CN112275031B - Preparation method of melt-blown electret polymer filter material - Google Patents
Preparation method of melt-blown electret polymer filter material Download PDFInfo
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- CN112275031B CN112275031B CN202011181411.7A CN202011181411A CN112275031B CN 112275031 B CN112275031 B CN 112275031B CN 202011181411 A CN202011181411 A CN 202011181411A CN 112275031 B CN112275031 B CN 112275031B
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 229920000642 polymer Polymers 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 89
- -1 polypropylene Polymers 0.000 claims abstract description 70
- 239000004743 Polypropylene Substances 0.000 claims abstract description 54
- 229920001155 polypropylene Polymers 0.000 claims abstract description 54
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 239000000155 melt Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 16
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 16
- 239000000022 bacteriostatic agent Substances 0.000 claims abstract description 15
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 238000006011 modification reaction Methods 0.000 claims abstract description 8
- 150000003918 triazines Chemical class 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 150000001451 organic peroxides Chemical class 0.000 claims abstract description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000005243 fluidization Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 235000010333 potassium nitrate Nutrition 0.000 claims description 9
- 239000004323 potassium nitrate Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 6
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 239000011246 composite particle Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- NRWCNEBHECBWRJ-UHFFFAOYSA-M trimethyl(propyl)azanium;chloride Chemical group [Cl-].CCC[N+](C)(C)C NRWCNEBHECBWRJ-UHFFFAOYSA-M 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- JJRDRFZYKKFYMO-UHFFFAOYSA-N 2-methyl-2-(2-methylbutan-2-ylperoxy)butane Chemical compound CCC(C)(C)OOC(C)(C)CC JJRDRFZYKKFYMO-UHFFFAOYSA-N 0.000 claims description 3
- 125000005336 allyloxy group Chemical group 0.000 claims description 3
- HQOVXPHOJANJBR-UHFFFAOYSA-N 2,2-bis(tert-butylperoxy)butane Chemical compound CC(C)(C)OOC(C)(CC)OOC(C)(C)C HQOVXPHOJANJBR-UHFFFAOYSA-N 0.000 claims description 2
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 2
- ROHTVIURAJBDES-UHFFFAOYSA-N 2-n,2-n-bis(prop-2-enyl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N(CC=C)CC=C)=N1 ROHTVIURAJBDES-UHFFFAOYSA-N 0.000 claims description 2
- PFBLRDXPNUJYJM-UHFFFAOYSA-N tert-butyl 2-methylpropaneperoxoate Chemical compound CC(C)C(=O)OOC(C)(C)C PFBLRDXPNUJYJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004744 fabric Substances 0.000 abstract description 28
- 230000007774 longterm Effects 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 5
- 239000007921 spray Substances 0.000 abstract 1
- 238000004804 winding Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 235000005078 Chaenomeles speciosa Nutrition 0.000 description 3
- 240000000425 Chaenomeles speciosa Species 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 241000700605 Viruses Species 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 150000001336 alkenes Chemical group 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- AYMDJPGTQFHDSA-UHFFFAOYSA-N 1-(2-ethenoxyethoxy)-2-ethoxyethane Chemical compound CCOCCOCCOC=C AYMDJPGTQFHDSA-UHFFFAOYSA-N 0.000 description 1
- 239000000370 acceptor Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- CGQIJXYITMTOBI-UHFFFAOYSA-N hex-5-enyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCC=C CGQIJXYITMTOBI-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Chemical group CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000734 polysilsesquioxane polymer Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- FYZFRYWTMMVDLR-UHFFFAOYSA-M trimethyl(3-trimethoxysilylpropyl)azanium;chloride Chemical compound [Cl-].CO[Si](OC)(OC)CCC[N+](C)(C)C FYZFRYWTMMVDLR-UHFFFAOYSA-M 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/08—Filter cloth, i.e. woven, knitted or interlaced material
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses a preparation method of a melt-blown electret polymer filter material, which comprises the following steps: s1: weighing a certain amount of polypropylene, organic peroxide, triazine derivative and bacteriostatic agent, uniformly mixing, and then extruding for modification reaction to obtain modified polypropylene master batch; s2: uniformly mixing the modified polypropylene master batch, the polytetrafluoroethylene master batch, the polypropylene master batch and the polypropylene grafted maleic anhydride, heating and melting, and then ejecting a melt through a spinneret plate; s3: the fluidized modified nano activated carbon particles are used as traction airflow to synchronously spray and stretch the melt, and a magnetic field is applied in the process, so that the concentration of the modified nano activated carbon particles is changed in a gradient manner from the center to two sides; corona discharge, cooling and winding to obtain the filtering material. The filter material prepared by the invention has the excellent characteristics of polypropylene and polytetrafluoroethylene materials, has high-efficiency filtering and antibacterial properties, and meets the use requirements of long-term harsh environments of filter materials such as melt-blown cloth and the like.
