that it exhibits a solubility in water of 5% by mass or more at 25 ° C. The materials exemplified in the present specification may be used alone or in combination of two or more. The content of each component in the composition means the total amount of the plurality of substances present in the composition when a plurality of substances corresponding to each component are present in the composition, unless otherwise specified.
<吸収性物品>
一実施形態に係る吸収性物品は、吸水コア、該吸水コアによる吸液を補助する補助シート、液体不透過性シート及び液体透過性シートを備える。吸収性物品において、液体不透過性シート、吸水コア及び液体透過性シートはこの順に配置されている。補助シートは、不透過性シート及び吸水コアの間、及び/又は、吸水コア及び液体透過性シートの間に配置される。 <Absorbent article>
The absorbent article according to one embodiment includes a water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet, and a liquid permeable sheet. In the absorbent article, the liquid impermeable sheet, the water absorbing core and the liquid permeable sheet are arranged in this order. The auxiliary sheet is arranged between the impermeable sheet and the water absorbing core and / or between the water absorbing core and the liquid permeable sheet.
一実施形態に係る吸収性物品は、吸水コア、該吸水コアによる吸液を補助する補助シート、液体不透過性シート及び液体透過性シートを備える。吸収性物品において、液体不透過性シート、吸水コア及び液体透過性シートはこの順に配置されている。補助シートは、不透過性シート及び吸水コアの間、及び/又は、吸水コア及び液体透過性シートの間に配置される。 <Absorbent article>
The absorbent article according to one embodiment includes a water absorbing core, an auxiliary sheet for assisting liquid absorption by the water absorbing core, a liquid impermeable sheet, and a liquid permeable sheet. In the absorbent article, the liquid impermeable sheet, the water absorbing core and the liquid permeable sheet are arranged in this order. The auxiliary sheet is arranged between the impermeable sheet and the water absorbing core and / or between the water absorbing core and the liquid permeable sheet.
[補助シート]
補助シートは、吸水性樹脂粒子を含む膨潤層を備える。補助シートは、吸水コアを備える吸収性物品において、吸水コアの吸液を補助するために用いられる。 [Auxiliary sheet]
The auxiliary sheet includes a swelling layer containing water-absorbent resin particles. The auxiliary sheet is used in an absorbent article provided with a water-absorbing core to assist the liquid absorption of the water-absorbing core.
補助シートは、吸水性樹脂粒子を含む膨潤層を備える。補助シートは、吸水コアを備える吸収性物品において、吸水コアの吸液を補助するために用いられる。 [Auxiliary sheet]
The auxiliary sheet includes a swelling layer containing water-absorbent resin particles. The auxiliary sheet is used in an absorbent article provided with a water-absorbing core to assist the liquid absorption of the water-absorbing core.
膨潤層に含まれる吸水性樹脂粒子の、以下のi)、ii)、iii)、iv)及びv)の順で行われる膨潤力試験で測定される膨潤力の10秒値は5N以上である。
The 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer, which is measured in the swelling force test performed in the order of i), ii), iii), iv) and v) below, is 5 N or more. ..
i)両端に開口部を有し、その一方の開口部にメッシュが装着された内径20mmのシリンダーを用意し、メッシュが装着された側を下になる向きでシリンダーを垂直に立てた状態で、シリンダー内でメッシュ上に0.1gの吸水性樹脂粒子を均一に散布し、その上に直径19.5mmの円筒形治具を置く。
ii)厚み5mmのガラスフィルターを、水平に設置されたシャーレ内に載置し、ガラスフィルターにその上面より僅かに下の位置まで生理食塩水を浸透させる。
iii)生理食塩水が浸透したガラスフィルターの上面に不透液シートを置き、該不透液シートの上に、吸水性樹脂粒子を含むシリンダーを、メッシュが下になる向きで垂直に立てる。
iv)不透液シートを取り除いて、吸水性樹脂粒子による吸水を開始させる。
v)不透液シートを取り除いてから10秒後の時点の、吸水性樹脂粒子の膨潤によって生じた円筒形治具を押し上げる力をロードセルによって測定し、10秒後の時点の測定値を膨潤力の10秒値として記録する。膨潤力の10秒値は、具体的には後述する実施例に記載の方法によって測定される。 i) Prepare a cylinder with an inner diameter of 20 mm, which has openings at both ends and has a mesh mounted on one of the openings, with the cylinder standing vertically with the side on which the mesh is mounted facing down. 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
ii) A glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
iii) An impermeable sheet is placed on the upper surface of a glass filter permeated with physiological saline, and a cylinder containing water-absorbent resin particles is erected vertically on the impermeable sheet with the mesh facing down.
iv) Remove the impermeable sheet and start water absorption by the water-absorbent resin particles.
v) The force to push up the cylindrical jig generated by the swelling of the water-absorbent resin particles at 10 seconds after removing the impermeable sheet is measured by the load cell, and the measured value at 10 seconds is the swelling force. Record as a 10-second value of. The 10-second value of the swelling force is specifically measured by the method described in Examples described later.
ii)厚み5mmのガラスフィルターを、水平に設置されたシャーレ内に載置し、ガラスフィルターにその上面より僅かに下の位置まで生理食塩水を浸透させる。
iii)生理食塩水が浸透したガラスフィルターの上面に不透液シートを置き、該不透液シートの上に、吸水性樹脂粒子を含むシリンダーを、メッシュが下になる向きで垂直に立てる。
iv)不透液シートを取り除いて、吸水性樹脂粒子による吸水を開始させる。
v)不透液シートを取り除いてから10秒後の時点の、吸水性樹脂粒子の膨潤によって生じた円筒形治具を押し上げる力をロードセルによって測定し、10秒後の時点の測定値を膨潤力の10秒値として記録する。膨潤力の10秒値は、具体的には後述する実施例に記載の方法によって測定される。 i) Prepare a cylinder with an inner diameter of 20 mm, which has openings at both ends and has a mesh mounted on one of the openings, with the cylinder standing vertically with the side on which the mesh is mounted facing down. 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
ii) A glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
iii) An impermeable sheet is placed on the upper surface of a glass filter permeated with physiological saline, and a cylinder containing water-absorbent resin particles is erected vertically on the impermeable sheet with the mesh facing down.
iv) Remove the impermeable sheet and start water absorption by the water-absorbent resin particles.
v) The force to push up the cylindrical jig generated by the swelling of the water-absorbent resin particles at 10 seconds after removing the impermeable sheet is measured by the load cell, and the measured value at 10 seconds is the swelling force. Record as a 10-second value of. The 10-second value of the swelling force is specifically measured by the method described in Examples described later.
膨潤層に含まれる吸水性樹脂粒子の膨潤力の10秒値は、5N以上であり、6N以上、7N以上、8N以上、9N以上、10N以上、又は11N以上であってよく、20N以下、18N以下、16N以下、14N以下、又は13N以下であってよい。膨潤層に含まれる吸水性樹脂粒子の膨潤力の10秒値は、5N以上20N以下、5N以上18N以下、5N以上16N以下、5N以上14N以下、又は5N以上13N以下であってよい。
The 10-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer may be 5N or more, 6N or more, 7N or more, 8N or more, 9N or more, 10N or more, or 11N or more, 20N or less, 18N or more. Hereinafter, it may be 16N or less, 14N or less, or 13N or less. The 10-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer may be 5N or more and 20N or less, 5N or more and 18N or less, 5N or more and 16N or less, 5N or more and 14N or less, or 5N or more and 13N or less.
膨潤力の10秒値は、例えば、吸水性樹脂粒子の形状を変化させて比表面積を調整すること、吸水性樹脂の表面を親水化するような表面処理を施すこと、内部の架橋と表面架橋とによる粒子一粒における架橋密度の濃淡のバランスを調整すること等により、制御することができる。
The 10-second value of the swelling force can be determined by, for example, changing the shape of the water-absorbent resin particles to adjust the specific surface area, performing surface treatment to make the surface of the water-absorbent resin hydrophilic, internal cross-linking and surface cross-linking. It can be controlled by adjusting the balance of the light and shade of the cross-linking density in one particle by the above.
本実施形態に係る吸収性物品では、まず、吸液対象となる液体が侵入すると、吸水コア及び補助シートによって吸液される。膨潤力の10秒値がある程度以上である吸水性樹脂粒子は、吸液初期段階において、より膨潤しやすい傾向があり、このような吸水性樹脂粒子を含む膨潤層を、吸水コアの短手方向の両端部上に長手方向に沿って配置することによって、吸液初期段階において膨潤した吸水性樹脂粒子が、その後に侵入した液体による短手方向の外側への液流れの発生を抑制し、この結果として、使用者の装着状態において、液体漏れが抑制されることになると考えられる。いわば吸水コアの両端に液流れをブロックするゲル層を発生させ短手方向(幅方向)への液体漏れを抑制していると考えられる。ただし、液体漏れが抑制される要因は、上記要因に限られない。
In the absorbent article according to the present embodiment, first, when a liquid to be absorbed invades, the liquid is absorbed by the water absorption core and the auxiliary sheet. The water-absorbent resin particles having a swelling force of 10 seconds or more tend to swell more easily in the initial stage of liquid absorption, and the swelling layer containing such water-absorbent resin particles is formed in the lateral direction of the water-absorbing core. By arranging it along the longitudinal direction on both ends of the water-absorbing resin particles, the water-absorbent resin particles swollen in the initial stage of liquid absorption suppress the generation of liquid flow to the outside in the lateral direction due to the liquid that has subsequently invaded. As a result, it is considered that liquid leakage is suppressed in the wearing state of the user. So to speak, it is considered that gel layers that block the liquid flow are generated at both ends of the water absorption core to suppress liquid leakage in the lateral direction (width direction). However, the factors that suppress liquid leakage are not limited to the above factors.
膨潤層に含まれる吸水性樹脂粒子の膨潤力の60秒値は、使用状態における液体漏れ抑制効果により一層優れる観点から、30N以下、20N以下、18N以下、15N以下、13N以下、10N以下、又は8N以下であってよく、6N以上、又は7N以上であってよい。膨潤層に含まれる吸水性樹脂粒子の膨潤力の60秒値は、使用状態における液体漏れ抑制効果により一層優れる観点から、6N以上30N以下、6N以上20N以下、6N以上18N以下、6N以上15N以下、7N以上30N以下、7N以上20N以下、7N以上18N以下、又は7N以上15N以下であってよい。
The 60-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer is 30 N or less, 20 N or less, 18 N or less, 15 N or less, 13 N or less, 10 N or less, or from the viewpoint of being more excellent in the liquid leakage suppressing effect in the used state. It may be 8N or less, 6N or more, or 7N or more. The 60-second value of the swelling power of the water-absorbent resin particles contained in the swelling layer is 6N or more and 30N or less, 6N or more and 20N or less, 6N or more and 18N or less, and 6N or more and 15N or less from the viewpoint of being more excellent in the liquid leakage suppressing effect in the used state. , 7N or more and 30N or less, 7N or more and 20N or less, 7N or more and 18N or less, or 7N or more and 15N or less.
膨潤力の60秒値は、上述したi)、ii)、iii)及びiv)並びに以下のvi)の順で行われる膨潤力試験で測定される。
vi)不透液シートを取り除いてから60秒後の時点の、吸水性樹脂粒子の膨潤によって生じた円筒形治具を押し上げる力をロードセルによって測定し、60秒後の時点の測定値を膨潤力の60秒値として記録する。膨潤力の60秒値は、具体的には後述する実施例に記載の方法によって測定される。 The 60-second value of the swelling force is measured by the swelling force test performed in the order of i), ii), iii) and iv) described above and vi) below.
vi) The force to push up the cylindrical jig generated by the swelling of the water-absorbent resin particles 60 seconds after removing the impermeable sheet is measured by the load cell, and the measured value at 60 seconds later is the swelling force. Record as a 60-second value of. The 60-second value of the swelling force is specifically measured by the method described in Examples described later.
vi)不透液シートを取り除いてから60秒後の時点の、吸水性樹脂粒子の膨潤によって生じた円筒形治具を押し上げる力をロードセルによって測定し、60秒後の時点の測定値を膨潤力の60秒値として記録する。膨潤力の60秒値は、具体的には後述する実施例に記載の方法によって測定される。 The 60-second value of the swelling force is measured by the swelling force test performed in the order of i), ii), iii) and iv) described above and vi) below.
vi) The force to push up the cylindrical jig generated by the swelling of the water-
膨潤力の60秒値は、例えば、内部の架橋と表面架橋とによる粒子一粒における架橋密度の濃淡のバランスを調整すること等により、制御することができる。
The 60-second value of the swelling force can be controlled, for example, by adjusting the balance of the density of the cross-linking in each particle due to the internal cross-linking and the surface cross-linking.
吸水性樹脂粒子の生理食塩水の吸水量は、例えば20~80g/g、30~70g/g、又は40~65g/gであってよい。吸水性樹脂粒子の吸水速度(Vortex法)は、例えば1~70秒、2~50秒、2~25秒、又は2~10秒であってよい。
The water absorption amount of the physiological saline of the water-absorbent resin particles may be, for example, 20 to 80 g / g, 30 to 70 g / g, or 40 to 65 g / g. The water absorption rate (Vortex method) of the water-absorbent resin particles may be, for example, 1 to 70 seconds, 2 to 50 seconds, 2 to 25 seconds, or 2 to 10 seconds.
生理食塩水の吸水量及び吸水速度は、後述する実施例に記載の方法により測定することができる。
The water absorption amount and the water absorption rate of the physiological saline can be measured by the method described in Examples described later.
本実施形態に係る吸水性樹脂粒子の形状は、特に限定されず、例えば略球状、破砕状又は顆粒状であってもよく、これらの形状を有する一次粒子が凝集した粒子が形成されていてもよい。
The shape of the water-absorbent resin particles according to the present embodiment is not particularly limited, and may be, for example, substantially spherical, crushed, or granular, and even if primary particles having these shapes are aggregated to form particles. Good.
吸水性樹脂粒子の中位粒子径は、100~800μm、150~700μm、200~600μm、又は250~500μmであってもよい。中位粒子径は、以下の方法で測定することができる。JIS標準篩を上から、目開き600μmの篩、目開き500μmの篩、目開き425μmの篩、目開き300μmの篩、目開き250μmの篩、目開き180μmの篩、目開き150μmの篩、及び、受け皿の順に組み合わせる。組み合わせた最上の篩に、吸水性樹脂粒子50gを入れ、ロータップ式振とう器(株式会社飯田製作所製)を用いてJIS Z 8815(1994)に準じて分級する。分級後、各篩上に残った粒子の質量を全量に対する質量百分率として算出し粒度分布を求める。この粒度分布に関して粒子径の大きい方から順に篩上を積算することにより、篩の目開きと篩上に残った粒子の質量百分率の積算値との関係を対数確率紙にプロットする。確率紙上のプロットを直線で結ぶことにより、積算質量百分率50質量%に相当する粒子径を中位粒子径として得る。
The medium particle size of the water-absorbent resin particles may be 100 to 800 μm, 150 to 700 μm, 200 to 600 μm, or 250 to 500 μm. The medium particle size can be measured by the following method. From the top, JIS standard sieves have a mesh size of 600 μm, a mesh size of 500 μm, a mesh size of 425 μm, a mesh size of 300 μm, a mesh size of 250 μm, a mesh size of 180 μm, a mesh size of 150 μm, and a sieve. , Combine in the order of the saucer. 50 g of water-absorbent resin particles are placed in the best combined sieve, and the mixture is classified according to JIS Z8815 (1994) using a low-tap shaker (manufactured by Iida Seisakusho Co., Ltd.). After classification, the mass of the particles remaining on each sieve is calculated as a mass percentage with respect to the total amount to obtain the particle size distribution. The relationship between the mesh size of the sieve and the integrated value of the mass percentage of the particles remaining on the sieve is plotted on the logarithmic probability paper by integrating the particles on the sieve in order from the one having the largest particle size with respect to this particle size distribution. By connecting the plots on the probability paper with a straight line, the particle size corresponding to the cumulative mass percentage of 50% by mass is obtained as the medium particle size.
吸水性樹脂粒子61aは、例えば、エチレン性不飽和単量体を含む単量体の重合により形成された重合体粒子を含むことができる。重合体粒子は、エチレン性不飽和単量体に由来する単量体単位として含む重合体を含有する吸水性の粒子であってもよい。エチレン性不飽和単量体は、水溶性の単量体であってもよく、その例としては、(メタ)アクリル酸及びその塩、2-(メタ)アクリルアミド-2-メチルプロパンスルホン酸及びその塩、(メタ)アクリルアミド、N,N-ジメチル(メタ)アクリルアミド、2-ヒドロキシエチル(メタ)アクリレート、N-メチロール(メタ)アクリルアミド、ポリエチレングリコールモノ(メタ)アクリレート、N,N-ジエチルアミノエチル(メタ)アクリレート、N,N-ジエチルアミノプロピル(メタ)アクリレート、並びにジエチルアミノプロピル(メタ)アクリルアミドが挙げられる。エチレン性不飽和単量体がアミノ基を有する場合、当該アミノ基は4級化されていてもよい。エチレン性不飽和単量体は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。上述の単量体のカルボキシル基、アミノ基等の官能基は、後述する表面架橋工程において架橋が可能な官能基として機能し得る。
The water-absorbent resin particles 61a can include, for example, polymer particles formed by polymerizing a monomer containing an ethylenically unsaturated monomer. The polymer particles may be water-absorbent particles containing a polymer contained as a monomer unit derived from an ethylenically unsaturated monomer. The ethylenically unsaturated monomer may be a water-soluble monomer, and examples thereof include (meth) acrylic acid and salts thereof, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts. Salt, (meth) acrylamide, N, N-dimethyl (meth) acrylamide, 2-hydroxyethyl (meth) acrylate, N-methylol (meth) acrylamide, polyethylene glycol mono (meth) acrylate, N, N-diethylaminoethyl (meth) ) Acrylate, N, N-diethylaminopropyl (meth) acrylate, and diethylaminopropyl (meth) acrylamide. When the ethylenically unsaturated monomer has an amino group, the amino group may be quaternized. The ethylenically unsaturated monomer may be used alone or in combination of two or more. Functional groups such as the carboxyl group and amino group of the above-mentioned monomers can function as functional groups capable of cross-linking in the surface cross-linking step described later.
エチレン性不飽和単量体は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。重合体粒子における、エチレン性不飽和単量体を単量体単位として含む重合体の割合は、重合体粒子の質量を基準として50~100質量%、60~100質量%、70~100質量%、又は80~100質量%であってもよい。重合体粒子は、(メタ)アクリル酸又は(メタ)アクリル酸塩のうち少なくとも一方を単量体単位として含む(メタ)アクリル酸系重合体を含有する粒子であってもよい。(メタ)アクリル酸系重合体における(メタ)アクリル酸又は(メタ)アクリル酸塩に由来する単量体単位の合計の割合は、重合体の質量を基準として70~100質量%であってよく、90~100質量%であってもよい。
The ethylenically unsaturated monomer may be used alone or in combination of two or more. The proportion of the polymer containing the ethylenically unsaturated monomer as a monomer unit in the polymer particles is 50 to 100% by mass, 60 to 100% by mass, and 70 to 100% by mass based on the mass of the polymer particles. , Or 80 to 100% by mass. The polymer particles may be particles containing a (meth) acrylic acid-based polymer containing at least one of (meth) acrylic acid or (meth) acrylate as a monomer unit. The total ratio of the monomer units derived from (meth) acrylic acid or (meth) acrylate in the (meth) acrylic acid-based polymer may be 70 to 100% by mass based on the mass of the polymer. , 90-100% by mass.
吸水性樹脂粒子61aは、エチレン性不飽和単量体を含む単量体を重合させる工程を含む方法により、製造することができる。重合方法としては、逆相懸濁重合法、水溶液重合法、バルク重合法、沈殿重合法等が挙げられる。得られる吸水性樹脂粒子の良好な吸水特性の確保、及び、重合反応の制御が容易である観点から、逆相懸濁重合法又は水溶液重合法を適用してもよい。以下においては、エチレン性不飽和単量体を重合させる方法として、逆相懸濁重合法を例にとって説明する。
The water-absorbent resin particles 61a can be produced by a method including a step of polymerizing a monomer containing an ethylenically unsaturated monomer. Examples of the polymerization method include a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method. From the viewpoint of ensuring good water absorption characteristics of the obtained water-absorbent resin particles and facilitating control of the polymerization reaction, a reverse phase suspension polymerization method or an aqueous solution polymerization method may be applied. In the following, as a method for polymerizing an ethylenically unsaturated monomer, a reverse phase suspension polymerization method will be described as an example.
工業的に入手が容易である観点から、エチレン性不飽和単量体は、(メタ)アクリル酸及びその塩、アクリルアミド、メタクリルアミド、並びに、N,N-ジメチルアクリルアミドからなる群より選ばれる少なくとも1種の化合物を含んでいてもよい。エチレン性不飽和単量体が、(メタ)アクリル酸及びその塩、並びに、アクリルアミドからなる群より選ばれる少なくとも1種の化合物を含んでいてもよい。吸水特性を更に高める観点から、エチレン性不飽和単量体は、(メタ)アクリル酸及びその塩からなる群より選ばれる少なくとも1種の化合物を含んでもよい。
From the viewpoint of industrial availability, the ethylenically unsaturated monomer is at least one selected from the group consisting of (meth) acrylic acid and salts thereof, acrylamide, methacrylamide, and N, N-dimethylacrylamide. It may contain a compound of the species. The ethylenically unsaturated monomer may contain (meth) acrylic acid and a salt thereof, and at least one compound selected from the group consisting of acrylamide. From the viewpoint of further enhancing the water absorption property, the ethylenically unsaturated monomer may contain at least one compound selected from the group consisting of (meth) acrylic acid and salts thereof.
エチレン性不飽和単量体は、水溶液として重合反応に用いることができる。エチレン性不飽和単量体を含む水溶液(以下、単に「単量体水溶液」という)におけるエチレン性不飽和単量体の濃度は、20質量%以上飽和濃度以下、25~70質量%、又は30~55質量%であってもよい。水溶液において使用される水としては、水道水、蒸留水、イオン交換水等が挙げられる。
The ethylenically unsaturated monomer can be used in the polymerization reaction as an aqueous solution. The concentration of the ethylenically unsaturated monomer in the aqueous solution containing the ethylenically unsaturated monomer (hereinafter, simply referred to as "monomeric aqueous solution") is 20% by mass or more and the saturation concentration or less, 25 to 70% by mass, or 30. It may be up to 55% by mass. Examples of the water used in the aqueous solution include tap water, distilled water, ion-exchanged water and the like.
吸水性樹脂粒子を得るための単量体として、上述のエチレン性不飽和単量体以外の単量体が使用されてもよい。このような単量体は、例えば、上述のエチレン性不飽和単量体を含む水溶液に混合して用いることができる。エチレン性不飽和単量体の使用量は、単量体全量に対して70~100モル%であってもよい。(メタ)アクリル酸及びその塩の割合が単量体全量に対して70~100モル%であってもよい。
As the monomer for obtaining the water-absorbent resin particles, a monomer other than the above-mentioned ethylenically unsaturated monomer may be used. Such a monomer can be used, for example, by mixing with an aqueous solution containing the above-mentioned ethylenically unsaturated monomer. The amount of the ethylenically unsaturated monomer used may be 70 to 100 mol% with respect to the total amount of the monomer. The ratio of (meth) acrylic acid and a salt thereof may be 70 to 100 mol% with respect to the total amount of the monomer.
エチレン性不飽和単量体が酸性基を有する場合、その酸性基をアルカリ性中和剤によって中和してから、単量体溶液を重合反応に用いてもよい。エチレン性不飽和単量体における、アルカリ性中和剤による中和度は、得られる吸水性樹脂粒子の浸透圧を高くし、吸水特性(吸水量等)を更に高める観点から、エチレン性不飽和単量体中の酸性基の10~100モル%、50~90モル%、又は60~80モル%であってもよい。アルカリ性中和剤としては、水酸化ナトリウム、炭酸ナトリウム、炭酸水素ナトリウム、水酸化カリウム、炭酸カリウム等のアルカリ金属塩;アンモニアなどが挙げられる。アルカリ性中和剤は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。アルカリ性中和剤は、中和操作を簡便にするために水溶液の状態で用いられてもよい。エチレン性不飽和単量体の酸性基の中和は、例えば、水酸化ナトリウム、水酸化カリウム等の水溶液を上述の単量体水溶液に滴下して混合することにより行うことができる。
When the ethylenically unsaturated monomer has an acidic group, the acidic group may be neutralized with an alkaline neutralizer and then the monomer solution may be used in the polymerization reaction. The degree of neutralization of an ethylenically unsaturated monomer by an alkaline neutralizing agent increases the osmotic pressure of the obtained water-absorbent resin particles and further enhances the water absorption characteristics (water absorption amount, etc.). It may be 10-100 mol%, 50-90 mol%, or 60-80 mol% of the acidic group in the body. Examples of the alkaline neutralizing agent include alkali metal salts such as sodium hydroxide, sodium carbonate, sodium hydrogen carbonate, potassium hydroxide and potassium carbonate; ammonia and the like. The alkaline neutralizer may be used alone or in combination of two or more. The alkaline neutralizer may be used in the form of an aqueous solution to simplify the neutralization operation. Neutralization of the acidic group of the ethylenically unsaturated monomer can be performed, for example, by dropping an aqueous solution of sodium hydroxide, potassium hydroxide or the like into the above-mentioned monomer aqueous solution and mixing them.
逆相懸濁重合法においては、界面活性剤の存在下、炭化水素分散媒中で単量体水溶液を分散し、ラジカル重合開始剤等を用いてエチレン性不飽和単量体の重合を行うことができる。ラジカル重合開始剤としては、水溶性ラジカル重合開始剤を用いることができる。
In the reverse phase suspension polymerization method, an aqueous monomer solution is dispersed in a hydrocarbon dispersion medium in the presence of a surfactant, and an ethylenically unsaturated monomer is polymerized using a radical polymerization initiator or the like. Can be done. As the radical polymerization initiator, a water-soluble radical polymerization initiator can be used.
界面活性剤としては、ノニオン系界面活性剤、アニオン系界面活性剤等が挙げられる。ノニオン系界面活性剤としては、ソルビタン脂肪酸エステル、(ポリ)グリセリン脂肪酸エステル(「(ポリ)」とは、「ポリ」の接頭語がある場合及びない場合の双方を意味するものとする。以下同じ。)、ショ糖脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル、ポリオキシエチレングリセリン脂肪酸エステル、ソルビトール脂肪酸エステル、ポリオキシエチレンソルビトール脂肪酸エステル、ポリオキシエチレンアルキルエーテル、ポリオキシエチレンアルキルフェニルエーテル、ポリオキシエチレンヒマシ油、ポリオキシエチレン硬化ヒマシ油、アルキルアリルホルムアルデヒド縮合ポリオキシエチレンエーテル、ポリオキシエチレンポリオキシプロピレンブロックコポリマー、ポリオキシエチレンポリオキシプロピルアルキルエーテル、ポリエチレングリコール脂肪酸エステル等が挙げられる。アニオン系界面活性剤としては、脂肪酸塩、アルキルベンゼンスルホン酸塩、アルキルメチルタウリン酸塩、ポリオキシエチレンアルキルフェニルエーテル硫酸エステル塩、ポリオキシエチレンアルキルエーテルスルホン酸塩、ポリオキシエチレンアルキルエーテルのリン酸エステル、及びポリオキシエチレンアルキルアリルエーテルのリン酸エステル等が挙げられる。界面活性剤は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。
Examples of the surfactant include nonionic surfactants, anionic surfactants and the like. As the nonionic surfactant, sorbitan fatty acid ester and (poly) glycerin fatty acid ester (“(poly)” means both with and without the prefix of “poly”. The same shall apply hereinafter. ), Sucrose fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, sorbitol fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene himashi Examples thereof include oil, polyoxyethylene hydrogenated castor oil, alkylallyl formaldehyde condensed polyoxyethylene ether, polyoxyethylene polyoxypropylene block copolymer, polyoxyethylene polyoxypropyl alkyl ether, polyethylene glycol fatty acid ester and the like. Anionic surfactants include fatty acid salts, alkylbenzene sulfonates, alkylmethyl taurates, polyoxyethylene alkylphenyl ether sulfates, polyoxyethylene alkyl ether sulfonates, and polyoxyethylene alkyl ether phosphates. , And the phosphate ester of polyoxyethylene alkyl allyl ether and the like. The surfactant may be used alone or in combination of two or more.
