CN109837605B - Two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and preparation method thereof - Google Patents
Two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and preparation method thereof Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229920000728 polyester Polymers 0.000 title claims abstract description 57
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 32
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000314 lubricant Substances 0.000 claims abstract description 21
- 239000004094 surface-active agent Substances 0.000 claims abstract description 21
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 15
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 32
- 238000009987 spinning Methods 0.000 claims description 23
- 239000008187 granular material Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052961 molybdenite Inorganic materials 0.000 claims description 5
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 14
- 239000000835 fiber Substances 0.000 abstract description 14
- 210000002268 wool Anatomy 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000000463 material Substances 0.000 description 13
- 238000001816 cooling Methods 0.000 description 10
- 239000002135 nanosheet Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 229920006351 engineering plastic Polymers 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention provides a two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and a preparation method thereof, belonging to the technical field of high polymer materials. The composite brush wire comprises the following components in parts by weight: 60-96 parts of polyester, modified two-dimensional ultrathin nano TiO20.1-20 parts of antioxidant, 0.5-2 parts of lubricant and 0.5-8 parts of lubricant; the modified two-dimensional ultrathin nanometer TiO2Is prepared from two-dimensional ultra-thin nano TiO2Adding a surfactant for surface modification; the modified two-dimensional ultrathin nanometer TiO2The thickness is less than 50nm, and the diameter-thickness ratio is more than 5. The invention also provides a preparation method of the two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire. The polyester brush silk fiber surface of the invention has obvious concave-convex feeling, and the performance and the structure are similar to those of wool.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and a preparation method thereof.
Background
Engineering plastics are widely applied in the fields of electrical and electronic appliances, automotive interior trim, building decoration, aerospace manufacturing and the like, and China has become the country with the fastest increase of the demand of the engineering plastics. Polyester is the most rapidly developed of five major engineering plastics due to its excellent properties, although it is relatively late in industrialization in the polymer field. The polyester has excellent mechanical property, chemical corrosion resistance and good flow property, but the polyester is crystalline engineering plastic, has small forming shrinkage ratio and poor dimensional stability, and easily causes overlarge wing curvature of a product in the forming process, thereby limiting the application range of the polyester product. In addition, the difficulty of developing a new high-performance material is high, the research and development period is long, and the capital and the energy are high. Therefore, in order to meet different purposes, the best approach is to fill and modify the polymer, and some inorganic fillers which have different physicochemical properties from the prior resin matrix are added into the polymer matrix for modification research, so that a novel composite material with excellent performance is prepared by using a chemical method or a physical method. The method has the advantages of simplicity, effectiveness, low cost and easy industrial production, and greatly improves the application value of the polymer in industry.
The inorganic filler has special physical and chemical properties, and can obviously improve the mechanical property, the forming property, the thermal property and the like of the polymer, so the inorganic filler is rapidly applied and developed in the polymer modification technology.
Disclosure of Invention
The invention aims to provide a two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and a preparation method thereof. The polyester nano composite brush wire has good spinnability.
The invention firstly provides two-dimensional ultrathin TiO2The modified polyester nano composite brush wire comprises the following components in parts by weight:
60-96 parts of polyester, modified two-dimensional ultrathin nano TiO20.1-20 parts of antioxidant, 0.5-2 parts of lubricant and 0.5-8 parts of lubricant;
the modified two-dimensional ultrathin nanometer TiO2Is prepared from two-dimensional ultra-thin nano TiO2Adding a surfactant for surface modification;
the modified two-dimensional ultrathin nanometer TiO2The thickness is less than 50nm, and the diameter-thickness ratio is more than 5.
Preferably, the surfactant is one or two of KH550, KH560 or hexamethyldisilazane.
Preferably, the polyester is one of PET or PBT.
Preferably, the antioxidant is one or two of antioxidants 1010, 1076, B900 and 3114.
Preferably, the lubricant is MoS2Or one or two of PETS-XY 201A.
The invention also provides a preparation method of the two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire, which comprises the following steps:
the method comprises the following steps: preparation of two-dimensional ultrathin nano TiO2
Adding titanium tetrachloride into ethylene glycol under the protection of nitrogen, heating to reflux, and then adding water for reaction to obtain two-dimensional ultrathin nano TiO2；
Step two: modified two-dimensional ultrathin nano TiO2
Mixing a surfactant and the two-dimensional ultrathin nano TiO obtained in the step one2Reacting to obtain modified two-dimensional ultrathin nano TiO2；
Step three: melt blending
Polyester modified two-dimensional ultrathin nano TiO2Stirring and mixing the antioxidant and the lubricant until the mixture is uniform, and extruding and granulating the obtained mixture through a double-screw extruder to obtain granules;
step four: spinning formation
And (4) spinning and forming the granules obtained in the step three to obtain the two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire.