Description
Technical Field
The invention relates to the technical field of melt-blown cloth, in particular to a preparation method of a melt-blown electret polymer filter material.
Background
With the increasing emphasis on personal health and safety, people are becoming more and more accustomed to wearing masks for personal protection. The mask can be divided into various types according to the requirements of the application occasions, including medical masks and N95 masks. Medical masks and N95 masks are generally composed of a spunbond layer, a meltblown layer and a spunbond layer, the conventional meltblown layer is made of a conventional polypropylene meltblown material, and the polymer material is polarized and can be kept in a polarization state permanently under the action of factors such as a strong external electric field, and the polymer material is called an electret polymer. Most of the existing melt-blown fabric filter materials are prepared only from polypropylene polymers, and are not modified or compounded with other functional substances for synergistic filtration treatment, so that the long-term high-efficiency filtration effect cannot be ensured, and the filter materials are usually discarded after being used for several hours, thereby causing serious waste of resources. Meanwhile, the surface charge of the melt-blown cloth filter material charged in the strong electric field can stay for a period of time to play a role in filtering viruses, bacteria, particles and the like, but along with the gradual failure of the melt-blown cloth, the inhibition effect of the melt-blown cloth on the viruses and the bacteria is gradually reduced, and the long-term antibacterial effect cannot be maintained.
Accordingly, there is a need to provide a melt-blown electret polymer filter material to meet the use requirements of melt-blown cloth filter materials in long-term harsh environments.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a preparation method of a melt-blown electret polymer filter material, so as to solve the problems that the existing melt-blown electret polymer filter material cannot inhibit bacteria for a long time, the filter effect is not uniformly distributed, and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of making a melt-blown electret polymer filter material, comprising the steps of:
s1: weighing 100 parts of polypropylene, 0.05-0.5 part of organic peroxide, 15-25 parts of triazine derivative and 10-20 parts of bacteriostatic agent by weight, adding into a high-speed mixer, stirring at a high speed, uniformly mixing, and performing modification reaction extrusion through an extruder to obtain modified polypropylene master batch;
s2: uniformly mixing the modified polypropylene master batch, the polytetrafluoroethylene master batch, the polypropylene master batch and the polypropylene grafted maleic anhydride obtained in the step S1, heating and melting, and then ejecting a melt through a spinneret plate;
s3: carrying out high-speed fluidization on the modified nano activated carbon particles by using high-temperature pressurized air, then synchronously jetting and stretching the melt sprayed out in the step S2 from one side of a spinneret plate as a traction air flow, and applying a magnetic field in the process to ensure that the concentration of the modified nano activated carbon particles is changed in a gradient manner from the center to two sides; and corona discharge is adopted in the gradual cooling process of the melt, and the melt-blown electret polymer filter material is obtained by rolling.
Preferably, the triazine derivative is at least one of 6-allyl-1, 3, 5-triazine-2, 4-diamine, 4, 6-bis (allyloxy) -N-butyl-1, 3, 5-triazine-2-amine, 4, 6-diallyloxy-N-octyl-1, 3, 5-triazine-2-amine, 2, 4-diamino-6-diallylamino-1, 3, 5-triazine. Due to the introduction of the triazine functional group, the prepared melt-blown fabric not only further improves the heat resistance and aging resistance of the melt-blown fabric, but also provides more active sites of electron acceptors for the melt-blown fabric, so that the electrostatic adsorption performance of the melt-blown fabric is further improved, and the melt-blown fabric has high-efficiency filtering performance.