W/O型逆相懸濁の状態が良好であり、好適な粒子径を有する吸水性樹脂粒子が得られやすく、工業的に入手が容易である観点から、界面活性剤は、ソルビタン脂肪酸エステル、ポリグリセリン脂肪酸エステル及びショ糖脂肪酸エステルからなる群より選ばれる少なくとも1種の化合物を含んでもよい。得られる吸水性樹脂粒子の吸水特性が向上しやすい観点から、界面活性剤は、ソルビタン脂肪酸エステル(例えばソルビタンモノラウレート)、及び/又はショ糖脂肪酸エステル(例えばショ糖ステアリン酸エステル)を用いてよい。これらの界面活性剤は、単独で用いられてもよいし、2種以上を組み合わせて用いられてもよい。
From the viewpoint that the W / O type reverse phase suspension is in a good state, water-absorbent resin particles having a suitable particle size can be easily obtained, and industrially available, the surfactant is a sorbitan fatty acid ester. It may contain at least one compound selected from the group consisting of polyglycerin fatty acid ester and sucrose fatty acid ester. From the viewpoint of easily improving the water absorption characteristics of the obtained water-absorbent resin particles, sorbitan fatty acid ester (for example, sorbitan monolaurate) and / or sucrose fatty acid ester (for example, sucrose stearic acid ester) are used as the surfactant. Good. These surfactants may be used alone or in combination of two or more.
界面活性剤の量は、単量体水溶液100質量部に対して、0.05~10質量部、0.08~5質量部、又は0.1~3質量部であってもよい。
The amount of the surfactant may be 0.05 to 10 parts by mass, 0.08 to 5 parts by mass, or 0.1 to 3 parts by mass with respect to 100 parts by mass of the aqueous monomer solution.
逆相懸濁重合では、上述の界面活性剤と共に高分子系分散剤を併せて用いてもよい。高分子系分散剤としては、無水マレイン酸変性ポリエチレン、無水マレイン酸変性ポリプロピレン、無水マレイン酸変性エチレン・プロピレン共重合体、無水マレイン酸変性EPDM(エチレン・プロピレン・ジエン・ターポリマー)、無水マレイン酸変性ポリブタジエン、無水マレイン酸・エチレン共重合体、無水マレイン酸・プロピレン共重合体、無水マレイン酸・エチレン・プロピレン共重合体、無水マレイン酸・ブタジエン共重合体、ポリエチレン、ポリプロピレン、エチレン・プロピレン共重合体、酸化型ポリエチレン、酸化型ポリプロピレン、酸化型エチレン・プロピレン共重合体、エチレン・アクリル酸共重合体、エチルセルロース、エチルヒドロキシエチルセルロース等が挙げられる。高分子系分散剤は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。高分子系分散剤は、単量体の分散安定性に優れる観点から、無水マレイン酸変性ポリエチレン、無水マレイン酸変性ポリプロピレン、無水マレイン酸変性エチレン・プロピレン共重合体、無水マレイン酸・エチレン共重合体、無水マレイン酸・プロピレン共重合体、無水マレイン酸・エチレン・プロピレン共重合体、ポリエチレン、ポリプロピレン、エチレン・プロピレン共重合体、酸化型ポリエチレン、酸化型ポリプロピレン、及び、酸化型エチレン・プロピレン共重合体からなる群より選ばれる少なくとも一種であってもよい。
In reverse phase suspension polymerization, a polymer-based dispersant may be used in combination with the above-mentioned surfactant. Examples of the polymer dispersant include maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, maleic anhydride-modified ethylene / propylene copolymer, maleic anhydride-modified EPDM (ethylene / propylene / diene / terpolymer), and maleic anhydride. Modified polybutadiene, maleic anhydride / ethylene copolymer, maleic anhydride / propylene copolymer, maleic anhydride / ethylene / propylene copolymer, maleic anhydride / butadiene copolymer, polyethylene, polypropylene, ethylene / propylene copolymer Examples thereof include coalescence, oxidized polyethylene, oxidized polypropylene, oxidized ethylene / propylene copolymer, ethylene / acrylic acid copolymer, ethyl cellulose, ethyl hydroxyethyl cellulose and the like. The polymer-based dispersant may be used alone or in combination of two or more. From the viewpoint of excellent dispersion stability of the monomer, the polymer-based dispersant includes maleic anhydride-modified polyethylene, maleic anhydride-modified polypropylene, maleic anhydride-modified ethylene / propylene copolymer, and maleic anhydride / ethylene copolymer. , Maleic anhydride / propylene copolymer, maleic anhydride / ethylene / propylene copolymer, polyethylene, polypropylene, ethylene / propylene copolymer, oxidized polyethylene, oxidized polypropylene, and oxidized ethylene / propylene copolymer It may be at least one selected from the group consisting of.
高分子系分散剤の量は、単量体水溶液100質量部に対して、0.05~10質量部、0.08~5質量部、又は0.1~3質量部であってもよい。
The amount of the polymer-based dispersant may be 0.05 to 10 parts by mass, 0.08 to 5 parts by mass, or 0.1 to 3 parts by mass with respect to 100 parts by mass of the aqueous monomer solution.
炭化水素分散媒は、炭素数6~8の鎖状脂肪族炭化水素、及び、炭素数6~8の脂環式炭化水素からなる群より選ばれる少なくとも1種の化合物を含んでいてもよい。炭化水素分散媒としては、n-ヘキサン、n-ヘプタン、2-メチルヘキサン、3-メチルヘキサン、2,3-ジメチルペンタン、3-エチルペンタン、n-オクタン等の鎖状脂肪族炭化水素;シクロヘキサン、メチルシクロヘキサン、シクロペンタン、メチルシクロペンタン、trans-1,2-ジメチルシクロペンタン、cis-1,3-ジメチルシクロペンタン、trans-1,3-ジメチルシクロペンタン等の脂環式炭化水素;ベンゼン、トルエン、キシレン等の芳香族炭化水素などが挙げられる。炭化水素分散媒は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。
The hydrocarbon dispersion medium may contain at least one compound selected from the group consisting of chain aliphatic hydrocarbons having 6 to 8 carbon atoms and alicyclic hydrocarbons having 6 to 8 carbon atoms. Hydrocarbon dispersion media include chain aliphatic hydrocarbons such as n-hexane, n-heptane, 2-methylhexane, 3-methylhexane, 2,3-dimethylpentane, 3-ethylpentane, and n-octane; cyclohexane. , Methylcyclohexane, cyclopentane, methylcyclopentane, trans-1,2-dimethylcyclopentane, cis-1,3-dimethylcyclopentane, trans-1,3-dimethylcyclopentane and other alicyclic hydrocarbons; benzene, Examples include aromatic hydrocarbons such as toluene and xylene. The hydrocarbon dispersion medium may be used alone or in combination of two or more.
工業的に入手が容易であり、かつ、品質が安定している観点から、炭化水素分散媒は、n-ヘプタン及びシクロヘキサンからなる群より選ばれる少なくとも一種を含んでいてもよい。また、同様の観点から、上述の炭化水素分散媒の混合物としては、例えば、市販されているエクソールヘプタン(エクソンモービル社製:n-ヘプタン及び異性体の炭化水素75~85%含有)を用いてもよい。
From the viewpoint of industrial availability and stable quality, the hydrocarbon dispersion medium may contain at least one selected from the group consisting of n-heptane and cyclohexane. From the same viewpoint, as the mixture of the above-mentioned hydrocarbon dispersion medium, for example, commercially available ExxonHeptane (manufactured by ExxonMobil: containing 75 to 85% of n-heptane and isomeric hydrocarbons) is used. You may.
炭化水素分散媒の量は、重合熱を適度に除去し、重合温度を制御しやすい観点から、単量体水溶液100質量部に対して、30~1000質量部、40~500質量部、又は50~300質量部であってもよい。炭化水素分散媒の量が30質量部以上であることにより、重合温度の制御が容易である傾向がある。炭化水素分散媒の量が1000質量部以下であることにより、重合の生産性が向上する傾向があり、経済的である。
The amount of the hydrocarbon dispersion medium is 30 to 1000 parts by mass, 40 to 500 parts by mass, or 50 parts by mass with respect to 100 parts by mass of the monomer aqueous solution from the viewpoint of appropriately removing the heat of polymerization and easily controlling the polymerization temperature. It may be up to 300 parts by mass. When the amount of the hydrocarbon dispersion medium is 30 parts by mass or more, the polymerization temperature tends to be easily controlled. When the amount of the hydrocarbon dispersion medium is 1000 parts by mass or less, the productivity of polymerization tends to be improved, which is economical.
ラジカル重合開始剤は水溶性であってもよい。水溶性ラジカル重合開始剤の例としては、過硫酸カリウム、過硫酸アンモニウム、過硫酸ナトリウム等の過硫酸塩;メチルエチルケトンパーオキシド、メチルイソブチルケトンパーオキシド、ジ-t-ブチルパーオキシド、t-ブチルクミルパーオキシド、t-ブチルパーオキシアセテート、t-ブチルパーオキシイソブチレート、t-ブチルパーオキシピバレート、過酸化水素等の過酸化物;2,2’-アゾビス(2-アミジノプロパン)2塩酸塩、2,2’-アゾビス[2-(N-フェニルアミジノ)プロパン]2塩酸塩、2,2’-アゾビス[2-(N-アリルアミジノ)プロパン]2塩酸塩、2,2'-アゾビス[2-(2-イミダゾリン-2-イル)プロパン]2塩酸塩、2,2’-アゾビス{2-[1-(2-ヒドロキシエチル)-2-イミダゾリン-2-イル]プロパン}2塩酸塩、2,2’-アゾビス{2-メチル-N-[1,1-ビス(ヒドロキシメチル)-2-ヒドロキシエチル]プロピオンアミド}、2,2’-アゾビス[2-メチル-N-(2-ヒドロキシエチル)-プロピオンアミド]、4,4’-アゾビス(4-シアノ吉草酸)等のアゾ化合物が挙げられる。ラジカル重合開始剤は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。ラジカル重合開始剤は、過硫酸カリウム、過硫酸アンモニウム、過硫酸ナトリウム、2,2’-アゾビス(2-アミジノプロパン)二塩酸塩、2,2'-アゾビス[2-(2-イミダゾリン-2-イル)プロパン]2塩酸塩、及び、2,2’-アゾビス{2-[1-(2-ヒドロキシエチル)-2-イミダゾリン-2-イル]プロパン}2塩酸塩からなる群より選ばれる少なくとも一種であってもよい。
The radical polymerization initiator may be water-soluble. Examples of water-soluble radical polymerization initiators include persulfates such as potassium persulfate, ammonium persulfate, and sodium persulfate; methyl ethyl ketone peroxide, methyl isobutyl ketone peroxide, di-t-butyl peroxide, and t-butyl cumylper. Peroxides such as oxides, t-butylperoxyacetate, t-butylperoxyisobutyrate, t-butylperoxypivalate, hydrogen peroxide; 2,2'-azobis (2-amidinopropane) dihydrochloride , 2,2'-azobis [2- (N-phenylamidino) propane] dihydrochloride, 2,2'-azobis [2- (N-allylamidino) propane] dihydrochloride, 2,2'-azobis [ 2- (2-imidazolin-2-yl) propane] 2 hydrochloride, 2,2'-azobis {2- [1- (2-hydroxyethyl) -2-imidazolin-2-yl] propane} 2 hydrochloride, 2,2'-azobis {2-methyl-N- [1,1-bis (hydroxymethyl) -2-hydroxyethyl] propionamide}, 2,2'-azobis [2-methyl-N- (2-hydroxy) Ethyl) -propionamide], azo compounds such as 4,4'-azobis (4-cyanovaleric acid) can be mentioned. The radical polymerization initiator may be used alone or in combination of two or more. Radical polymerization initiators are potassium persulfate, ammonium persulfate, sodium persulfate, 2,2'-azobis (2-amidinopropane) dihydrochloride, 2,2'-azobis [2- (2-imidazolin-2-yl). ) Propane] 2 hydrochloride and 2,2'-azobis {2- [1- (2-hydroxyethyl) -2-imidazolin-2-yl] propane} 2 hydrochloride, at least one selected from the group. There may be.
ラジカル重合開始剤の量は、エチレン性不飽和単量体1モルに対して0.00005~0.01モルであってよい。ラジカル重合開始剤の使用量が0.00005モル以上であると、重合反応に長時間を要さず、効率的である。ラジカル重合開始剤の量が0.01モル以下であると、急激な重合反応が起こることを抑制しやすい。
The amount of the radical polymerization initiator may be 0.00005 to 0.01 mol per 1 mol of the ethylenically unsaturated monomer. When the amount of the radical polymerization initiator used is 0.00005 mol or more, the polymerization reaction does not require a long time and is efficient. When the amount of the radical polymerization initiator is 0.01 mol or less, it is easy to suppress the occurrence of a rapid polymerization reaction.
例示されたラジカル重合開始剤は、亜硫酸ナトリウム、亜硫酸水素ナトリウム、硫酸第一鉄、L-アスコルビン酸等の還元剤と併用して、レドックス重合開始剤として用いることもできる。
The exemplified radical polymerization initiator can also be used as a redox polymerization initiator in combination with a reducing agent such as sodium sulfite, sodium hydrogen sulfite, ferrous sulfate, and L-ascorbic acid.
重合反応の際、単量体水溶液は、連鎖移動剤を含んでいてもよい。連鎖移動剤としては、次亜リン酸塩類、チオール類、チオール酸類、第2級アルコール類、アミン類等が挙げられる。
At the time of the polymerization reaction, the aqueous monomer solution may contain a chain transfer agent. Examples of the chain transfer agent include hypophosphates, thiols, thiolic acids, secondary alcohols, amines and the like.
吸水性樹脂粒子の粒子径を制御するために、重合に用いる単量体水溶液は、増粘剤を含んでいてもよい。増粘剤としては、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース、メチルセルロース、カルボキシメチルセルロース、ポリアクリル酸、ポリエチレングリコール、ポリアクリルアミド、ポリエチレンイミン、デキストリン、アルギン酸ナトリウム、ポリビニルアルコール、ポリビニルピロリドン、ポリエチレンオキサイド等が挙げられる。重合時の攪拌速度が同じであれば、単量体水溶液の粘度が高いほど、得られる粒子の中位粒子径は大きくなる傾向にある。
The monomer aqueous solution used for polymerization may contain a thickener in order to control the particle size of the water-absorbent resin particles. Examples of the thickener include hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, carboxymethyl cellulose, polyacrylic acid, polyethylene glycol, polyacrylamide, polyethyleneimine, dextrin, sodium alginate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide and the like. If the stirring speed at the time of polymerization is the same, the higher the viscosity of the aqueous monomer solution, the larger the medium particle size of the obtained particles tends to be.
重合の際に自己架橋による架橋が生じうるが、更に内部架橋剤を用いることで架橋を施してもよい。内部架橋剤を用いると、吸水性樹脂粒子の吸水特性を制御しやすい。内部架橋剤は、通常、重合反応の際に反応液に添加される。内部架橋剤としては、例えば、エチレングリコール、プロピレングリコール、トリメチロールプロパン、グリセリン、ポリオキシエチレングリコール、ポリオキシプロピレングリコール、ポリグリセリン等のポリオール類のジ又はトリ(メタ)アクリル酸エステル類;上述のポリオール類と不飽和酸(マレイン酸、フマール酸等)とを反応させて得られる不飽和ポリエステル類;N,N’-メチレンビス(メタ)アクリルアミド等のビス(メタ)アクリルアミド類;ポリエポキシドと(メタ)アクリル酸とを反応させて得られるジ又はトリ(メタ)アクリル酸エステル類;ポリイソシアネート(トリレンジイソシアネート、ヘキサメチレンジイソシアネート等)と(メタ)アクリル酸ヒドロキシエチルとを反応させて得られるジ(メタ)アクリル酸カルバミルエステル類;アリル化澱粉、アリル化セルロース、ジアリルフタレート、N,N’,N”-トリアリルイソシアヌレート、ジビニルベンゼン等の,重合性不飽和基を2個以上有する化合物;(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)プロピレングリコールジグリシジルエーテル、(ポリ)グリセリンジグリシジルエーテル、(ポリ)グリセリントリグリシジルエーテル、(ポリ)プロピレングリコールポリグリシジルエーテル、ポリグリセロールポリグリシジルエーテル等のポリグリシジル化合物;エピクロロヒドリン、エピブロムヒドリン、α-メチルエピクロロヒドリン等のハロエポキシ化合物;イソシアネート化合物(2,4-トリレンジイソシアネート、ヘキサメチレンジイソシアネート等)などの、反応性官能基を2個以上有する化合物が挙げられる。内部架橋剤は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。内部架橋剤としては、ポリグリシジル化合物であってもよく、ジグリシジルエーテル化合物であってもよい。内部架橋剤が、(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)プロピレングリコールジグリシジルエーテル、及び、(ポリ)グリセリンジグリシジルエーテルからなる群より選ばれる少なくとも一種を含んでもよい。
Cross-linking by self-cross-linking may occur during polymerization, but cross-linking may be further performed by using an internal cross-linking agent. When an internal cross-linking agent is used, it is easy to control the water absorption characteristics of the water-absorbent resin particles. The internal cross-linking agent is usually added to the reaction solution during the polymerization reaction. Examples of the internal cross-linking agent include di or tri (meth) acrylic acid esters of polyols such as ethylene glycol, propylene glycol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; Unsaturated polyesters obtained by reacting polyols with unsaturated acids (maleic acid, fumaric acid, etc.); bis (meth) acrylamides such as N, N'-methylenebis (meth) acrylamide; polyepoxides and (meth) Di or tri (meth) acrylic acid esters obtained by reacting with acrylic acid; di (meth) obtained by reacting polyisocyanate (tolylene diisocyanate, hexamethylene diisocyanate, etc.) with hydroxyethyl (meth) acrylate. ) Acrylic acid carbamil esters; compounds having two or more polymerizable unsaturated groups such as allylated starch, allylated cellulose, diallyl phthalate, N, N', N "-triallyl isocyanurate, divinylbenzene; Poly such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, polyglycerol polyglycidyl ether, etc. Glyceridyl compound; haloepoxy compound such as epichlorohydrin, epibromhydrin, α-methylepichlorohydrin; 2 reactive functional groups such as isocyanate compound (2,4-tolylene diisocyanate, hexamethylene diisocyanate, etc.) Examples thereof include compounds having more than one. The internal cross-linking agent may be used alone or in combination of two or more. The internal cross-linking agent may be a polyglycidyl compound or diglycidyl. It may be an ether compound. The internal cross-linking agent comprises at least one selected from the group consisting of (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, and (poly) glycerin diglycidyl ether. It may be.
内部架橋剤の量は、上述の単量体水溶液の重合により得られる重合体が適度に架橋されることにより水溶性の性質が抑制され、充分な吸水量が得られやすい観点から、エチレン性不飽和単量体1モル当たり、0ミリモル以上、0.01ミリモル以上、0.015ミリモル以上、又は0.020ミリモル以上であってもよく、0.1モル以下であってもよい。
The amount of the internal cross-linking agent is not ethylenically from the viewpoint that the water-soluble property is suppressed by appropriately cross-linking the polymer obtained by the polymerization of the above-mentioned monomer aqueous solution, and a sufficient water absorption amount can be easily obtained. It may be 0 mmol or more, 0.01 mmol or more, 0.015 mmol or more, 0.020 mmol or more, or 0.1 mol or less, per 1 mol of saturated monomer.
エチレン性不飽和単量体、ラジカル重合開始剤、必要に応じて内部架橋剤等を含む水相と、炭化水素系分散剤と必要に応じて界面活性剤、高分子系分散剤等を含む油相を混合した状態において攪拌下で加熱し、油中水系において逆相懸濁重合を行うことができる。
An aqueous phase containing an ethylenically unsaturated monomer, a radical polymerization initiator, an internal cross-linking agent, etc., if necessary, and an oil containing a hydrocarbon-based dispersant and, if necessary, a surfactant, a polymer-based dispersant, etc. Reversed phase suspension polymerization can be carried out in an aqueous system in oil by heating with stirring in a state where the phases are mixed.
逆相懸濁重合を行う際には、界面活性剤(必要に応じて更に、高分子系分散剤)の存在下で、エチレン性不飽和単量体を含む単量体水溶液を炭化水素分散媒に分散させる。このとき、重合反応を開始する前であれば、界面活性剤、高分子系分散剤等の添加時期は、単量体水溶液の添加の前後どちらであってもよい。
When performing reverse phase suspension polymerization, a monomer aqueous solution containing an ethylenically unsaturated monomer is used as a hydrocarbon dispersion medium in the presence of a surfactant (and, if necessary, a polymer-based dispersant). Disperse in. At this time, the timing of adding the surfactant, the polymer-based dispersant, or the like may be either before or after the addition of the aqueous monomer solution, as long as it is before the start of the polymerization reaction.
得られる吸水性樹脂に残存する炭化水素分散媒の量を低減しやすい観点から、高分子系分散剤を分散させた炭化水素分散媒に単量体水溶液を分散させた後に界面活性剤を添加して更に分散させてから重合を行ってもよい。
From the viewpoint of easily reducing the amount of the hydrocarbon dispersion medium remaining in the obtained water-absorbent resin, a surfactant is added after dispersing the monomer aqueous solution in the hydrocarbon dispersion medium in which the polymer-based dispersant is dispersed. The polymer may be further dispersed and then polymerized.
逆相懸濁重合は、1段、又は、2段以上の多段で行うことができる。逆相懸濁重合は、生産性を高める観点から、2段又は3段で行ってもよい。
Reverse phase suspension polymerization can be carried out in one stage or in multiple stages of two or more stages. Reversed phase suspension polymerization may be carried out in two or three stages from the viewpoint of increasing productivity.
2段以上の多段で逆相懸濁重合を行う場合、1段目の逆相懸濁重合を行った後、1段目の重合反応で得られた反応混合物にエチレン性不飽和単量体を添加して混合し、1段目と同様の方法で2段目以降の逆相懸濁重合を行えばよい。2段目以降の各段における逆相懸濁重合では、エチレン性不飽和単量体の他に、上述のラジカル重合開始剤を、2段目以降の各段における逆相懸濁重合の際に添加するエチレン性不飽和単量体の量を基準として、上述のエチレン性不飽和単量体に対する各成分のモル比の範囲内で添加して逆相懸濁重合を行ってもよい。2段目以降の各段における逆相懸濁重合では、必要に応じて内部架橋剤を用いてもよい。内部架橋剤を用いる場合は、各段に供するエチレン性不飽和単量体の量を基準として、上述のエチレン性不飽和単量体に対する各成分のモル比の範囲内で添加して逆相懸濁重合を行ってもよい。
When reverse phase suspension polymerization is carried out in two or more stages, an ethylenically unsaturated monomer is added to the reaction mixture obtained in the first step polymerization reaction after the first step reverse phase suspension polymerization is carried out. It may be added and mixed, and the reverse phase suspension polymerization of the second and subsequent steps may be carried out in the same manner as in the first step. In the reverse phase suspension polymerization in each stage of the second and subsequent stages, in addition to the ethylenically unsaturated monomer, the above-mentioned radical polymerization initiator is used in the reverse phase suspension polymerization in each stage of the second and subsequent stages. Based on the amount of the ethylenically unsaturated monomer to be added, it may be added within the range of the molar ratio of each component to the above-mentioned ethylenically unsaturated monomer to carry out reverse phase suspension polymerization. In the reverse phase suspension polymerization in each stage after the second stage, an internal cross-linking agent may be used if necessary. When an internal cross-linking agent is used, it is added within the range of the molar ratio of each component to the above-mentioned ethylenically unsaturated monomer based on the amount of the ethylenically unsaturated monomer provided in each stage, and the suspension is reversed. Muddy polymerization may be carried out.
重合反応の温度は、使用するラジカル重合開始剤によって異なるが、重合を迅速に進行させ、重合時間を短くすることにより、経済性を高めると共に、容易に重合熱を除去して円滑に反応を行う観点から、20~150℃、又は40~120℃であってもよい。反応時間は、通常、0.5~4時間である。重合反応の終了は、例えば、反応系内の温度上昇の停止により確認することができる。これにより、エチレン性不飽和単量体の重合体は、通常、含水ゲル状重合体の状態で得られる。
The temperature of the polymerization reaction varies depending on the radical polymerization initiator used, but by rapidly advancing the polymerization and shortening the polymerization time, the efficiency is improved and the heat of polymerization is easily removed to carry out the reaction smoothly. From the viewpoint, it may be 20 to 150 ° C. or 40 to 120 ° C. The reaction time is usually 0.5-4 hours. The completion of the polymerization reaction can be confirmed, for example, by stopping the temperature rise in the reaction system. As a result, the polymer of the ethylenically unsaturated monomer is usually obtained in the state of a hydrogel-like polymer.
重合後、得られた含水ゲル状重合体に架橋剤を添加して加熱することで、重合後架橋を施してもよい。重合後架橋を行なうことで含水ゲル状重合体の架橋度を高め、それにより吸水性樹脂粒子の吸水特性を更に向上させることができる。
After polymerization, cross-linking may be performed after polymerization by adding a cross-linking agent to the obtained hydrogel polymer and heating it. By performing cross-linking after the polymerization, the degree of cross-linking of the hydrogel polymer can be increased, whereby the water-absorbing characteristics of the water-absorbent resin particles can be further improved.
重合後架橋を行うための架橋剤としては、例えば、エチレングリコール、プロピレングリコール、1,4-ブタンジオール、トリメチロールプロパン、グリセリン、ポリオキシエチレングリコール、ポリオキシプロピレングリコール、ポリグリセリン等のポリオール;(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)プロピレングリコールジグリシジルエーテル、及び(ポリ)グリセリンジグリシジルエーテル等の2個以上のエポキシ基を有する化合物;エピクロルヒドリン、エピブロムヒドリン、及びα-メチルエピクロルヒドリン等のハロエポキシ化合物;2,4-トリレンジイソシアネート、及びヘキサメチレンジイソシアネート等の2個以上のイソシアネート基を有する化合物;1,2-エチレンビスオキサゾリン等のオキサゾリン化合物;エチレンカーボネート等のカーボネート化合物;ビス[N,N-ジ(β-ヒドロキシエチル)]アジプアミド等のヒドロキシアルキルアミド化合物等が挙げられる。重合後架橋のための架橋剤が、(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)グリセリンジグリシジルエーテル、(ポリ)グリセリントリグリシジルエーテル、(ポリ)プロピレングリコールポリグリシジルエーテル、及びポリグリセロールポリグリシジルエーテル等のポリグリシジル化合物であってもよい。これらの架橋剤は、単独で用いられてもよいし、2種以上を組み合わせて用いられてもよい。
Examples of the cross-linking agent for performing post-polymerization cross-linking include polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; Compounds having two or more epoxy groups such as (poly) ethylene glycol diglycidyl ether, (poly) propylene glycol diglycidyl ether, and (poly) glycerin diglycidyl ether; epichlorohydrin, epibromhydrin, α-methylepicrolhydrin and the like. Haloepoxy compounds; compounds having two or more isocyanate groups such as 2,4-tolylene diisocyanate and hexamethylene diisocyanate; oxazoline compounds such as 1,2-ethylene bisoxazoline; carbonate compounds such as ethylene carbonate; bis [N , N-di (β-hydroxyethyl)] hydroxyalkylamide compounds such as adipamide can be mentioned. Cross-linking agents for post-polymerization cross-linking are (poly) ethylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, and polyglycerol polyglycidyl ether. It may be a polyglycidyl compound such as. These cross-linking agents may be used alone or in combination of two or more.
