CN116770451A - Preparation method of novel cool-feeling cool jade fiber with multiple functions - Google Patents
Preparation method of novel cool-feeling cool jade fiber with multiple functions Download PDFInfo
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- CN116770451A CN116770451A CN202310621132.5A CN202310621132A CN116770451A CN 116770451 A CN116770451 A CN 116770451A CN 202310621132 A CN202310621132 A CN 202310621132A CN 116770451 A CN116770451 A CN 116770451A
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- 239000000835 fiber Substances 0.000 title claims abstract description 62
- 239000010977 jade Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 206010016326 Feeling cold Diseases 0.000 title claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000009987 spinning Methods 0.000 claims abstract description 36
- 239000004005 microsphere Substances 0.000 claims abstract description 35
- 238000005406 washing Methods 0.000 claims abstract description 18
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 26
- 229920002873 Polyethylenimine Polymers 0.000 claims description 25
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 25
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 25
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 20
- 229920000642 polymer Polymers 0.000 claims description 19
- 238000007334 copolymerization reaction Methods 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 15
- 239000003995 emulsifying agent Substances 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 8
- 238000006136 alcoholysis reaction Methods 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 claims description 4
- UICXTANXZJJIBC-UHFFFAOYSA-N 1-(1-hydroperoxycyclohexyl)peroxycyclohexan-1-ol Chemical compound C1CCCCC1(O)OOC1(OO)CCCCC1 UICXTANXZJJIBC-UHFFFAOYSA-N 0.000 claims description 3
- MMEDJBFVJUFIDD-UHFFFAOYSA-N 2-[2-(carboxymethyl)phenyl]acetic acid Chemical compound OC(=O)CC1=CC=CC=C1CC(O)=O MMEDJBFVJUFIDD-UHFFFAOYSA-N 0.000 claims description 3
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 229920001577 copolymer Polymers 0.000 claims 1
- 238000005469 granulation Methods 0.000 claims 1
- 230000003179 granulation Effects 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 20
- 238000002156 mixing Methods 0.000 abstract description 13
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 239000004744 fabric Substances 0.000 abstract description 7
- 241000222122 Candida albicans Species 0.000 abstract description 5
- 241000588724 Escherichia coli Species 0.000 abstract description 5
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 5
- 229940095731 candida albicans Drugs 0.000 abstract description 5
- 239000004952 Polyamide Substances 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000004220 aggregation Methods 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- 229920002647 polyamide Polymers 0.000 abstract description 3
- 229920006149 polyester-amide block copolymer Polymers 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000004482 other powder Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 19
- 239000002245 particle Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 12
- 230000000694 effects Effects 0.000 description 7
- 230000006750 UV protection Effects 0.000 description 6
- 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 5
- 150000001450 anions Chemical class 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 5
- 241000205585 Aquilegia canadensis Species 0.000 description 4
- 240000006891 Artemisia vulgaris Species 0.000 description 4
- 235000003261 Artemisia vulgaris Nutrition 0.000 description 4
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- 238000004132 cross linking Methods 0.000 description 4
- 229940002508 ginger extract Drugs 0.000 description 4
- 235000020708 ginger extract Nutrition 0.000 description 4
- 229940094952 green tea extract Drugs 0.000 description 4
- 235000020688 green tea extract Nutrition 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
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- 238000009740 moulding (composite fabrication) Methods 0.000 description 4
- 210000004243 sweat Anatomy 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 3
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
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- 230000006872 improvement Effects 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 2
- 229920000053 polysorbate 80 Polymers 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000004769 CoolMax Substances 0.000 description 1
- 241001602762 Sophista Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- VBICKXHEKHSIBG-UHFFFAOYSA-N beta-monoglyceryl stearate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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Landscapes
- Artificial Filaments (AREA)
Abstract
The invention provides a preparation method of novel cool-feeling cool jade fiber with multiple functions, which comprises the steps of preparing functional microspheres, preparing functional master batches and spinning. Coating and modifying ice jade powder, plant source powder, nano titanium dioxide and other powder to obtain functional microsphere, and melt blending with polyester or polyamide to obtain special-shaped productThe cross section spinning molding, the product has various composite functions such as natural cool feeling, suction and exhaust, and the like, and effectively solves the problems of infinite aggregation, uneven distribution, unstable product functionality, blockage of spinning holes, strength reduction and the like of functional powder in the processes of blending spinning and special-shaped spinning. The ice jade fiber prepared by the invention is woven into a fabric, and after 50 times of washing, the antibacterial rate to staphylococcus aureus is measured to be more than 99%, the antibacterial rate to escherichia coli is measured to be more than 99%, and the antibacterial rate to candida albicans is measured to be more than 97%; the contact cool feeling coefficient is greater than 0.2J/(cm) 2 S) the average value of the moisture absorption quick-drying property after 5 times of water washing is 5 grades.