Preferably, the bacteriostatic agent is shown in chemical formula I:
in the formula: r is propyl-N, N, N-trimethyl ammonium chloride.
The bacteriostatic agent adopted by the invention takes cage type polysilsesquioxane as a main body structure, a quaternary ammonium salt containing olefin functional groups and a plurality of active sites with positive charges is grafted on a Si atom, olefin double bonds participate in the crosslinking modification reaction of polypropylene, and the quaternary ammonium salt with the active sites with positive charges can interact with protein on the surface of bacteria to inhibit the bacteria from absorbing nutrient substances from the outside, so that after the bacteriostatic agent is introduced into the polypropylene to prepare the melt-blown cloth, the antibacterial capability of the melt-blown cloth can be effectively improved.
Polyhedral oligomeric silsesquioxane (POSS) is called as POSS for short, POSS groups belong to an organic-inorganic hybrid structure and have the characteristic of cage structure, the structure has certain flexibility, the wrinkle resistance of the meltblown fabric is improved, the thermal stability of the meltblown fabric is improved, and the propyl-N, N, N-trimethyl ammonium chloride connected to the Si atom of the POSS groups can effectively improve the long-acting antibacterial property of the meltblown fabric.
Preferably, in step S2, the mass ratio of the modified polypropylene masterbatch, the polytetrafluoroethylene masterbatch, the polypropylene masterbatch and the polypropylene grafted maleic anhydride is 15-25: 3-8: 100: 1 to 10. The polytetrafluoroethylene and the polypropylene are blended and modified, so that the melt-blown electret polymer filter material has the characteristics of both the polytetrafluoroethylene and the polypropylene, and the polypropylene grafted maleic anhydride is added to facilitate the increase of the compatibility of the polytetrafluoroethylene and the polypropylene in the blending and modifying process, so that the overall performance of the filter material is improved.
Preferably, the modified nano activated carbon particles are prepared by the following steps:
s1: weighing 25-65 parts by weight of activated carbon, dispersing the activated carbon in 50-80 parts by weight of deionized water and 20-40 parts by weight of ethanol, adding 6-15 parts by weight of ferrous hydroxide, stirring at room temperature for 1-3 hours, and uniformly mixing to obtain a mixed solution;
s2: carrying out ultrasonic oscillation on the mixed solution for 10-30 min, adding 35-80 parts of potassium nitrate solution at the speed of 1-5 g/min, and keeping the stirring speed of 800-1500 rpm in the adding process to obtain a suspension of ferroferric oxide coated activated carbon; preferably, in the adding process, oxygen is introduced at the speed of 200-800 mL/min;
s3: standing and aging the obtained suspension for 3-5 times and washing the suspension with deionized water, and then carrying out centrifugal filtration for 20-40 min at a centrifugal speed of 3000-8000 rpm to obtain a solid filter cake;
s4: and drying the solid filter cake obtained by centrifugal filtration at the temperature of 80-120 ℃ for 0.5-3 hours, and sieving the dried solid filter cake by using a 300-mesh vibrating screen to obtain the spherical composite particles of the modified nano activated carbon.
In the preparation process, the potassium nitrate is slowly oxidized to oxidize the ferrous hydroxide, and a standing aging reaction needs to be carried out for a long time, so that further, oxygen can be introduced into the reaction solution in the step S2 to accelerate the reaction process, thereby obtaining the ferroferric oxide coated activated carbon structure; in addition, the reasonable proportion of ferrous hydroxide and active carbon particles is controlled, so that the outer layer of ferroferric oxide cannot cause serious interference on the adsorption of the active carbon.
The melt-blown cloth filter material compounded by the activated carbon particles is beneficial to further improving the filtering performance of the filter material, and the ferroferric oxide coats the activated carbon structure, so that the concentration of the activated carbon particles is changed in a gradient manner from the center of the melt-blown cloth filter material to two sides under the action of a magnetic field by the modified nano activated carbon particles.
Preferably, the particle size of the activated carbon is 100-500 nm.
Preferably, the mass concentration of the potassium nitrate solution is 20-30%.
Preferably, the temperature of the fluidization operation is 110-150 ℃; the pressure of the air flow in the fluidization operation is 0.15-0.25 MPa.