重合後架橋に用いられる架橋剤の量は、得られる含水ゲル状重合体が適度に架橋されることにより好適な吸水特性を示すようにする観点から、水溶性エチレン性不飽和単量体1モル当たり、0~0.03モル、0~0.01モル、又は0.00001~0.005モルであってもよい。
The amount of the cross-linking agent used for post-polymerization cross-linking is 1 mol of the water-soluble ethylenically unsaturated monomer from the viewpoint of appropriately cross-linking the obtained hydrogel-like polymer to exhibit suitable water absorption characteristics. It may be 0 to 0.03 mol, 0 to 0.01 mol, or 0.00001 to 0.005 mol.
重合後架橋のための架橋剤は、エチレン性不飽和単量体の重合反応後に反応液に添加される。多段重合の場合、多段重合後に重合後架橋のための架橋剤を添加してもよい。重合時および重合後の発熱、工程遅延による滞留、架橋剤添加時の系の開放、及び架橋剤添加に伴う水の添加等による水分の変動を考慮して、重合後架橋のための架橋剤は、含水率(後述)の観点から、[重合直後の含水率±3質量%]の領域で添加してもよい。
The cross-linking agent for post-polymerization cross-linking is added to the reaction solution after the polymerization reaction of the ethylenically unsaturated monomer. In the case of multi-stage polymerization, a cross-linking agent for post-polymerization cross-linking may be added after the multi-stage polymerization. Considering the fluctuation of water content due to heat generation during and after polymerization, retention due to process delay, opening of the system when adding a cross-linking agent, and addition of water due to addition of a cross-linking agent, the cross-linking agent for post-polymerization cross-linking is , From the viewpoint of water content (described later), it may be added in the region of [water content immediately after polymerization ± 3% by mass].
引き続き、得られた含水ゲル状重合体から水分が除去される。水分の除去する乾燥により、エチレン性不飽和単量体の重合体を含む重合体粒子が得られる。乾燥方法としては、例えば、(a)含水ゲル状重合体が炭化水素分散媒に分散した状態で共沸蒸留により水分を除去する方法、(b)デカンテーションにより含水ゲル状重合体を取り出し、減圧乾燥する方法、(c)フィルターにより含水ゲル状重合体をろ別し、減圧乾燥する方法等が挙げられる。
Subsequently, water is removed from the obtained hydrogel-like polymer. Drying to remove water gives polymer particles containing a polymer of ethylenically unsaturated monomers. Examples of the drying method include (a) a method of removing water by azeotropic distillation in a state where the hydrogel polymer is dispersed in a hydrocarbon dispersion medium, and (b) a method of taking out the hydrogel polymer by decantation and reducing the pressure. Examples thereof include a method of drying, and (c) a method of filtering the hydrogel polymer by a filter and drying under reduced pressure.
重合反応時の攪拌機の回転数を調整することによって、あるいは、重合反応後又は乾燥の初期において凝集剤を系内に添加することによって吸水性樹脂粒子の粒子径を調整することができる。凝集剤を添加することにより、得られる吸水性樹脂粒子の粒子径を大きくすることができる。凝集剤としては、無機凝集剤を用いることができる。無機凝集剤(例えば粉末状無機凝集剤)としては、シリカ、ゼオライト、ベントナイト、酸化アルミニウム、タルク、二酸化チタン、カオリン、クレイ、ハイドロタルサイト等が挙げられる。凝集効果に優れる観点から、凝集剤が、シリカ、酸化アルミニウム、タルク及びカオリンからなる群より選ばれる少なくとも一種であってもよい。
The particle size of the water-absorbent resin particles can be adjusted by adjusting the rotation speed of the stirrer during the polymerization reaction, or by adding a flocculant into the system after the polymerization reaction or in the early stage of drying. By adding a flocculant, the particle size of the obtained water-absorbent resin particles can be increased. As the flocculant, an inorganic flocculant can be used. Examples of the inorganic flocculant (for example, powdered inorganic flocculant) include silica, zeolite, bentonite, aluminum oxide, talc, titanium dioxide, kaolin, clay, hydrotalcite and the like. From the viewpoint of excellent aggregating effect, the aggregating agent may be at least one selected from the group consisting of silica, aluminum oxide, talc and kaolin.
逆相懸濁重合において、重合で用いられるものと同種の炭化水素分散媒又は水に凝集剤を予め分散させてから、これを、攪拌下で、含水ゲル状重合体を含む炭化水素分散媒中に混合してもよい。
In reverse phase suspension polymerization, a coagulant is previously dispersed in a hydrocarbon dispersion medium of the same type as that used in the polymerization or water, and then this is placed in a hydrocarbon dispersion medium containing a hydrogel polymer under stirring. May be mixed with.
凝集剤の量は、重合に使用するエチレン性不飽和単量体100質量部に対して、0.001~1質量部、0.005~0.5質量部、又は0.01~0.2質量部であってもよい。凝集剤の量がこれら範囲内であることによって、目的とする粒度分布を有する吸水性樹脂粒子が得られやすい。
The amount of the flocculant is 0.001 to 1 part by mass, 0.005 to 0.5 part by mass, or 0.01 to 0.2 with respect to 100 parts by mass of the ethylenically unsaturated monomer used for the polymerization. It may be a mass part. When the amount of the flocculant is within these ranges, it is easy to obtain water-absorbent resin particles having a desired particle size distribution.
重合反応は、攪拌翼を有する各種攪拌機を用いて行うことができる。攪拌翼としては、平板翼、格子翼、パドル翼、プロペラ翼、アンカー翼、タービン翼、ファウドラー翼、リボン翼、フルゾーン翼、マックスブレンド翼等を用いることができる。平板翼は、軸(撹拌軸)と、軸の周囲に配置された平板部(撹拌部)とを有している。さらに、平板部は、スリット等を有していてもよい。
The polymerization reaction can be carried out using various stirrers having stirring blades. As the stirring blade, a flat plate blade, a lattice blade, a paddle blade, a propeller blade, an anchor blade, a turbine blade, a Faudler blade, a ribbon blade, a full zone blade, a max blend blade and the like can be used. The flat plate blade has a shaft (stirring shaft) and a flat plate portion (stirring portion) arranged around the shaft. Further, the flat plate portion may have a slit or the like.
吸水性樹脂粒子61aの製造においては、乾燥工程又はそれ以降のいずれかの工程において、架橋剤を用いて含水ゲル状重合体の表面部分の架橋(表面架橋)が行われてもよい。表面架橋を行うことで、吸水性樹脂粒子の吸水特性を制御しやすい。表面架橋される含水ゲル状重合体の含水率が、5~50質量%、10~40質量%、又は15~35質量%であってもよい。含水ゲル状重合体の含水率(質量%)は、次の式で算出される。
含水率=[Ww/(Ww+Ws)]×100
Ww:全重合工程の重合前の単量体水溶液に含まれる水分量から、乾燥工程により系外部に排出された水分量を差し引いた量に、凝集剤、表面架橋剤等を混合する際に必要に応じて用いられる水分量を加えることで算出される含水ゲル状重合体の水分量。 In the production of the water-absorbent resin particles 61a, cross-linking (surface cross-linking) of the surface portion of the hydrogel polymer may be carried out using a cross-linking agent in any of the drying step and subsequent steps. By performing surface cross-linking, it is easy to control the water absorption characteristics of the water-absorbent resin particles. The water content of the surface-crosslinked hydrogel polymer may be 5 to 50% by mass, 10 to 40% by mass, or 15 to 35% by mass. The water content (mass%) of the water-containing gel polymer is calculated by the following formula.
Moisture content = [Ww / (Ww + Ws)] x 100
Ww: Necessary when mixing a flocculant, a surface cross-linking agent, etc. to the amount obtained by subtracting the amount of water discharged to the outside of the system by the drying step from the amount of water contained in the monomer aqueous solution before polymerization in the entire polymerization step. The amount of water in the hydrogel polymer calculated by adding the amount of water used according to.
含水率=[Ww/(Ww+Ws)]×100
Ww:全重合工程の重合前の単量体水溶液に含まれる水分量から、乾燥工程により系外部に排出された水分量を差し引いた量に、凝集剤、表面架橋剤等を混合する際に必要に応じて用いられる水分量を加えることで算出される含水ゲル状重合体の水分量。 In the production of the water-
Moisture content = [Ww / (Ww + Ws)] x 100
Ww: Necessary when mixing a flocculant, a surface cross-linking agent, etc. to the amount obtained by subtracting the amount of water discharged to the outside of the system by the drying step from the amount of water contained in the monomer aqueous solution before polymerization in the entire polymerization step. The amount of water in the hydrogel polymer calculated by adding the amount of water used according to.
Ws:含水ゲル状重合体を構成するエチレン性不飽和単量体、架橋剤、開始剤等の材料の仕込量から算出される固形分量。
Ws: The amount of solid content calculated from the amount of materials such as ethylenically unsaturated monomers, cross-linking agents, and initiators that make up the hydrogel polymer.
表面架橋を行うための架橋剤(表面架橋剤)としては、例えば、反応性官能基を2個以上有する化合物を挙げることができる。表面架橋剤の例としては、例えば、エチレングリコール、プロピレングリコール、1,4-ブタンジオール、トリメチロールプロパン、グリセリン、ポリオキシエチレングリコール、ポリオキシプロピレングリコール、ポリグリセリン等のポリオール類;(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)グリセリンジグリシジルエーテル、(ポリ)グリセリントリグリシジルエーテル、トリメチロールプロパントリグリシジルエーテル(ポリ)プロピレングリコールポリグリシジルエーテル、(ポリ)グリセロールポリグリシジルエーテル等のポリグリシジル化合物;エピクロロヒドリン、エピブロムヒドリン、α-メチルエピクロロヒドリン等のハロエポキシ化合物;2,4-トリレンジイソシアネート、ヘキサメチレンジイソシアネート等のイソシアネート化合物;3-メチル-3-オキセタンメタノール、3-エチル-3-オキセタンメタノール、3-ブチル-3-オキセタンメタノール、3-メチル-3-オキセタンエタノール、3-エチル-3-オキセタンエタノール、3-ブチル-3-オキセタンエタノール等のオキセタン化合物;1,2-エチレンビスオキサゾリン等のオキサゾリン化合物;エチレンカーボネート等のカーボネート化合物;ビス[N,N-ジ(β-ヒドロキシエチル)]アジプアミド等のヒドロキシアルキルアミド化合物などが挙げられる。表面架橋剤は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。表面架橋剤は、ポリグリシジル化合物であってよく、(ポリ)エチレングリコールジグリシジルエーテル、(ポリ)グリセリンジグリシジルエーテル、(ポリ)グリセリントリグリシジルエーテル、(ポリ)プロピレングリコールポリグリシジルエーテル、及び、ポリグリセロールポリグリシジルエーテルからなる群より選ばれる少なくとも1種であってよい。
Examples of the cross-linking agent (surface cross-linking agent) for performing surface cross-linking include compounds having two or more reactive functional groups. Examples of surface cross-linking agents include, for example, polyols such as ethylene glycol, propylene glycol, 1,4-butanediol, trimethylolpropane, glycerin, polyoxyethylene glycol, polyoxypropylene glycol, and polyglycerin; (poly) ethylene. Polyglycidyl compounds such as glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, trimethylpropan triglycidyl ether (poly) propylene glycol polyglycidyl ether, (poly) glycerol polyglycidyl ether; Haloepoxy compounds such as chlorohydrin, epibromhydrin, α-methylepichlorohydrin; isocyanate compounds such as 2,4-tolylene diisocyanate, hexamethylene diisocyanate; 3-methyl-3-oxetane methanol, 3-ethyl- Oxetane compounds such as 3-oxetane methanol, 3-butyl-3-oxetane methanol, 3-methyl-3-oxetaneethanol, 3-ethyl-3-oxetaneethanol, 3-butyl-3-oxetaneethanol; 1,2-ethylene Examples thereof include oxazoline compounds such as bisoxazoline; carbonate compounds such as ethylene carbonate; and hydroxyalkylamide compounds such as bis [N, N-di (β-hydroxyethyl)] adipamide. The surface cross-linking agent may be used alone or in combination of two or more. The surface cross-linking agent may be a polyglycidyl compound, and may be (poly) ethylene glycol diglycidyl ether, (poly) glycerin diglycidyl ether, (poly) glycerin triglycidyl ether, (poly) propylene glycol polyglycidyl ether, and poly. It may be at least one selected from the group consisting of glycerol polyglycidyl ether.
表面架橋剤の使用量は、好適な吸水特性が得られやすい観点から、重合に使用するエチレン性不飽和単量体1モルに対して、0.01~20ミリモル、0.05~10ミリモル、0.1~5ミリモル、0.15~3ミリモル、又は0.2~1ミリモルであってよい。
The amount of the surface cross-linking agent used is 0.01 to 20 mmol, 0.05 to 10 mmol, based on 1 mol of the ethylenically unsaturated monomer used for the polymerization, from the viewpoint that suitable water absorption characteristics can be easily obtained. It may be 0.1-5 mmol, 0.15-3 mmol, or 0.2-1 mmol.
吸水性樹脂粒子61aの製造においては、乾燥工程(水分除去工程)又はそれ以降のいずれかの工程において、表面改質剤を用いて含水ゲル状重合体の表面部分を処理(表面改質)してもよい。表面改質は、例えば、表面架橋工程の前、途中又は後に行われてよい。表面改質は、なかでも表面架橋後に行われてよい。
In the production of the water-absorbent resin particles 61a, the surface portion of the hydrogel polymer is treated (surface modification) with a surface modifier in either the drying step (moisture removal step) or a subsequent step. You may. The surface modification may be carried out, for example, before, during or after the surface cross-linking step. Surface modification may be carried out after surface cross-linking.
表面改質剤は、例えば、ノニオン界面活性剤、陰イオン界面活性剤、陽イオン界面活性剤、両性界面活性剤等の界面活性剤であってよい。例えば、表面改質剤として用いられるノニオン界面活性剤のHLB値は、例えば、3~12、又は6~10であってよい。ノニオン界面活性剤としては、例えば、ソルビタンモノラウレート等のソルビタン脂肪酸エステルが挙げられる。HLB値は、グリフィン法により測定される。
The surface modifier may be, for example, a surfactant such as a nonionic surfactant, an anionic surfactant, a cationic surfactant, or an amphoteric surfactant. For example, the HLB value of the nonionic surfactant used as the surface modifier may be, for example, 3 to 12, or 6 to 10. Examples of the nonionic surfactant include sorbitan fatty acid esters such as sorbitan monolaurate. The HLB value is measured by the Griffin method.
表面改質剤の量は、重合に使用するエチレン性不飽和単量体100質量部に対して、0.01~0.50質量部、0.02~0.40質量部、又は0.04~0.30質量部であってもよい。
The amount of the surface modifier is 0.01 to 0.50 parts by mass, 0.02 to 0.40 parts by mass, or 0.04 with respect to 100 parts by mass of the ethylenically unsaturated monomer used for the polymerization. It may be ~ 0.30 parts by mass.
必要に応じて、表面架橋及び/又は表面改質が行われた後、含水ゲル状重合体から水及び炭化水素分散媒を留去すること等により、乾燥品である重合体粒子を得ることができる。
If necessary, after surface cross-linking and / or surface modification, water and a hydrocarbon dispersion medium can be distilled off from the hydrogel polymer to obtain polymer particles which are dry products. it can.
吸水性樹脂粒子61aは、重合体粒子のみから構成されていてもよいが、例えば、ゲル安定剤、金属キレート剤、及び流動性向上剤(滑剤)等から選ばれる各種の追加の成分を更に含むことができる。追加の成分は、重合体粒子の内部、重合体粒子の表面上、又はそれらの両方に配置され得る。追加の成分は、流動性向上剤(滑剤)であってもよい。流動性向上剤は無機粒子を含んでいてもよい。無機粒子としては、例えば、非晶質シリカ等のシリカ粒子が挙げられる。
The water-absorbent resin particles 61a may be composed of only polymer particles, but further contain various additional components selected from, for example, a gel stabilizer, a metal chelating agent, a fluidity improver (lubricant), and the like. be able to. Additional components may be placed inside the polymer particles, on the surface of the polymer particles, or both. The additional component may be a fluidity improver (lubricant). The fluidity improver may contain inorganic particles. Examples of the inorganic particles include silica particles such as amorphous silica.
吸水性樹脂粒子61aは、重合体粒子の表面上に配置された複数の無機粒子を含んでいてもよい。例えば、重合体粒子と無機粒子とを混合することにより、重合体粒子の表面上に無機粒子を配置することができる。この無機粒子は、非晶質シリカ等のシリカ粒子であってもよい。吸水性樹脂粒子61aが重合体粒子の表面上に配置された無機粒子を含む場合、重合体粒子の質量に対する無機粒子の量の割合は、0.2質量%以上、0.5質量%以上、1.0質量%以上、又は1.5質量%以上であってもよく、5.0質量%以下、又は3.5質量%以下であってもよい。ここでの無機粒子は、通常、重合体粒子の大きさと比較して微小な大きさを有する。例えば、無機粒子の平均粒子径が、0.1~50μm、0.5~30μm、又は1~20μmであってもよい。ここでの平均粒子径は、動的光散乱法、又はレーザー回折・散乱法によって測定される値であることができる。
The water-absorbent resin particles 61a may contain a plurality of inorganic particles arranged on the surface of the polymer particles. For example, by mixing the polymer particles and the inorganic particles, the inorganic particles can be arranged on the surface of the polymer particles. The inorganic particles may be silica particles such as amorphous silica. When the water-absorbent resin particles 61a contain inorganic particles arranged on the surface of the polymer particles, the ratio of the amount of the inorganic particles to the mass of the polymer particles is 0.2% by mass or more, 0.5% by mass or more, It may be 1.0% by mass or more, 1.5% by mass or more, 5.0% by mass or less, or 3.5% by mass or less. The inorganic particles here usually have a minute size as compared with the size of the polymer particles. For example, the average particle size of the inorganic particles may be 0.1 to 50 μm, 0.5 to 30 μm, or 1 to 20 μm. The average particle size here can be a value measured by a dynamic light scattering method or a laser diffraction / scattering method.
図1は、一実施形態に係る短冊状の補助シートを示す断面図である。図1に示す補助シート60は、膨潤層61と、2枚のシート基材62a,62bとを有する。シート基材62a,62bは、膨潤層61の両側に配置されている。言い換えると、膨潤層61は、シート基材62a,62bの内側に配置されている。膨潤層61は、2枚のシート基材62a,62bの間に挟まれることにより、保形されている。シート基材62a,62bは、2枚のシートであってもよいし、折り返された1枚のシート、又は1枚の袋体であってもよい。
FIG. 1 is a cross-sectional view showing a strip-shaped auxiliary sheet according to an embodiment. The auxiliary sheet 60 shown in FIG. 1 has a swelling layer 61 and two sheet base materials 62a and 62b. The sheet base materials 62a and 62b are arranged on both sides of the swelling layer 61. In other words, the swelling layer 61 is arranged inside the sheet base materials 62a and 62b. The swelling layer 61 is held in shape by being sandwiched between the two sheet base materials 62a and 62b. The sheet base materials 62a and 62b may be two sheets, one folded sheet, or one bag.
補助シート60は、シート基材62aと膨潤層61との間に介在する接着剤63aを更に有していてもよく、シート基材62bと膨潤層61との間に介在する接着剤63bを更に有していてもよい。接着剤63a,63bとしては、例えば水性接着剤、溶剤型接着剤、弾性接着剤、エアゾール接着剤、ホットメルト接着剤等であってよい。
The auxiliary sheet 60 may further have an adhesive 63a interposed between the sheet base material 62a and the swelling layer 61, and further has an adhesive 63b interposed between the sheet base material 62b and the swelling layer 61. You may have. The adhesives 63a and 63b may be, for example, a water-based adhesive, a solvent-based adhesive, an elastic adhesive, an aerosol adhesive, a hot melt adhesive, or the like.
補助シート60の長手方向の長さは、乾燥状態で、例えば20cm以上、22cm以上、24cm以上、又は26cm以上であってよく、60cm以下、50cm以下、40cm以下、38cm以下、36cm以下、34cm以下、又は32cm以下であってよい。あるいは、補助シート60の長手方向の長さは、乾燥状態で、吸収性物品に同梱される吸水コアの長さに対し、その0.8~1.2倍の長さであってもよく、同じ長さであってもよい。
The length of the auxiliary sheet 60 in the longitudinal direction may be, for example, 20 cm or more, 22 cm or more, 24 cm or more, or 26 cm or more in a dry state, and is 60 cm or less, 50 cm or less, 40 cm or less, 38 cm or less, 36 cm or less, 34 cm or less. , Or 32 cm or less. Alternatively, the length of the auxiliary sheet 60 in the longitudinal direction may be 0.8 to 1.2 times the length of the water absorbing core included in the absorbent article in the dry state. , May be the same length.
補助シート60の短手方向の長さは、乾燥状態で、例えば0.5cm以上、1cm以上、1.5cm以上、又は2cm以上であってよく、6.5cm以下、5.5cm以下、4.5cm以下、3.5cm以下、3.0cm以下、又は2.5cm以下であってよい。
The length of the auxiliary sheet 60 in the lateral direction may be, for example, 0.5 cm or more, 1 cm or more, 1.5 cm or more, or 2 cm or more in a dry state, and may be 6.5 cm or less, 5.5 cm or less, 4. It may be 5 cm or less, 3.5 cm or less, 3.0 cm or less, or 2.5 cm or less.
また、補助シート60中の膨潤層61の存在領域の短手方向の長さは、乾燥状態で吸収性物品に同梱される吸水コアの幅Wに対し、1/2W未満であり、吸水コアの短手方向の両端部に配置しても、吸水コア全体を覆うことは無い。
Further, the length of the region where the swelling layer 61 exists in the auxiliary sheet 60 in the lateral direction is less than 1 / 2W with respect to the width W of the water absorption core included in the absorbent article in the dry state, and the water absorption core. Even if it is placed at both ends in the lateral direction, it does not cover the entire water absorption core.
補助シート60の厚さは、乾燥状態で、例えば3.0mm以下、2.5mm以下、2.0mm以下、又は1.8mm以下であってよく、0.1mm以上、0.3mm以上、又は0.5mm以上であってもよい。厚さは、例えば、尾崎製作所製ダイヤルシックネスゲージJ-B(測定子はφ50mmのアルミ製)を用いて測定することができる。
The thickness of the auxiliary sheet 60 may be, for example, 3.0 mm or less, 2.5 mm or less, 2.0 mm or less, or 1.8 mm or less in a dry state, and is 0.1 mm or more, 0.3 mm or more, or 0. It may be 5.5 mm or more. The thickness can be measured using, for example, a dial thickness gauge JB manufactured by Ozaki Seisakusho Co., Ltd. (the stylus is made of aluminum having a diameter of 50 mm).
補助シート60において、吸水性樹脂粒子の目付量(単位面積当たりの吸水性樹脂粒子の質量)は、10~100g/m2、15~60g/m2、又は18~45g/m2であってよい。
In the auxiliary sheet 60, the amount of water-absorbent resin particles (mass of water-absorbent resin particles per unit area) is 10 to 100 g / m 2 , 15 to 60 g / m 2 , or 18 to 45 g / m 2. Good.
膨潤層61は、上述の実施形態に係る吸水性樹脂粒子61aと、繊維状物を含む繊維層61bとを有する。膨潤層61は、繊維層61bを有していなくてもよい。膨潤層における吸水性樹脂粒子の含有量は、膨潤層61の質量を基準として、70~100質量%、80~100質量%、又は90~100質量%であってもよい。
The swelling layer 61 has the water-absorbent resin particles 61a according to the above-described embodiment and the fiber layer 61b containing a fibrous material. The swelling layer 61 does not have to have the fiber layer 61b. The content of the water-absorbent resin particles in the swelling layer may be 70 to 100% by mass, 80 to 100% by mass, or 90 to 100% by mass based on the mass of the swelling layer 61.
膨潤層61の厚さは、乾燥状態で、例えば2.0mm以下、1.5mm以下、1.0mm以下、又は0.8mm以下であってよく、0.1mm以上、又は0.3mm以上であってもよい。膨潤層61の単位面積当たりの質量は、100g/m2以下、80g/m2以下、60g/m2以下、又は40g/m2以下であってもよく、10g/m2以上、20g/m2以上、又は25g/m2以上であってもよい。
The thickness of the swelling layer 61 may be, for example, 2.0 mm or less, 1.5 mm or less, 1.0 mm or less, or 0.8 mm or less in a dry state, and is 0.1 mm or more, or 0.3 mm or more. You may. The mass per unit area of the swelling layer 61 may be 100 g / m 2 or less, 80 g / m 2 or less, 60 g / m 2 or less, or 40 g / m 2 or less, 10 g / m 2 or more, 20 g / m. It may be 2 or more, or 25 g / m 2 or more.
繊維層61bを構成する繊維状物は、例えば、セルロース系繊維、合成繊維、又はこれらの組み合わせであることができる。セルロース系繊維の例としては、粉砕された木材パルプ、コットン、コットンリンター、レーヨン、セルロースアセテートが挙げられる。合成繊維の例としては、ポリアミド繊維、ポリエステル繊維、及びポリオレフィン繊維が挙げられる。繊維状物が親水性繊維(例えばパルプ)であってもよい。
The fibrous material constituting the fiber layer 61b can be, for example, a cellulosic fiber, a synthetic fiber, or a combination thereof. Examples of cellulosic fibers include crushed wood pulp, cotton, cotton linters, rayon and cellulosic acetate. Examples of synthetic fibers include polyamide fibers, polyester fibers, and polyolefin fibers. The fibrous material may be hydrophilic fibers (for example, pulp).
膨潤層61は、無機粒子(例えば非晶質シリカ)、消臭剤、抗菌剤、香料等を更に含んでもよい。
The swelling layer 61 may further contain inorganic particles (for example, amorphous silica), a deodorant, an antibacterial agent, a fragrance, and the like.
シート基材62a,62bは、例えば、不織布、又はティッシュ等であってもよい。2枚のシート基材62a,62bが、同一又は異なる不織布であることができる。不織布は、短繊維(すなわちステープル)で構成される不織布(短繊維不織布)であってもよく、長繊維(すなわちフィラメント)で構成される不織布(長繊維不織布)であってもよい。ステープルは、一般的には数百mm以下の繊維長を有していてよい。
The sheet base materials 62a and 62b may be, for example, a non-woven fabric, a tissue, or the like. The two sheet base materials 62a and 62b can be the same or different non-woven fabrics. The non-woven fabric may be a non-woven fabric composed of short fibers (that is, staples) (short-fiber non-woven fabric) or a non-woven fabric composed of long fibers (that is, filaments) (long-fiber non-woven fabric). The staples may generally have a fiber length of several hundred mm or less.
シート基材62a,62bとして用いられる不織布は、サーマルボンド不織布、エアスルー不織布、レジンボンド不織布、スパンボンド不織布、メルトブロー不織布、エアレイド不織布、スパンレース不織布、ポイントボンド不織布、又はこれらから選ばれる2種以上の不織布を含む積層体であってよい。
The non-woven fabrics used as the sheet base materials 62a and 62b are thermal-bonded non-woven fabrics, air-through non-woven fabrics, resin-bonded non-woven fabrics, spunbonded non-woven fabrics, melt-blown non-woven fabrics, air-laid non-woven fabrics, spunlaced non-woven fabrics, point-bonded non-woven fabrics, or two or more kinds selected from these. It may be a laminate containing a non-woven fabric.