Preferably, the volume ratio of the ethylene glycol to the titanium tetrachloride in the first step is (5-100): 1, the volume ratio of titanium tetrachloride to water is (1-4): 1.
preferably, the reaction temperature of the second step is 60-80 ℃, and the reaction time is 2-6 h.
Preferably, the extrusion temperature in the third step is 220-.
Preferably, the spinning forming temperature of the step four is 220-260 ℃.
The invention has the advantages of
The invention provides two-dimensional ultrathin TiO2The modified polyester nanometer composite brush wire and the preparation method thereof, the method adds modified two-dimensional ultrathin nanometer TiO into the polyester material2By the pair of ultra-thin TiO2The nano sheets are subjected to surface modification, and polyester is filled in the nano sheets, so that the nano sheets are uniformly dispersed in a polyester matrix and have good compatibility, polyester fibers have good spinnability, the powder adhesion amount of polyester brush filaments is increased, the quality is stable, the fiber surfaces have obvious concave-convex feeling, the performance and the structure of the nano sheets are similar to those of wool, the added value of products is high, and the nano sheets can be widely applied to toothbrushes, dust removing brushes, various brushes in the cosmetic industry and the like.
Drawings
FIG. 1 is a scanning electron micrograph of a pure polyester spun at 250 times magnification.
FIG. 2 is a scanning electron micrograph of a pure polyester spun at 1000 times magnification.
FIG. 3 shows two-dimensional ultra-thin nano TiO prepared in example 2 of the present invention2Scanning electron microscope photograph of the modified polyester nano composite spinning at 650 times of magnification.
FIG. 4 shows two-dimensional ultra-thin nano TiO prepared in example 2 of the present invention2Scanning electron microscope photograph of the modified polyester nano composite spinning at 1000 times of magnification.
Detailed Description
The invention firstly provides a two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire which comprises the following components in parts by weight:
60-96 parts of polyester, modified two-dimensional ultrathin nano TiO20.1-20 parts of antioxidant, 0.5-2 parts of lubricant and 0.5-8 parts of lubricant; preferably: 92-96 parts of polyester, modified two-dimensional ultrathin nano TiO20.5-4 parts of antioxidant, 1 part of lubricant and 2.5-3 parts of lubricant;
the modified two-dimensional ultrathin nanometer TiO2Is prepared from two-dimensional ultra-thin nano TiO2Adding a surfactant for surface modification; the surfactant is preferably one or two of KH550, KH560 or hexamethyldisilazane. The invention uses the surface active agent to process two-dimensional ultrathin nanometer TiO2Surface modification is carried out to ensure that two-dimensional ultrathin nano TiO2The dispersion in the polyester matrix resin is better, so that the performance of the polyester material is improved.
The modified two-dimensional ultrathin nanometer TiO2Is less than 50nm, preferably 20nm, and has a diameter-thickness ratio of more than 5, preferably 10. The invention limits the modified two-dimensional ultrathin nanometer TiO2When the thickness ratio is too small, the dispersibility of a nano-sheet layer material in a polyester matrix can be influenced, the spinning effect is influenced, the concave-convex feeling on the surface of the nano-composite brush wire can be influenced, the lamella is too small, the concave-convex feeling on the surface of the nano-composite brush wire is not caused, and the sheep-like sheep cannot be imitatedThe microstructure of the surface of the hair causes the sticky powder amount of the nano composite brush wire to be greatly reduced. .
According to the invention, the polyester is preferably one of PET and PBT, the antioxidant and the lubricant are preferably auxiliary agents conventional in the field, and the antioxidant is preferably one or two of antioxidants 1010, 1076, B900 and 3114; the lubricant is preferably MoS2Or one or two of PETS-XY 201A.
