CN117089948A - Cooling factor modified nylon fiber with special-shaped cross section, preparation method and application thereof in cool sense anti-ultraviolet fabric - Google Patents
Cooling factor modified nylon fiber with special-shaped cross section, preparation method and application thereof in cool sense anti-ultraviolet fabric Download PDFInfo
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- CN117089948A CN117089948A CN202311348847.4A CN202311348847A CN117089948A CN 117089948 A CN117089948 A CN 117089948A CN 202311348847 A CN202311348847 A CN 202311348847A CN 117089948 A CN117089948 A CN 117089948A
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- change material
- nylon fiber
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- 239000004744 fabric Substances 0.000 title claims abstract description 68
- 238000001816 cooling Methods 0.000 title claims abstract description 61
- 229920001778 nylon Polymers 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000011787 zinc oxide Substances 0.000 claims abstract description 60
- 239000012782 phase change material Substances 0.000 claims abstract description 55
- 238000002156 mixing Methods 0.000 claims abstract description 43
- GXEBTZBJBFEOQS-SREVYHEPSA-N (z)-4-(5-methyl-2-propan-2-ylcyclohexyl)oxy-4-oxobut-2-enoic acid Chemical compound CC(C)C1CCC(C)CC1OC(=O)\C=C/C(O)=O GXEBTZBJBFEOQS-SREVYHEPSA-N 0.000 claims abstract description 41
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229940041616 menthol Drugs 0.000 claims abstract description 28
- YJKHMSPWWGBKTN-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)F YJKHMSPWWGBKTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 claims abstract description 23
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 22
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000005507 spraying Methods 0.000 claims abstract description 11
- 238000009987 spinning Methods 0.000 claims abstract description 9
- 239000004677 Nylon Substances 0.000 claims abstract description 7
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims abstract 3
- 238000003756 stirring Methods 0.000 claims description 97
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 64
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 50
- 238000006243 chemical reaction Methods 0.000 claims description 47
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 43
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 38
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 36
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 36
- 239000004246 zinc acetate Substances 0.000 claims description 36
- 239000000178 monomer Substances 0.000 claims description 35
- 239000007864 aqueous solution Substances 0.000 claims description 33
- 238000001914 filtration Methods 0.000 claims description 33
- 238000005406 washing Methods 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 24
- 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 20
- 239000000155 melt Substances 0.000 claims description 20
- 238000010992 reflux Methods 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000009965 tatting Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 24
- 230000006750 UV protection Effects 0.000 abstract description 20
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- NOOLISFMXDJSKH-KXUCPTDWSA-N (-)-Menthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@H]1O NOOLISFMXDJSKH-KXUCPTDWSA-N 0.000 description 26
- 229960001701 chloroform Drugs 0.000 description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 14
- 239000000706 filtrate Substances 0.000 description 14
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 14
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 238000010025 steaming Methods 0.000 description 8
- 229920006052 Chinlon® Polymers 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 7
- 239000012074 organic phase Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- 238000001132 ultrasonic dispersion Methods 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 229920002301 cellulose acetate Polymers 0.000 description 3
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229920002292 Nylon 6 Polymers 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000035597 cooling sensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000010977 jade Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 244000061354 Manilkara achras Species 0.000 description 1
- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 235000002899 Mentha suaveolens Nutrition 0.000 description 1
- 235000001636 Mentha x rotundifolia Nutrition 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FFFGUEPPLOPQAT-UHFFFAOYSA-N bis(5-methyl-2-propan-2-ylcyclohexyl) 2-hydroxybutanedioate Chemical compound CC(C)C1CCC(C)CC1OC(=O)CC(O)C(=O)OC1CC(C)CCC1C(C)C FFFGUEPPLOPQAT-UHFFFAOYSA-N 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- VAMFXQBUQXONLZ-UHFFFAOYSA-N n-alpha-eicosene Natural products CCCCCCCCCCCCCCCCCCC=C VAMFXQBUQXONLZ-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D13/00—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft
- D03D13/008—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft characterised by weave density or surface weight
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
- D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/30—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the structure of the fibres or filaments
- D03D15/37—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the structure of the fibres or filaments with specific cross-section or surface shape
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/22—Physical properties protective against sunlight or UV radiation
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2501/00—Wearing apparel
- D10B2501/04—Outerwear; Protective garments
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of fabrics, in particular to a cool factor modified nylon fiber with a special-shaped cross section, a preparation method and application thereof in cool sense ultraviolet resistant fabrics. The preparation method of the cool factor modified nylon fiber with the special-shaped cross section comprises the following steps: preparing maleic acid monomenthyl ester by using maleic anhydride and menthol to react; coating the phase change material with nano zinc oxide to obtain a nano zinc oxide coated phase change material; the method comprises the steps of (1) reacting monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate, hydroxyethyl acrylate and nano zinc oxide coated phase change material to obtain a cooling factor; and (3) melt blending the cooling factors and the nylon slices, spraying out the special-shaped spinneret orifices, and drawing and chopping to obtain the cooling factor modified nylon fiber with the special-shaped cross section. And (3) spinning the fibers into a fabric to obtain the cool-feeling ultraviolet-resistant fabric. The fabric has the advantages of comfort in wearing, good cool feeling, ultraviolet resistance and the like, and can be used for manufacturing summer clothing.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a cool factor modified nylon fiber with a special-shaped cross section, a preparation method and application thereof in cool sense ultraviolet resistant fabrics.