シート基材62a,62bとして用いられる不織布は、合成繊維、天然繊維、又はこれらの組み合わせによって形成された不織布であることができる。合成繊維の例としては、ポリエチレン(PE)及びポリプロピレン(PP)等のポリオレフィン、ポリエチレンテレフタレート(PET)、ポリトリメチレンテレフタレート(PTT)及びポリエチレンナフタレート(PEN)等のポリエステル、ナイロン等のポリアミド、並びにレーヨンから選ばれる合成樹脂を含む繊維が挙げられる。天然繊維の例としては、綿、絹、麻、又はパルプ(セルロース)を含む繊維が挙げられる。不織布を形成する繊維が、ポリオレフィン繊維、ポリエステル繊維又はこれらの組み合わせであってよい。シート基材62a,62bがティッシュであってもよい。
The non-woven fabric used as the sheet base materials 62a and 62b can be a non-woven fabric formed of synthetic fibers, natural fibers, or a combination thereof. Examples of synthetic fibers include polyolefins such as polyethylene (PE) and polypropylene (PP), polyesters such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN), polyamides such as nylon, and Examples thereof include fibers containing a synthetic resin selected from rayon. Examples of natural fibers include fibers containing cotton, silk, hemp, or pulp (cellulose). The fibers forming the non-woven fabric may be polyolefin fibers, polyester fibers or a combination thereof. The sheet base materials 62a and 62b may be tissues.
シート基材62a,62bとして用いられるティッシュは、天然繊維、あるいは天然繊維に合成繊維を配合したものであってもよい。ティッシュの単位面積当たりの質量は、16±2g/m2であってもよい。ティッシュの厚みは、0.12±0.02mmであってもよい。
The tissues used as the sheet base materials 62a and 62b may be natural fibers or natural fibers mixed with synthetic fibers. The mass per unit area of the tissue may be 16 ± 2 g / m 2. The thickness of the tissue may be 0.12 ± 0.02 mm.
シート基材62a,62bは、膨潤層61の主面よりも広い主面を有していてよい。すなわち、シート基材62a,62bの外縁部は、膨潤層61の周囲に延在していてよい。シート基材62a,62bは、膨潤層61の周囲に延在する外縁部において、互いに接着されていてもよい。
The sheet base materials 62a and 62b may have a main surface wider than the main surface of the swelling layer 61. That is, the outer edges of the sheet base materials 62a and 62b may extend around the swelling layer 61. The sheet base materials 62a and 62b may be adhered to each other at the outer edge portion extending around the swelling layer 61.
補助シート60は、例えば、膨潤層61をシート基材62a,62bの間に挟み、形成された構造体を必要により加熱しながら加圧する方法により、得ることができる。必要により、シート基材62a,62bと、膨潤層61との間に接着剤63a,63bが配置される。
The auxiliary sheet 60 can be obtained, for example, by sandwiching the swelling layer 61 between the sheet base materials 62a and 62b and pressurizing the formed structure while heating it as necessary. If necessary, the adhesives 63a and 63b are arranged between the sheet base materials 62a and 62b and the swelling layer 61.
補助シート60は、例えば各種の吸収性物品を製造するために用いられる。吸収性物品の例としては、おむつ(例えば紙おむつ)、トイレトレーニングパンツ、失禁パッド、衛生材料(生理用ナプキン、タンポン等)、汗取りパッド、ペットシート、簡易トイレ用部材、及び動物排泄物処理材が挙げられる。
The auxiliary sheet 60 is used, for example, for producing various absorbent articles. Examples of absorbent articles include diapers (eg paper diapers), toilet training pants, incontinence pads, sanitary materials (sanitary napkins, tampons, etc.), sweat pads, pet sheets, toilet components, and animal waste treatment materials. Can be mentioned.
[吸収性物品]
図2は、一実施形態に係る吸収性物品の短手方向の断面図である。図2に示す吸収性物品100は、短冊状の吸水コア50と、補助シート60と、液体透過性シート30と、液体不透過性シート40とを備える。 [Absorbent article]
FIG. 2 is a cross-sectional view of the absorbent article according to the embodiment in the lateral direction. Theabsorbent article 100 shown in FIG. 2 includes a strip-shaped water absorbing core 50, an auxiliary sheet 60, a liquid permeable sheet 30, and a liquid permeable sheet 40.
図2は、一実施形態に係る吸収性物品の短手方向の断面図である。図2に示す吸収性物品100は、短冊状の吸水コア50と、補助シート60と、液体透過性シート30と、液体不透過性シート40とを備える。 [Absorbent article]
FIG. 2 is a cross-sectional view of the absorbent article according to the embodiment in the lateral direction. The
図2に示す吸収性物品100において、膨潤層61を備える補助シート60は、吸水コア50及び液体透過性シート30の間に配置されている。補助シート60は、吸水コア50及び液体透過性シート30の間に配置されることに代えて、不透過性シート40及び吸水コア50の間に配置されていてよい。また、補助シート60は、吸水コア50及び液体透過性シート30の間、並びに、吸水コア50及び液体透過性シート30の間に、配置されていてもよい。使用状態における液体漏れ抑制効果により一層優れる観点から、補助シートは、吸水コア及び液体透過性シートの間に配置されていてよい。
In the absorbent article 100 shown in FIG. 2, the auxiliary sheet 60 provided with the swelling layer 61 is arranged between the water absorbing core 50 and the liquid permeable sheet 30. The auxiliary sheet 60 may be arranged between the impermeable sheet 40 and the water absorbing core 50 instead of being arranged between the water absorbing core 50 and the liquid permeable sheet 30. Further, the auxiliary sheet 60 may be arranged between the water absorption core 50 and the liquid permeable sheet 30, and between the water absorption core 50 and the liquid permeable sheet 30. The auxiliary sheet may be arranged between the water absorption core and the liquid permeable sheet from the viewpoint of being more excellent in the liquid leakage suppressing effect in the use state.
図2に示す補助シート60は、吸水コア50の使用者が装着した際の使用者側の主面上に配置されているが、使用者が装着した際の使用者側とは反対側(外側)に配置されていてもよく、使用者側及び外側の両側に配置されていてもよい。
The auxiliary sheet 60 shown in FIG. 2 is arranged on the main surface of the user side when the water absorption core 50 is worn by the user, but is opposite to the user side (outside) when the water absorption core 50 is worn by the user. ), And may be arranged on both the user side and the outer side.
補助シート60は、吸水性樹脂粒子61aを含む膨潤層61を有する。膨潤層61は、吸水コア50の短手方向の両端部上に吸水コア50の長手方向に沿って設けられている。膨潤層61及びシート基材62a,62bを備える補助シート60において、吸水コアの一方の端部上の膨潤層と他方の端部上の膨潤層とは、別々のシート基材上に設けられていてもよいし、1枚のシート基材上に設けられていてもよい。
The auxiliary sheet 60 has a swelling layer 61 containing water-absorbent resin particles 61a. The swelling layer 61 is provided on both ends of the water absorption core 50 in the lateral direction along the longitudinal direction of the water absorption core 50. In the auxiliary sheet 60 including the swelling layer 61 and the sheet base materials 62a and 62b, the swelling layer on one end of the water absorption core and the swelling layer on the other end are provided on separate sheet base materials. It may be provided on one sheet base material.
補助シート60における膨潤層61は、吸水コア50の長手方向の両端部上に、吸水コア50の短手方向に沿って更に設けられていてもよい。この場合、吸水コア50の端部上に外周(縁部)に沿って設けられた膨潤層61を有する一枚の補助シートを用いることができる。
The swelling layer 61 in the auxiliary sheet 60 may be further provided on both ends of the water absorption core 50 in the longitudinal direction along the lateral direction of the water absorption core 50. In this case, one auxiliary sheet having a swelling layer 61 provided along the outer circumference (edge) on the end of the water absorption core 50 can be used.
吸収性物品100は、吸水コア50の短手方向の両端部上に長手方向に沿って設けられた膨潤層の間に、上述した膨潤力の10秒値が5N以上である吸水性樹脂粒子を含まない領域を有する。言い換えると、吸収性物品100は、吸水コア50の中央部上に上述した膨潤力の10秒値が5N以上である吸水性樹脂粒子を含まない領域を有する。当該領域には、例えば、上述した膨潤力の10秒値が5N以上である吸水性樹脂粒子以外の物質が必要に応じて配置されていてもよく、当該領域は、空隙であってもよい。
The absorbent article 100 has water-absorbent resin particles having a 10-second value of the above-mentioned swelling force of 5 N or more between the swelling layers provided along the longitudinal direction on both ends of the water-absorbing core 50 in the lateral direction. It has an area that does not include it. In other words, the absorbent article 100 has a region on the central portion of the water absorbing core 50 that does not contain the water absorbing resin particles having the above-mentioned 10-second value of the swelling force of 5 N or more. For example, a substance other than the water-absorbent resin particles having a 10-second value of the swelling force of 5 N or more may be arranged in the region, if necessary, and the region may be a void.
吸水コア50は、吸収層10と、2枚のコアラップシート20a,20bとを有する。コアラップシート20a,20bは、吸収層10の両側に配置されている。言い換えると、吸収層10は、コアラップシート20a,20bの内側に配置されており、上記2枚のコアラップシートの間に挟まれることにより、保形されている。コアラップシート20a,20bは、別々のシートであってもよいし、折り返された1枚のシート、又は1枚の袋体であってもよい。但し、吸水コア50は、2枚のコアラップシート20a,20bのうち一方又は両方を有していなくてもよい。例えば、吸収層10と、補助シート60との間にコアラップシート20aが配置されていなくてもよい。吸収層10と、補助シート60との間にコアラップシートが配置されていない場合、例えば、吸収層10は、1枚のコアラップシート20bと、補助シート60との間に挟まれることにより、保形される。
The water absorption core 50 has an absorption layer 10 and two core wrap sheets 20a and 20b. The core wrap sheets 20a and 20b are arranged on both sides of the absorption layer 10. In other words, the absorbent layer 10 is arranged inside the core wrap sheets 20a and 20b, and is held in shape by being sandwiched between the two core wrap sheets. The core wrap sheets 20a and 20b may be separate sheets, one folded sheet, or one bag body. However, the water absorption core 50 does not have to have one or both of the two core wrap sheets 20a and 20b. For example, the core wrap sheet 20a may not be arranged between the absorption layer 10 and the auxiliary sheet 60. When the core wrap sheet is not arranged between the absorption layer 10 and the auxiliary sheet 60, for example, the absorption layer 10 is sandwiched between one core wrap sheet 20b and the auxiliary sheet 60. It is kept in shape.
吸水コア50は、コアラップシート20aと吸収層10との間に介在する接着剤を更に有していてもよく、コアラップシート20bと吸収層10との間に介在する接着剤を更に有していてもよい。両側のコアラップシート20a,20bと吸収層10との間に接着層が介在してもよい。図3は、コアラップシート上に形成された接着剤の塗布パターンの一例を示す平面図である。図3に示される接着剤21は、コアラップシート20a上で間隔を空けながら配列された複数の線状部分から構成される塗布パターンを形成している。なお、接着剤21の塗布パターンは、直線状、曲線状、ドット状、又はこれらの組み合わせ等であってもよい。接着剤は、例えば水性接着剤、溶剤型接着剤、ホットメルト接着剤であってもよい。
The water absorption core 50 may further have an adhesive interposed between the core wrap sheet 20a and the absorption layer 10, and further has an adhesive interposed between the core wrap sheet 20b and the absorption layer 10. May be. An adhesive layer may be interposed between the core wrap sheets 20a and 20b on both sides and the absorption layer 10. FIG. 3 is a plan view showing an example of an adhesive application pattern formed on the core wrap sheet. The adhesive 21 shown in FIG. 3 forms a coating pattern composed of a plurality of linear portions arranged at intervals on the core wrap sheet 20a. The coating pattern of the adhesive 21 may be linear, curved, dot-shaped, or a combination thereof. The adhesive may be, for example, a water-based adhesive, a solvent-based adhesive, or a hot-melt adhesive.
吸収層10は、吸水性樹脂粒子10aと、繊維状物を含む繊維層10bとを有する。吸収層10は、繊維層10bを有していなくてもよい。吸収層における吸水性樹脂粒子の含有量は、吸収層10の質量を基準として、70~100質量%、80~100質量%、又は90~100質量%であってもよい。
The absorption layer 10 has water-absorbent resin particles 10a and a fiber layer 10b containing a fibrous material. The absorption layer 10 does not have to have the fiber layer 10b. The content of the water-absorbent resin particles in the absorption layer may be 70 to 100% by mass, 80 to 100% by mass, or 90 to 100% by mass based on the mass of the absorption layer 10.
吸水性樹脂粒子10aは、エチレン性不飽和単量体を単量体単位として含む重合体を含む粒子であってもよい。エチレン性不飽和単量体は、水溶性の単量体であってもよく、その例としては、(メタ)アクリル酸及びその塩、2-(メタ)アクリルアミド-2-メチルプロパンスルホン酸及びその塩、(メタ)アクリルアミド、N,N-ジメチル(メタ)アクリルアミド、2-ヒドロキシエチル(メタ)アクリレート、N-メチロール(メタ)アクリルアミド、ポリエチレングリコールモノ(メタ)アクリレート、N,N-ジエチルアミノエチル(メタ)アクリレート、N,N-ジエチルアミノプロピル(メタ)アクリレート、並びにジエチルアミノプロピル(メタ)アクリルアミドが挙げられる。エチレン性不飽和単量体は、単独で用いられてもよく、2種以上を組み合わせて用いられてもよい。エチレン性不飽和単量体がカルボキシル基、アミノ基等の官能基を有する場合、それらは重合体を架橋させる官能基として機能し得る。吸水性樹脂粒子は、(メタ)アクリル酸又は(メタ)アクリル酸の塩のうち少なくとも一方を単量体単位として含む重合体を含む粒子であってもよい。
The water-absorbent resin particles 10a may be particles containing a polymer containing an ethylenically unsaturated monomer as a monomer unit. The ethylenically unsaturated monomer may be a water-soluble monomer, and examples thereof include (meth) acrylic acid and salts thereof, 2- (meth) acrylamide-2-methylpropanesulfonic acid and its salts. Salt, (meth) acrylamide, N, N-dimethyl (meth) acrylamide, 2-hydroxyethyl (meth) acrylate, N-methylol (meth) acrylamide, polyethylene glycol mono (meth) acrylate, N, N-diethylaminoethyl (meth) ) Acrylate, N, N-diethylaminopropyl (meth) acrylate, and diethylaminopropyl (meth) acrylamide. The ethylenically unsaturated monomer may be used alone or in combination of two or more. When the ethylenically unsaturated monomer has a functional group such as a carboxyl group or an amino group, they can function as a functional group for cross-linking the polymer. The water-absorbent resin particles may be particles containing a polymer containing at least one of (meth) acrylic acid or a salt of (meth) acrylic acid as a monomer unit.
吸水性樹脂粒子10aは、例えば、エチレン性不飽和単量体を含む単量体を重合することを含む方法によって、製造することができる。単量体の重合方法は、例えば、逆相懸濁重合法、水溶液重合法、バルク重合法、及び沈殿重合法から選択され得る。吸水性樹脂粒子の良好な吸水特性の確保、及び、重合反応の容易な制御の観点から、逆相懸濁重合法又は水溶液重合法を採用してもよい。
The water-absorbent resin particles 10a can be produced, for example, by a method including polymerizing a monomer containing an ethylenically unsaturated monomer. The polymerization method of the monomer can be selected from, for example, a reverse phase suspension polymerization method, an aqueous solution polymerization method, a bulk polymerization method, and a precipitation polymerization method. From the viewpoint of ensuring good water absorption characteristics of the water-absorbent resin particles and easily controlling the polymerization reaction, a reverse phase suspension polymerization method or an aqueous solution polymerization method may be adopted.
吸水性樹脂粒子10aを構成する重合体は、架橋重合体であってもよい。この場合、重合体は、自己架橋、架橋剤との反応による架橋、又はこれらの両方によって架橋されていてもよい。吸水性樹脂粒子が、少なくともその表層部分の重合体を架橋剤で架橋することによって表面架橋されていてもよい。
The polymer constituting the water-absorbent resin particles 10a may be a crosslinked polymer. In this case, the polymer may be crosslinked by self-crosslinking, cross-linking by reaction with a cross-linking agent, or both. The water-absorbent resin particles may be surface-crosslinked by cross-linking at least the polymer of the surface layer portion with a cross-linking agent.
吸水性樹脂粒子10aは、エチレン性不飽和単量体の重合体に加えて、各種の追加の成分を含んでいてもよい。追加の成分の例としては、ゲル安定剤、金属キレート剤、及び流動性向上剤(滑剤)が挙げられる。追加の成分は、重合体を含む重合体粒子の内部、重合体粒子の表面上、又はそれらの両方に配置され得る。追加の成分は、流動性向上剤(滑剤)であってもよい。流動性向上剤は、無機粒子を含んでいてもよい。無機粒子としては、例えば、非晶質シリカ等のシリカ粒子が挙げられる。
The water-absorbent resin particles 10a may contain various additional components in addition to the polymer of the ethylenically unsaturated monomer. Examples of additional ingredients include gel stabilizers, metal chelating agents, and fluidity improvers (lubricants). Additional components may be placed inside the polymer particles, including the polymer, on the surface of the polymer particles, or both. The additional component may be a fluidity improver (lubricant). The fluidity improver may contain inorganic particles. Examples of the inorganic particles include silica particles such as amorphous silica.
吸水性樹脂粒子10aの形状は、例えば略球状、破砕状又は顆粒状であってもよく、これらの形状を有する一次粒子が凝集した粒子が形成されていてもよい。吸水性樹脂粒子の中位粒子径は、250~850μm、300~700μm、又は、300~600μmであってよい。また、吸水性樹脂粒子10aの吸水特性としては、例えば生理食塩水の吸水量が、20~80g/g、30~70g/g、又は40~65g/gであってよい。
The shape of the water-absorbent resin particles 10a may be, for example, substantially spherical, crushed or granular, and particles having these shapes may be aggregated. The medium particle size of the water-absorbent resin particles may be 250 to 850 μm, 300 to 700 μm, or 300 to 600 μm. As for the water absorption characteristics of the water-absorbent resin particles 10a, for example, the water absorption amount of the physiological saline may be 20 to 80 g / g, 30 to 70 g / g, or 40 to 65 g / g.
吸水性樹脂粒子10aのゲル膨潤力の10秒値は、使用者の装着状態における液体漏れ抑制効果をより一層高める観点から、5N未満であってよく、4N以下であってよく、0N以上であってよい。吸水性樹脂粒子10aのゲル膨潤力の60秒値は、使用者の装着状態における液体漏れ抑制効果をより一層高める観点から、20N以下、16N以下、12N以下、8N以下、7N未満、又は5N以下であってよく、0N以上、又は2N以上であってよい。ゲル膨潤力の10秒値及び60秒値の測定方法は、上述したとおりである。
The 10-second value of the gel swelling force of the water-absorbent resin particles 10a may be less than 5N, may be 4N or less, and may be 0N or more from the viewpoint of further enhancing the liquid leakage suppressing effect in the wearing state of the user. You can. The 60-second value of the gel swelling force of the water-absorbent resin particles 10a is 20 N or less, 16 N or less, 12 N or less, 8 N or less, less than 7 N, or 5 N or less from the viewpoint of further enhancing the liquid leakage suppressing effect in the wearing state of the user. It may be 0N or more, or 2N or more. The method for measuring the 10-second value and the 60-second value of the gel swelling force is as described above.
吸収層10の厚さは、乾燥状態で、例えば20mm以下、15mm以下、10mm以下、5mm以下、4mm以下、又は3mm以下であってよく、0.1mm以上、又は0.3mm以上であってもよい。吸収層10の単位面積当たりの質量は、1000g/m2以下、800g/m2以下、又は600g/m2以下であってもよく、100g/m2以上、又は200g/m2以上であってもよい。
The thickness of the absorption layer 10 may be, for example, 20 mm or less, 15 mm or less, 10 mm or less, 5 mm or less, 4 mm or less, or 3 mm or less, even if it is 0.1 mm or more, or 0.3 mm or more in a dry state. Good. The mass per unit area of the absorption layer 10 may be 1000 g / m 2 or less, 800 g / m 2 or less, or 600 g / m 2 or less, 100 g / m 2 or more, or 200 g / m 2 or more. May be good.
繊維層10bを構成する繊維状物は、例えば、セルロース系繊維、合成繊維、又はこれらの組み合わせであることができる。セルロース系繊維の例としては、粉砕された木材パルプ、コットン、コットンリンター、レーヨン、セルロースアセテートが挙げられる。合成繊維の例としては、ポリアミド繊維、ポリエステル繊維、及びポリオレフィン繊維が挙げられる。繊維状物が親水性繊維(例えばパルプ)であってもよい。
The fibrous material constituting the fiber layer 10b can be, for example, a cellulosic fiber, a synthetic fiber, or a combination thereof. Examples of cellulosic fibers include crushed wood pulp, cotton, cotton linters, rayon and cellulosic acetate. Examples of synthetic fibers include polyamide fibers, polyester fibers, and polyolefin fibers. The fibrous material may be hydrophilic fibers (for example, pulp).
吸収層10は、無機粒子(例えば非晶質シリカ)、消臭剤、抗菌剤、香料等を更に含んでもよい。吸水性樹脂粒子10aが無機粒子を含む場合、吸収層10は吸水性樹脂粒子10a中の無機粒子とは別に無機粒子を含んでいてもよい。
The absorption layer 10 may further contain inorganic particles (for example, amorphous silica), a deodorant, an antibacterial agent, a fragrance, and the like. When the water-absorbent resin particles 10a contain inorganic particles, the absorption layer 10 may contain inorganic particles in addition to the inorganic particles in the water-absorbent resin particles 10a.
コアラップシート20a,20bは、例えば不織布であってもよい。2枚のコアラップシート20a,20bが、同一又は異なる不織布であることができる。不織布は、短繊維(すなわちステープル)で構成される不織布(短繊維不織布)であってもよく、長繊維(すなわちフィラメント)で構成される不織布(長繊維不織布)であってもよい。ステープルは、一般的には数百mm以下の繊維長を有していてよい。
The core wrap sheets 20a and 20b may be, for example, a non-woven fabric. The two core wrap sheets 20a and 20b can be the same or different non-woven fabrics. The non-woven fabric may be a non-woven fabric composed of short fibers (that is, staples) (short-fiber non-woven fabric) or a non-woven fabric composed of long fibers (that is, filaments) (long-fiber non-woven fabric). The staples may generally have a fiber length of several hundred mm or less.
コアラップシート20a,20bは、サーマルボンド不織布、エアスルー不織布、レジンボンド不織布、スパンボンド不織布、メルトブロー不織布、エアレイド不織布、スパンレース不織布、ポイントボンド不織布、又はこれらから選ばれる2種以上の不織布を含む積層体であってよい。
The core wrap sheets 20a and 20b are laminated including a thermal bond non-woven fabric, an air-through non-woven fabric, a resin bond non-woven fabric, a spunbond non-woven fabric, a melt blow non-woven fabric, an air-laid non-woven fabric, a spunlace non-woven fabric, a point bond non-woven fabric, or two or more kinds of non-woven fabrics selected from these. It can be a body.
コアラップシート20a,20bとして用いられる不織布は、合成繊維、天然繊維、又はこれらの組み合わせによって形成された不織布であることができる。合成繊維の例としては、ポリエチレン(PE)及びポリプロピレン(PP)等のポリオレフィン、ポリエチレンテレフタレート(PET)、ポリトリメチレンテレフタレート(PTT)及びポリエチレンナフタレート(PEN)等のポリエステル、ナイロン等のポリアミド、並びにレーヨンから選ばれる合成樹脂を含む繊維が挙げられる。天然繊維の例としては、綿、絹、麻、又はパルプ(セルロース)を含む繊維が挙げられる。不織布を形成する繊維が、ポリオレフィン繊維、ポリエステル繊維又はこれらの組み合わせであってよい。コアラップシート20a,20bがティッシュであってもよい。
The non-woven fabric used as the core wrap sheets 20a and 20b can be a non-woven fabric formed of synthetic fibers, natural fibers, or a combination thereof. Examples of synthetic fibers include polyolefins such as polyethylene (PE) and polypropylene (PP), polyesters such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN), polyamides such as nylon, and Examples thereof include fibers containing a synthetic resin selected from rayon. Examples of natural fibers include fibers containing cotton, silk, hemp, or pulp (cellulose). The fibers forming the non-woven fabric may be polyolefin fibers, polyester fibers or a combination thereof. The core wrap sheets 20a and 20b may be tissues.
吸水コア50は、例えば、吸水性樹脂粒子10a、又は吸水性樹脂粒子10aと繊維状物とを含む混合物とコアラップシート20a,20bの間に挟み、形成された構造体を必要により加熱しながら加圧する方法により、得ることができる。必要により、コアラップシート20a,20bと、吸水性樹脂粒子10a、又はこれを含む混合物との間に接着剤が配置される。
The water-absorbing core 50 is sandwiched between, for example, the water-absorbent resin particles 10a or a mixture containing the water-absorbent resin particles 10a and the fibrous material and the core wrap sheets 20a and 20b, and the formed structure is heated as necessary. It can be obtained by the method of pressurizing. If necessary, an adhesive is placed between the core wrap sheets 20a and 20b and the water-absorbent resin particles 10a or a mixture containing the same.
吸水コア50は、コアラップシート20a、吸水性樹脂粒子10a及び繊維層10bからなる吸収層10及びコアラップシート20bがこの順に配置されている吸水コアのほかに、全体が繊維層を実質的に含まないシート状であってもよい。吸水コアは、複数(例えば2つ)の吸収層を含んでいてもよい。吸水コアが複数の吸収層を含む場合、吸収層の間には、コアラップシートが配置されていてよい。当該複数の吸収層に含まれる吸水性樹脂粒子は、同種であっても異種であってもよい。複数の吸収層それぞれの単位面積当たりの質量及び厚さは同一であっても異なっていてもよい。
The water-absorbing core 50 includes a water-absorbing core in which the core wrap sheet 20a, the water-absorbent resin particles 10a, the absorbent layer 10 composed of the fiber layer 10b, and the core wrap sheet 20b are arranged in this order, and substantially the entire fiber layer. It may be in the form of a sheet that does not include it. The water absorption core may include a plurality of (for example, two) absorption layers. When the water absorption core includes a plurality of absorption layers, a core wrap sheet may be arranged between the absorption layers. The water-absorbent resin particles contained in the plurality of absorption layers may be of the same type or different types. The mass and thickness per unit area of each of the plurality of absorption layers may be the same or different.
液体透過性シート30は、吸収対象の液が浸入する側の最外層の位置に配置されている。液体透過性シート30は、コアラップシート20bに接した状態でコアラップシート20bの外側に配置されている。液体不透過性シート40は、吸収性物品100において液体透過性シート30とは反対側の最外層の位置に配置されている。液体不透過性シート40は、コアラップシート20aに接した状態でコアラップシート20aの外側に配置されている。液体透過性シート30及び液体不透過性シート40は、吸水コア50の主面よりも広い主面を有しており、液体透過性シート30及び液体不透過性シート40の外縁部は、吸収層10及びコアラップシート20a,20bの周囲に延在している。ただし、吸収層10、コアラップシート20a,20b、補助シート60、液体透過性シート30、及び、液体不透過性シート40の大小関係は、吸収性物品の用途等に応じて適宜調整される。
The liquid permeable sheet 30 is arranged at the position of the outermost layer on the side where the liquid to be absorbed enters. The liquid permeable sheet 30 is arranged on the outside of the core wrap sheet 20b in contact with the core wrap sheet 20b. The liquid permeable sheet 40 is arranged at the position of the outermost layer on the side opposite to the liquid permeable sheet 30 in the absorbent article 100. The liquid impermeable sheet 40 is arranged on the outside of the core wrap sheet 20a in a state of being in contact with the core wrap sheet 20a. The liquid permeable sheet 30 and the liquid permeable sheet 40 have a main surface wider than the main surface of the water absorbing core 50, and the outer edges of the liquid permeable sheet 30 and the liquid permeable sheet 40 are an absorbing layer. It extends around 10 and the core wrap sheets 20a and 20b. However, the magnitude relationship of the absorbent layer 10, the core wrap sheets 20a and 20b, the auxiliary sheet 60, the liquid permeable sheet 30, and the liquid permeable sheet 40 is appropriately adjusted according to the use of the absorbent article and the like.