The invention also provides a preparation method of the two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire, which comprises the following steps:
the method comprises the following steps: preparation of two-dimensional ultrathin nano TiO2
Under the protection of nitrogen, adding titanium tetrachloride into ethylene glycol, heating to reflux, then adding water for reaction, after the reaction is finished, cooling to room temperature, centrifugally separating and washing to obtain the two-dimensional ultrathin nano TiO2(ii) a The reaction time is preferably 30min-5 h; more preferably 2-4h, and the volume ratio of the ethylene glycol to the titanium tetrachloride is preferably (5-100): 1, more preferably (5-6): 1, the volume ratio of titanium tetrachloride to water is preferably (1-4): 1, more preferably (1-1.25): 1; the glycol is used as a guiding agent;
step two: modified two-dimensional ultrathin nano TiO2
Mixing a surfactant and the two-dimensional ultrathin nano TiO obtained in the step one2Reacting to obtain modified two-dimensional ultrathin nano TiO2(ii) a Specifically, it is preferable that: mixing two-dimensional ultrathin nano TiO2Back dispersing in a mixed solution of water and ethanol, performing ultrasonic dispersion, wherein the dispersion time is preferably 50-60min, adding a surfactant for reaction, the reaction temperature is preferably 60-80 ℃, the time is preferably 2-6h, cooling, centrifuging, and drying, wherein the centrifugal rotation speed is preferably 4000-6000r/min, the drying temperature is preferably 60-140 ℃, and the drying time is preferably 12-24 h; the addition of the surfactant is two-dimensional ultrathin nano TiO22-10% by mass, more preferably 5%;
step three: melt blending
Polyester modified two-dimensional ultrathin nano TiO2Stirring and mixing the antioxidant and the lubricant until the mixture is uniform, and extruding and granulating the obtained mixture through a double-screw extruder to obtain granules; the polyester and the modified two-dimensional ultrathin nanometer TiO2Before mixing, preferably drying the materials respectively to improve the processing performance of the materials, wherein the drying temperature is preferably 95-125 ℃, and the drying time is preferably 2-8 hours; the extrusion temperature is preferably 220-260 ℃, more preferably 230-240 ℃, and the screw rotation speed is preferably 100-150r/min, more preferably 150 r/min;
step four: spinning formation
Spinning and forming the granules obtained in the third step, cutting the granules, soaking the obtained composite spinning fiber in NaOH solution for sharpening to obtain two-dimensional ultrathin TiO2Modified polyester nano composite brush filaments. The spinning forming temperature is preferably 220-260 ℃, and more preferably 230-235 ℃; the concentration of the NaOH solution is preferably 30%.
The present invention is described in further detail below with reference to specific examples, in which the starting materials are all commercially available.
Example 1
Adding 0.5L titanium tetrachloride into 3.0L ethylene glycol under the protection of nitrogen, heating to reflux, adding 0.5L water to react with the titanium tetrachloride, after reacting for 2.0h, cooling to room temperature, performing centrifugal separation and washing to obtain two-dimensional ultrathin nano TiO2。
Mixing two-dimensional ultrathin nano TiO2Back dispersing in mixed solution of water and ethanol (volume ratio of water to ethanol is 9:1), performing ultrasonic dispersion for 50min, adding surfactant KH550, reacting at 70 deg.C for 4h, cooling, centrifuging at 5000r/min, drying at 100 deg.C overnight, wherein the addition amount of the surfactant is two-dimensional ultrathin nanometer TiO25% of the mass; obtaining modified two-dimensional ultrathin nano TiO2M (thickness of 20nm, thickness to diameter ratio of 15).
PBT material and modified two-dimensional ultrathin nanosheet TiO2Drying at 110 ℃ for 6 hours by using the drying method of-M, wherein the spinnability of the fiber can be improved; then, mixing the PBT material in parts by weight: 96 parts of modified two-dimensional ultrathin nano TiO2-M: 0.5 part, antioxidant 1076: 1 part, lubricant PETS-XY 201A: 2.5 parts of the mixture is stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 230 deg.C and screw rotation speed of 150r/min to obtain granules;
then drying the granules in a vacuum oven at 110 ℃; extruding and spinning the granules at 230 ℃, cutting, soaking the obtained composite spinning fiber in 30% NaOH solution for sharpening to obtain the two-dimensional ultrathin TiO2Modified PBT nanometer composite brush wire.
The performance test data of the composite brush filaments prepared in example 1 are shown in table 1.
Example 2
Adding 0.5L titanium tetrachloride into 3.0L ethylene glycol under the protection of nitrogen, heating to reflux, adding 0.5L water to react with the titanium tetrachloride, after reacting for 2.0h, cooling to room temperature, performing centrifugal separation and washing to obtain two-dimensional ultrathin nano TiO2。
Mixing two-dimensional ultrathin nano TiO2Back dispersing in mixed solution of water and ethanol (volume ratio of water to ethanol is 9:1), performing ultrasonic dispersion for 50min, adding surfactant KH550, reacting at 70 deg.C for 4h, cooling, centrifuging at 5000r/min, drying at 100 deg.C overnight, wherein the addition amount of the surfactant is two-dimensional ultrathin nanometer TiO25% of the mass; obtaining modified two-dimensional ultrathin nano TiO2M (thickness of 20nm, thickness to diameter ratio of 15).