Background
As the global air temperature increases gradually, the wearing comfort of people for summer clothing increases gradually, and cool feeling fibers gradually enter the vision of people. The clothing made of cool feeling fiber has cool feeling compared with the clothing made of common fiber, and has the advantages of heat conduction, cooling, moisture absorption and quick drying.
Chinese patent CN111118695B discloses a cool multifunctional elastic fabric, wherein mint extracts are dissolved in an organic solvent, cellulose acetate is added for stirring and dissolving to prepare an inner-layer fiber solution, jade powder, polyether polyol, organic acid, a cellulose solvent, cotton fibers and a thickener are uniformly mixed to prepare an outer-layer fiber solution, the outer-layer fiber solution is prepared into cool composite fiber yarns through solution spinning, the cool performance of the fiber yarns is ensured through compounding of two cool substances, but cellulose acetate and cotton fibers contain a large number of hydroxyl groups and carboxyl groups, the cellulose acetate and the cotton fibers are combined with water molecules through hydrogen bonds, water absorption is easy, dehydration is difficult, the moisture conductivity is relatively poor, and a large amount of organic solvents are needed for solution spinning and are difficult to recover; chinese patent CN113914003B discloses a method for preparing ultraviolet-proof cool feeling fabric, which comprises mixing submicron jade powder and polyester fiber to obtain cool feeling polyester fiber, blending at least two fibers to obtain inner and outer woven layers of fabric, weaving the inner and outer layers into fabric, wherein the fiber comprises modal fiber, polyester fiber, cotton fiber and fibrilia, the inner layer comprises cool feeling polyester fiber, and soaking the fabric in nanometer Ag/TiO 2 In the sol, the ultraviolet-proof cool fabric is obtained, but the fabric has an inner layer and an outer layer, has relatively large thickness and passes through nano Ag/TiO 2 The sol is adhered to the surface layer of the fabric by dipping and is easy to be washed away by water.
Disclosure of Invention
In order to solve the problems, the invention provides the cool factor modified nylon fiber with the special-shaped cross section, the preparation method and the application thereof in the cool sense ultraviolet resistant fabric, which solve the problems that the fabric has good moisture absorption performance but poor moisture permeability and the double-layer fabric has larger thickness.
In order to achieve the aim, the invention provides a preparation method of a cooling factor modified nylon fiber with a special-shaped cross section, which comprises the following steps:
step (1), preparing a maleic acid monomenthyl ester and nano zinc oxide coated phase change material; wherein, the preparation of the maleic acid monomenthyl ester comprises the following steps: mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, reacting under stirring, separating, purifying and drying after the reaction is finished to obtain maleic acid monomenthyl ester; wherein, preparing nano zinc oxide coated phase change material comprises: adding phase change material and sodium dodecyl sulfate into N, N-dimethylformamide, stirring at constant temperature, dropwise adding zinc acetate solution into emulsion formed by stirring after stirring, continuing stirring after dropwise adding, dropwise adding alkali precipitant after stirring, stirring again after dropwise adding, heating and standing after stirring, filtering, washing and drying after standing to obtain nano zinc oxide coated phase change material;
uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing the nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic treatment, adding the mixed monomer and azodiisobutyronitrile, reacting under stirring, filtering, washing and drying after the reaction is finished to obtain a cooling factor;
and (3) melting and blending the cooling factors and the nylon slices to obtain a melt, spraying the melt through the special-shaped spinneret orifices, and drawing and chopping to obtain the cooling factor modified special-shaped cross-section nylon fibers.
Preferably, in the step (1), when the monomenthyl maleate is prepared, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform participating in the reaction is 155: (125-145): (12-15): (620-700), the reaction conditions are: reacting at 40-50 deg.c for 24-28 hr.
Preferably, in the step (1), when monomenthyl maleate is prepared, the separation and purification comprises: filtering, washing, extracting, drying, filtering and rotary steaming.
Preferably, in the step (1), when the nano zinc oxide coated phase change material is prepared, the mass ratio of the phase change material, sodium dodecyl sulfate, N-dimethylformamide, zinc acetate solution and alkali precipitant is (8-12): (1.5-2.5): (90-100): (100-110): 150, the constant temperature stirring conditions are as follows: stirring at 45-55deg.C and 300-500r/min for 1-2h, continuously stirring at 45-55deg.C and 300-500r/min for 2-3h, stirring again at 45-55deg.C and 300-500r/min for 1-2h, heating and standing: standing at 80-90deg.C for 4-6 hr.