Description
Technical Field
The invention belongs to the technical field of fibers, and particularly relates to a preparation method of novel cool-feeling cool jade fibers with multiple functions.
Background
In order to meet the requirements of people on comfort and coolness of summer clothing, low-carbon clothing life is realized, and development of fibers with a multifunctional cooling function becomes a focus of attention in the current chemical fiber industry. The fabric woven by the cool feeling fiber has excellent contact cool feeling and also has good additional functions of moisture absorption, sweat discharge and the like. The principle of adding substances with high heat conductivity into the fiber by a blending melt spinning or in-situ polymerization method is to increase the conduction and heat dissipation of a human body, and the human body can rapidly transfer heat when contacting with substances with higher heat conductivity, so that a cool feeling is obtained. At present, the common cool feeling fiber in the market is usually realized by adding jade powder or mica powder, and the heat conductivity of the jade powder is more than 5 times of that of chemical fiber, so that the chemical fiber can generate contact cool feeling by adding the jade powder, or the evaporation of human sweat can be accelerated by designing the special-shaped fiber section so as to release heat.
The common special-shaped cross section of the cool sense fiber is provided with a plurality of grooves, the capillary effect is strong, the conduction of moisture on the fabric is promoted, the specific surface area of the fiber is large, the evaporation speed of sweat distributed on the surface of the special-shaped fiber can be greatly increased, more moisture conduction paths are arranged among the flat fibers, the contact area with a human body is large, and the heat conduction and the heat dissipation are more facilitated.
Dupont CoolMax is a PET fiber of profiled cross section, which has a flat cross-section, thus having a unique hollow four-tube cross-section structure. The cross-section structure greatly enhances the capillary effect of the fiber, greatly increases the specific surface area, endows the fabric with excellent moisture absorption and perspiration performance, and can quickly conduct body surface perspiration to the surface of the fabric and evaporate, so that a cool feeling is generated, and the skin can be kept dry and comfortable in hot summer.
The Sophista of Japanese colali company is a sheath-core composite fiber, the sheath layer is polyvinyl alcohol with strong hygroscopicity, the core layer is common polyester fiber, the polyvinyl alcohol on the surface layer has hydrophilic groups, all the moisture absorption and water absorption are excellent, and the human body can generate cool feeling through heat conduction and dissipation of moisture.