PBT material and modified two-dimensional ultrathin nano TiO2Drying at 110 ℃ for 6 hours by using the drying method of-M, wherein the spinnability of the fiber can be improved; then preparing the PBT material according to the parts by weight: 95.5 parts of modified two-dimensional ultrathin nano TiO2-M: 1.0 part, antioxidant 1010: 1 part of lubricant MoS2: 2.5 parts of the mixture is stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 230 deg.C and screw rotation speed of 150r/min to obtain granules;
then drying the granules in a vacuum oven at 110 ℃; extruding and spinning the granules at the temperature ofCutting at 230 ℃, soaking the obtained composite spinning fiber in 30% NaOH solution for sharpening to obtain two-dimensional ultrathin TiO2Modified PBT nanometer composite brush wire.
FIGS. 1 and 2 are scanning electron micrographs of pure polyester spun yarn at 250 and 1000 times magnification, respectively. FIGS. 3 and 4 show two-dimensional ultra-thin nanometer TiO prepared in example 2 of the present invention2Scanning electron microscope photographs of the modified polyester nanocomposite spun yarn at magnification of 650 and 1000 times. Compared with pure polyester spinning, the surface of the fiber has obvious concave-convex feeling, which indicates that the structure of the fiber is similar to that of wool.
The performance test data of the composite brush wire prepared in example 2 is shown in table 1.
Example 3
Adding 1.0L of titanium tetrachloride into 5.0L of ethylene glycol under the protection of nitrogen, heating to reflux, adding 0.8L of water to react with the titanium tetrachloride, cooling to room temperature after reacting for 4.0h, performing centrifugal separation and washing to obtain the two-dimensional ultrathin nano TiO2。
Mixing two-dimensional ultrathin nano TiO2Back dispersing in mixed solution of water and ethanol (volume ratio of water to ethanol is 9:1), performing ultra-living dispersion for 50min, adding surfactant KH560, reacting at 70 deg.C for 4h, cooling, centrifuging at 5000r/min, drying at 100 deg.C overnight, wherein the addition amount of the surfactant is two-dimensional ultrathin nanometer TiO25% of the mass; obtaining modified two-dimensional ultrathin nano TiO2M (thickness of 15nm, thickness to diameter ratio of 20).
PET material and modified two-dimensional ultrathin nano TiO2Drying at 110 ℃ for 6 hours by using the drying method of-M, wherein the spinnability of the fiber can be improved; then, the PET material in parts by weight: 94 portions of modified two-dimensional ultrathin nano TiO2-M: 2.0 parts of antioxidant 1010: 1 part, lubricant PETS-XY 201A: 3 parts of the mixture is stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 240 deg.c and screw rotation speed of 150r/min to obtain granular material;
then drying the granules in a vacuum oven at 110 ℃; extruding and spinning the granules at a certain temperatureThe temperature is 235 ℃, the obtained composite spinning fiber is soaked in 30 percent NaOH solution for sharpening after being sheared, and the two-dimensional ultrathin TiO is obtained2Modified PET nano composite brush filaments.
The performance test data of the composite brush wire prepared in example 3 is shown in table 1.
Example 4
Adding 1.0L of titanium tetrachloride into 5.0L of ethylene glycol under the protection of nitrogen, heating to reflux, adding 0.8L of water to react with the titanium tetrachloride, cooling to room temperature after reacting for 4.0h, performing centrifugal separation and washing to obtain the two-dimensional ultrathin nano TiO2。
Mixing two-dimensional ultrathin nano TiO2Back dispersing in mixed solution of water and ethanol (volume ratio of water to ethanol is 9:1), performing ultra-living dispersion for 50min, adding surfactant KH560, reacting at 70 deg.C for 4h, cooling, centrifuging at 5000r/min, drying at 100 deg.C overnight, wherein the addition amount of the surfactant is two-dimensional ultrathin nanometer TiO25% of the mass; obtaining modified two-dimensional ultrathin nano TiO2M (thickness of 15nm, thickness to diameter ratio of 20).