Preferably, in the step (1), when preparing the nano zinc oxide coated phase change material, the phase change material comprises N-eicosane, the zinc acetate solution comprises zinc acetate and N, N-dimethylformamide, and the mass ratio of the zinc acetate to the N, N-dimethylformamide is 11:95, the alkali precipitant comprises sodium hydroxide aqueous solution, wherein the sodium hydroxide aqueous solution is 1mol/L sodium hydroxide aqueous solution.
Further, the dripping time of the zinc acetate solution is 1h, and the dripping time of the sodium hydroxide aqueous solution is 1-2h.
Preferably, in the step (2), the mass ratio of the maleic acid monomenthyl ester, the glycidyl acrylate, the dodecafluoroheptyl methacrylate and the hydroxyethyl acrylate is (40-55): (25-35): 5: (5-10).
Preferably, in the step (2), the mass ratio of the acetone, the isobutanol, the nano zinc oxide coated phase change material, the mixed monomer and the azodiisobutyronitrile is (150-160): (150-160): (160-200): 90: (1.6-2), the conditions of the ultrasound are: ultrasonic treatment is carried out for 20-40min at the frequency of 20-40kHz, and the reaction conditions are as follows: reflux reaction is carried out for 8-12h at 70-80 ℃, and the drying conditions are as follows: drying at 40-50deg.C for 6-10 hr.
Preferably, in the step (3), the mass ratio of the cooling factor to the nylon chips is (10-20): (80-90) and the temperature of melt blending is 260-270 ℃.
Preferably, in the step (3), the cross-sectional shape of the profiled spinneret orifice includes a cross shape.
Further, the nylon slices comprise nylon 6 slices.
Preferably, the cooling factor modified special-shaped section nylon fiber prepared by the cooling factor modified special-shaped section nylon fiber preparation method is adopted.
Preferably, the method for applying the cool-feeling ultraviolet-resistant fabric to the cool-feeling ultraviolet-resistant fabric by adopting the cool factor modified nylon fiber with the special-shaped cross section comprises the following steps of: spinning the cool factor modified nylon fibers with special-shaped cross sections into warp yarns and weft yarns respectively, and spinning the warp yarns and the weft yarns into blended fabrics through a tatting process to obtain cool-feeling ultraviolet-resistant fabrics; wherein, the count of the warp yarn is 40S, and the count of the weft yarn is 40S; the warp density of the blended fabric is 550 roots/10 cm, and the weft density is 320 roots/10 cm.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, a mixed monomer obtained by mixing maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate reacts with a nano zinc oxide coated phase change material under the initiation of azodiisobutyronitrile to prepare a cooling factor, the cooling factor is mixed with nylon fiber, and the nylon fiber is subjected to melt spinning to obtain the cooling factor modified special-shaped section nylon fiber, wherein the fiber has good cooling sense, thermal conductivity and ultraviolet resistance, the design of the special-shaped section can endow the nylon fiber with better moisture conductivity, and the nylon fiber is used for preparing cool sense ultraviolet resistant fabric with good cooling sense and ultraviolet resistance; the nano zinc oxide is an inorganic additive with good heat conducting property and ultraviolet resistance, and can be doped into nylon fibers to improve the heat conducting property and ultraviolet resistance of the fibers; menthol is a cooling agent, when the menthol contacts with skin, the skin can feel cool, but the menthol has a lower melting point and a smaller relative molecular mass, and the menthol is easy to migrate when the menthol is directly mixed in nylon fiber, so that maleic anhydride reacts with the menthol to prepare maleic acid monomenthyl ester, carboxyl and double bond are introduced, and then the maleic acid monomenthyl ester reacts with glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate under the initiation of azodiisobutyronitrile, and simultaneously carboxyl on the maleic acid monomenthyl ester reacts with hydroxyl on the surface of nano zinc oxide in the nano zinc oxide coated phase-change material to obtain a cooling factor, the polarity of the nano zinc oxide coated phase-change material is reduced, the compatibility of the maleic acid monomenthyl ester and the amino and carboxyl in nylon is enhanced by utilizing the epoxy group on the cooling factor, and the separation of the nano zinc oxide coated material and a fiber base material is prevented.