The patent number CN201711238655.2 is named as a preparation method of superfine denier absorbing and discharging cool antibacterial fiber, nano cool jade powder and polyester melt are mixed at high speed, and then are sprayed and formed by adopting a cross-section spinneret orifice, but the nano cool jade powder has small particle size and is easy to aggregate to form larger-size aggregates, so that the nano particles cannot be uniformly dispersed in a single state, the improvement effect of the nano particles on the polymer performance is reduced, and the loss rate of the jade powder is increased by special-section spinneret, so that the contact cool feeling coefficient is less than 0.15, and the national standard requirement is not met. The single cool fiber has poor functional diversity, can not meet the requirements of consumers, and has the functional effects of cool, antibacterial, ultraviolet resistance and the like, so that the fiber is popular with people.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a novel cool-feeling cool jade fiber with multiple functions, which is characterized in that ultra-fine nano powder such as cool jade powder, plant source powder and titanium dioxide is modified and then is melt-blended with polyester or polyamide, and is formed by special-shaped cross-section spinning, so that the product has multiple composite functions such as natural cool feeling and suction and discharge, and the problems of infinite aggregation, uneven distribution, unstable product functionality and strong decline of functional powder in the special-shaped spinning process are effectively solved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of novel cool-feeling cool jade fiber with multiple functions comprises the following steps:
s1, preparation of functional microspheres
Stirring unsaturated polyester resin, polyethyleneimine and functional powder at a high speed for 15-20min, wherein the stirring speed is 2000-2400rpm, adding an initiator and an accelerator, stirring at 40-50 ℃ for reacting for 60-90min, and performing copolymerization and cross-linking on the polyethyleneimine and the double bonds of the unsaturated polyester resin at the stirring speed of 600-700rpm to obtain a copolymerization mixture gel; adding the copolymerization mixture gel into an aqueous phase, stirring for 30-40min at a stirring speed of 200-300rpm, performing suction filtration and washing, washing the product with distilled water at 95-98 ℃, forming a coating layer on the surface of the functional powder, and drying to obtain the functional microsphere with a particle size of 1-2 μm.
Preferably, the unsaturated polyester resin is o-benzene unsaturated polyester resin, and the viscosity at 25 ℃ is 0.85-1.25 Pa.s; the molecular weight of the polyethyleneimine is 1200-1800, and the viscosity at 25 ℃ is 8000-10000 MPa.s.
Preferably, the functional powder is one or more of ice jade powder, nano titanium dioxide and plant source powder; the particle size of the ice jade powder is 500nm, the particle size of the nano titanium dioxide is 20-50nm, the particle size of the plant source powder is 300-400nm, and the mass ratio of the ice jade powder to the nano titanium dioxide to the plant source powder is 10-12:4-6:10-12.
Further, the plant source powder is one or more of honeysuckle extract, mugwort extract, ginger extract, green tea extract and the like.
Preferably, the mass ratio of the unsaturated polyester resin to the polyethyleneimine to the functional powder is 60-75:20-30:10-15.
Preferably, the initiator is one or more of benzoyl peroxide, lauroyl peroxide, cyclohexanone peroxide and azobisisobutyronitrile; the promoter is one or more of cobalt naphthenate, cobalt octoate and dimethylaniline.
Preferably, the initiator is added in an amount of 1 to 1.5wt% of the unsaturated polyester resin; the addition amount of the accelerator is 0.5-0.8wt% of the unsaturated polyester resin.
Preferably, the water phase is a mixture of polyvinyl alcohol, an emulsifying agent and distilled water; the mass ratio of the polyvinyl alcohol to the emulsifier to the distilled water is 10-15:0.9-1.2:100-110; the alcoholysis degree of the polyvinyl alcohol is more than 99%.
Further, the emulsifier is one or more of Span80 and Tween80.
Preferably, the volume ratio of the polymer gel blend to the aqueous phase is 1:3-5.
S2, preparing functional master batch
Crushing the polymer slice to 10-20 mu m, blending with the functional microsphere, granulating by adopting a double screw extruder, and vacuum drying at 100-120 ℃ after granulating to obtain the functional master batch.
Preferably, the mass ratio of the functional microsphere to the polymer slice is 10-15:85-90; the polymer slice is one of PET or PA.
S3, spinning
And (3) blending and melting the functional master batch and the polymer slice, feeding the blend into a spinning box body, extruding out through a spinning hole, oiling after cooling through blowing, and winding and forming to obtain the ice jade fiber.
Preferably, the mass ratio of the functional master batch to the polymer slice is 6-9:91-94.
Preferably, the spinneret orifice has a cross-shaped cross section.
Preferably, additives such as lubricants, antioxidants and the like can be added in the spinning process; the lubricant is one or more of zinc stearate, stearic acid monoglyceride, ethylene bisstearamide and oleamide, and the antioxidant is one or more of antioxidant 1010 and antioxidant 168.
Preferably, the lubricant is added in an amount of 0.5 to 0.7wt% of the polymer chip, and the antioxidant is added in an amount of 0.2 to 0.3wt% of the polymer chip.