Preferably, the magnetic field intensity of the magnetic field is 0.5-1.5T.
Preferably, the discharge voltage of the corona discharge is 30-50 KV.
Preferably, the organic peroxide is at least one of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, di-t-amyl peroxide, t-butyl peroxyisobutyrate or 2, 2-bis (t-butylperoxy) butane.
The invention has the beneficial effects that:
the invention relates to a preparation method of a melt-blown electret polymer filter material, which takes triazine derivatives and bacteriostatic agents with terminal olefin functional groups as cross-linking agents, and the triazine derivatives and the bacteriostatic agents with terminal olefin functional groups perform cross-linking modification reaction with polypropylene under the action of organic peroxides to obtain modified polypropylene; further, the improved polypropylene, the polytetrafluoroethylene and the polypropylene are blended and modified, a melt-blown cloth filter material is formed in a melt-blown mode, and a layer of modified nano activated carbon particles with gradient change in mass concentration is compounded on the surface of the filter material; the finally prepared melt-blown fabric has high-efficiency filtering performance and antibacterial performance under the long-term high-humidity environment polluted by particles, bacteria, viruses and the like, the problem that the filtering performance of the melt-blown fabric is remarkably reduced or loses efficacy is solved, the long-term use requirement of the melt-blown fabric is met, and meanwhile, the melt-blown fabric has excellent thermal stability, hydrophobicity and flexibility and can be repeatedly used after being washed.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments described below are by way of example only, and other obvious variations will occur to those skilled in the art.
Example 1
The preparation method of the melt-blown electret polymer filter material of the embodiment comprises the following steps:
s1: weighing 100 parts of polypropylene, 0.1 part of dicumyl peroxide, 15 parts of 6-allyl-1, 3, 5-triazine-2, 4-diamine and 10 parts of bacteriostatic agent by weight, adding into a high-speed mixer, stirring at a high speed, uniformly mixing, and performing modification reaction extrusion through an extruder to obtain the modified polypropylene master batch.
S2: uniformly mixing the modified polypropylene master batch, the polytetrafluoroethylene master batch, the polypropylene master batch and the polypropylene grafted maleic anhydride obtained in the step S1, heating and melting, and then spraying a melt through a spinneret plate; the mass ratio of the modified polypropylene master batch to the polytetrafluoroethylene master batch to the polypropylene grafted maleic anhydride is 15: 3: 100: 2.
s3: carrying out high-speed fluidization on the modified nano activated carbon particles by using high-temperature pressurized air, then synchronously jetting and stretching the melt jetted by the step S2 from one side of a spinneret plate as a traction airflow, and applying a magnetic field in the process to ensure that the concentration of the modified nano activated carbon particles is changed in a gradient manner from the center to two sides; and corona discharge is adopted in the gradual cooling process of the melt, and the melt-blown electret polymer filter material is obtained by rolling. The total weight of the active carbon of the prepared melt-blown electret polymer filter material accounts for 1 percent of the total mass of the filter material. The temperature of the fluidization operation is 130 ℃; the pressure of the fluidized air flow is 0.2MPa, the magnetic field intensity of the magnetic field is 1.0T, and the discharge voltage of the corona discharge is 40 KV.
The bacteriostatic agent is shown in a chemical formula I:
in the formula: r is propyl-N, N, N-trimethyl ammonium chloride.
The monofunctional POSS shown in the chemical formula I is synthesized by adopting a method of 'cap on top', namely N-trimethoxysilylpropyl-N, N, N-trimethyl ammonium chloride is hydrolyzed in aqueous solution of acetone to prepare T7(OH)3(i.e. also one vertex is not closed, three hydroxyl groups respectivelyAnd then adding a triethylamine solution of 5-hexenyltrimethoxysilane to perform a ring closing reaction to obtain the compound.