Drawings
FIG. 1 is a process flow diagram of preparing a cooling factor modified nylon fiber with special-shaped cross section in the invention;
FIG. 2 is a bar graph of cooling sensation testing results of the cooling sensation anti-ultraviolet fabric prepared by the invention;
FIG. 3 is a bar graph showing the result of ultraviolet resistance test of cool feeling ultraviolet resistant fabric prepared by the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
The embodiment discloses a preparation method of a cooling factor modified nylon fiber with a special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 40 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 40 ℃, reacting for 28 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 35 ℃ for 8 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:125:12:620;
(2) Adding N-dodecane and sodium dodecyl sulfonate into N, N-dimethylformamide, stirring at a stirring speed of 500r/min for 1h at a temperature of 55 ℃, maintaining the temperature at 55 ℃, dropwise adding zinc acetate solution into the emulsion at a stirring speed of 500r/min for 1h, continuously stirring at a stirring speed of 500r/min for 2h at a temperature of 55 ℃ after the dropwise adding, dropwise adding 1mol/L sodium hydroxide aqueous solution after the dropwise adding, stirring again for 1h at a stirring speed of 500r/min at a temperature of 55 ℃ after the dropwise adding, heating to 80 ℃, standing for 6h at a temperature of 80 ℃, filtering, washing, and drying at a temperature of 40 ℃ for 10h to obtain the nano zinc oxide coated phase change material; wherein, the mass ratio of N-dodecane, sodium dodecyl sulfonate, N-dimethylformamide, zinc acetate solution and 1mol/L sodium hydroxide aqueous solution is 8:1.5:90:100:150, the mass ratio of zinc acetate to N, N-dimethylformamide in the zinc acetate solution is 11:95;
(3) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic dispersion for 40min at 20kHz frequency, adding mixed monomers and azodiisobutyronitrile, stirring and heating to 70 ℃ at the stirring speed of 500r/min, performing reflux reaction for 12h, filtering after the reaction is finished, washing with acetone, and drying at the temperature of 40 ℃ for 10h to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 40:35:5:10, acetone, isobutanol, nano zinc oxide coated phase change material, mixed monomer and azodiisobutyronitrile with the mass ratio of 150:150:160:90:1.6;
(4) Cooling factors and chinlon 6 slices are mixed according to the mass ratio of 10:90, melt blending at 260 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain the cool factor modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Example 2
The embodiment discloses a preparation method of a cooling factor modified nylon fiber with a special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 45 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 45 ℃, reacting for 26 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 40 ℃ for 6 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:130:13.5:640, a base;
(2) Adding N-dodecane and sodium dodecyl sulfonate into N, N-dimethylformamide, stirring at the temperature of 45 ℃ and the stirring speed of 300r/min for 2 hours, maintaining the temperature at 45 ℃, dropwise adding zinc acetate solution into the emulsion at the stirring speed of 300r/min for 1 hour, continuously stirring at the temperature of 45 ℃ and the stirring speed of 300r/min for 3 hours after the dropwise addition, dropwise adding 1mol/L sodium hydroxide aqueous solution after the dropwise addition, stirring again at the stirring speed of 300r/min for 2 hours after the dropwise addition, heating to 85 ℃, standing at the temperature of 85 ℃, standing for 5 hours, filtering, washing, and drying at the temperature of 45 ℃ for 8 hours to obtain the nano zinc oxide coated phase change material; wherein, the mass ratio of N-dodecane, sodium dodecyl sulfonate, N-dimethylformamide, zinc acetate solution and 1mol/L sodium hydroxide aqueous solution is 9:1.75:92.5:102.5:150, the mass ratio of zinc acetate to N, N-dimethylformamide in the zinc acetate solution is 11:95;
(3) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic dispersion for 30min at the frequency of 30kHz, adding mixed monomers and azodiisobutyronitrile, stirring and heating to 75 ℃ at the stirring speed of 500r/min, performing reflux reaction for 10h, filtering after the reaction is finished, washing with acetone, and drying at the temperature of 45 ℃ for 8h to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 45:35:5:5, the mass ratio of the acetone, the isobutanol and the nano zinc oxide coated phase change material to the mixed monomer to the azodiisobutyronitrile is 160:160:170:90:1.8;
(4) Cooling factors and chinlon 6 slices are prepared according to a mass ratio of 12:88, melt blending at 265 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain the cooling factor modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Example 3
The embodiment discloses a preparation method of a cooling factor modified nylon fiber with a special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 45 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 45 ℃, reacting for 26 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 40 ℃ for 6 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:135:13.5:660;