液体透過性シート30は、不織布であってもよい。液体透過性シート30として用いられる不織布は、吸収性物品の液体吸収性能の観点から、適度な親水性を有していてもよい。その観点から、液体透過性シート30は、紙パルプ技術協会による紙パルプ試験方法No.68(2000)の測定方法に従って測定される親水度が5~200の不織布であってもよい。不織布の親水度は、10~150であってもよい。紙パルプ試験方法No.68の詳細については、例えばWO2011/086843号を参照することができる。
The liquid permeable sheet 30 may be a non-woven fabric. The non-woven fabric used as the liquid permeable sheet 30 may have appropriate hydrophilicity from the viewpoint of the liquid absorption performance of the absorbent article. From this point of view, the liquid permeable sheet 30 is obtained from the pulp and paper test method No. 1 by the Paper and Pulp Technology Association. A non-woven fabric having a hydrophilicity of 5 to 200 measured according to the measuring method of 68 (2000) may be used. The hydrophilicity of the non-woven fabric may be 10 to 150. Pulp and paper test method No. For details of 68, for example, WO2011 / 086843 can be referred to.
親水性を有する不織布は、例えば、レーヨン繊維のように適度な親水度を示す繊維によって形成されたものでもよいし、ポリオレフィン繊維、ポリエステル繊維のような疎水性の化学繊維を親水化処理して得た繊維によって形成されたものであってもよい。親水化処理された疎水性の化学繊維を含む不織布を得る方法としては、例えば、疎水性の化学繊維に親水化剤を混合したものを用いてスパンボンド法にて不織布を得る方法、疎水性化学繊維でスパンボンド不織布を作製する際に親水化剤を同伴させる方法、疎水性の化学繊維を用いて得たスパンボンド不織布に親水化剤を含浸させる方法が挙げられる。親水化剤としては、脂肪族スルホン酸塩、高級アルコール硫酸エステル塩等のアニオン系界面活性剤、第4級アンモニウム塩等のカチオン系界面活性剤、ポリエチレングリコール脂肪酸エステル、ポリグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル等のノニオン系界面活性剤、ポリオキシアルキレン変性シリコーン等のシリコーン系界面活性剤、及びポリエステル系、ポリアミド系、アクリル系、ウレタン系の樹脂からなるステイン・リリース剤等が用いられる。
The non-woven fabric having hydrophilicity may be formed of fibers showing appropriate hydrophilicity such as rayon fiber, or obtained by hydrophilizing a hydrophobic chemical fiber such as polyolefin fiber or polyester fiber. It may be formed of rayon fibers. Examples of a method for obtaining a non-woven fabric containing hydrophobic chemical fibers that have been hydrophilized include a method for obtaining a non-woven fabric by a spunbond method using a mixture of hydrophobic chemical fibers and a hydrophilic agent, and hydrophobic chemistry. Examples thereof include a method of accommodating a hydrophilic agent when producing a spunbonded non-woven fabric from fibers, and a method of impregnating a spunbonded non-woven fabric obtained by using hydrophobic chemical fibers with a hydrophilicizing agent. Hydrophilic agents include anionic surfactants such as aliphatic sulfonates and higher alcohol sulfates, cationic surfactants such as quaternary ammonium salts, polyethylene glycol fatty acid esters, polyglycerin fatty acid esters, and sorbitan fatty acids. Nonionic surfactants such as esters, silicone-based surfactants such as polyoxyalkylene-modified silicones, and stain-releasing agents made of polyester-based, polyamide-based, acrylic-based, and urethane-based resins are used.
液体透過性シート30として用いられる不織布の目付量(単位面積当たりの質量)は、吸収性物品に、良好な液体浸透性、柔軟性、強度及びクッション性を付与できる観点、及び吸収性物品の液体浸透速度を速める観点から、5~200g/m2、8~150g/m2、又は10~100g/m2であってもよい。液体透過性シート30の厚さは、20~1400μm、50~1200μm、又は80~1000μmであってもよい。
The amount of texture (mass per unit area) of the non-woven fabric used as the liquid permeable sheet 30 is from the viewpoint of imparting good liquid permeability, flexibility, strength and cushioning property to the absorbent article, and the liquid of the absorbent article. From the viewpoint of increasing the permeation rate, it may be 5 to 200 g / m 2 , 8 to 150 g / m 2 , or 10 to 100 g / m 2 . The thickness of the liquid permeable sheet 30 may be 20 to 1400 μm, 50 to 1200 μm, or 80 to 1000 μm.
液体不透過性シート40は、吸収層10又は膨潤層61に吸収された液体が液体不透過性シート40側から外部へ漏れ出すのを防止する。液体不透過性シート40は、樹脂シート、又は不織布であってもよい。樹脂シートは、ポリエチレン、ポリプロピレン、ポリ塩化ビニル等の合成樹脂からなるシートであってもよい。不織布は、耐水性のメルトブロー不織布を高強度のスパンボンド不織布で挟んだスパンボンド/メルトブロー/スパンボンド(SMS)不織布であってもよい。また、液体不透過性シート40が、樹脂シートと不織布(例えば、スパンボンド不織布、スパンレース不織布)との複合シートであってもよい。液体不透過性シート40は、装着時のムレが低減されて、着用者に与える不快感を軽減することができる等の観点から、通気性を有していてもよい。通気性を有する液体不透過性シート40として、例えば低密度ポリエチレン(LDPE)樹脂のシートを用いることができる。
The liquid impermeable sheet 40 prevents the liquid absorbed by the absorption layer 10 or the swelling layer 61 from leaking to the outside from the liquid impermeable sheet 40 side. The liquid impermeable sheet 40 may be a resin sheet or a non-woven fabric. The resin sheet may be a sheet made of a synthetic resin such as polyethylene, polypropylene, or polyvinyl chloride. The non-woven fabric may be a spunbond / meltblow / spunbond (SMS) non-woven fabric in which a water-resistant melt-blow non-woven fabric is sandwiched between high-strength spunbond non-woven fabrics. Further, the liquid permeable sheet 40 may be a composite sheet of a resin sheet and a non-woven fabric (for example, a spunbonded non-woven fabric or a spunlaced non-woven fabric). The liquid impermeable sheet 40 may have breathability from the viewpoint that stuffiness at the time of wearing is reduced and discomfort given to the wearer can be reduced. As the liquid impermeable sheet 40 having breathability, for example, a sheet of low density polyethylene (LDPE) resin can be used.
吸収性物品の着用感を損なわないよう、柔軟性を確保する観点から、液体不透過性シート40の目付量(単位面積当たりの質量)が5~100g/m2、又は10~50g/m2であってもよい。
From the viewpoint of ensuring flexibility so as not to impair the wearing feeling of the absorbent article, the basis weight (mass per unit area) of the liquid impermeable sheet 40 is 5 to 100 g / m 2 or 10 to 50 g / m 2. It may be.
吸収性物品100は、例えば、短冊状の吸水コア50、液体透過性シート30及び液体不透過性シート40を備える吸収性物品において、補助シート60を液体不透過性シート40と吸水コア50との間、及び/又は吸水コア50と液体透過性シート30との間に配置することを含む方法により、製造することができる。液体不透過性シート40、吸水コア50及び液体透過性シート30をこの順に備え、補助シート60が、液体不透過性シート40と吸水コア50との間及び/又は吸水コアと液体透過性シート30との間に配置されている積層体が、必要により加圧される。各構成単位間を接着剤で結合させてもよい。
The absorbent article 100 is, for example, in an absorbent article including a strip-shaped water absorbing core 50, a liquid permeable sheet 30, and a liquid impermeable sheet 40, and the auxiliary sheet 60 is a liquid impermeable sheet 40 and a water absorbing core 50. It can be manufactured by a method including placing between and / or between the water absorbing core 50 and the liquid permeable sheet 30. The liquid permeable sheet 40, the water absorbing core 50 and the liquid permeable sheet 30 are provided in this order, and the auxiliary sheet 60 is provided between the liquid permeable sheet 40 and the water absorbing core 50 and / or between the water absorbing core and the liquid permeable sheet 30. The laminate arranged between and is pressurized if necessary. The structural units may be bonded with an adhesive.
<液体漏れを抑制する方法>
本実施形態によれば、本実施形態に係る補助シートを用いた液体漏れの抑制方法を提供することができる。本実施形態に係る液体漏れの抑制方法は、短冊状の吸水コア、液体不透過性シート及び液体透過性シートを備える吸収性物品において、上記膨潤層を有する補助シートを、吸水コアの短手方向の両端部上に、上記膨潤層が長手方向に沿うように配置することを含む。 <Method of suppressing liquid leakage>
According to the present embodiment, it is possible to provide a method for suppressing liquid leakage using the auxiliary sheet according to the present embodiment. The method for suppressing liquid leakage according to the present embodiment is to use an auxiliary sheet having the swelling layer in an absorbent article provided with a strip-shaped water absorbing core, a liquid impermeable sheet and a liquid permeable sheet in the lateral direction of the water absorbing core. The swelling layer is arranged along the longitudinal direction on both ends of the swelling layer.
本実施形態によれば、本実施形態に係る補助シートを用いた液体漏れの抑制方法を提供することができる。本実施形態に係る液体漏れの抑制方法は、短冊状の吸水コア、液体不透過性シート及び液体透過性シートを備える吸収性物品において、上記膨潤層を有する補助シートを、吸水コアの短手方向の両端部上に、上記膨潤層が長手方向に沿うように配置することを含む。 <Method of suppressing liquid leakage>
According to the present embodiment, it is possible to provide a method for suppressing liquid leakage using the auxiliary sheet according to the present embodiment. The method for suppressing liquid leakage according to the present embodiment is to use an auxiliary sheet having the swelling layer in an absorbent article provided with a strip-shaped water absorbing core, a liquid impermeable sheet and a liquid permeable sheet in the lateral direction of the water absorbing core. The swelling layer is arranged along the longitudinal direction on both ends of the swelling layer.
以下、実施例を挙げて本発明についてさらに具体的に説明する。ただし、本発明はこれら実施例に限定されるものではない。
Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.
<吸水性樹脂粒子の製造>
<Manufacturing of water-absorbent resin particles>
製造例1 吸水性樹脂粒子a
還流冷却器、滴下ロート、窒素ガス導入管、及び、撹拌機(翼径5cmの4枚傾斜パドル翼(フッ素樹脂にて表面処理したもの)を2段有する撹拌翼)を備えた内径11cm、内容積2Lの、4箇所の側壁バッフル付き丸底円筒型セパラブルフラスコ(バッフル長さ:10cm、バッフル幅:7mm)を準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン451.4gを添加し、界面活性剤としてソルビタンモノラウレート(ノニオンLP-20R、HLB値:8.6、日油株式会社製)1.288gを添加することにより混合物を得た。この混合物を撹拌機の回転数300rpmで撹拌しつつ50℃まで昇温することによりソルビタンモノラウレートをn-ヘプタンに溶解させた後、混合物を40℃まで冷却した。 Production Example 1 Water-absorbent resin particles a
Inner diameter 11 cm, contents equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirrer (a stirrer blade having two stages of four inclined paddle blades (surface treated with fluororesin) with a blade diameter of 5 cm). A round-bottomed cylindrical separable flask with a stack of 2 L and four side wall baffles (baffle length: 10 cm, baffle width: 7 mm) was prepared. To this flask, 451.4 g of n-heptane as a hydrocarbon dispersion medium was added, and 1.288 g of sorbitan monolaurate (Nonion LP-20R, HLB value: 8.6, manufactured by NOF CORPORATION) was added as a surfactant. The mixture was obtained by addition. The sorbitan monolaurate was dissolved in n-heptane by heating the mixture to 50 ° C. while stirring at a stirring speed of 300 rpm, and then the mixture was cooled to 40 ° C.
還流冷却器、滴下ロート、窒素ガス導入管、及び、撹拌機(翼径5cmの4枚傾斜パドル翼(フッ素樹脂にて表面処理したもの)を2段有する撹拌翼)を備えた内径11cm、内容積2Lの、4箇所の側壁バッフル付き丸底円筒型セパラブルフラスコ(バッフル長さ:10cm、バッフル幅:7mm)を準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン451.4gを添加し、界面活性剤としてソルビタンモノラウレート(ノニオンLP-20R、HLB値:8.6、日油株式会社製)1.288gを添加することにより混合物を得た。この混合物を撹拌機の回転数300rpmで撹拌しつつ50℃まで昇温することによりソルビタンモノラウレートをn-ヘプタンに溶解させた後、混合物を40℃まで冷却した。 Production Example 1 Water-absorbent resin particles a
Inner diameter 11 cm, contents equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirrer (a stirrer blade having two stages of four inclined paddle blades (surface treated with fluororesin) with a blade diameter of 5 cm). A round-bottomed cylindrical separable flask with a stack of 2 L and four side wall baffles (baffle length: 10 cm, baffle width: 7 mm) was prepared. To this flask, 451.4 g of n-heptane as a hydrocarbon dispersion medium was added, and 1.288 g of sorbitan monolaurate (Nonion LP-20R, HLB value: 8.6, manufactured by NOF CORPORATION) was added as a surfactant. The mixture was obtained by addition. The sorbitan monolaurate was dissolved in n-heptane by heating the mixture to 50 ° C. while stirring at a stirring speed of 300 rpm, and then the mixture was cooled to 40 ° C.
次に、内容積500mLの三角フラスコに80.5質量%のアクリル酸水溶液92.0g(アクリル酸:1.03モル)を入れた。続いて、外部より氷冷しながら20.9質量%水酸化ナトリウム水溶液147.7gを滴下することによってアクリル酸の中和を行うことによりアクリル酸部分中和物水溶液を得た。次に、水溶性ラジカル重合開始剤として過硫酸カリウム0.1012g(0.374ミリモル)をアクリル酸部分中和物水溶液に加えた後に溶解させることにより単量体水溶液を調製した。
Next, 92.0 g (acrylic acid: 1.03 mol) of an 80.5 mass% acrylic acid aqueous solution was placed in an Erlenmeyer flask having an internal volume of 500 mL. Subsequently, 147.7 g of a 20.9 mass% sodium hydroxide aqueous solution was added dropwise from the outside while cooling with ice to neutralize the acrylic acid, thereby obtaining an aqueous solution of a partially neutralized acrylic acid. Next, 0.1012 g (0.374 mmol) of potassium persulfate as a water-soluble radical polymerization initiator was added to the acrylic acid partially neutralized aqueous solution and then dissolved to prepare a monomer aqueous solution.
上述の単量体水溶液を上述のセパラブルフラスコに添加した後、系内を窒素で充分に置換した。その後、撹拌機の回転数700rpmで撹拌しつつ、フラスコを70℃の水浴に浸漬した後に60分間保持して重合を完了させることにより含水ゲル状重合体を得た。
After adding the above-mentioned monomer aqueous solution to the above-mentioned separable flask, the inside of the system was sufficiently replaced with nitrogen. Then, the flask was immersed in a water bath at 70 ° C. and held for 60 minutes to complete the polymerization while stirring at a rotation speed of 700 rpm of the stirrer to obtain a hydrogel polymer.
その後、撹拌機の回転数1000rpmで撹拌しつつ、生成した含水ゲル状重合体、n-ヘプタン及び界面活性剤を含む重合液に、粉末状無機凝集剤として非晶質シリカ(オリエンタルシリカズコーポレーション、トクシールNP-S)0.092gを予めn-ヘプタン100gに分散させることにより得られた分散液を添加した後、10分間混合した。その後、反応液を含むフラスコを125℃の油浴に浸漬し、n-ヘプタンと水との共沸蒸留によりn-ヘプタンを還流しながら98.0gの水を系外へ抜き出した。その後、表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液4.14g(エチレングリコールジグリシジルエーテル:0.475ミリモル)を添加した後、内温83±2℃で2時間保持した。
Then, while stirring at a stirring speed of 1000 rpm, amorphous silica (Oriental Silicas Corporation, oriental silicas corporation, etc.) was added to the polymer solution containing the produced hydrogel polymer, n-heptane and a surfactant as a powdery inorganic flocculant. A dispersion obtained by previously dispersing 0.092 g of Toxile NP-S) in 100 g of n-heptane was added and then mixed for 10 minutes. Then, the flask containing the reaction solution was immersed in an oil bath at 125 ° C., and 98.0 g of water was extracted from the system while refluxing n-heptane by azeotropic distillation of n-heptane and water. Then, 4.14 g (ethylene glycol diglycidyl ether: 0.475 mmol) of 2% by mass of an ethylene glycol diglycidyl ether aqueous solution was added as a surface cross-linking agent, and the mixture was maintained at an internal temperature of 83 ± 2 ° C. for 2 hours.
次いで、n-ヘプタン6.62gに界面活性剤であるソルビタンモノラウレート(商品名:ノニオンLP-20R、HLB値8.6、日油株式会社製)0.074gが溶解した界面活性剤溶液をフラスコ内に添加した。
Next, a surfactant solution in which 0.074 g of sorbitan monolaurate (trade name: Nonion LP-20R, HLB value 8.6, manufactured by Nichiyu Co., Ltd.), which is a surfactant, was dissolved in 6.62 g of n-heptane was added. Added in a flask.
その後、水及びn-ヘプタンを125℃の油浴で加熱して蒸発させ、系内からの蒸発物がほとんど留出されなくなるまで乾燥させることにより、重合体粒子の乾燥品を得た。この重合体粒子を目開き850μmの篩に通すことにより吸水性樹脂粒子aを90.1g得た。吸水性樹脂粒子aの中位粒子径は352μmであった。
Then, water and n-heptane were heated in an oil bath at 125 ° C. to evaporate, and dried until almost no evaporation from the system was distilled off to obtain a dried product of polymer particles. The polymer particles were passed through a sieve having an opening of 850 μm to obtain 90.1 g of water-absorbent resin particles a. The medium particle size of the water-absorbent resin particles a was 352 μm.
製造例2 吸水性樹脂粒子b
共沸蒸留により104.0gの水を系外へ抜き出したこと、表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液8.28g(エチレングリコールジグリシジルエーテル:0.951ミリモル)に変更したこと以外は製造例1と同様にして、吸水性樹脂粒子bを90.3g得た。吸水性樹脂粒子bの中位粒子径は420μmであった。 Production Example 2 Water-absorbent resin particles b
104.0 g of water was extracted from the system by azeotropic distillation, and the surface cross-linking agent was changed to 8.28 g of a 2 mass% ethylene glycol diglycidyl ether aqueous solution (ethylene glycol diglycidyl ether: 0.951 mmol). 90.3 g of water-absorbent resin particles b were obtained in the same manner as in Production Example 1 except for the above. The medium particle size of the water-absorbent resin particles b was 420 μm.
共沸蒸留により104.0gの水を系外へ抜き出したこと、表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液8.28g(エチレングリコールジグリシジルエーテル:0.951ミリモル)に変更したこと以外は製造例1と同様にして、吸水性樹脂粒子bを90.3g得た。吸水性樹脂粒子bの中位粒子径は420μmであった。 Production Example 2 Water-absorbent resin particles b
104.0 g of water was extracted from the system by azeotropic distillation, and the surface cross-linking agent was changed to 8.28 g of a 2 mass% ethylene glycol diglycidyl ether aqueous solution (ethylene glycol diglycidyl ether: 0.951 mmol). 90.3 g of water-absorbent resin particles b were obtained in the same manner as in Production Example 1 except for the above. The medium particle size of the water-absorbent resin particles b was 420 μm.
製造例3 吸水性樹脂粒子c
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 Production Example 3 Water-absorbent resin particles c
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 Production Example 3 Water-absorbent resin particles c
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
内容積300mLのビーカーに、水溶性エチレン性不飽和単量体として80.5質量%のアクリル酸水溶液92.0g(1.03モル)をとり、外部より冷却しつつ、20.9質量%の水酸化ナトリウム水溶液147.7gを滴下して75モル%の中和を行った後、増粘剤としてヒドロキシルエチルセルロース0.092g(住友精化株式会社、HECAW-15F)、水溶性ラジカル重合開始剤として過硫酸カリウム0.0736g(0.272ミリモル)、内部架橋剤としてエチレングリコールジグリシジルエーテル0.010g(0.057ミリモル)を加えて溶解し、第1段目の単量体水溶液を調製した。
In a beaker having an internal volume of 300 mL, 92.0 g (1.03 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer was placed, and while being cooled from the outside, 20.9 mass% was added. After adding 147.7 g of an aqueous sodium hydroxide solution to neutralize 75 mol%, 0.092 g of hydroxylethyl cellulose (Sumitomo Seika Co., Ltd., HECAW-15F) as a thickener, as a water-soluble radical polymerization initiator. 0.0736 g (0.272 mmol) of potassium persulfate and 0.010 g (0.057 mmol) of ethylene glycol diglycidyl ether as an internal cross-linking agent were added and dissolved to prepare a first-stage monomer aqueous solution.
そして、上記にて調製した第1段目の単量体水溶液をセパラブルフラスコに添加して、10分間攪拌した後、n-ヘプタン6.62gに界面活性剤としてHLB3のショ糖ステアリン酸エステル(三菱化学フーズ株式会社、リョートーシュガーエステルS-370)0.736gを加熱溶解した界面活性剤溶液を、さらに添加して、撹拌機の回転数を500rpmとして攪拌しながら系内を窒素で十分に置換した後、フラスコを70℃の水浴に浸漬して昇温し、重合を60分間行うことにより、第1段目の重合スラリー液を得た。
Then, the first-stage monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, 6.62 g of n-heptane was added as a surfactant to the sucrose stearic acid ester of HLB3. Mitsubishi Chemical Foods Co., Ltd., Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution dissolved by heating is further added, and the inside of the system is sufficiently filled with nitrogen while stirring at a stirring speed of 500 rpm. After the replacement, the flask was immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization was carried out for 60 minutes to obtain a first-stage polymerized slurry solution.
内容積500mLのビーカーに水溶性エチレン性不飽和単量体として80.5質量%のアクリル酸水溶液128.8g(1.44モル)をとり、外部より冷却しつつ、27質量%の水酸化ナトリウム水溶液159.0gを滴下して75モル%の中和を行った後、水溶性ラジカル重合開始剤として過硫酸カリウム0.090g(0.333ミリモル)、内部架橋剤としてエチレングリコールジグリシジルエーテル0.0116g(0.067ミリモル)を加えて溶解し、第2段目の単量体水溶液を調製した。
128.8 g (1.44 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer was placed in a beaker having an internal volume of 500 mL, and 27 mass% sodium hydroxide was cooled from the outside. After 159.0 g of the aqueous solution was added dropwise to neutralize 75 mol%, 0.090 g (0.333 mmol) of potassium persulfate was used as the water-soluble radical polymerization initiator, and ethylene glycol diglycidyl ether was used as the internal cross-linking agent. 0116 g (0.067 mmol) was added and dissolved to prepare a second-stage monomer aqueous solution.
撹拌機の回転数を1000rpmとして撹拌しながら、上記のセパラブルフラスコ系内を25℃に冷却した後、上記第2段目の単量体水溶液の全量を、第1段目の重合スラリー液に添加して、系内を窒素で30分間置換した後、再度、フラスコを70℃の水浴に浸漬して昇温し、重合反応を60分間行って、含水ゲル状重合体を得た。
After cooling the inside of the separable flask system to 25 ° C. while stirring at a stirring speed of 1000 rpm, the entire amount of the monomer aqueous solution in the second stage is added to the polymerized slurry liquid in the first stage. After adding and replacing the inside of the system with nitrogen for 30 minutes, the flask was again immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization reaction was carried out for 60 minutes to obtain a hydrogel polymer.
重合後、得られた含水ゲル状重合体に、45質量%のジエチレントリアミン5酢酸5ナトリウム水溶液0.589gを攪拌下で添加した。その後、125℃に設定した油浴にフラスコを浸漬し、n-ヘプタンと水との共沸蒸留により、n-ヘプタンを還流しながら、257.2gの水を系外へ抜き出した。その後、フラスコに表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液4.42g(0.507ミリモル)を添加し、83℃で2時間保持した。
After the polymerization, 0.589 g of a 45% by mass diethylenetriamine-5 sodium acetate aqueous solution was added to the obtained hydrogel polymer under stirring. Then, the flask was immersed in an oil bath set at 125 ° C., and 257.2 g of water was extracted from the system while refluxing n-heptane by azeotropic distillation of n-heptane and water. Then, 4.42 g (0.507 mmol) of a 2% by mass ethylene glycol diglycidyl ether aqueous solution was added to the flask as a surface cross-linking agent, and the flask was kept at 83 ° C. for 2 hours.
その後、n-ヘプタンと水を125℃の油浴で加熱して蒸発させて乾燥させることによって、重合体粒子の乾燥品を得た。この重合体粒子を目開き850μmの篩に通過させ、重合体粒子の質量に対して0.2質量%の非晶質シリカ(オリエンタルシリカズコーポレーション、トクシールNP-S)を重合体粒子と混合し、非晶質シリカを含む吸水性樹脂粒子cを231.2g得た。吸水性樹脂粒子cの中位粒子径は359μmであった。
Then, n-heptane and water were heated in an oil bath at 125 ° C. to evaporate and dry to obtain a dried product of polymer particles. The polymer particles are passed through a sieve having an opening of 850 μm, and 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) with respect to the mass of the polymer particles is mixed with the polymer particles. , 231.2 g of water-absorbent resin particles c containing amorphous silica were obtained. The medium particle size of the water-absorbent resin particles c was 359 μm.
製造例4 吸水性樹脂粒子d
第1段目の重合反応において、界面活性剤溶液添加後に調節する撹拌機の回転数を550rpmとしたこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により256.8gの水を系外へ抜き出したこと、重合体粒子と混合する非晶質シリカの量を重合体粒子質量に対して0.5質量%に変更したこと以外は、製造例3と同様にして、吸水性樹脂粒子dを230.2g得た。吸水性樹脂粒子dの中位粒子径は358μmであった。 Production Example 4 Water-absorbent resin particles d
In the first-stage polymerization reaction, the rotation speed of the stirrer adjusted after the addition of the surfactant solution was set to 550 rpm, and in the hydrogel polymer after the second-stage polymerization, 256.8 g by co-boiling distillation. In the same manner as in Production Example 3, except that the water was extracted from the system and the amount of amorphous silica mixed with the polymer particles was changed to 0.5% by mass with respect to the mass of the polymer particles. 230.2 g of water-absorbent resin particles d were obtained. The medium particle size of the water-absorbent resin particles d was 358 μm.