The modified nano activated carbon particles are prepared by the following steps:
s1: weighing 25 parts by weight of activated carbon, dispersing the activated carbon in 50 parts by weight of deionized water and 20 parts by weight of ethanol, adding 6 parts by weight of ferrous hydroxide, stirring at room temperature for 1 hour, and uniformly mixing to obtain a mixed solution; the particle size of the active carbon is 100 nm;
s2: carrying out ultrasonic oscillation on the mixed solution for 10min, adding 35 parts of potassium nitrate solution at the speed of 1g/min, wherein the mass concentration of the potassium nitrate solution is 20%, and keeping the stirring speed of 800rpm in the adding process to obtain a suspension of the ferroferric oxide coated activated carbon;
s3: standing and aging the obtained suspension for 3 times and washing the suspension with deionized water, and then carrying out centrifugal filtration for 20min at the centrifugal speed of 3000rpm to obtain a solid filter cake;
s4: and drying the solid filter cake obtained by centrifugal filtration at 120 ℃ for 0.5 hour, and sieving the dried solid filter cake by using a 300-mesh vibrating screen to obtain the spherical composite particles of the modified nano activated carbon.
Example 2
The preparation method of the melt-blown electret polymer filter material of the embodiment comprises the following steps:
s1: weighing 100 parts of polypropylene, 0.3 part of di-tert-amyl peroxide, 20 parts of 4, 6-bis (allyloxy) -N-butyl-1, 3, 5-triazine-2-amine and 15 parts of bacteriostatic agent by weight, adding into a high-speed mixer, stirring and mixing uniformly at a high speed, and performing modification reaction and extrusion through an extruder to obtain the modified polypropylene master batch.
S2: uniformly mixing the modified polypropylene master batch, the polytetrafluoroethylene master batch, the polypropylene master batch and the polypropylene grafted maleic anhydride obtained in the step S1, heating and melting, and then ejecting a melt through a spinneret plate; the mass ratio of the modified polypropylene master batch to the polytetrafluoroethylene master batch to the polypropylene grafted maleic anhydride is 20: 6: 100: 5.
s3: carrying out high-speed fluidization on the modified nano activated carbon particles by using high-temperature pressurized air, then synchronously jetting and stretching the melt jetted by the step S2 from one side of a spinneret plate as a traction airflow, and applying a magnetic field in the process to ensure that the concentration of the modified nano activated carbon particles is changed in a gradient manner from the center to two sides; and corona discharge is adopted in the gradual cooling process of the melt, and the melt-blown electret polymer filter material is obtained by rolling. The total weight of the active carbon of the prepared melt-blown electret polymer filter material accounts for 3 percent of the total mass of the filter material. The temperature of the fluidization operation is 150 ℃; the pressure of the fluidized air flow is 0.15MPa, the magnetic field intensity of the magnetic field is 1.5T, and the discharge voltage of the corona discharge is 40 KV.
The structural formula of the bacteriostatic agent is as shown in the chemical formula I in the example 1.
The modified nano activated carbon particles are prepared by the following steps:
s1: weighing 35 parts by weight of activated carbon, dispersing the activated carbon in 60 parts by weight of deionized water and 30 parts by weight of ethanol, adding 10 parts by weight of ferrous hydroxide, stirring for 2 hours at room temperature, and uniformly mixing to obtain a mixed solution; the particle size of the active carbon is 300 nm;
s2: carrying out ultrasonic oscillation on the mixed solution for 20min, adding 50 parts of potassium nitrate solution at the speed of 3g/min, wherein the mass concentration of the potassium nitrate solution is 25%, introducing oxygen at the speed of 500mL/min in the adding process, and keeping the stirring speed of 1200rpm to obtain a suspension of ferroferric oxide coated activated carbon;
s3: standing and aging the obtained suspension for 5 times and washing the suspension with deionized water, and then carrying out centrifugal filtration for 30min at the centrifugal speed of 5000rpm to obtain a solid filter cake;
s4: and drying the solid filter cake obtained by centrifugal filtration at 100 ℃ for 2 hours, and sieving the dried solid filter cake by using a 300-mesh vibrating screen to obtain the spherical composite particles of the modified nano activated carbon.
Example 3
The preparation method of the melt-blown electret polymer filter material of the embodiment comprises the following steps:
s1: weighing 100 parts of polypropylene, 0.5 part of tert-butyl peroxyisobutyrate, 25 parts of 4, 6-diallyl-N-octyl-1, 3, 5-triazine-2-amine and 20 parts of bacteriostatic agent, adding into a high-speed mixer, stirring and mixing uniformly at a high speed, and performing modification reaction and extrusion through an extruder to obtain the modified polypropylene master batch.