By adopting the technical scheme, the invention has the following technical effects:
1. the novel cool-feeling cool jade fiber prepared by the invention has multiple effects of cool contact, antibiosis, anion, moisture absorption, sweat release, ultraviolet resistance and the like, can be applied to various aspects such as knitting (T-shirts, underwear, socks and the like), weaving (shirts, jeans, leisure and the like), home textile and the like, and can be particularly applied to summer clothing, and is cool and comfortable when being worn.
2. The ice jade fiber prepared by the invention has excellent multiple functions, the fiber is woven into the fabric, after 50 times of washing, the antibacterial rate to staphylococcus aureus is more than 99%, the antibacterial rate to escherichia coli is more than 99%, the antibacterial rate to candida albicans is more than 97%, and the fabric meets the 3A-level antibacterial standard (according to GB/T20944.3-2008, the evaluation of the antibacterial property of textiles, part 3: vibration method); the contact cool feeling coefficient is greater than 0.2J/(cm) 2 S) (measured according to GB/T35263-2017), the average value of the moisture absorption and quick drying performance after 5 times of water washing is 5 grades (measured according to GB/T21655.2-2019), the UPF value of ultraviolet resistance is more than 50 (measured according to GB/T18830-2009), and the negative ion generation amount is not less than 700 per cm 3 (measured according to GB/T30128-2013).
3. The functional microspheres prepared by coating and modifying the ice jade powder, the plant source powder, the nano titanium dioxide and other powder are not limitlessly aggregated into large particles among the microspheres in the melt blending process with polyester or polyamide and the special-shaped cross-section spinning forming process, so that the stability of the product function is ensured, and the problems of infinite aggregation, uneven distribution, unstable product functionality, blocking of spinning holes, strength reduction and the like of the functional powder in the blending spinning process and the special-shaped spinning process are effectively solved.
4. The unsaturated polyester resin and the polyethyleneimine are copolymerized and crosslinked to coat the functional powder, so that the thermal stability and the compatibility with polymer slices of the powder are improved, the loss of the functional powder is reduced, and the functional durability of the product is further improved; meanwhile, the defects of high brittleness and poor mechanical property of the unsaturated polyester resin are overcome by copolymerizing the polyethyleneimine and the unsaturated polyester resin, and the polyethyleneimine has polar amino groups and amphipathy, and is added into the fiber after being copolymerized with the unsaturated polyester resin, so that the dispersibility is improved, and the hygroscopicity of the fiber is further improved; polyvinyl alcohol is added into the water phase, the alcoholysis degree of the polyvinyl alcohol is more than 99%, so the polyvinyl alcohol is insoluble in water at normal temperature and doped into the copolymerization mixture, the microspheres are formed and then doped on the surfaces of the microspheres, the polyvinyl alcohol on the surfaces is removed after the microspheres are washed with high temperature, the surfaces of the microspheres are microporous, the specific surface area is increased, the hygroscopicity is better, and the functional powder can also play a role better.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1
S1, preparation of functional microspheres
Stirring unsaturated polyester resin, polyethyleneimine and functional powder at a high speed for 15-20min, wherein the stirring speed is 2200rpm, adding an initiator and an accelerator, stirring at 45 ℃ for reacting for 80min, and performing copolymerization and crosslinking on the polyethyleneimine and the double bonds of the unsaturated polyester resin at the stirring speed of 600rpm to obtain a copolymerization mixture gel; adding the copolymerization mixture gel into the water phase, stirring for 35min at the stirring speed of 300rpm, filtering, washing the product with 97 ℃ distilled water, forming a coating layer on the surface of the functional powder, and drying to obtain the functional microsphere with the particle size of 1 μm.
The unsaturated polyester resin is o-benzene unsaturated polyester resin, and the viscosity of the unsaturated polyester resin is 0.95 Pa.s at 25 ℃; the molecular weight of the polyethyleneimine is 1500, and the viscosity at 25 ℃ is 9000 MPa.s.