(2) Adding N-dodecane and sodium dodecyl sulfonate into N, N-dimethylformamide, stirring at the temperature of 50 ℃ and the stirring speed of 400r/min for 1h, maintaining the temperature of 50 ℃, dropwise adding zinc acetate solution into the emulsion at the stirring speed of 500r/min for 1h, continuously stirring at the temperature of 50 ℃ and the stirring speed of 400r/min for 2.5h after the dropwise addition, dropwise adding 1mol/L sodium hydroxide aqueous solution after the dropwise addition, stirring again at the stirring speed of 400r/min for 1.5h at the temperature of 50 ℃ after the dropwise addition, heating to 85 ℃, standing for 5h at the temperature of 85 ℃, filtering, washing, and drying at the temperature of 45 ℃ for 8h to obtain the nano zinc oxide coated material; wherein, the mass ratio of N-dodecane, sodium dodecyl sulfonate, N-dimethylformamide, zinc acetate solution and 1mol/L sodium hydroxide aqueous solution is 10:2:95:105:150, the mass ratio of zinc acetate to N, N-dimethylformamide in the zinc acetate solution is 11:95;
(3) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic dispersion for 30min at the frequency of 30kHz, adding mixed monomers and azodiisobutyronitrile, stirring and heating to 75 ℃ at the stirring speed of 500r/min, performing reflux reaction for 10h, filtering after the reaction is finished, washing with acetone, and drying at the temperature of 45 ℃ for 8h to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 50:30:5:5, the mass ratio of the acetone, the isobutanol and the nano zinc oxide coated phase change material to the mixed monomer to the azodiisobutyronitrile is 160:160:180:90:1.8;
(4) Cooling factors and chinlon 6 slices are mixed according to a mass ratio of 15:85, melt blending at 265 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain the cooling factor modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Example 4
The embodiment discloses a preparation method of a cooling factor modified nylon fiber with a special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 45 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 45 ℃, reacting for 26 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 40 ℃ for 6 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:140:13.5:680, respectively;
(2) Adding N-dodecane and sodium dodecyl sulfonate into N, N-dimethylformamide, stirring at the temperature of 50 ℃ and the stirring speed of 400r/min for 1h, maintaining the temperature of 50 ℃, dropwise adding zinc acetate solution into the emulsion at the stirring speed of 500r/min for 1h, continuously stirring at the temperature of 50 ℃ and the stirring speed of 400r/min for 2.5h after the dropwise addition, dropwise adding 1mol/L sodium hydroxide aqueous solution after the dropwise addition, stirring again at the stirring speed of 400r/min for 1.5h at the temperature of 50 ℃ after the dropwise addition, heating to 85 ℃, standing for 5h at the temperature of 85 ℃, filtering, washing, and drying at the temperature of 45 ℃ for 8h to obtain the nano zinc oxide coated material; wherein, the mass ratio of N-dodecane, sodium dodecyl sulfonate, N-dimethylformamide, zinc acetate solution and 1mol/L sodium hydroxide aqueous solution is 11:2.25:97.5:107.5:150, the mass ratio of zinc acetate to N, N-dimethylformamide in the zinc acetate solution is 11:95;
(3) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic dispersion for 30min at the frequency of 30kHz, adding mixed monomers and azodiisobutyronitrile, stirring and heating to 75 ℃ at the stirring speed of 500r/min, performing reflux reaction for 10h, filtering after the reaction is finished, washing with acetone, and drying at the temperature of 45 ℃ for 8h to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 50:25:5:10, acetone, isobutanol, nano zinc oxide coated phase change material, mixed monomer and azodiisobutyronitrile with the mass ratio of 160:160:190:90:1.8;
(4) Cooling factors and chinlon 6 slices are prepared according to the mass ratio of 18:82, melt blending at 265 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain the cool factor modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm;
wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Example 5
The embodiment discloses a preparation method of a cooling factor modified nylon fiber with a special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 50 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 50 ℃, reacting for 24 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 45 ℃ for 4 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:145:15:700;
(2) Adding N-dodecane and sodium dodecyl sulfonate into N, N-dimethylformamide, stirring at a stirring speed of 500r/min for 1h at a temperature of 55 ℃, maintaining the temperature at 55 ℃, dropwise adding zinc acetate solution into the emulsion at a stirring speed of 500r/min for 1h, continuously stirring at a stirring speed of 500r/min for 2h at a temperature of 55 ℃ after the dropwise adding, dropwise adding 1mol/L sodium hydroxide aqueous solution after the dropwise adding, stirring again for 1h at a stirring speed of 500r/min at a temperature of 55 ℃ after the dropwise adding, heating to 90 ℃, standing for 4h at a temperature of 90 ℃, filtering, washing, and drying at a temperature of 50 ℃ for 6h to obtain the nano zinc oxide coated phase change material; wherein, the mass ratio of N-dodecane, sodium dodecyl sulfonate, N-dimethylformamide, zinc acetate solution and 1mol/L sodium hydroxide aqueous solution is 12:2.5:100:110:150, the mass ratio of zinc acetate to N, N-dimethylformamide in the zinc acetate solution is 11:95;