S2: uniformly mixing the modified polypropylene master batch, the polytetrafluoroethylene master batch, the polypropylene master batch and the polypropylene grafted maleic anhydride obtained in the step S1, heating and melting, and then ejecting a melt through a spinneret plate; the mass ratio of the modified polypropylene master batch to the polytetrafluoroethylene master batch to the polypropylene grafted maleic anhydride is 25: 8: 100: 10.
s3: carrying out high-speed fluidization on the modified nano activated carbon particles by using high-temperature pressurized air, then synchronously jetting and stretching the melt sprayed out in the step S2 from one side of a spinneret plate as a traction air flow, and applying a magnetic field in the process to ensure that the concentration of the modified nano activated carbon particles is changed in a gradient manner from the center to two sides; and corona discharge is adopted in the gradual cooling process of the melt, and the melt-blown electret polymer filter material is obtained by rolling. The total weight of the active carbon of the prepared melt-blown electret polymer filter material accounts for 5 percent of the total mass of the filter material. The temperature of the fluidization operation is 150 ℃; the pressure of the fluidized air flow is 0.15MPa, the magnetic field intensity of the magnetic field is 0.5T, and the discharge voltage of the corona discharge is 50 KV.
The structural formula of the bacteriostatic agent is as shown in the chemical formula I in the example 1.
The preparation method of the modified nano activated carbon particles is the same as that shown in example 2.
Comparative example 1
The preparation method of the melt-blown electret polymer filter material of the comparative example does not include the modified nano activated carbon particle compounding operation in step S3, and the other operation steps are the same as those in example 1.
The performance of the filter materials prepared in examples 1 to 3 and comparative example 1 was tested, and the performance results are shown in table 1:
wherein, a Boke G506 type particulate matter filtration efficiency tester, a Boke mask bacterial filtration efficiency [ BFE ] tester and a Boke G285 type gas exchange pressure difference tester, which are manufactured by Shandong Boke scientific instruments Co.
And (3) hydrophobic property test: and soaking the melt-blown fabric in water for 24 hours, taking out the melt-blown fabric, and then testing the performance of PM2.5 such as filtration efficiency, air permeability, bacteriostasis rate and the like.
And (3) testing heat resistance: and (3) placing the melt-blown fabric for 168 hours in an environment with constant temperature of 85 ℃ and constant humidity of 95%, and taking out the melt-blown fabric for testing the performances of PM2.5 filtration efficiency, air permeability, bacteriostasis rate and the like.
TABLE 1
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed.
Claims (9)
1. A method for preparing a melt-blown electret polymer filter material, which comprises the following steps:
s1: weighing 100 parts of polypropylene, 0.05-0.5 part of organic peroxide, 15-25 parts of triazine derivative and 10-20 parts of bacteriostatic agent by weight, adding into a high-speed mixer, stirring at a high speed, uniformly mixing, and performing modification reaction extrusion through an extruder to obtain modified polypropylene master batch;
s2: uniformly mixing the modified polypropylene master batch, the polytetrafluoroethylene master batch, the polypropylene master batch and the polypropylene grafted maleic anhydride obtained in the step S1, heating and melting, and then ejecting a melt through a spinneret plate;
s3: carrying out high-speed fluidization on the modified nano activated carbon particles by using high-temperature pressurized air, then synchronously jetting and stretching the melt sprayed out in the step S2 from one side of a spinneret plate as a traction air flow, and applying a magnetic field in the process to ensure that the concentration of the modified nano activated carbon particles is changed in a gradient manner from the center to two sides; corona discharge is adopted in the gradual cooling process of the melt, and the melt-blown electret polymer filter material is obtained by rolling;
the triazine derivative is at least one of 6-allyl-1, 3, 5-triazine-2, 4-diamine, 4, 6-bis (allyloxy) -N-butyl-1, 3, 5-triazine-2-amine, 4, 6-diallyloxy-N-octyl-1, 3, 5-triazine-2-amine and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine; the organic peroxide is at least one of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, di-tert-amyl peroxide, tert-butyl peroxyisobutyrate or 2, 2-bis (tert-butylperoxy) butane.