The functional powder is ice jade powder, nano titanium dioxide and plant source powder; the particle size of the ice jade powder is 500nm, the particle size of the nano titanium dioxide is 20nm, the particle size of the plant source powder is 300nm, and the mass ratio of the ice jade powder to the nano titanium dioxide to the plant source powder is 11:5:11.
The plant source powder is prepared from honeysuckle extract, mugwort extract, ginger extract and green tea extract in a mass ratio of 1:1:1:1.
The mass ratio of the unsaturated polyester resin to the polyethyleneimine to the functional powder is 68:15:13.
the initiator is benzoyl peroxide; the promoter is cobalt naphthenate.
The addition amount of the initiator is 1.4wt% of the unsaturated polyester resin; the addition amount of the accelerator is 0.6wt% of the unsaturated polyester resin.
The water phase is a mixture of polyvinyl alcohol, an emulsifying agent and distilled water; the mass ratio of the polyvinyl alcohol to the emulsifier to the distilled water is 12:1:105; the alcoholysis degree of the polyvinyl alcohol is 99.2%; the emulsifier is Span80.
The volume ratio of the polymer gel blend to the aqueous phase was 1:4.
S2, preparing functional master batch
And (3) crushing the PET slices to 10 mu m, blending the PET slices with the functional microspheres, granulating by adopting a double-screw extruder, and vacuum drying at 110 ℃ for 5 hours after granulating to obtain the functional master batch.
The mass ratio of the functional microsphere to the PET slice is 12:88.
S3, spinning
And (3) blending and melting the functional master batch and the PET slice, feeding the blend into a spinning box body, extruding out through a spinneret orifice, oiling after cooling through blowing, and winding and forming to obtain the ice jade fiber.
The mass ratio of the functional master batch to the PET slice is 8:92; the spinneret orifice is in a cross-shaped section.
The temperature of the spinning box body is 270 ℃, the spinning speed is 600m/min, and the blowing temperature is 15 ℃.
Zinc stearate and an antioxidant 1010 are added in the spinning process; the addition amount of the zinc stearate is 0.6wt% of the PET slice, and the addition amount of the antioxidant 1010 is 0.25wt% of the PET slice.
The ice jade fiber prepared in the example 1 has the breaking strength of 4.2cN/dtex, and after 50 times of water washing, the antibacterial rate to staphylococcus aureus is 99.55%, the antibacterial rate to escherichia coli is 99.36%, and the antibacterial rate to candida albicans is 98.2%; the contact cool feeling coefficient was measured to be 0.26J/(cm) 2 S), after washing for 5 times, the average value of the moisture absorption and quick drying performance is 5 level, the UPF value of the ultraviolet resistance is more than 50, and the anion generation amount is 800 per cm 3 The fiber moisture regain is 3.7%, and the functional powder loss rate is 1.36%.
Example 2
S1, preparation of functional microspheres
Stirring unsaturated polyester resin, polyethyleneimine and functional powder at a high speed for 15min, wherein the stirring speed is 2000rpm, adding an initiator and an accelerator, stirring at 40 ℃ for reacting for 60min, and performing copolymerization and crosslinking on the double bonds of the polyethyleneimine and the unsaturated polyester resin at the stirring speed of 600rpm to obtain a copolymerization mixture gel; adding the copolymerization mixture gel into the water phase, stirring for 30min at the stirring speed of 200rpm, filtering, washing the product with distilled water at 95 ℃, forming a coating layer on the surface of the functional powder, and drying to obtain the functional microsphere with the particle size of 1.6 mu m.
The unsaturated polyester resin is o-benzene unsaturated polyester resin, and the viscosity of the unsaturated polyester resin is 0.85 Pa.s at 25 ℃; the molecular weight of the polyethyleneimine is 1200, and the viscosity at 25 ℃ is 8000 MPa.s.
The functional powder is ice jade powder, nano titanium dioxide and plant source powder; the particle size of the ice jade powder is 500nm, the particle size of the nano titanium dioxide is 50nm, the particle size of the plant source powder is 400nm, and the mass ratio of the ice jade powder to the nano titanium dioxide to the plant source powder is 10:4:10.
The plant source powder is prepared from honeysuckle extract, mugwort extract, ginger extract and green tea extract in a mass ratio of 1:1:1:1.