第1段目の重合反応において、界面活性剤溶液添加後に調節する撹拌機の回転数を550rpmとしたこと、第2段目の重合後の含水ゲル状重合体において、共沸蒸留により256.8gの水を系外へ抜き出したこと、重合体粒子と混合する非晶質シリカの量を重合体粒子質量に対して0.5質量%に変更したこと以外は、製造例3と同様にして、吸水性樹脂粒子dを230.2g得た。吸水性樹脂粒子dの中位粒子径は358μmであった。 Production Example 4 Water-absorbent resin particles d
In the first-stage polymerization reaction, the rotation speed of the stirrer adjusted after the addition of the surfactant solution was set to 550 rpm, and in the hydrogel polymer after the second-stage polymerization, 256.8 g by co-boiling distillation. In the same manner as in Production Example 3, except that the water was extracted from the system and the amount of amorphous silica mixed with the polymer particles was changed to 0.5% by mass with respect to the mass of the polymer particles. 230.2 g of water-absorbent resin particles d were obtained. The medium particle size of the water-absorbent resin particles d was 358 μm.
製造例5 吸水性樹脂粒子e
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 Production Example 5 Water-absorbent resin particles e
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
還流冷却器、滴下ロート、窒素ガス導入管、並びに、攪拌機として、翼径5cmの4枚傾斜パドル翼を2段で有する攪拌翼を備えた内径11cm、2L容の丸底円筒型セパラブルフラスコを準備した。このフラスコに、炭化水素分散媒としてn-ヘプタン293gをとり、高分子系分散剤として無水マレイン酸変性エチレン・プロピレン共重合体(三井化学株式会社、ハイワックス1105A)0.736gを添加し、攪拌しつつ80℃まで昇温して分散剤を溶解した後、50℃まで冷却した。 Production Example 5 Water-absorbent resin particles e
A round-bottomed cylindrical separable flask with an inner diameter of 11 cm and a volume of 2 L equipped with a reflux condenser, a dropping funnel, a nitrogen gas introduction pipe, and a stirring blade having four inclined paddle blades with a blade diameter of 5 cm in two stages as a stirrer. Got ready. To this flask, take 293 g of n-heptane as a hydrocarbon dispersion medium, add 0.736 g of a maleic anhydride-modified ethylene-propylene copolymer (Mitsui Chemicals Co., Ltd., High Wax 1105A) as a polymer-based dispersant, and stir. The temperature was raised to 80 ° C. to dissolve the dispersant, and then cooled to 50 ° C.
内容積300mLのビーカーに、水溶性エチレン性不飽和単量体として80.5質量%のアクリル酸水溶液92.0g(1.03モル)をとり、外部より冷却しつつ、20.9質量%の水酸化ナトリウム水溶液147.7gを滴下して75モル%の中和を行った後、増粘剤としてヒドロキシルエチルセルロース0.092g(住友精化株式会社、HECAW-15F)、水溶性ラジカル重合開始剤として過硫酸カリウム0.0736g(0.272ミリモル)、内部架橋剤としてエチレングリコールジグリシジルエーテル0.010g(0.057ミリモル)を加えて溶解し、第1段目の単量体水溶液を調製した。
In a beaker having an internal volume of 300 mL, 92.0 g (1.03 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer was placed, and while being cooled from the outside, 20.9 mass% was added. After adding 147.7 g of an aqueous sodium hydroxide solution to neutralize 75 mol%, 0.092 g of hydroxylethyl cellulose (Sumitomo Seika Co., Ltd., HECAW-15F) as a thickener, as a water-soluble radical polymerization initiator. 0.0736 g (0.272 mmol) of potassium persulfate and 0.010 g (0.057 mmol) of ethylene glycol diglycidyl ether as an internal cross-linking agent were added and dissolved to prepare a first-stage monomer aqueous solution.
そして、上記にて調製した第1段目の単量体水溶液をセパラブルフラスコに添加して、10分間攪拌した後、n-ヘプタン6.62gに界面活性剤としてHLB3のショ糖ステアリン酸エステル(三菱化学フーズ株式会社、リョートーシュガーエステルS-370)0.736gを加熱溶解した界面活性剤溶液を、さらに添加して、撹拌機の回転数を550rpmとして攪拌しながら系内を窒素で十分に置換した後、フラスコを70℃の水浴に浸漬して昇温し、重合を60分間行うことにより、第1段目の重合スラリー液を得た。
Then, the first-stage monomer aqueous solution prepared above was added to the separable flask, and after stirring for 10 minutes, 6.62 g of n-heptane was added as a surfactant to the sucrose stearic acid ester of HLB3. Mitsubishi Chemical Foods Co., Ltd., Ryoto Sugar Ester S-370) 0.736 g of a surfactant solution dissolved by heating is further added, and the inside of the system is sufficiently filled with nitrogen while stirring at a stirring speed of 550 rpm. After the replacement, the flask was immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization was carried out for 60 minutes to obtain a first-stage polymerized slurry solution.
内容積500mLのビーカーに水溶性エチレン性不飽和単量体として80.5質量%のアクリル酸水溶液128.8g(1.44モル)をとり、外部より冷却しつつ、27質量%の水酸化ナトリウム水溶液159.0gを滴下して75モル%の中和を行った後、水溶性ラジカル重合開始剤として過硫酸カリウム0.090g(0.333ミリモル)、内部架橋剤としてエチレングリコールジグリシジルエーテル0.0116g(0.067ミリモル)を加えて溶解し、第2段目の単量体水溶液を調製した。
128.8 g (1.44 mol) of an 80.5 mass% acrylic acid aqueous solution as a water-soluble ethylenically unsaturated monomer was placed in a beaker having an internal volume of 500 mL, and 27 mass% sodium hydroxide was cooled from the outside. After 159.0 g of the aqueous solution was added dropwise to neutralize 75 mol%, 0.090 g (0.333 mmol) of potassium persulfate was used as the water-soluble radical polymerization initiator, and ethylene glycol diglycidyl ether was used as the internal cross-linking agent. 0116 g (0.067 mmol) was added and dissolved to prepare a second-stage monomer aqueous solution.
撹拌機の回転数を1000rpmとして撹拌しながら、上記のセパラブルフラスコ系内を44℃に冷却した後、上記第2段目の単量体水溶液の全量を、第1段目の重合スラリー液に添加して、系内を窒素で30分間置換した後、再度、フラスコを70℃の水浴に浸漬して昇温し、重合反応を60分間行って、含水ゲル状重合体を得た。
After cooling the inside of the separable flask system to 44 ° C. while stirring at a stirring speed of 1000 rpm, the entire amount of the monomer aqueous solution in the second stage is added to the polymerized slurry liquid in the first stage. After adding and replacing the inside of the system with nitrogen for 30 minutes, the flask was again immersed in a water bath at 70 ° C. to raise the temperature, and the polymerization reaction was carried out for 60 minutes to obtain a hydrogel polymer.
重合後、得られた含水ゲル状重合体に、45質量%のジエチレントリアミン5酢酸5ナトリウム水溶液0.589gを攪拌下で添加した。その後、125℃に設定した油浴にフラスコを浸漬し、n-ヘプタンと水との共沸蒸留により、n-ヘプタンを還流しながら、275.8gの水を系外へ抜き出した。その後、フラスコに表面架橋剤として2質量%のエチレングリコールジグリシジルエーテル水溶液4.42g(0.507ミリモル)を添加し、83℃で2時間保持した。
After the polymerization, 0.589 g of a 45% by mass diethylenetriamine-5 sodium acetate aqueous solution was added to the obtained hydrogel polymer under stirring. Then, the flask was immersed in an oil bath set at 125 ° C., and 275.8 g of water was extracted from the system while refluxing n-heptane by azeotropic distillation of n-heptane and water. Then, 4.42 g (0.507 mmol) of a 2% by mass ethylene glycol diglycidyl ether aqueous solution was added to the flask as a surface cross-linking agent, and the flask was kept at 83 ° C. for 2 hours.
その後、n-ヘプタンと水を125℃の油浴で加熱して蒸発させて乾燥させることによって、重合体粒子の乾燥品を得た。この重合体粒子を目開き850μmの篩に通過させ、重合体粒子の質量に対して0.2質量%の非晶質シリカ(オリエンタルシリカズコーポレーション、トクシールNP-S)を重合体粒子と混合し、非晶質シリカを含む吸水性樹脂粒子eを233.0g得た。該吸水性樹脂粒子eの中位粒子径は128μmであった。
Then, n-heptane and water were heated in an oil bath at 125 ° C. to evaporate and dry to obtain a dried product of polymer particles. The polymer particles are passed through a sieve having an opening of 850 μm, and 0.2% by mass of amorphous silica (Oriental Silicas Corporation, Toxile NP-S) with respect to the mass of the polymer particles is mixed with the polymer particles. , 233.0 g of water-absorbent resin particles e containing amorphous silica were obtained. The medium particle size of the water-absorbent resin particles e was 128 μm.
製造例6 試験用吸水コアの製造方法
試験用の吸水コアの製造のため、以下の材料を準備した。
(接着剤)
・ホットメルト接着剤(ヘンケルジャパン株式会社 軟化点96℃ ME-765E)
(試験用吸水コアの基材)
・エアレイド不織布(KNH Enterprise Co.,Ltd.、6190516-1A01、目付量40g/m2)
・エアスルー不織布(Hualong(Nanjing)、目付量45g/m2) Production Example 6 Method for Manufacturing Test Water Absorption Core The following materials were prepared for manufacturing the test water absorption core.
(adhesive)
・ Hot melt adhesive (Henkel Japan Ltd. Softening point 96 ℃ ME-765E)
(Base material of water absorption core for test)
Air-laid non-woven fabric (KNH Enterprise Co., Ltd., 6190516-1A01, basis weight 40 g / m 2 )
・ Air-through non-woven fabric (Hualong (Nanjining), basis weight 45 g / m 2 )
試験用の吸水コアの製造のため、以下の材料を準備した。
(接着剤)
・ホットメルト接着剤(ヘンケルジャパン株式会社 軟化点96℃ ME-765E)
(試験用吸水コアの基材)
・エアレイド不織布(KNH Enterprise Co.,Ltd.、6190516-1A01、目付量40g/m2)
・エアスルー不織布(Hualong(Nanjing)、目付量45g/m2) Production Example 6 Method for Manufacturing Test Water Absorption Core The following materials were prepared for manufacturing the test water absorption core.
(adhesive)
・ Hot melt adhesive (Henkel Japan Ltd. Softening point 96 ℃ ME-765E)
(Base material of water absorption core for test)
Air-laid non-woven fabric (KNH Enterprise Co., Ltd., 6190516-1A01, basis weight 40 g / m 2 )
・ Air-through non-woven fabric (Hualong (Nanjining), basis weight 45 g / m 2 )
エアレイド不織布を10cm×30cmのサイズに2枚分裁断し、エアレイド不織布―1、2とした。エアレイド不織布―1に10cm×30cmのサイズに裁断したエアスルー不織布を載置し、気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用い、1.5gの吸水性樹脂粒子(住友精化株式会社製のアクアキープSA60S、生理食塩水の吸水量60g/g、中位粒子径342μm)を均一に散布させた。
The air-laid non-woven fabric was cut into two pieces to a size of 10 cm × 30 cm to obtain air-laid non-woven fabric-1 and 2. An air-through non-woven fabric cut to a size of 10 cm x 30 cm is placed on the air-laid non-woven fabric-1, and 1.5 g of water-absorbent resin particles (Sumitomo Seika Chemical Co., Ltd.) are used using an airflow type mixer (Padformer manufactured by Otec Co., Ltd.). Aquakeep SA60S manufactured by Co., Ltd., water absorption of physiological saline 60 g / g, medium particle size 342 μm) were uniformly sprayed.
エアレイド不織布―2にホットメルト塗工機(株式会社ハリーズ、ポンプ:Marshal150、テーブル:XA-DT、タンク設定温度:150℃、ホース内設定温度:165℃、ガンヘッド設定温度:170℃)で、全量0.2gのホットメルト接着剤(ヘンケルジャパン株式会社、ME-765E)を、基材に対し長編方向にそって、図3のように10mm間隔で10本塗布した。接着剤の塗布パターンは、スパイラルストライプであった。エアレイド系不織布―2のホットメルトが付着した面を、エアスルー不織布の吸水性樹脂粒子を散布された面に両端を揃えて合わせ、剥離紙で挟み、上下反転させた。その後、剥離紙およびエアレイド不織布―1を取り除いた。
Air-laid non-woven fabric-2 with hot melt coating machine (Henkel Co., Ltd., pump: Marshal150, table: XA-DT, tank set temperature: 150 ° C, hose set temperature: 165 ° C, gun head set temperature: 170 ° C) Ten 0.2 g of hot melt adhesive (Henkel Japan Ltd., ME-765E) was applied to the base material along the length direction as shown in FIG. 3 at 10 mm intervals. The adhesive application pattern was a spiral stripe. The surface of the air-laid non-woven fabric-2 to which the hot melt was attached was aligned with the surface on which the water-absorbent resin particles of the air-through non-woven fabric were sprayed, sandwiched between release papers, and turned upside down. Then, the release paper and the air-laid non-woven fabric-1 were removed.
エアスルー不織布のうち、吸水性樹脂粒子を散布した面とは逆の面に対し、気流型混合装置を用い、4.8gの吸水性樹脂粒子(住友精化株式会社製のアクアキープSA60S、生理食塩水の吸水量60g/g、中位粒子径342μm)を均一に散布した。取り除いていたエアレイド系不織布―1に上記と同様の操作にてホットメルトを0.2g塗布した。エアスルー不織布の上からエアレイド不織布―1を接着剤塗布面が下側になるよう両端を揃えて合わせ、剥離紙で挟み、ラミネート機(株式会社ハシマ、Straight Linear Fussing Press、型式HP-600LFS、110℃、0.1MPa)にてプレスして張り合わせ、試験用の吸水コアを作製した。試験用吸水コアは上から、エアレイド不織布―1、ホットメルト接着剤、吸水性樹脂粒子からなる吸収層、エアスルー不織布、吸水性樹脂粒子からなる吸収層、ホットメルト接着剤、エアレイド不織布―2の順で配置されている。
Of the air-through non-woven fabric, 4.8 g of water-absorbent resin particles (Aquakeep SA60S manufactured by Sumitomo Seika Co., Ltd., physiological salt) was used on the surface opposite to the surface on which the water-absorbent resin particles were sprayed. A water absorption amount of 60 g / g and a medium particle size of 342 μm) were uniformly sprayed. 0.2 g of hot melt was applied to the removed air-laid nonwoven fabric-1 by the same operation as described above. From the top of the air-through non-woven fabric, align both ends of the air-laid non-woven fabric-1 so that the adhesive coating surface is on the lower side, sandwich it with release paper, and use a laminating machine (Hashima Co., Ltd., Straight Liner Fusion Press, model HP-600LFS, 110 ° C.). , 0.1 MPa) and pasted together to prepare a water-absorbing core for testing. From the top, the test water-absorbing core is in the order of air-laid non-woven fabric-1, hot melt adhesive, absorbent layer made of water-absorbent resin particles, air-through non-woven fabric, absorbent layer made of water-absorbent resin particles, hot-melt adhesive, and air-laid non-woven fabric-2. It is arranged in.
[試験用の吸収性物品の作製]
実施例1
(補助シートの作製)
目付量16g/m2のティッシュを10cm×30cmのサイズに2枚分裁断し、補助シートの上部シート基材、下部シート基材とした。下部シート基材のロール内側面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した後、速やかに気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用いて、製造例1にて作製した吸水性樹脂粒子a1.1gを均一に散布した。上部シート基材に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した。上部シート基材の接着剤を塗布した面を下部シート基材の吸水性樹脂粒子が散布された面に両端を揃えて合わせ重ね、面全体を接着させ、補助シート用吸水シートを得た。 [Preparation of absorbent articles for testing]
Example 1
(Preparation of auxiliary sheet)
Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 10 cm × 30 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (3M Spray Glue 77, manufactured by 3M Japan Ltd.) to the inner surface of the roll of the lower sheet base material, a flow-type mixer (pad former, manufactured by Otec Co., Ltd.) was promptly applied. Was used to uniformly spray 1.1 g of the water-absorbent resin particles a1 prepared in Production Example 1. 0.3 g of an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to the upper sheet base material. The surface coated with the adhesive of the upper sheet base material was overlapped with the surface on which the water-absorbent resin particles of the lower sheet base material were sprayed so that both ends were aligned, and the entire surface was adhered to obtain a water-absorbent sheet for an auxiliary sheet.
実施例1
(補助シートの作製)
目付量16g/m2のティッシュを10cm×30cmのサイズに2枚分裁断し、補助シートの上部シート基材、下部シート基材とした。下部シート基材のロール内側面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した後、速やかに気流型混合装置(有限会社オーテック社製、パッドフォーマー)を用いて、製造例1にて作製した吸水性樹脂粒子a1.1gを均一に散布した。上部シート基材に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した。上部シート基材の接着剤を塗布した面を下部シート基材の吸水性樹脂粒子が散布された面に両端を揃えて合わせ重ね、面全体を接着させ、補助シート用吸水シートを得た。 [Preparation of absorbent articles for testing]
Example 1
(Preparation of auxiliary sheet)
Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 10 cm × 30 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (
(試験用の吸収性物品の作製)
得られた補助シート用吸水シートを3cm×30cmのサイズに2枚分裁断し補助シートとした。補助シートの片面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.1g均一に塗布した。補助シートの接着剤を塗布した面を下向きにし、補助シートを、製造例6にて作製した試験用吸水コアのエアレイド不織布―1の面上に、該吸水コア主面の短手方向の両端部に、吸水コアの長手方向に沿ってはり合わせて、接着した。これにより、実施例1の試験用吸収性物品を得た。 (Preparation of absorbent articles for testing)
The obtained water-absorbing sheet for auxiliary sheet was cut into two pieces having a size of 3 cm × 30 cm to obtain an auxiliary sheet. 0.1 g of an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to one side of the auxiliary sheet. With the adhesive-coated side of the auxiliary sheet facing down, the auxiliary sheet is placed on the surface of the air-laid non-woven fabric-1 of the test water-absorbing core produced in Production Example 6 at both ends in the lateral direction of the main surface of the water-absorbing core. Was glued together along the longitudinal direction of the water absorption core. As a result, a test absorbent article of Example 1 was obtained.
得られた補助シート用吸水シートを3cm×30cmのサイズに2枚分裁断し補助シートとした。補助シートの片面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.1g均一に塗布した。補助シートの接着剤を塗布した面を下向きにし、補助シートを、製造例6にて作製した試験用吸水コアのエアレイド不織布―1の面上に、該吸水コア主面の短手方向の両端部に、吸水コアの長手方向に沿ってはり合わせて、接着した。これにより、実施例1の試験用吸収性物品を得た。 (Preparation of absorbent articles for testing)
The obtained water-absorbing sheet for auxiliary sheet was cut into two pieces having a size of 3 cm × 30 cm to obtain an auxiliary sheet. 0.1 g of an adhesive (
実施例1における補助シートは、ティッシュ、接着剤、吸水性樹脂粒子からなる膨潤層、接着剤及びティッシュがこの順に配置されている。実施例1における膨潤層は、吸水コアの短手方向の両端部上に、吸水コアの長手方向に沿って設けられている。実施例1の試験用の吸収性物品において、補助シートは、装着した際の使用者側(液体が侵入する側)に配置されている。実施例1の試験用の吸収性物品は、図4A(上面図)及びB(試験用吸収性物品の長手方向の一方からみた側面図)に示す構成と同様の構成を有する。
In the auxiliary sheet of Example 1, a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order. The swollen layers in Example 1 are provided on both ends of the water absorbing core in the lateral direction along the longitudinal direction of the water absorbing core. In the test absorbent article of Example 1, the auxiliary sheet is arranged on the user side (the side where the liquid invades) when it is attached. The test absorbent article of Example 1 has the same configuration as shown in FIGS. 4A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
実施例2
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例2にて作製した吸水性樹脂粒子bに変更したこと以外は実施例1と同様にして、実施例2の試験用吸収性物品を得た。 Example 2
The test-absorbent article of Example 2 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles b produced in Production Example 2. Got
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例2にて作製した吸水性樹脂粒子bに変更したこと以外は実施例1と同様にして、実施例2の試験用吸収性物品を得た。 Example 2
The test-absorbent article of Example 2 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles b produced in Production Example 2. Got
実施例3
補助シート用吸水シートの作製に用いた吸水性樹脂粒子の使用量を0.6gに変更したこと以外は実施例1と同様にして実施例3の試験用吸収性物品を得た。 Example 3
The test-absorbent article of Example 3 was obtained in the same manner as in Example 1 except that the amount of the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet was changed to 0.6 g.
補助シート用吸水シートの作製に用いた吸水性樹脂粒子の使用量を0.6gに変更したこと以外は実施例1と同様にして実施例3の試験用吸収性物品を得た。 Example 3
The test-absorbent article of Example 3 was obtained in the same manner as in Example 1 except that the amount of the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet was changed to 0.6 g.
実施例4
補助シートとして裁断するサイズを4cm×30cmに変更したこと以外は実施例1と同様にして、実施例4の試験用吸収性物品を得た。 Example 4
The test absorbent article of Example 4 was obtained in the same manner as in Example 1 except that the size to be cut as an auxiliary sheet was changed to 4 cm × 30 cm.
補助シートとして裁断するサイズを4cm×30cmに変更したこと以外は実施例1と同様にして、実施例4の試験用吸収性物品を得た。 Example 4
The test absorbent article of Example 4 was obtained in the same manner as in Example 1 except that the size to be cut as an auxiliary sheet was changed to 4 cm × 30 cm.
実施例5
補助シートとして裁断するサイズを1cm×30cmに変更したこと以外は実施例1と同様にして実施例5の試験用吸収性物品を得た。 Example 5
The test absorbent article of Example 5 was obtained in the same manner as in Example 1 except that the size to be cut as an auxiliary sheet was changed to 1 cm × 30 cm.
補助シートとして裁断するサイズを1cm×30cmに変更したこと以外は実施例1と同様にして実施例5の試験用吸収性物品を得た。 Example 5
The test absorbent article of Example 5 was obtained in the same manner as in Example 1 except that the size to be cut as an auxiliary sheet was changed to 1 cm × 30 cm.
実施例6
補助シートの設置個所をエアレイド不織布―2の面に変更したこと以外は実施例1と同様にして実施例6の試験用の吸収性物品を得た。実施例6の試験用の吸収性物品は、吸水コアと、補助シートとを備えている。 Example 6
An absorbent article for testing in Example 6 was obtained in the same manner as in Example 1 except that the installation location of the auxiliary sheet was changed to the surface of the air-laid nonwoven fabric-2. The test absorbent article of Example 6 comprises a water absorption core and an auxiliary sheet.
補助シートの設置個所をエアレイド不織布―2の面に変更したこと以外は実施例1と同様にして実施例6の試験用の吸収性物品を得た。実施例6の試験用の吸収性物品は、吸水コアと、補助シートとを備えている。 Example 6
An absorbent article for testing in Example 6 was obtained in the same manner as in Example 1 except that the installation location of the auxiliary sheet was changed to the surface of the air-laid nonwoven fabric-2. The test absorbent article of Example 6 comprises a water absorption core and an auxiliary sheet.
実施例6における補助シートは、ティッシュ、接着剤、吸水性樹脂粒子からなる膨潤層、接着剤及びティッシュがこの順に配置されている。実施例6における膨潤層は、吸水コアの短手方向の両端部上に、吸水コアの長手方向に沿って設けられている。実施例6の試験用の吸収性物品において、補助シートは、装着した際の使用者側(液体が侵入する側)とは反対側に配置されている。実施例6の試験用の吸収性物品は、図7A(上面図)及びB(試験用吸収性物品の長手方向の一方からみた側面図)に示す構成と同様の構成を有する。
In the auxiliary sheet of Example 6, a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order. The swollen layers in Example 6 are provided on both ends of the water absorbing core in the lateral direction along the longitudinal direction of the water absorbing core. In the test absorbent article of Example 6, the auxiliary sheet is arranged on the side opposite to the user side (the side where the liquid invades) when it is attached. The test absorbent article of Example 6 has the same configuration as shown in FIGS. 7A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
実施例7
目付量16g/m2のティッシュを10cm×30cmのサイズに2枚分裁断し、補助シートの上部シート基材、下部シート基材とした。下部シート基材のロール内側面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した後、下部シート基材中央の短辺4cm、長辺30cmの長方形状の領域以外の領域に、製造例1にて作製した吸水性樹脂粒子a0.7gを均一に散布した。上部シート基材に接着剤を塗布し、接着剤を塗布した面を下部シート基材の吸水性樹脂粒子が散布された面に両端を揃えて合わせ重ねて、面全体を接着させ、補助シートを得た。 Example 7
Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 10 cm × 30 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) to the inner surface of the roll of the lower sheet base material, a rectangular shape with a short side of 4 cm and a long side of 30 cm in the center of the lower sheet base material. 0.7 g of the water-absorbent resin particles a produced in Production Example 1 was uniformly sprayed on a region other than the region. An adhesive is applied to the upper sheet base material, and the surface to which the adhesive is applied is overlapped with the surface on which the water-absorbent resin particles of the lower sheet base material are sprayed so that both ends are aligned, and the entire surface is adhered to form an auxiliary sheet. Obtained.
目付量16g/m2のティッシュを10cm×30cmのサイズに2枚分裁断し、補助シートの上部シート基材、下部シート基材とした。下部シート基材のロール内側面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した後、下部シート基材中央の短辺4cm、長辺30cmの長方形状の領域以外の領域に、製造例1にて作製した吸水性樹脂粒子a0.7gを均一に散布した。上部シート基材に接着剤を塗布し、接着剤を塗布した面を下部シート基材の吸水性樹脂粒子が散布された面に両端を揃えて合わせ重ねて、面全体を接着させ、補助シートを得た。 Example 7
Two pieces of tissue having a basis weight of 16 g / m 2 were cut into a size of 10 cm × 30 cm to obtain an upper sheet base material and a lower sheet base material of the auxiliary sheet. After uniformly applying 0.3 g of adhesive (
得られた補助シートの片面に接着剤(スリーエムジャパン株式会社製、3Mスプレーのり77)を0.3g均一に塗布した。補助シートの接着剤を塗布した面を下向きにし、補助シートを、製造例6にて作製した試験用吸水コアのエアレイド不織布―1の全面に貼り付けた。これにより、実施例7の試験用吸収性物品を得た。
0.3 g of an adhesive (3M spray glue 77 manufactured by 3M Japan Ltd.) was uniformly applied to one side of the obtained auxiliary sheet. The adhesive-coated side of the auxiliary sheet was turned downward, and the auxiliary sheet was attached to the entire surface of the air-laid nonwoven fabric-1 of the test water-absorbing core produced in Production Example 6. As a result, a test absorbent article of Example 7 was obtained.
実施例7の試験用吸収性物品において、補助シートは、ティッシュをシート基材とし、10cm×30cmの大きさを有し、その短手方向の両端の3cm×30cmの範囲に膨潤層が設けられている。実施例7における補助シート中央の4cm×30cmの範囲には、シート基材としてのティッシュ及び接着剤のみが配置されている。
In the test absorbent article of Example 7, the auxiliary sheet is made of tissue as a sheet base material, has a size of 10 cm × 30 cm, and swelling layers are provided in a range of 3 cm × 30 cm at both ends in the lateral direction thereof. ing. Only the tissue and the adhesive as the sheet base material are arranged in the range of 4 cm × 30 cm in the center of the auxiliary sheet in Example 7.