(3) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic dispersion for 20min at 40kHz frequency, adding mixed monomers and azodiisobutyronitrile, stirring and heating to 80 ℃ at a stirring speed of 500r/min, performing reflux reaction for 8h, filtering after the reaction is finished, washing with acetone, and drying at 50 ℃ for 6h to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 55:25:5:5, the mass ratio of the acetone, the isobutanol and the nano zinc oxide coated phase change material to the mixed monomer to the azodiisobutyronitrile is 160:160:200:90:2;
(4) Cooling factors and chinlon 6 slices are prepared according to the mass ratio of 20:80, melt blending at 270 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain the cooling factor modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Comparative example 1
The comparative example discloses a preparation method of modified nylon fiber with special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 45 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 45 ℃, reacting for 26 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 40 ℃ for 6 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:130:13.5:640, a base;
(2) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing nano zinc oxide, acetone and isobutanol, performing ultrasonic dispersion for 30min at the frequency of 30kHz, adding mixed monomers and azodiisobutyronitrile, stirring and heating to 75 ℃ at the stirring speed of 500r/min, performing reflux reaction for 10h, filtering after the reaction is finished, washing with acetone, and drying at the temperature of 45 ℃ for 8h to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 45:35:5:5, acetone, isobutanol, nano zinc oxide, mixed monomers and azodiisobutyronitrile in a mass ratio of 160:160:170:90:1.8;
(3) Cooling factors and chinlon 6 slices are prepared according to a mass ratio of 12:88, melt blending at 265 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Comparative example 2
The comparative example discloses a preparation method of modified nylon fiber with special-shaped cross section, which comprises the following steps:
(1) Adding N-dodecane and sodium dodecyl sulfonate into N, N-dimethylformamide, stirring at the temperature of 45 ℃ and the stirring speed of 300r/min for 2 hours, maintaining the temperature at 45 ℃, dropwise adding zinc acetate solution into the emulsion at the stirring speed of 300r/min for 1 hour, continuously stirring at the temperature of 45 ℃ and the stirring speed of 300r/min for 3 hours after the dropwise addition, dropwise adding 1mol/L sodium hydroxide aqueous solution after the dropwise addition, stirring again at the stirring speed of 300r/min for 2 hours after the dropwise addition, heating to 85 ℃, standing at the temperature of 85 ℃, standing for 5 hours, filtering, washing, and drying at the temperature of 45 ℃ for 8 hours to obtain the nano zinc oxide coated phase change material; wherein, the mass ratio of N-dodecane, sodium dodecyl sulfonate, N-dimethylformamide, zinc acetate solution and 1mol/L sodium hydroxide aqueous solution is 9:1.75:92.5:102.5:150, the mass ratio of zinc acetate to N, N-dimethylformamide in the zinc acetate solution is 11:95;
(2) The nano zinc oxide coated phase change material and nylon 6 slices are prepared according to the mass ratio of 12:88, melt blending at 265 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Comparative example 3
The comparative example discloses a preparation method of modified nylon fiber with special-shaped cross section, which comprises the following steps:
(1) Uniformly mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, stirring and heating to 45 ℃ at a stirring speed of 180r/min, maintaining the reaction temperature at 45 ℃, reacting for 26 hours, filtering after the reaction is finished, washing with chloroform, collecting filtrate, adding 10wt% of sodium carbonate aqueous solution, washing, standing for layering, taking an upper solution, adding 10wt% of hydrochloric acid aqueous solution to adjust the pH value to 3, extracting twice with ethyl acetate, taking an organic phase, adding anhydrous magnesium sulfate for drying, filtering, rotationally steaming the filtrate at 70 ℃ to remove a solvent, standing at room temperature for 0.5 hour to solidify a product, crushing, and vacuum drying at 40 ℃ for 6 hours to obtain maleic acid monomenthyl ester; wherein, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and trichloromethane participating in the reaction is 155:130:13.5:640, a base;
(2) Uniformly mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing acetone and isobutanol, adding mixed monomers and azodiisobutyronitrile, stirring at a stirring speed of 500r/min, heating to 75 ℃, carrying out reflux reaction for 10 hours, filtering after the reaction is finished, washing with acetone, and drying at a temperature of 45 ℃ for 8 hours to obtain a cooling factor; wherein, in the mixed monomer, the mass ratio of maleic acid monomenthyl ester, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate is 45:35:5:5, the mass ratio of the acetone, the isobutanol, the mixed monomer and the azodiisobutyronitrile is 160:160:90:1.8;
(3) Cooling factors and chinlon 6 slices are prepared according to a mass ratio of 12:88, melt blending at 265 ℃ to obtain a melt, spraying the melt through a special-shaped spinneret orifice, wherein the cross section of the special-shaped spinneret orifice is cross-shaped, and drawing and chopping to obtain the cooling factor modified special-shaped cross section nylon fiber with the thickness of 1.5D and the length of 38 mm; wherein the drafting temperature is 80 ℃ and the drafting speed is 430m/min.