The mass ratio of the unsaturated polyester resin to the polyethyleneimine to the functional powder is 60:20:10.
the initiator is cyclohexanone peroxide; the promoter is cobalt naphthenate.
The addition amount of the initiator is 1wt% of the unsaturated polyester resin; the addition amount of the accelerator is 0.8wt% of the unsaturated polyester resin.
The water phase is a mixture of polyvinyl alcohol, an emulsifying agent and distilled water; the mass ratio of the polyvinyl alcohol to the emulsifier to the distilled water is 10:0.9:100; the alcoholysis degree of the polyvinyl alcohol is 99.2%; the emulsifier is Tween80.
The volume ratio of the polymer gel blend to the aqueous phase was 1:3.
S2, preparing functional master batch
And (3) crushing the PET slices to 20 mu m, blending the PET slices with the functional microspheres, granulating by adopting a double-screw extruder, and vacuum drying at 100 ℃ for 5 hours after granulating to obtain the functional master batch.
The mass ratio of the functional microsphere to the PET slice is 10:90.
S3, spinning
And (3) blending and melting the functional master batch and the PET slice, feeding the blend into a spinning box body, extruding out through a spinneret orifice, oiling after cooling through blowing, and winding and forming to obtain the ice jade fiber.
The mass ratio of the functional master batch to the PET slice is 6:94; the spinneret orifice is in a cross-shaped section.
The temperature of the spinning box body is 270 ℃, the spinning speed is 600m/min, and the blowing temperature is 15 ℃.
Adding ethylene bis-stearamide and an antioxidant 168 in the spinning process; the addition amount of the ethylene bis stearamide is 0.5wt% of the PET slice, and the addition amount of the antioxidant 168 is 0.2wt% of the PET slice.
The ice jade fiber prepared in the example 2 has the breaking strength of 4.05cN/dtex, and after 50 times of water washing, the antibacterial rate to staphylococcus aureus is 99.34%, the antibacterial rate to escherichia coli is 99.27%, and the antibacterial rate to candida albicans is 97.85%; the contact cool feeling coefficient was measured to be 0.23J/(cm) 2 S), after washing for 5 times, the average value of the moisture absorption and quick drying performance is 5 level, the UPF value of the ultraviolet resistance is more than 50, and the anion generation amount is 700 per cm 3 The fiber moisture regain is 3.3%, and the functional powder loss rate is 1.78%.
Example 3
S1, preparation of functional microspheres
Stirring unsaturated polyester resin, polyethyleneimine and functional powder at a high speed for 20min, wherein the stirring speed is 2400rpm, adding an initiator and an accelerator, stirring at 50 ℃ for reacting for 90min, and performing copolymerization and crosslinking on the double bonds of the polyethyleneimine and the unsaturated polyester resin at the stirring speed of 700rpm to obtain a copolymerization mixture gel; adding the copolymerization mixture gel into the water phase, stirring for 40min at the stirring speed of 200rpm, filtering, washing the product with 98 ℃ distilled water, forming a coating layer on the surface of the functional powder, and drying to obtain the functional microsphere with the particle size of 2 mu m.
The unsaturated polyester resin is o-benzene unsaturated polyester resin, and the viscosity at 25 ℃ is 1.25 Pa.s; the molecular weight of the polyethyleneimine is 1800, and the viscosity at 25 ℃ is 10000 MPa.s.
The functional powder is ice jade powder, nano titanium dioxide and plant source powder; the particle size of the ice jade powder is 500nm, the particle size of the nano titanium dioxide is 20nm, the particle size of the plant source powder is 300nm, and the mass ratio of the ice jade powder to the nano titanium dioxide to the plant source powder is 12:6:12.
The plant source powder is prepared from honeysuckle extract, mugwort extract, ginger extract and green tea extract in a mass ratio of 1:1:1:1.
The mass ratio of the unsaturated polyester resin to the polyethyleneimine to the functional powder is 75:30:15.
the initiator is benzoyl peroxide; the promoter is cobalt octoate.