実施例7における補助シートは、ティッシュ、接着剤、吸水性樹脂粒子からなる膨潤層、接着剤、及びティッシュがこの順に配置されている。実施例7における膨潤層は、吸水コアの短手方向の両端部上に、吸水コアの長手方向に沿って設けられている。実施例7の試験用の吸収性物品において、補助シートは、装着した際の使用者側(液体が侵入する側)とは反対側に配置されている。実施例7の試験用の吸収性物品は、図5A(上面図)及びB(試験用吸収性物品の長手方向の一方からみた側面図)に示す構成と同様の構成を有する。
In the auxiliary sheet of Example 7, a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order. The swollen layers in Example 7 are provided on both ends of the water absorbing core in the lateral direction along the longitudinal direction of the water absorbing core. In the test absorbent article of Example 7, the auxiliary sheet is arranged on the side opposite to the user side (the side where the liquid invades) when it is attached. The test absorbent article of Example 7 has the same configuration as shown in FIGS. 5A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
実施例8
補助シート用の基材をスパンレース不織布(株式会社クラレ、70%レーション;20%PET;10%PP/PE、目付量35g/m2)に変更したこと以外は実施例1と同様にして、実施例8の試験用吸収性物品を得た。 Example 8
The same as in Example 1 except that the base material for the auxiliary sheet was changed to a spunlace non-woven fabric (Kuraray Co., Ltd., 70% ration; 20% PET; 10% PP / PE, basis weight 35 g / m 2). A test absorbent article of Example 8 was obtained.
補助シート用の基材をスパンレース不織布(株式会社クラレ、70%レーション;20%PET;10%PP/PE、目付量35g/m2)に変更したこと以外は実施例1と同様にして、実施例8の試験用吸収性物品を得た。 Example 8
The same as in Example 1 except that the base material for the auxiliary sheet was changed to a spunlace non-woven fabric (Kuraray Co., Ltd., 70% ration; 20% PET; 10% PP / PE, basis weight 35 g / m 2). A test absorbent article of Example 8 was obtained.
実施例9
補助シート用の基材をスパンボンド不織布(Toray Polytech(Nantong)Co.,Ltd.、LIVSEN親水 SSSS、目付量17g/m2)に変更したこと以外は実施例1と同様にして、実施例9の試験用吸収性物品を得た。 Example 9
Example 9 in the same manner as in Example 1 except that the base material for the auxiliary sheet was changed to a spunbonded non-woven fabric (Toray Polytech (Nantong) Co., Ltd., LIVESEN hydrophilic SSSS, basis weight 17 g / m 2). A test absorbent article was obtained.
補助シート用の基材をスパンボンド不織布(Toray Polytech(Nantong)Co.,Ltd.、LIVSEN親水 SSSS、目付量17g/m2)に変更したこと以外は実施例1と同様にして、実施例9の試験用吸収性物品を得た。 Example 9
Example 9 in the same manner as in Example 1 except that the base material for the auxiliary sheet was changed to a spunbonded non-woven fabric (Toray Polytech (Nantong) Co., Ltd., LIVESEN hydrophilic SSSS, basis weight 17 g / m 2). A test absorbent article was obtained.
実施例10
実施例1に記載の方法と同様の方法で補助シート用吸水シート(短辺10cm、長辺30cmの大きさを有する)を準備した。前記吸水シート中央部に位置する、短辺4cm、長辺24cmの大きさを有する長方形状の領域を裁断した。これにより得られた中央部の所定領域が除去された前記吸水シートを、実施例10の吸収性物品作製用の補助シートとした。当該補助シートをエアレイド不織布―1全面に接着するように変更したこと以外は実施例1と同様にして実施例10の試験用吸収性物品を得た。 Example 10
A water absorption sheet for an auxiliary sheet (having a size of 10 cm on the short side and 30 cm on the long side) was prepared by the same method as that described in Example 1. A rectangular region having a short side of 4 cm and a long side of 24 cm, located at the center of the water absorption sheet, was cut. The water-absorbing sheet from which the predetermined region in the central portion was removed was used as an auxiliary sheet for producing an absorbent article of Example 10. The test absorbent article of Example 10 was obtained in the same manner as in Example 1 except that the auxiliary sheet was changed so as to adhere to the entire surface of the air-laid nonwoven fabric-1.
実施例1に記載の方法と同様の方法で補助シート用吸水シート(短辺10cm、長辺30cmの大きさを有する)を準備した。前記吸水シート中央部に位置する、短辺4cm、長辺24cmの大きさを有する長方形状の領域を裁断した。これにより得られた中央部の所定領域が除去された前記吸水シートを、実施例10の吸収性物品作製用の補助シートとした。当該補助シートをエアレイド不織布―1全面に接着するように変更したこと以外は実施例1と同様にして実施例10の試験用吸収性物品を得た。 Example 10
A water absorption sheet for an auxiliary sheet (having a size of 10 cm on the short side and 30 cm on the long side) was prepared by the same method as that described in Example 1. A rectangular region having a short side of 4 cm and a long side of 24 cm, located at the center of the water absorption sheet, was cut. The water-absorbing sheet from which the predetermined region in the central portion was removed was used as an auxiliary sheet for producing an absorbent article of Example 10. The test absorbent article of Example 10 was obtained in the same manner as in Example 1 except that the auxiliary sheet was changed so as to adhere to the entire surface of the air-laid nonwoven fabric-1.
実施例10における補助シートは、ティッシュ、接着剤、吸水性樹脂粒子からなる膨潤層、接着剤及びティッシュがこの順に配置されている。実施例10における膨潤層は、吸水コア上の外周(縁部)に沿って設けられている。実施例10の試験用の吸収性物品において、補助シートは、装着した際の使用者側(液体が侵入する側)に配置されている。実施例10の試験用の吸収性物品は、図6A(上面図)及びB(試験用の吸収性物品の長手方向の一方からみた側面図)に示す構成と同様の構成を有する。
In the auxiliary sheet of Example 10, a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order. The swollen layer in Example 10 is provided along the outer circumference (edge) on the water absorption core. In the test absorbent article of Example 10, the auxiliary sheet is arranged on the user side (the side where the liquid invades) when it is attached. The test absorbent article of Example 10 has the same configuration as shown in FIGS. 6A (top view) and B (side view from one side in the longitudinal direction of the test absorbent article).
比較例1
補助シートを用いずに製造例6にて作製した吸水コアのみを比較例1の試験用吸収性物品とした。比較例1の試験用吸収性物品は、吸水コアのみを備えており、図8A(上面図)及びB(試験用の吸収性物品の長手方向の一方からみた側面図)に示す構成と同様の構成を有している。 Comparative Example 1
Only the water-absorbing core produced in Production Example 6 without using the auxiliary sheet was used as the test-absorbing article of Comparative Example 1. The test-absorbent article of Comparative Example 1 includes only a water-absorbing core, and has the same configuration as that shown in FIGS. 8A (top view) and B (side view from one side in the longitudinal direction of the test-absorbent article). It has a structure.
補助シートを用いずに製造例6にて作製した吸水コアのみを比較例1の試験用吸収性物品とした。比較例1の試験用吸収性物品は、吸水コアのみを備えており、図8A(上面図)及びB(試験用の吸収性物品の長手方向の一方からみた側面図)に示す構成と同様の構成を有している。 Comparative Example 1
Only the water-absorbing core produced in Production Example 6 without using the auxiliary sheet was used as the test-absorbing article of Comparative Example 1. The test-absorbent article of Comparative Example 1 includes only a water-absorbing core, and has the same configuration as that shown in FIGS. 8A (top view) and B (side view from one side in the longitudinal direction of the test-absorbent article). It has a structure.
比較例2
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例3にて作製した吸水性樹脂粒子cに変更したこと以外は実施例1と同様にして、比較例2の試験用吸収性物品を得た。 Comparative Example 2
The test-absorbent article of Comparative Example 2 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles c produced in Production Example 3. Got
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例3にて作製した吸水性樹脂粒子cに変更したこと以外は実施例1と同様にして、比較例2の試験用吸収性物品を得た。 Comparative Example 2
The test-absorbent article of Comparative Example 2 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles c produced in Production Example 3. Got
比較例3
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例4にて作製した吸水性樹脂粒子dに変更したこと以外は実施例1と同様にして、比較例3の試験用吸収性物品を得た。 Comparative Example 3
The test-absorbent article of Comparative Example 3 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles d produced in Production Example 4. Got
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例4にて作製した吸水性樹脂粒子dに変更したこと以外は実施例1と同様にして、比較例3の試験用吸収性物品を得た。 Comparative Example 3
The test-absorbent article of Comparative Example 3 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles d produced in Production Example 4. Got
比較例4
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例5にて作製した吸水性樹脂粒子eに変更したこと以外は実施例1と同様にして、比較例4の試験用吸収性物品を得た。 Comparative Example 4
The test-absorbent article of Comparative Example 4 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles e produced in Production Example 5. Got
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を製造例5にて作製した吸水性樹脂粒子eに変更したこと以外は実施例1と同様にして、比較例4の試験用吸収性物品を得た。 Comparative Example 4
The test-absorbent article of Comparative Example 4 in the same manner as in Example 1 except that the water-absorbent resin particles used for producing the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles e produced in Production Example 5. Got
比較例5
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を日本販売の大王製紙株式会社の生理用ナプキン「エリス 朝まで超安心 CLINICS」(2017年購入)から採取した吸水性樹脂粒子fに変更したこと以外は実施例1と同様にして、比較例5の試験用吸収性物品を得た。 Comparative Example 5
The water-absorbent resin particles used to prepare the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles f collected from the sanitary napkin "Eris Morning Super Safe CLIINS" (purchased in 2017) of Daio Paper Corporation sold in Japan. Except for the above, a test absorbent article of Comparative Example 5 was obtained in the same manner as in Example 1.
補助シート用吸水シートの作製に用いた吸水性樹脂粒子を日本販売の大王製紙株式会社の生理用ナプキン「エリス 朝まで超安心 CLINICS」(2017年購入)から採取した吸水性樹脂粒子fに変更したこと以外は実施例1と同様にして、比較例5の試験用吸収性物品を得た。 Comparative Example 5
The water-absorbent resin particles used to prepare the water-absorbent sheet for the auxiliary sheet were changed to the water-absorbent resin particles f collected from the sanitary napkin "Eris Morning Super Safe CLIINS" (purchased in 2017) of Daio Paper Corporation sold in Japan. Except for the above, a test absorbent article of Comparative Example 5 was obtained in the same manner as in Example 1.
比較例6
補助シートとして裁断するサイズを3cm×10cmとし、補助シートの長辺をエアレイド不織布―1の面上に、吸水コアの短辺に沿ってはりあわせて接着するように変更したこと以外は実施例1と同様にして、比較例6の試験用吸収性物品を得た。 Comparative Example 6
Example 1 except that the size to be cut as an auxiliary sheet is set to 3 cm × 10 cm, and the long side of the auxiliary sheet is changed so as to be adhered to the surface of the air-laid non-woven fabric-1 along the short side of the water absorption core. In the same manner as above, a test absorbent article of Comparative Example 6 was obtained.
補助シートとして裁断するサイズを3cm×10cmとし、補助シートの長辺をエアレイド不織布―1の面上に、吸水コアの短辺に沿ってはりあわせて接着するように変更したこと以外は実施例1と同様にして、比較例6の試験用吸収性物品を得た。 Comparative Example 6
Example 1 except that the size to be cut as an auxiliary sheet is set to 3 cm × 10 cm, and the long side of the auxiliary sheet is changed so as to be adhered to the surface of the air-laid non-woven fabric-1 along the short side of the water absorption core. In the same manner as above, a test absorbent article of Comparative Example 6 was obtained.
比較例6における補助シートは、ティッシュ、接着剤、吸水性樹脂粒子からなる膨潤層、接着剤及びティッシュがこの順に配置されている。比較例6における膨潤層は、吸水コアの長手方向の両端部に、吸水コアの短手方向に沿って設けられている。比較例6の試験用の吸収性物品において、補助シートは、装着した際の使用者側(液体が侵入する側)に配置されている。比較例6の試験用の吸収性物品は、図9A(上面図)及びB(長手方向の一方からみた側面図)に示す構成と同様の構成を有している。
In the auxiliary sheet in Comparative Example 6, a tissue, an adhesive, a swelling layer made of water-absorbent resin particles, an adhesive, and a tissue are arranged in this order. The swollen layers in Comparative Example 6 are provided at both ends in the longitudinal direction of the water absorption core along the lateral direction of the water absorption core. In the test absorbent article of Comparative Example 6, the auxiliary sheet is arranged on the user side (the side where the liquid invades) when it is attached. The test absorbent article of Comparative Example 6 has a configuration similar to that shown in FIGS. 9A (top view) and B (side view seen from one side in the longitudinal direction).
以下、吸水性樹脂粒子の諸性能の測定及び液体漏れ試験については特に記載がない場合は、温度25±2℃、湿度50±10%の環境下で行なわれた。
Hereinafter, unless otherwise specified, the measurement of various performances of the water-absorbent resin particles and the liquid leakage test were carried out in an environment of a temperature of 25 ± 2 ° C. and a humidity of 50 ± 10%.
<中位粒子径>
吸水性樹脂粒子の上述の中位粒子径は下記手順により測定した。すなわち、JIS標準篩を上から、目開き600μmの篩、目開き500μmの篩、目開き425μmの篩、目開き300μmの篩、目開き250μmの篩、目開き180μmの篩、目開き150μmの篩、及び、受け皿の順に組み合わせた。組み合わせた最上の篩に、吸水性樹脂粒子50gを入れ、ロータップ式振とう器(株式会社飯田製作所製)を用いてJIS Z 8815(1994)に準じて分級した。分級後、各篩上に残った粒子の質量を全量に対する質量百分率として算出し粒度分布を求めた。この粒度分布に関して粒子径の大きい方から順に篩上を積算することにより、篩の目開きと篩上に残った粒子の質量百分率の積算値との関係を対数確率紙にプロットした。確率紙上のプロットを直線で結ぶことにより、積算質量百分率50質量%に相当する粒子径を中位粒子径として得た。 <Medium particle size>
The above-mentioned medium particle size of the water-absorbent resin particles was measured by the following procedure. That is, from the top of the JIS standard sieve, a sieve with a mesh size of 600 μm, a sieve with a mesh size of 500 μm, a sieve with a mesh size of 425 μm, a sieve with a mesh size of 300 μm, a sieve with a mesh size of 250 μm, a sieve with a mesh size of 180 μm, and a sieve with a mesh size of 150 μm. , And the saucer in that order. 50 g of water-absorbent resin particles were placed in the best combined sieve, and the mixture was classified according to JIS Z 8815 (1994) using a low-tap shaker (manufactured by Iida Seisakusho Co., Ltd.). After classification, the mass of the particles remaining on each sieve was calculated as a mass percentage with respect to the total amount, and the particle size distribution was obtained. The relationship between the mesh size of the sieve and the integrated value of the mass percentage of the particles remaining on the sieve was plotted on a logarithmic probability paper by integrating on the sieve in order from the one having the largest particle size with respect to this particle size distribution. By connecting the plots on the probability paper with a straight line, the particle size corresponding to the cumulative mass percentage of 50% by mass was obtained as the medium particle size.
吸水性樹脂粒子の上述の中位粒子径は下記手順により測定した。すなわち、JIS標準篩を上から、目開き600μmの篩、目開き500μmの篩、目開き425μmの篩、目開き300μmの篩、目開き250μmの篩、目開き180μmの篩、目開き150μmの篩、及び、受け皿の順に組み合わせた。組み合わせた最上の篩に、吸水性樹脂粒子50gを入れ、ロータップ式振とう器(株式会社飯田製作所製)を用いてJIS Z 8815(1994)に準じて分級した。分級後、各篩上に残った粒子の質量を全量に対する質量百分率として算出し粒度分布を求めた。この粒度分布に関して粒子径の大きい方から順に篩上を積算することにより、篩の目開きと篩上に残った粒子の質量百分率の積算値との関係を対数確率紙にプロットした。確率紙上のプロットを直線で結ぶことにより、積算質量百分率50質量%に相当する粒子径を中位粒子径として得た。 <Medium particle size>
The above-mentioned medium particle size of the water-absorbent resin particles was measured by the following procedure. That is, from the top of the JIS standard sieve, a sieve with a mesh size of 600 μm, a sieve with a mesh size of 500 μm, a sieve with a mesh size of 425 μm, a sieve with a mesh size of 300 μm, a sieve with a mesh size of 250 μm, a sieve with a mesh size of 180 μm, and a sieve with a mesh size of 150 μm. , And the saucer in that order. 50 g of water-absorbent resin particles were placed in the best combined sieve, and the mixture was classified according to JIS Z 8815 (1994) using a low-tap shaker (manufactured by Iida Seisakusho Co., Ltd.). After classification, the mass of the particles remaining on each sieve was calculated as a mass percentage with respect to the total amount, and the particle size distribution was obtained. The relationship between the mesh size of the sieve and the integrated value of the mass percentage of the particles remaining on the sieve was plotted on a logarithmic probability paper by integrating on the sieve in order from the one having the largest particle size with respect to this particle size distribution. By connecting the plots on the probability paper with a straight line, the particle size corresponding to the cumulative mass percentage of 50% by mass was obtained as the medium particle size.
<吸水量(生理食塩水)>
容量500mLのビーカーに、生理食塩水500gを量り取った。そこに、スターラーバー(8mmφ×30mm、リング無し)を用い600rpmで撹拌しながら、吸水性樹脂粒子2.0gを、ママコが発生しないように分散させた。その状態で60分間放置し、吸水性樹脂粒子を十分に膨潤させた。続いてビーカー中の内容物を、目開き75μm標準篩(質量Ma(g))を用いてろ過した。篩を水平に対して約30度の傾斜角となるように傾けた状態で30分間放置することにより、篩上の膨潤ゲルから余剰の水分をろ別した。その後、篩と篩上の膨潤ゲルとの合計質量Mb(g)を測定した。以下の式により、生理食塩水の吸水量を求めた。
生理食塩水の吸水量[g/g]=(Mb-Ma)/2.0 <Water absorption (saline)>
500 g of physiological saline was weighed in a beaker having a capacity of 500 mL. There, 2.0 g of water-absorbent resin particles were dispersed so as not to generate mamaco while stirring at 600 rpm using a stirrer bar (8 mmφ × 30 mm, without ring). It was left in that state for 60 minutes to sufficiently swell the water-absorbent resin particles. Subsequently, the contents in the beaker were filtered using a standard sieve having a mesh size of 75 μm (mass Ma (g)). Excess water was filtered off from the swollen gel on the sieve by allowing the sieve to be tilted at an inclination angle of about 30 degrees with respect to the horizontal for 30 minutes. Then, the total mass Mb (g) of the sieve and the swollen gel on the sieve was measured. The amount of water absorption of physiological saline was determined by the following formula.
Water absorption of saline [g / g] = (Mb-Ma) /2.0
容量500mLのビーカーに、生理食塩水500gを量り取った。そこに、スターラーバー(8mmφ×30mm、リング無し)を用い600rpmで撹拌しながら、吸水性樹脂粒子2.0gを、ママコが発生しないように分散させた。その状態で60分間放置し、吸水性樹脂粒子を十分に膨潤させた。続いてビーカー中の内容物を、目開き75μm標準篩(質量Ma(g))を用いてろ過した。篩を水平に対して約30度の傾斜角となるように傾けた状態で30分間放置することにより、篩上の膨潤ゲルから余剰の水分をろ別した。その後、篩と篩上の膨潤ゲルとの合計質量Mb(g)を測定した。以下の式により、生理食塩水の吸水量を求めた。
生理食塩水の吸水量[g/g]=(Mb-Ma)/2.0 <Water absorption (saline)>
500 g of physiological saline was weighed in a beaker having a capacity of 500 mL. There, 2.0 g of water-absorbent resin particles were dispersed so as not to generate mamaco while stirring at 600 rpm using a stirrer bar (8 mmφ × 30 mm, without ring). It was left in that state for 60 minutes to sufficiently swell the water-absorbent resin particles. Subsequently, the contents in the beaker were filtered using a standard sieve having a mesh size of 75 μm (mass Ma (g)). Excess water was filtered off from the swollen gel on the sieve by allowing the sieve to be tilted at an inclination angle of about 30 degrees with respect to the horizontal for 30 minutes. Then, the total mass Mb (g) of the sieve and the swollen gel on the sieve was measured. The amount of water absorption of physiological saline was determined by the following formula.
Water absorption of saline [g / g] = (Mb-Ma) /2.0
[吸水速度(Vortex法)]
吸水性樹脂粒子の生理食塩水に対する吸水速度を、Vortex法に基づき下記手順で測定した。まず、恒温水槽にて25±0.2℃の温度に調整した生理食塩水50±0.1gを容量100mLのビーカーに量りとった。次に、マグネチックスターラーバー(8mmφ×30mm、リング無し)を用いて600rpmで撹拌することにより渦を発生させた。吸水性樹脂粒子2.0±0.002gを生理食塩水中に一度に添加した。吸水性樹脂粒子の添加後から、液面の渦が収束する時点までの時間[秒]を測定し、当該時間を吸水性樹脂粒子の吸水速度として記録した。 [Water absorption rate (Vortex method)]
The water absorption rate of the water-absorbent resin particles with respect to physiological saline was measured by the following procedure based on the Vortex method. First, 50 ± 0.1 g of physiological saline adjusted to a temperature of 25 ± 0.2 ° C. in a constant temperature water tank was weighed in a beaker having a capacity of 100 mL. Next, a vortex was generated by stirring at 600 rpm using a magnetic stirrer bar (8 mmφ × 30 mm, without ring). 2.0 ± 0.002 g of water-absorbent resin particles were added to physiological saline at one time. The time [seconds] from the addition of the water-absorbent resin particles to the time when the vortex on the liquid surface converged was measured, and the time was recorded as the water absorption rate of the water-absorbent resin particles.
吸水性樹脂粒子の生理食塩水に対する吸水速度を、Vortex法に基づき下記手順で測定した。まず、恒温水槽にて25±0.2℃の温度に調整した生理食塩水50±0.1gを容量100mLのビーカーに量りとった。次に、マグネチックスターラーバー(8mmφ×30mm、リング無し)を用いて600rpmで撹拌することにより渦を発生させた。吸水性樹脂粒子2.0±0.002gを生理食塩水中に一度に添加した。吸水性樹脂粒子の添加後から、液面の渦が収束する時点までの時間[秒]を測定し、当該時間を吸水性樹脂粒子の吸水速度として記録した。 [Water absorption rate (Vortex method)]
The water absorption rate of the water-absorbent resin particles with respect to physiological saline was measured by the following procedure based on the Vortex method. First, 50 ± 0.1 g of physiological saline adjusted to a temperature of 25 ± 0.2 ° C. in a constant temperature water tank was weighed in a beaker having a capacity of 100 mL. Next, a vortex was generated by stirring at 600 rpm using a magnetic stirrer bar (8 mmφ × 30 mm, without ring). 2.0 ± 0.002 g of water-absorbent resin particles were added to physiological saline at one time. The time [seconds] from the addition of the water-absorbent resin particles to the time when the vortex on the liquid surface converged was measured, and the time was recorded as the water absorption rate of the water-absorbent resin particles.
<吸水性樹脂粒子の膨潤力の測定>
図10に示す装置を用いて、吸水性樹脂粒子の膨潤力試験を行った。膨潤力試験は以下に示す手順で実施した。吸水性樹脂粒子の膨潤力の測定には、株式会社島津製作所製 小型卓上試験機EZ-Testを用いた。 <Measurement of swelling power of water-absorbent resin particles>
The swelling power test of the water-absorbent resin particles was performed using the apparatus shown in FIG. The swelling power test was carried out according to the procedure shown below. A small tabletop tester EZ-Test manufactured by Shimadzu Corporation was used to measure the swelling power of the water-absorbent resin particles.
図10に示す装置を用いて、吸水性樹脂粒子の膨潤力試験を行った。膨潤力試験は以下に示す手順で実施した。吸水性樹脂粒子の膨潤力の測定には、株式会社島津製作所製 小型卓上試験機EZ-Testを用いた。 <Measurement of swelling power of water-absorbent resin particles>
The swelling power test of the water-absorbent resin particles was performed using the apparatus shown in FIG. The swelling power test was carried out according to the procedure shown below. A small tabletop tester EZ-Test manufactured by Shimadzu Corporation was used to measure the swelling power of the water-absorbent resin particles.
(1)両端に開口部を有し、その一方の開口部にナイロン(登録商標)メッシュ71(255メッシュ)が装着された内径20mm(底面積3.14cm2)かつ高さ50mmのアクリル樹脂製シリンダー72を用意した。
(2)上記ナイロン(登録商標)メッシュ71が装着された側の開口部が下になる向きで上記シリンダー72を垂直に立てた状態で、上記シリンダー72の上記ナイロン(登録商標)メッシュ71上に0.1gの吸水性樹脂粒子73を均一に散布した。均一であることは、目視にて確認した。必要により、シリンダー72を揺らすことで吸水性樹脂粒子73が均一になるように調整した。シリンダー72内に直径19.5mm、高さ59mmで質量20.5gのアクリル樹脂製の円筒形治具74(円筒形おもり)を挿入して、吸水性樹脂粒子73の上に円筒形治具74を配置した。
(3)EZ-Testの測定テーブル上に、直径100mmのシャーレ75を水平に載置した。直径50mm、厚み5mmの乾燥したガラスフィルター76(フィルター孔径G1)を、上記シャーレ75内の中央部に置き、上記ガラスフィルター76の上面より僅かに下の位置までの生理食塩水77を注入した(約20ml)。
(4)生理食塩水77が浸透した上記ガラスフィルター76の上面中央付近に、50mm×50mmの不透液シート78を置き、該不透液シート78の上に、上記吸水性樹脂粒子73を含む上記シリンダー72を、上記ナイロン(登録商標)メッシュ71が下になる向きで垂直に載置した。
(5)EZ-Testのロードセル79に接続された直径20mmの感圧部をシリンダー72内の円筒形治具74の上方直近に位置するよう、ロードセル79を配置した。より具体的には、ロードセル部測定テーブルを上下させることで、ロードセル79に接続された感圧部をアクリル樹脂製円筒形治具74に近接させ、接触による僅かな圧力が観測された時点で停止した。次に、ロードセル部測定テーブルを僅かずつ上方向に移動させ、圧力指示値が0±0.05(単位ニュートン:N)となった位置を測定開始点とした。
(6)上記不透液シート78をすみやかに取り除いて、上記吸水性樹脂粒子73による吸水を開始させた。
(7)上記不透液シート78を取り除いた時点を経過時間t=0[秒]とし、生理食塩水77を吸水した吸水性樹脂粒子73の膨潤によって生じる力の経時変化をロードセル79によって60秒間測定を行い、t=10[秒]の値を膨潤力の10秒値とし、t=10[秒]の値を膨潤力の60秒値とした。 (1) Made of acrylic resin having an inner diameter of 20 mm (bottom area 3.14 cm 2 ) and a height of 50 mm, which has openings at both ends and nylon (registered trademark) mesh 71 (255 mesh) is attached to one of the openings. Acylinder 72 was prepared.
(2) On the nylon (registered trademark)mesh 71 of the cylinder 72, with the cylinder 72 standing vertically with the opening on the side where the nylon (registered trademark) mesh 71 is mounted facing down. 0.1 g of water-absorbent resin particles 73 were uniformly sprayed. It was visually confirmed that it was uniform. If necessary, the cylinder 72 was shaken to make the water-absorbent resin particles 73 uniform. A cylindrical jig 74 (cylindrical weight) made of acrylic resin having a diameter of 19.5 mm and a height of 59 mm and a mass of 20.5 g is inserted into the cylinder 72, and the cylindrical jig 74 is placed on the water-absorbent resin particles 73. Was placed.
(3) Apetri dish 75 having a diameter of 100 mm was horizontally placed on the measurement table of EZ-Test. A dry glass filter 76 (filter hole diameter G1) having a diameter of 50 mm and a thickness of 5 mm was placed in the central portion of the petri dish 75, and physiological saline 77 was injected to a position slightly below the upper surface of the glass filter 76 ( About 20 ml).
(4) A 50 mm × 50 mmimpermeable liquid sheet 78 is placed near the center of the upper surface of the glass filter 76 in which the physiological saline 77 has permeated, and the impermeable resin sheet 78 contains the water-absorbent resin particles 73. The cylinder 72 was placed vertically with the nylon (registered trademark) mesh 71 facing down.