PET material and modified two-dimensional ultrathin nano TiO2Drying at 110 ℃ for 6 hours by using the drying method of-M, wherein the spinnability of the fiber can be improved; then, the PET material in parts by weight: 92 parts of modified two-dimensional ultrathin nano TiO2-M: 4 parts, antioxidant 1076: 1 part of lubricant MoS2: 3 parts of the mixture is stirred and mixed to be uniform, and the mixture is extruded and granulated by a double-screw extruder by adopting a melt blending method; extruding at 240 deg.c and screw rotation speed of 150r/min to obtain granular material;
then drying the granules in a vacuum oven at 110 ℃; spinning the granules; extruding and spinning the granules at 235 ℃, cutting, soaking the obtained composite spinning fiber in 30% NaOH solution for sharpening to obtain the two-dimensional ultrathin TiO2Modified PET nano composite brush filaments.
The performance test data of the composite brush wire prepared in example 4 is shown in table 1.
TABLE 1
The technical solutions provided by the embodiments of the present invention are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the embodiments are only used to help understanding the principles of the embodiments of the present invention; meanwhile, for a person skilled in the art, according to the embodiments of the present invention, there may be variations in the specific implementation and application ranges, and in summary, the content of the present description should not be construed as a limitation to the present invention.
Claims (10)
1. The two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire is characterized by comprising the following components in parts by weight:
60-96 parts of polyester, modified two-dimensional ultrathin nano TiO20.1-20 parts of antioxidant, 0.5-2 parts of lubricant and 0.5-8 parts of lubricant;
the modified two-dimensional ultrathin nanometer TiO2Is prepared from two-dimensional ultra-thin nano TiO2Adding a surfactant for surface modification;
the modified two-dimensional ultrathin nanometer TiO2The thickness is less than 50nm, and the diameter-thickness ratio is more than 5.
2. The two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush filaments according to claim 1, wherein the surfactant is one or two of KH550, KH560 or hexamethyldisilazane.
3. The two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush wire according to claim 1, wherein the polyester is one of PET or PBT.
4. The two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush wire according to claim 1, wherein the antioxidant is one or two of antioxidants 1010, 1076, B900 and 3114.
5. The two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush wire according to claim 1, wherein the lubricant is MoS2Or one or two of PETS-XY 201A.
6. The method for preparing the two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire as claimed in claim 1, is characterized by comprising the following steps:
the method comprises the following steps: preparation of two-dimensional ultrathin nano TiO2
Adding titanium tetrachloride into ethylene glycol under the protection of nitrogen, heating to reflux, and then adding water for reaction to obtain two-dimensional ultrathin nano TiO2；
Step two: modified two-dimensional ultrathin nano TiO2
Mixing a surfactant and the two-dimensional ultrathin nano TiO obtained in the step one2Reacting to obtain modified two-dimensional ultrathin nano TiO2；
Step three: melt blending
Polyester modified two-dimensional ultrathin nano TiO2Stirring and mixing the antioxidant and the lubricant until the mixture is uniform, and extruding and granulating the obtained mixture through a double-screw extruder to obtain granules;
step four: spinning formation
Spinning and forming the granules obtained in the third step to obtain two-dimensional ultrathin TiO2Modified polyester nano composite brush filaments.
7. The method for preparing the two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush filaments according to claim 6, wherein the volume ratio of the ethylene glycol to the titanium tetrachloride in the first step is (5-100): 1, the volume ratio of titanium tetrachloride to water is (1-4): 1.
8. the preparation method of the two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush wire according to claim 6, wherein the reaction temperature in the second step is 60-80 ℃ and the reaction time is 2-6 hours.
9. The method for preparing a two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush wire as claimed in claim 6, wherein the extrusion temperature in the third step is 220-260 ℃, and the screw rotation speed is 100-150 r/min.
10. The method for preparing two-dimensional ultrathin titanium dioxide modified polyester nanocomposite brush wires as claimed in claim 6, wherein the spinning molding temperature in the fourth step is 220-260 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910089521.1A CN109837605B (en) | 2019-01-30 | 2019-01-30 | Two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and preparation method thereof |
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| CN201910089521.1A CN109837605B (en) | 2019-01-30 | 2019-01-30 | Two-dimensional ultrathin titanium dioxide modified polyester nano composite brush wire and preparation method thereof |
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| Publication Number | Publication Date |
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| CN116145280A (en) * | 2022-12-31 | 2023-05-23 | 诸暨市锦晨纺织有限公司 | TiO (titanium dioxide) 2 PHMG composite modified PET antibacterial fabric and preparation method thereof |
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