Menthol in all the above examples and comparative examples was from Shanghai Ala Biochemical technologies Co., ltd, with CAS number 2216-51-5; maleic anhydride from Ji Xin Yibang Biotechnology Co., ltd. With CAS number 108-31-6; 4-dimethylaminopyridine is from the biological technology Co.Ltd, jixin Yibang, wuhan with CAS number 1122-58-3; n-eicosane is from the scientific and technological Co., ltd., bajingzhi, CAS number 112-95-8; sodium dodecyl sulfonate is available from Shanghai Ala Biochemical technology Co., ltd, with CAS number 2386-53-0; zinc acetate is from Nantong Runfeng petrochemical industry Co., ltd, with CAS number 557-34-6; glycidyl acrylate is from Anhui chemical industry Co., ltd, with CAS number 106-90-1; dodecafluoroheptyl methacrylate is available from halbine chiku fluorosilicone limited under CAS number 2261-99-6; hydroxyethyl acrylate is available from Jiangsu Runfeng synthetic technology Co., ltd, and has CAS number 868-77-9.
Example 6
Spinning the cool factor modified nylon fiber with the special-shaped cross section prepared in the examples 1-5 and the modified nylon fiber with the special-shaped cross section prepared in the comparative examples 1-3 into warp yarns and weft yarns respectively in sequence, spinning the warp yarns and the weft yarns into blended fabrics through a tatting process, and sequentially marking the blended fabrics as fabrics 1-8 respectively; wherein, the count of the warp yarn is 40S, and the count of the weft yarn is 40S; the warp density of the blended fabric is 550 roots/10 cm, and the weft density is 320 roots/10 cm;
test examples
Test (1) cool feeling energy test: the cool feeling performance test is carried out on the fabrics 1-8 according to GB/T35263-2017 test and evaluation of the instant cool feeling performance of textile contact, and the contact cool feeling (instant maximum heat flow Q m ) The test results are shown in table 1:
as can be seen from the test results in Table 1, the fabric prepared by the invention has good cool feeling performance. The nano zinc oxide in the cooling factors coats the phase change material, the heat conductivity coefficient of the zinc oxide is larger, the heat conductivity of the fiber can be well improved when the nano zinc oxide is doped in the fiber, meanwhile, the zinc oxide is coated with the phase change material, and the phase change material absorbs heat when heated, so that the contact cooling feeling is greatly improved. Comparing the test results of the fabric 6 and the fabric 2, the cool feeling of the fabric is reduced because the nano zinc oxide in the cool factors is not coated with the phase change material, because the zinc oxide increases the heat conductivity of the fabric, but the phase change material does not absorb heat, and the heat of the fabric is transferred to the air slowly, so the contact cool feeling of the fabric is reduced; compared with the fabric 7 and the fabric 2, the menthol is not introduced, but the nano zinc oxide coated phase change material has good heat conduction effect, and the contact cool feeling of the fabric 7 is similar to that of the fabric 2; the menthol type cooling agent can make people feel cool when contacting with the skin of people, but only stimulates cold receptors of the skin of the human body, and does not play a role in reducing the temperature, compared with the fabric 8 and the fabric 2, the cooling factor does not contain nano zinc oxide to coat the phase change material, does not have the heat conduction performance of nano zinc oxide and the heat absorption performance of the phase change material, and the contact cool feeling value of the fabric 8 is greatly reduced.
Test (2) ultraviolet resistance test: the anti-ultraviolet performance of the fabrics 1-8 is measured according to GB/T18830-2009 evaluation of anti-ultraviolet performance of textiles, and is expressed by UPF values, and the test results are shown in Table 2:
as can be seen from Table 2, the fabric prepared by the method has good ultraviolet resistance. As can be seen from the fabric 1-5, the UPF value of the fabric is gradually increased along with the increase of the content of the cooling factors in the fabric, and the ultraviolet resistance is better, because the cooling factors contain nano zinc oxide coated phase change materials, the zinc oxide has excellent ultraviolet resistance, and the ultraviolet resistance of the fiber can be well improved when the nano zinc oxide coated phase change materials are doped in the fiber; as can be seen from the fabric 6, the fabric 7 and the fabric 2, when the zinc oxide is not coated with the phase-change material, the ultraviolet resistance of the fabric is basically not affected, because the phase-change material does not have ultraviolet resistance, the coating of the phase-change material on the zinc oxide does not affect the ultraviolet resistance of the zinc oxide, and the modifying agent prepared from the menthyl maleate does not have active groups of an organic ultraviolet resistance agent and has no ultraviolet resistance effect, so that the ultraviolet resistance of the fabric 6, the fabric 7 and the fabric 2 are similar; as can be seen from the fabric 8 and the fabric 2, when the nano zinc oxide is not contained in the fiber to cover the phase change material, the ultraviolet resistance of the fabric is greatly reduced, because the ultraviolet resistance of the fabric is mainly from zinc oxide, and when the zinc oxide is not contained, the ultraviolet resistance of the fabric is poor.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the cool factor modified nylon fiber with the special-shaped cross section is characterized by comprising the following steps of:
step (1), preparing a maleic acid monomenthyl ester and nano zinc oxide coated phase change material; wherein, the preparation of the maleic acid monomenthyl ester comprises the following steps: mixing menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform, reacting under stirring, separating, purifying and drying after the reaction is finished to obtain maleic acid monomenthyl ester; wherein, preparing nano zinc oxide coated phase change material comprises: adding phase change material and sodium dodecyl sulfate into N, N-dimethylformamide, stirring at constant temperature, dropwise adding zinc acetate solution into emulsion formed by stirring after stirring, continuing stirring after dropwise adding, dropwise adding alkali precipitant after stirring, stirring again after dropwise adding, heating and standing after stirring, filtering, washing and drying after standing to obtain nano zinc oxide coated phase change material;
step (2), mixing monomenthyl maleate, glycidyl acrylate, dodecafluoroheptyl methacrylate and hydroxyethyl acrylate to obtain a mixed monomer; mixing the nano zinc oxide coated phase change material, acetone and isobutanol, performing ultrasonic treatment, adding the mixed monomer and azodiisobutyronitrile, reacting under stirring, filtering, washing and drying after the reaction is finished to obtain a cooling factor;
and (3) melting and blending the cooling factors and the nylon slices to obtain a melt, spraying the melt through the special-shaped spinneret orifices, and drawing and chopping to obtain the cooling factor modified special-shaped cross-section nylon fibers.