The addition amount of the initiator is 1.5wt% of the unsaturated polyester resin; the addition amount of the accelerator is 0.5wt% of the unsaturated polyester resin.
The water phase is a mixture of polyvinyl alcohol, an emulsifying agent and distilled water; the mass ratio of the polyvinyl alcohol to the emulsifier to the distilled water is 15:1.2:110; the alcoholysis degree of the polyvinyl alcohol is 99.2%; the emulsifier is Span80.
The volume ratio of the polymer gel blend to the aqueous phase was 1:5.
S2, preparing functional master batch
And (3) crushing the PET slices to 15 mu m, blending the PET slices with the functional microspheres, granulating by adopting a double-screw extruder, and vacuum drying at-120 ℃ for 5 hours after granulating to obtain the functional master batch.
The mass ratio of the functional microsphere to the PET slice is 15:85.
S3, spinning
And (3) blending and melting the functional master batch and the PET slice, feeding the blend into a spinning box body, extruding out through a spinneret orifice, oiling after cooling through blowing, and winding and forming to obtain the ice jade fiber.
The mass ratio of the functional master batch to the PET slice is 9:91; the spinneret orifice is in a cross-shaped section.
The temperature of the spinning box body is 270 ℃, the spinning speed is 600m/min, and the blowing temperature is 15 ℃.
Zinc stearate and an antioxidant 1010 are added in the spinning process; the addition amount of the zinc stearate is 0.7wt% of the PET slice, and the addition amount of the antioxidant 1010 is 0.3wt% of the PET slice.
The ice jade fiber prepared in the example 3 has the breaking strength of 4.12cN/dtex, and after 50 times of water washing, the antibacterial rate to staphylococcus aureus is 99.64%, the antibacterial rate to escherichia coli is 99.5%, and the antibacterial rate to candida albicans is 98.41%; the contact cool feeling coefficient was measured to be 0.28J/(cm) 2 S), after washing for 5 times, the average value of the moisture absorption and quick drying performance is 5 levels, the UPF value of the ultraviolet resistance is more than 50, and the anion generation amount is 860 per cm 3 The fiber moisture regain is 3.85%, and the functional powder loss rate is 1.52%.
Comparative example 1
This comparative example was different from example 1 in that the polyethyleneimine in S1 was removed and the unsaturated polyester resin was coated on the functional powder alone to form microspheres, and the rest was the same as example 1, as comparative example 1.
The ice jade fiber prepared by adopting the comparative example 1 has obviously reduced strength and hygroscopicity, 3.4cN/dtex of breaking strength and 2% of fiber moisture regain, which proves that the defects of high brittleness and poor mechanical property of the unsaturated polyester resin are overcome by utilizing the copolymerization of the polyethyleneimine and the unsaturated polyester resin, and the polyethyleneimine has polar amino groups, so that the hygroscopicity of the fiber is further improved.
Comparative example 2
This comparative example was different from example 1 in that the polyvinyl alcohol in S1 was removed and distilled water at 97℃was used for washing, and the remainder was identical to example 1 as comparative example 2.
The ice jade fiber prepared in the comparative example 2 has obviously reduced hygroscopicity, the fiber moisture regain is reduced to 2.8%, and the fact that polyvinyl alcohol is doped in the copolymerization mixture to form microspheres, the polyvinyl alcohol is doped on the surfaces of the microspheres, the polyvinyl alcohol on the surfaces is removed after the microspheres are washed with water, the surfaces of the microspheres are microporous, the specific surface area is increased, and the moisture absorption performance of the fiber is better is shown.
Comparative example 3
The comparative example was different from example 1 in that the functional microspheres in S1 were removed, and an equivalent amount of functional powder was directly blended with PET chips and spun, and the other was the same as example 1, except that the same amount was used as comparative example 3.