2. The method of making a melt-blown electret polymer filter material of claim 1 wherein the bacteriostatic agent is of formula I:
in the formula: r is propyl-N, N, N-trimethyl ammonium chloride.
3. The method for preparing the melt-blown electret polymer filter material of claim 1, wherein in step S2, the mass ratio of the modified polypropylene masterbatch, the polytetrafluoroethylene masterbatch, the polypropylene masterbatch and the polypropylene-grafted maleic anhydride is 15-25: 3-8: 100: 1 to 10.
4. The method of making a melt-blown electret polymer filter material of claim 1 wherein the modified nano-activated carbon particles are prepared by:
s1: weighing 25-65 parts by weight of activated carbon, dispersing the activated carbon in 50-80 parts by weight of deionized water and 20-40 parts by weight of ethanol, adding 6-15 parts by weight of ferrous hydroxide, stirring at room temperature for 1-3 hours, and uniformly mixing to obtain a mixed solution;
s2: carrying out ultrasonic oscillation on the mixed solution for 10-30 min, adding 35-80 parts of potassium nitrate solution at the speed of 1-5 g/min, and keeping the stirring speed of 800-1500 rpm in the adding process to obtain a suspension of ferroferric oxide coated activated carbon;
s3: standing and aging the obtained suspension for 3-5 times and washing the suspension with deionized water, and then carrying out centrifugal filtration for 20-40 min at a centrifugal speed of 3000-8000 rpm to obtain a solid filter cake;
s4: and drying the solid filter cake obtained by centrifugal filtration at the temperature of 80-120 ℃ for 0.5-3 hours, and sieving the dried solid filter cake by using a 300-mesh vibrating screen to obtain the spherical composite particles of the modified nano activated carbon.
5. The method of claim 4, wherein the particle size of the activated carbon is 100-500 nm.
6. The method for preparing a melt-blown electret polymer filter material according to claim 4, wherein the mass concentration of the potassium nitrate solution is 20-30%.
7. The method of making a melt-blown electret polymer filter material of claim 1 wherein the temperature of the fluidization is 110 to 150 ℃; the pressure of the air flow in the fluidization operation is 0.15-0.25 MPa.
8. The method of making a melt-blown electret polymer filter material of claim 1 wherein the magnetic field has a field strength of 0.5 to 1.5T.
9. The method for preparing a melt-blown electret polymer filter material according to claim 1, wherein the corona discharge has a discharge voltage of 30 to 50 KV.
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| CN113279139B (en) * | 2021-04-26 | 2022-06-17 | 杭州诗蓝过滤科技有限公司 | Preparation method of high-strength fluffy melt-blown fabric |
| CN114288756A (en) * | 2021-12-31 | 2022-04-08 | 浙江金海高科股份有限公司 | Preparation method of air filter screen, air filter screen and application of air filter screen |
| CN114504951B (en) * | 2022-01-24 | 2023-09-22 | 华南理工大学 | A recyclable electret filter membrane and its preparation method, cleaning and charge regeneration method |
| CN115284689A (en) * | 2022-07-22 | 2022-11-04 | 中采实业新材料(滁州)有限公司 | Air filtering melt-blown material with uniform ventilation |
| CN115251497A (en) * | 2022-08-24 | 2022-11-01 | 浙江圣蓝新材科技有限公司 | Mask with low-resistance melt-blown interlayer and preparation process thereof |
| CN115226975A (en) * | 2022-08-31 | 2022-10-25 | 浙江圣蓝新材科技有限公司 | Mask with electrostatic cotton interlayer and preparation process thereof |
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| JP2010076139A (en) * | 2008-09-24 | 2010-04-08 | Fujifilm Corp | Method for manufacturing laminated body |
| CN101905101B (en) * | 2010-07-30 | 2012-03-21 | 杭州电子科技大学 | Method for preparing melt-blown polypropylene electret filter material |
| CN103085374B (en) * | 2013-02-05 | 2014-12-10 | 宁波市奇兴无纺布有限公司 | Melt-blown activated carbon non-woven fabric and its production technology |
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