(5) Theload cell 79 was arranged so that the pressure-sensitive portion having a diameter of 20 mm connected to the load cell 79 of the EZ-Test was located immediately above the cylindrical jig 74 in the cylinder 72. More specifically, by moving the load cell measurement table up and down, the pressure-sensitive part connected to the load cell 79 is brought close to the acrylic resin cylindrical jig 74, and stops when a slight pressure due to contact is observed. did. Next, the load cell measurement table was moved upward little by little, and the position where the pressure indicated value became 0 ± 0.05 (unit: Newton: N) was set as the measurement start point.
(6) Theimpermeable sheet 78 was promptly removed to start water absorption by the water-absorbent resin particles 73.
(7) The time when theimpermeable sheet 78 is removed is set to the elapsed time t = 0 [seconds], and the change over time of the force generated by the swelling of the water-absorbent resin particles 73 that have absorbed the physiological saline 77 is measured by the load cell 79 for 60 seconds. The measurement was performed, and the value of t = 10 [seconds] was defined as the 10-second value of the swelling force, and the value of t = 10 [seconds] was defined as the 60-second value of the swelling force.
(2)上記ナイロン(登録商標)メッシュ71が装着された側の開口部が下になる向きで上記シリンダー72を垂直に立てた状態で、上記シリンダー72の上記ナイロン(登録商標)メッシュ71上に0.1gの吸水性樹脂粒子73を均一に散布した。均一であることは、目視にて確認した。必要により、シリンダー72を揺らすことで吸水性樹脂粒子73が均一になるように調整した。シリンダー72内に直径19.5mm、高さ59mmで質量20.5gのアクリル樹脂製の円筒形治具74(円筒形おもり)を挿入して、吸水性樹脂粒子73の上に円筒形治具74を配置した。
(3)EZ-Testの測定テーブル上に、直径100mmのシャーレ75を水平に載置した。直径50mm、厚み5mmの乾燥したガラスフィルター76(フィルター孔径G1)を、上記シャーレ75内の中央部に置き、上記ガラスフィルター76の上面より僅かに下の位置までの生理食塩水77を注入した(約20ml)。
(4)生理食塩水77が浸透した上記ガラスフィルター76の上面中央付近に、50mm×50mmの不透液シート78を置き、該不透液シート78の上に、上記吸水性樹脂粒子73を含む上記シリンダー72を、上記ナイロン(登録商標)メッシュ71が下になる向きで垂直に載置した。
(5)EZ-Testのロードセル79に接続された直径20mmの感圧部をシリンダー72内の円筒形治具74の上方直近に位置するよう、ロードセル79を配置した。より具体的には、ロードセル部測定テーブルを上下させることで、ロードセル79に接続された感圧部をアクリル樹脂製円筒形治具74に近接させ、接触による僅かな圧力が観測された時点で停止した。次に、ロードセル部測定テーブルを僅かずつ上方向に移動させ、圧力指示値が0±0.05(単位ニュートン:N)となった位置を測定開始点とした。
(6)上記不透液シート78をすみやかに取り除いて、上記吸水性樹脂粒子73による吸水を開始させた。
(7)上記不透液シート78を取り除いた時点を経過時間t=0[秒]とし、生理食塩水77を吸水した吸水性樹脂粒子73の膨潤によって生じる力の経時変化をロードセル79によって60秒間測定を行い、t=10[秒]の値を膨潤力の10秒値とし、t=10[秒]の値を膨潤力の60秒値とした。 (1) Made of acrylic resin having an inner diameter of 20 mm (bottom area 3.14 cm 2 ) and a height of 50 mm, which has openings at both ends and nylon (registered trademark) mesh 71 (255 mesh) is attached to one of the openings. A
(2) On the nylon (registered trademark)
(3) A
(4) A 50 mm × 50 mm
(5) The
(6) The
(7) The time when the
表1に吸水量、吸水速度、並びに膨潤力の10秒値及び60秒値の測定結果が示される。
Table 1 shows the measurement results of water absorption, water absorption rate, and swelling power for 10 seconds and 60 seconds.
<液体漏れ試験>
(人工尿の調製)
以下に示す配合で、人工尿を調製した。
・イオン交換水:9865.75g
・NaCl:100.0g
・CaCl2・H2O:3.0g
・MgCl2・6H2O:6.0g
・トリトン X-100(1%):25.0g
・食用青色1号(着色用):0.25g <Liquid leak test>
(Preparation of artificial urine)
Artificial urine was prepared with the formulation shown below.
-Ion-exchanged water: 9865.75 g
-NaCl: 100.0 g
・ CaCl 2・ H 2 O: 3.0 g
· MgCl 2 · 6H 2 O: 6.0g
-Triton X-100 (1%): 25.0 g
-Edible blue No. 1 (for coloring): 0.25 g
(人工尿の調製)
以下に示す配合で、人工尿を調製した。
・イオン交換水:9865.75g
・NaCl:100.0g
・CaCl2・H2O:3.0g
・MgCl2・6H2O:6.0g
・トリトン X-100(1%):25.0g
・食用青色1号(着色用):0.25g <Liquid leak test>
(Preparation of artificial urine)
Artificial urine was prepared with the formulation shown below.
-Ion-exchanged water: 9865.75 g
-NaCl: 100.0 g
・ CaCl 2・ H 2 O: 3.0 g
· MgCl 2 · 6H 2 O: 6.0g
-Triton X-100 (1%): 25.0 g
-Edible blue No. 1 (for coloring): 0.25 g
(股漏れ試験)
図11に示す装置を用いて、股漏れ試験を行った。図11に示す装置は、立位及び座位を模した装置であり、当該装置に試験用吸収性物品を載置し、試験用吸収性物品中心の鉛直上方から滴下漏斗にて人工尿を投入することにより、試験用吸収性物品の短手方向からの人工尿の漏れ量が評価される。 (Crotch leak test)
A crotch leak test was performed using the device shown in FIG. The device shown in FIG. 11 is a device that imitates a standing position and a sitting position. A test absorbent article is placed on the device, and artificial urine is injected from vertically above the center of the test absorbent article with a dropping funnel. Thereby, the amount of artificial urine leaked from the short side of the test absorbent article is evaluated.
図11に示す装置を用いて、股漏れ試験を行った。図11に示す装置は、立位及び座位を模した装置であり、当該装置に試験用吸収性物品を載置し、試験用吸収性物品中心の鉛直上方から滴下漏斗にて人工尿を投入することにより、試験用吸収性物品の短手方向からの人工尿の漏れ量が評価される。 (Crotch leak test)
A crotch leak test was performed using the device shown in FIG. The device shown in FIG. 11 is a device that imitates a standing position and a sitting position. A test absorbent article is placed on the device, and artificial urine is injected from vertically above the center of the test absorbent article with a dropping funnel. Thereby, the amount of artificial urine leaked from the short side of the test absorbent article is evaluated.
(1)アルミニウム製型枠54を、アルミニウム製部品54a,54b(アルミニウム製フレームの幅は3cm)を、アルミニウム製部品内側間の水平距離が15cmとなるように組み立てた。
(2)10cm×40cmに切り出した不透液シート53(株式会社セイニチ製ポリエチレン製チャック付きビニール袋ユニパックLサイズを加工して使用)のうち短手方向の一方の端部を、アルミニウム製部品54aのうち部品54b側の端に、もう一方の端部を部品54bのうち部品54a側の端にとりつけた。このとき不透液シート53の最もたるむ部分は、測定装置を設置した面(水平面)から鉛直上側9cmとなる位置とした。 (1) Thealuminum formwork 54 was assembled by assembling aluminum parts 54a and 54b (the width of the aluminum frame is 3 cm) so that the horizontal distance between the insides of the aluminum parts was 15 cm.
(2) Of theimpermeable sheet 53 cut out to a size of 10 cm x 40 cm (used by processing Unipack L size, a plastic bag with a polyethylene zipper manufactured by Seinichi Co., Ltd.), one end in the lateral direction is made of aluminum part 54a. The other end was attached to the end of the component 54b on the component 54b side, and the other end was attached to the end of the component 54b on the component 54a side. At this time, the most slack portion of the impermeable sheet 53 was set at a position 9 cm vertically above the surface (horizontal plane) on which the measuring device was installed.
(2)10cm×40cmに切り出した不透液シート53(株式会社セイニチ製ポリエチレン製チャック付きビニール袋ユニパックLサイズを加工して使用)のうち短手方向の一方の端部を、アルミニウム製部品54aのうち部品54b側の端に、もう一方の端部を部品54bのうち部品54a側の端にとりつけた。このとき不透液シート53の最もたるむ部分は、測定装置を設置した面(水平面)から鉛直上側9cmとなる位置とした。 (1) The
(2) Of the
(4)作製した試験用吸収性物品200の中心にしるしをつけた。
(5)試験用吸収性物品200を測定装置のバックシートを模した不透液シート53に、試験用吸収性物品200の中心が最も不透液シート53がたるむ部分に載置した。このとき、試験用吸収性物品200を、吸収性物品200が露出された状態で配置し、トップシート等は使用しなかった。
(6)試験用吸収性物品200の中心となる点の鉛直方向上部1cmの位置(装置を設置した面から上に10cm)を投入点とし、滴下速度を8ml/秒に調整した滴下漏斗52(株式会社コスモスビード製 滴下ロート300ml容、先端部の内径が8mm×6mm)を用いて、液温25度に調整した人工尿51を40ml注入した。
(7)試験用吸収性物品200から漏れ出た人工尿51は、あらかじめ試験用吸収性物品200の下方向に設置しておいた、天秤56上に配置されたSUS製トレー55に回収し、回収した人工尿51を天秤56を用いて計量した。 (4) A mark was placed at the center of the prepared testabsorbent article 200.
(5) The testabsorbent article 200 was placed on the impermeable sheet 53 imitating the back sheet of the measuring device, and the center of the test absorbent article 200 was placed on the most slack portion of the impermeable sheet 53. At this time, the test absorbent article 200 was placed in a state where the absorbent article 200 was exposed, and no top sheet or the like was used.
(6) Dropping funnel 52 (dropping funnel 52) whose dropping speed was adjusted to 8 ml / sec, with the position 1 cm above the center of the testabsorbent article 200 in the vertical direction (10 cm above the surface on which the device was installed) as the loading point. Using a 300 ml dropping funnel manufactured by Cosmos Bead Co., Ltd. and an inner diameter of the tip of 8 mm × 6 mm), 40 ml of artificial urine 51 adjusted to a liquid temperature of 25 ° C. was injected.
(7) The artificial urine 51 leaked from the testabsorbent article 200 was collected in a SUS tray 55 arranged on the balance 56, which was previously installed in the downward direction of the test absorbent article 200. The collected artificial urine 51 was weighed using a balance 56.
(5)試験用吸収性物品200を測定装置のバックシートを模した不透液シート53に、試験用吸収性物品200の中心が最も不透液シート53がたるむ部分に載置した。このとき、試験用吸収性物品200を、吸収性物品200が露出された状態で配置し、トップシート等は使用しなかった。
(6)試験用吸収性物品200の中心となる点の鉛直方向上部1cmの位置(装置を設置した面から上に10cm)を投入点とし、滴下速度を8ml/秒に調整した滴下漏斗52(株式会社コスモスビード製 滴下ロート300ml容、先端部の内径が8mm×6mm)を用いて、液温25度に調整した人工尿51を40ml注入した。
(7)試験用吸収性物品200から漏れ出た人工尿51は、あらかじめ試験用吸収性物品200の下方向に設置しておいた、天秤56上に配置されたSUS製トレー55に回収し、回収した人工尿51を天秤56を用いて計量した。 (4) A mark was placed at the center of the prepared test
(5) The test
(6) Dropping funnel 52 (dropping funnel 52) whose dropping speed was adjusted to 8 ml / sec, with the position 1 cm above the center of the test
(7) The artificial urine 51 leaked from the test
表2は、補助シートの構成及び評価結果を示す。表2中の「使用者側」は、補助シートを吸水コア主面上の使用者が装着した際の使用者側(液体が侵入する側)に配置したことを、「外側」は補助シートを吸水コア主面上の使用者が装着した際の使用者側とは反対側に配置したことを意味する。
Table 2 shows the composition of the auxiliary sheet and the evaluation results. In Table 2, the "user side" means that the auxiliary sheet is placed on the user side (the side where the liquid invades) when the user wears the auxiliary sheet on the main surface of the water absorption core, and the "outside" means that the auxiliary sheet is placed. It means that it is placed on the side opposite to the user side when it is worn by the user on the main surface of the water absorption core.
表2中の「長手両端」は、膨潤層が、吸水コアの短手方向の両端部上に吸水コアの長手方向に沿って設けられていることを意味する。
The "longitudinal ends" in Table 2 mean that the swelling layer is provided on both ends of the water absorption core in the lateral direction along the longitudinal direction of the water absorption core.
補助シート上の所定位置に吸水性樹脂粒子を含む膨潤層を設け、膨潤層に含まれる吸水性樹脂粒子の膨潤力の10秒値を特定の数値に制御することによって、使用者の装着状態における液体漏れ(股漏れ)が抑制されることが示された。
By providing a swelling layer containing the water-absorbent resin particles at a predetermined position on the auxiliary sheet and controlling the 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer to a specific value, the user is in a wearing state. It was shown that liquid leakage (crotch leakage) was suppressed.
(腹漏れ、背漏れ試験)
図12に示す装置を用いて、股漏れ及び背漏れ試験を行った。図12に示す装置は、仰向け及びうつぶせを模した装置であり、試験用吸収性物品200を載置し、試験用吸収性物品200中心に向けて送液ポンプにて人工尿を投入することによって、人工尿の漏れ量が評価される。 (Abdominal leak, back leak test)
A crotch leak and back leak test were performed using the device shown in FIG. The device shown in FIG. 12 is a device that imitates lying on the back and lying down, and by placing the testabsorbent article 200 on the device and injecting artificial urine toward the center of the test absorbent article 200 with a liquid feed pump. , The amount of artificial urine leaked is evaluated.
図12に示す装置を用いて、股漏れ及び背漏れ試験を行った。図12に示す装置は、仰向け及びうつぶせを模した装置であり、試験用吸収性物品200を載置し、試験用吸収性物品200中心に向けて送液ポンプにて人工尿を投入することによって、人工尿の漏れ量が評価される。 (Abdominal leak, back leak test)
A crotch leak and back leak test were performed using the device shown in FIG. The device shown in FIG. 12 is a device that imitates lying on the back and lying down, and by placing the test
(1)U字形状のアクリル樹脂製器具81に試験用吸収性物品200を、試験用吸収性物品200の中心が器具の中心になるように載置し、ずれないように任意の箇所をテープで固定した。
(2)アクリル樹脂製器具81を、水平方向に向けて開口した状態で、測定台84上に設置し、試験用吸収性物品200の中心かつ試験用吸収性物品200から水平方向に1cm離れた点を投入点とし、液投入用の送液ポンプ82(INTEGRA Bioscience AG、モデル:DOSE IT P910)の排液口(直径0.4cm)を配置した。
(3)8ml/秒の速度にて液温25℃に調整した人工尿80mlを注入した。試験用吸収性物品200から漏れ出た人工尿は、あらかじめ試験用吸収性物品200の下方向に設置され、天秤83上に載置されたSUS製トレー82によって回収、計量される。 (1) Place the testabsorbent article 200 on the U-shaped acrylic resin instrument 81 so that the center of the test absorbent article 200 is the center of the instrument, and tape any part so that it does not shift. Fixed with.
(2) Theacrylic resin instrument 81 was installed on the measuring table 84 in a state of being opened in the horizontal direction, and was separated from the center of the test absorbent article 200 and the test absorbent article 200 in the horizontal direction by 1 cm. A point was set as a charging point, and a drainage port (diameter 0.4 cm) of a liquid feeding pump 82 (INTERGRA Bioscience AG, model: DOSEI IT P910) for liquid charging was arranged.
(3) 80 ml of artificial urine adjusted to a liquid temperature of 25 ° C. was injected at a rate of 8 ml / sec. The artificial urine leaked from the testabsorbent article 200 is previously installed in the downward direction of the test absorbent article 200, and is collected and measured by a SUS tray 82 placed on the balance 83.
(2)アクリル樹脂製器具81を、水平方向に向けて開口した状態で、測定台84上に設置し、試験用吸収性物品200の中心かつ試験用吸収性物品200から水平方向に1cm離れた点を投入点とし、液投入用の送液ポンプ82(INTEGRA Bioscience AG、モデル:DOSE IT P910)の排液口(直径0.4cm)を配置した。
(3)8ml/秒の速度にて液温25℃に調整した人工尿80mlを注入した。試験用吸収性物品200から漏れ出た人工尿は、あらかじめ試験用吸収性物品200の下方向に設置され、天秤83上に載置されたSUS製トレー82によって回収、計量される。 (1) Place the test
(2) The
(3) 80 ml of artificial urine adjusted to a liquid temperature of 25 ° C. was injected at a rate of 8 ml / sec. The artificial urine leaked from the test
表3は、補助シートの構成及び評価結果を示す。表3中の「使用者側」、「長手両端」は表2と同意義である。表3中の「長手・短手両端」は、膨潤層が、吸水コアの長手方向の両端部上に、吸水コアの短手方向に沿って設けられ、かつ、短手方向の両端部上に、吸水コアの長手方向に沿って設けられていることを、「短手両端」は、膨潤層が、吸水コアの長手方向の両端部上に吸水コアの短手方向に沿って設けられていることを意味する。
Table 3 shows the composition of the auxiliary sheet and the evaluation results. “User side” and “longitudinal end” in Table 3 have the same meaning as in Table 2. In "longitudinal and short ends" in Table 3, swelling layers are provided on both ends of the water absorption core in the longitudinal direction along the short direction of the water absorption core, and on both ends in the short direction. In the "short end", the swelling layer is provided on both ends of the water absorption core in the longitudinal direction along the longitudinal direction of the water absorption core. Means that.
補助シート上の所定位置に吸水性樹脂粒子を含む膨潤層を設け、膨潤層に含まれる吸水性樹脂粒子の膨潤力の10秒値を特定の数値に制御することによって、使用者の装着状態における液体漏れ(腹漏れ及び背漏れ)が抑制されることが示された。
By providing a swelling layer containing the water-absorbent resin particles at a predetermined position on the auxiliary sheet and controlling the 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer to a specific value, the user is in a wearing state. It was shown that liquid leakage (abdominal leakage and back leakage) was suppressed.
10…吸収層、10a…吸水性樹脂粒子、10b…繊維層、20a,20b…コアラップシート、21…接着剤、30…液体透過性シート、40…液体不透過性シート、50…吸水コア、60…補助シート、61…膨潤層、61a…吸水性樹脂粒子、61b…繊維層、62a,62b…シート基材、63a,63b…接着剤、100…吸収性物品。
10 ... Absorbent layer, 10a ... Water-absorbent resin particles, 10b ... Fiber layer, 20a, 20b ... Core wrap sheet, 21 ... Adhesive, 30 ... Liquid permeable sheet, 40 ... Liquid impermeable sheet, 50 ... Water-absorbing core, 60 ... Auxiliary sheet, 61 ... Swelling layer, 61a ... Water-absorbent resin particles, 61b ... Fiber layer, 62a, 62b ... Sheet base material, 63a, 63b ... Adhesive, 100 ... Absorbent article.
10 ... Absorbent layer, 10a ... Water-absorbent resin particles, 10b ... Fiber layer, 20a, 20b ... Core wrap sheet, 21 ... Adhesive, 30 ... Liquid permeable sheet, 40 ... Liquid impermeable sheet, 50 ... Water-absorbing core, 60 ... Auxiliary sheet, 61 ... Swelling layer, 61a ... Water-absorbent resin particles, 61b ... Fiber layer, 62a, 62b ... Sheet base material, 63a, 63b ... Adhesive, 100 ... Absorbent article.
Claims (4)
- 短冊状の吸水コア、該吸水コアによる吸液を補助する補助シート、液体不透過性シート及び液体透過性シートを備え、
前記液体不透過性シート、前記吸水コア及び前記液体透過性シートがこの順に配置され、
前記補助シートが、前記不透過性シートと前記吸水コアとの間、及び/又は、前記吸水コアと前記液体透過性シートとの間に配置されており、
前記補助シートが、吸水性樹脂粒子を含む膨潤層を有し、
前記膨潤層が、前記吸水コアの短手方向の両端部上に前記吸水コアの長手方向に沿って設けられており、
前記膨潤層に含まれる前記吸水性樹脂粒子の、以下のi)、ii)、iii)、iv)及びv)の順で行われる膨潤力試験で測定される膨潤力の10秒値が5N以上である、吸収性物品。
i)両端に開口部を有し、その一方の開口部にメッシュが装着された内径20mmのシリンダーを用意し、前記メッシュが装着された側を下になる向きで前記シリンダーを垂直に立てた状態で、前記シリンダー内で前記メッシュ上に0.1gの吸水性樹脂粒子を均一に散布し、その上に直径19.5mmの円筒形治具を置く。
ii)厚み5mmのガラスフィルターを、水平に設置されたシャーレ内に載置し、前記ガラスフィルターにその上面より僅かに下の位置まで生理食塩水を浸透させる。
iii)前記生理食塩水が浸透した前記ガラスフィルターの上面に不透液シートを置き、該不透液シートの上に、前記吸水性樹脂粒子を含む前記シリンダーを、前記メッシュが下になる向きで垂直に立てる。
iv)前記不透液シートを取り除いて、前記吸水性樹脂粒子による吸水を開始させる。
v)前記不透液シートを取り除いてから10秒後の時点の、前記吸水性樹脂粒子の膨潤によって生じた前記円筒形治具を押し上げる力をロードセルによって測定し、膨潤力の10秒値として記録する。 It is provided with a strip-shaped water absorption core, an auxiliary sheet for assisting liquid absorption by the water absorption core, a liquid impermeable sheet, and a liquid permeable sheet.
The liquid permeable sheet, the water absorption core, and the liquid permeable sheet are arranged in this order.
The auxiliary sheet is arranged between the impermeable sheet and the water absorbing core and / or between the water absorbing core and the liquid permeable sheet.
The auxiliary sheet has a swelling layer containing water-absorbent resin particles and has a swelling layer.
The swelling layer is provided on both ends of the water absorption core in the lateral direction along the longitudinal direction of the water absorption core.
The 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer measured in the swelling force test performed in the order of i), ii), iii), iv) and v) below is 5 N or more. Is an absorbent article.
i) A cylinder having openings at both ends and having a mesh mounted on one of the openings and having an inner diameter of 20 mm is prepared, and the cylinder is vertically erected with the side on which the mesh is mounted facing downward. Then, 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
ii) A glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
iii) An impermeable sheet is placed on the upper surface of the glass filter in which the physiological saline has permeated, and the cylinder containing the water-absorbent resin particles is placed on the impermeable sheet so that the mesh faces downward. Stand vertically.
iv) The impermeable sheet is removed to start water absorption by the water-absorbent resin particles.
v) The force for pushing up the cylindrical jig generated by the swelling of the water-absorbent resin particles 10 seconds after the impermeable sheet is removed is measured by a load cell and recorded as a 10-second value of the swelling force. To do. - 前記膨潤層が、前記吸水コアの長手方向の両端部上に、前記吸水コアの短手方向に沿って更に設けられている、請求項1に記載の吸収性物品。 The absorbent article according to claim 1, wherein the swollen layer is further provided on both ends of the water absorbing core in the longitudinal direction along the lateral direction of the water absorbing core.
- おむつである、請求項1又は2に記載の吸収性物品。 The absorbent article according to claim 1 or 2, which is a diaper.
- 短冊状の吸水コアを備える吸収性物品において、前記吸水コアの吸液を補助するために用いられる補助シートであって、
吸水性樹脂粒子を含む膨潤層を備え、
前記膨潤層に含まれる吸水性樹脂粒子の、以下のi)、ii)、iii)、iv)及びv)の順で行われる膨潤力試験で測定される膨潤力の10秒値が5N以上である、補助シート。
i)両端に開口部を有し、その一方の開口部にメッシュが装着された内径20mmのシリンダーを用意し、前記メッシュが装着された側を下になる向きで前記シリンダーを垂直に立てた状態で、前記シリンダー内で前記メッシュ上に0.1gの吸水性樹脂粒子を均一に散布し、その上に直径19.5mmの円筒形治具を置く。
ii)厚み5mmのガラスフィルターを、水平に設置されたシャーレ内に載置し、前記ガラスフィルターにその上面より僅かに下の位置まで生理食塩水を浸透させる。
iii)前記生理食塩水が浸透した前記ガラスフィルターの上面に不透液シートを置き、該不透液シートの上に、前記吸水性樹脂粒子を含む前記シリンダーを、前記メッシュが下になる向きで垂直に立てる。
iv)前記不透液シートを取り除いて、前記吸水性樹脂粒子による吸水を開始させる。
v)前記不透液シートを取り除いてから10秒後の時点の、前記吸水性樹脂粒子の膨潤によって生じた前記円筒形治具を押し上げる力をロードセルによって測定し、膨潤力の10秒値として記録する。 An auxiliary sheet used to assist the absorption of liquid in the water absorption core in an absorbent article provided with a strip-shaped water absorption core.
With a swollen layer containing water-absorbent resin particles,
When the 10-second value of the swelling force of the water-absorbent resin particles contained in the swelling layer is 5 N or more, which is measured in the swelling force test performed in the order of i), ii), iii), iv) and v) below. There is an auxiliary sheet.
i) A cylinder having openings at both ends and having a mesh mounted on one of the openings and having an inner diameter of 20 mm is prepared, and the cylinder is vertically erected with the side on which the mesh is mounted facing downward. Then, 0.1 g of water-absorbent resin particles are uniformly sprayed on the mesh in the cylinder, and a cylindrical jig having a diameter of 19.5 mm is placed on the mesh.
ii) A glass filter having a thickness of 5 mm is placed in a horizontally installed petri dish, and the glass filter is impregnated with physiological saline to a position slightly below the upper surface thereof.
iii) An impermeable sheet is placed on the upper surface of the glass filter in which the physiological saline has permeated, and the cylinder containing the water-absorbent resin particles is placed on the impermeable sheet so that the mesh faces downward. Stand vertically.
iv) The impermeable sheet is removed to start water absorption by the water-absorbent resin particles.
v) The force for pushing up the cylindrical jig generated by the swelling of the water-absorbent resin particles 10 seconds after the impermeable sheet is removed is measured by a load cell and recorded as a 10-second value of the swelling force. To do.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115670804A (en) * | 2021-07-22 | 2023-02-03 | 常州爱丽葆康护理用品股份有限公司 | Novel absorb health supplies of core and applied this absorption core |
WO2023233925A1 (en) * | 2022-05-30 | 2023-12-07 | 住友精化株式会社 | Absorbent body and absorbent article |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018181548A1 (en) * | 2017-03-31 | 2018-10-04 | 住友精化株式会社 | Water-absorbent resin particles |
JP2019146753A (en) * | 2018-02-27 | 2019-09-05 | ユニ・チャーム株式会社 | Absorbent article |
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2020
- 2020-10-15 WO PCT/JP2020/038951 patent/WO2021075508A1/en active Application Filing
- 2020-10-15 JP JP2021552439A patent/JPWO2021075508A1/ja active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2018181548A1 (en) * | 2017-03-31 | 2018-10-04 | 住友精化株式会社 | Water-absorbent resin particles |
JP2019146753A (en) * | 2018-02-27 | 2019-09-05 | ユニ・チャーム株式会社 | Absorbent article |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115670804A (en) * | 2021-07-22 | 2023-02-03 | 常州爱丽葆康护理用品股份有限公司 | Novel absorb health supplies of core and applied this absorption core |
WO2023233925A1 (en) * | 2022-05-30 | 2023-12-07 | 住友精化株式会社 | Absorbent body and absorbent article |
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