2. The method for preparing the cooling factor modified nylon fiber with the special-shaped cross section according to claim 1, wherein in the step (1), when the monomenthyl maleate is prepared, the mass ratio of menthol, maleic anhydride, 4-dimethylaminopyridine and chloroform participating in the reaction is 155: (125-145): (12-15): (620-700), the reaction conditions are: reacting at 40-50 deg.c for 24-28 hr.
3. The method for preparing the cooling factor modified nylon fiber with the special-shaped cross section according to claim 1, wherein in the step (1), when the nano zinc oxide coated phase change material is prepared, the mass ratio of the phase change material to the sodium dodecyl sulfate to the N, N-dimethylformamide to the zinc acetate solution to the alkali precipitant is (8-12): (1.5-2.5): (90-100): (100-110): 150, the constant temperature stirring conditions are as follows: stirring at 45-55deg.C and 300-500r/min for 1-2h, continuously stirring at 45-55deg.C and 300-500r/min for 2-3h, stirring again at 45-55deg.C and 300-500r/min for 1-2h, heating and standing: standing at 80-90deg.C for 4-6 hr.
4. The method for preparing the cooling factor modified nylon fiber with the special-shaped cross section according to claim 1, wherein in the step (1), when the nano zinc oxide coated phase change material is prepared, the phase change material comprises N-eicosane, a zinc acetate solution comprises zinc acetate and N, N-dimethylformamide, and the mass ratio of the zinc acetate to the N, N-dimethylformamide is 11:95, the alkali precipitant comprises sodium hydroxide aqueous solution, wherein the sodium hydroxide aqueous solution is 1mol/L sodium hydroxide aqueous solution.
5. The method for preparing the cooling factor modified nylon fiber with the special-shaped cross section according to claim 1, wherein in the step (2), the mass ratio of the maleic acid monomenthyl ester, the glycidyl acrylate, the dodecafluoroheptyl methacrylate and the hydroxyethyl acrylate is (40-55): (25-35): 5: (5-10).
6. The method for preparing the cooling factor modified nylon fiber with the special-shaped cross section according to claim 1, wherein in the step (2), the mass ratio of the acetone, the isobutanol, the nano zinc oxide coated phase-change material, the mixed monomer and the azodiisobutyronitrile is (150-160): (150-160): (160-200): 90: (1.6-2), the conditions of the ultrasound are: ultrasonic treatment is carried out for 20-40min at the frequency of 20-40kHz, and the reaction conditions are as follows: reflux reaction is carried out for 8-12h at 70-80 ℃.
7. The method for preparing the nylon fiber with the cooling factor modified special-shaped cross section according to claim 1, wherein in the step (3), the mass ratio of the cooling factor to the nylon chips is (10-20): (80-90) and the temperature of melt blending is 260-270 ℃.
8. The method for preparing the cooling-factor-modified profiled-section nylon fiber according to claim 1, wherein in the step (3), the profiled-section spinneret orifice has a cross-shaped cross-section.
9. A cooling factor modified profiled cross-section nylon fiber prepared by the cooling factor modified profiled cross-section nylon fiber preparation method according to any one of claims 1-8.
10. A method for applying the cool factor modified special-shaped section nylon fiber of claim 9 to cool feeling anti-ultraviolet fabric, comprising the following steps: spinning the cool factor modified nylon fibers with special-shaped cross sections into warp yarns and weft yarns respectively, and spinning the warp yarns and the weft yarns into blended fabrics through a tatting process to obtain cool-feeling ultraviolet-resistant fabrics; wherein, the count of the warp yarn is 40S, and the count of the weft yarn is 40S; the warp density of the blended fabric is 550 roots/10 cm, and the weft density is 320 roots/10 cm.
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