The ice jade fiber prepared in comparative example 3 had a breaking strength of 2.6cN/dtex, a fiber moisture regain of 0.5%, and a contact cool feeling coefficient of 0.1J/(cm) 2 S) the average value of the moisture absorption and quick drying performance after washing for 5 times is 3 grades, and the anion generation amount is 200 per cm 3 The loss rate of the functional powder is more than 50%, the antibacterial effect is also greatly reduced, and the phenomenon of blocking of spinneret orifices occurs during spinning, because the functional powder is unevenly dispersed in the PET slice, some powder is blocked in the spinneret orifices to cause loss, and the plant source powder is greatly lost at high temperature, and the performances of fiber strength, cool feeling effect and the like are reduced.
The proportions are mass proportions, and the percentages are mass percentages, unless otherwise specified; the raw materials are all commercially available.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the novel cool-feeling cool jade fiber with multiple functions is characterized by comprising the steps of preparing functional microspheres, preparing functional master batches and spinning.
2. The preparation method of the novel cool and refreshing jade fiber with multiple functions according to claim 1, wherein the preparation of the functional microspheres is that unsaturated polyester resin, polyethyleneimine and functional powder are stirred at a high speed for 15-20min, the stirring speed is 2000-2400rpm, then initiator and accelerator are added, stirring reaction is carried out for 60-90min at 40-50 ℃, and the stirring speed is 600-700rpm, so as to obtain copolymer mixture gel; adding the copolymerization mixture gel into the water phase, stirring for 30-40min at the stirring speed of 200-300rpm, filtering, washing the product with distilled water at 95-98 ℃, and drying to obtain the functional microsphere.
3. The method for preparing the novel cool and refreshing jade fiber with multiple functions according to claim 2, wherein the functional powder is one or more of refreshing jade powder, nano titanium dioxide and plant source powder.
4. The method for preparing the novel cool and refreshing jade fiber with multiple functions according to claim 2, wherein the unsaturated polyester resin is o-benzene type unsaturated polyester resin, and the viscosity at 25 ℃ is 0.85-1.25 Pa.s; the molecular weight of the polyethyleneimine is 1200-1800, and the viscosity at 25 ℃ is 8000-10000 MPa.s.
5. The preparation method of the novel cool and refreshing jade fiber with multiple functions according to claim 2, which is characterized in that the mass ratio of the unsaturated polyester resin to the polyethyleneimine to the functional powder is (60-75:20-30): 10-15.
6. The method for preparing the novel cool and refreshing jade fiber with multiple functions according to claim 2, wherein the initiator is one or more of benzoyl peroxide, lauroyl peroxide, cyclohexanone peroxide and azobisisobutyronitrile; the promoter is one or more of cobalt naphthenate, cobalt octoate and dimethylaniline.
7. The method for preparing the novel cool and refreshing jade fiber with multiple functions according to claim 2, wherein the addition amount of the initiator is 1-1.5wt% of the unsaturated polyester resin; the addition amount of the accelerator is 0.5-0.8wt% of the unsaturated polyester resin.
8. The method for preparing the novel cool and refreshing jade fiber with multiple functions according to claim 2, wherein the water phase is a mixture of polyvinyl alcohol, an emulsifying agent and distilled water; the mass ratio of the polyvinyl alcohol to the emulsifier to the distilled water is 10-15:0.9-1.2:100-110; the alcoholysis degree of the polyvinyl alcohol is more than 99%;
the volume ratio of the polymer gel blend to the aqueous phase is 1:3-5.
9. The preparation method of the novel cool and refreshing jade fiber with multiple functions according to claim 1, which is characterized in that the preparation of the functional master batch is characterized in that polymer slices are crushed to 10-20 mu m, and are mixed with functional microspheres and then are granulated by a double screw extruder, and the functional master batch is obtained by vacuum drying at 100-120 ℃ after granulation;
the mass ratio of the functional microsphere to the polymer slice is 10-15:85-90; the polymer slice is one of PET or PA.
10. The preparation method of the novel cool and refreshing jade fiber with multiple functions, which is characterized in that the spinning is carried out, functional master batch and polymer slices are mixed and melted into a spinning box body, and the spinning box body is oiled and coiled to form after being extruded by a spinning hole and cooled by blowing, so as to obtain the cool and refreshing jade fiber;
the mass ratio of the functional master batch to the polymer slice is 6-9:91-94; the spinneret orifice is in a cross-shaped section.
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