CN115627633A - Cold-proof breathable fabric and preparation method thereof - Google Patents
Cold-proof breathable fabric and preparation method thereof Download PDFInfo
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- CN115627633A CN115627633A CN202211152833.0A CN202211152833A CN115627633A CN 115627633 A CN115627633 A CN 115627633A CN 202211152833 A CN202211152833 A CN 202211152833A CN 115627633 A CN115627633 A CN 115627633A
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- 239000004744 fabric Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000004964 aerogel Substances 0.000 claims abstract description 72
- 239000002131 composite material Substances 0.000 claims abstract description 35
- PGJYYCIOYBZTPU-UHFFFAOYSA-N 2,3,4,5,6-pentafluorobenzyl alcohol Chemical compound OCC1=C(F)C(F)=C(F)C(F)=C1F PGJYYCIOYBZTPU-UHFFFAOYSA-N 0.000 claims abstract description 25
- -1 3- (aminomethyl) -2-hydroxypentanal Chemical compound 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 13
- LCPNYLRZLNERIG-ZETCQYMHSA-N (2S)-6-amino-2-[2-(oxomethylidene)hydrazinyl]hexanoyl isocyanate Chemical compound NCCCC[C@H](NN=C=O)C(=O)N=C=O LCPNYLRZLNERIG-ZETCQYMHSA-N 0.000 claims abstract description 11
- XSPASXKSXBJFKB-UHFFFAOYSA-N 11-trimethoxysilylundecan-1-amine Chemical compound CO[Si](OC)(OC)CCCCCCCCCCCN XSPASXKSXBJFKB-UHFFFAOYSA-N 0.000 claims abstract description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 11
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 11
- LWCNCHYFFPUDIH-UHFFFAOYSA-N methyl 3-[dichloro(methyl)silyl]propanoate Chemical compound COC(=O)CC[Si](C)(Cl)Cl LWCNCHYFFPUDIH-UHFFFAOYSA-N 0.000 claims abstract description 11
- YMTRNELCZAZKRB-UHFFFAOYSA-N 3-trimethoxysilylaniline Chemical compound CO[Si](OC)(OC)C1=CC=CC(N)=C1 YMTRNELCZAZKRB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 17
- 238000007142 ring opening reaction Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- 229960004624 perflexane Drugs 0.000 claims description 7
- ZJIJAJXFLBMLCK-UHFFFAOYSA-N perfluorohexane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F ZJIJAJXFLBMLCK-UHFFFAOYSA-N 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 238000003483 aging Methods 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 claims 1
- 238000001764 infiltration Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 21
- 239000003921 oil Substances 0.000 abstract description 12
- 230000035699 permeability Effects 0.000 abstract description 8
- 210000004243 sweat Anatomy 0.000 abstract description 8
- 238000004321 preservation Methods 0.000 abstract description 5
- 238000009423 ventilation Methods 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 37
- 230000000052 comparative effect Effects 0.000 description 21
- 239000000499 gel Substances 0.000 description 14
- 229910000077 silane Inorganic materials 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 210000003746 feather Anatomy 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000005661 hydrophobic surface Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 125000004492 methyl ester group Chemical group 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/34—Polyamides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/08—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/01—Stain or soil resistance
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/11—Oleophobic properties
Abstract
The invention discloses a cold-proof breathable fabric and a preparation method thereof, and relates to the technical field of fabrics. According to the invention, the nylon 6 fabric is modified by using 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride, sweat on the surface of a human body can be combined, and heat energy is generated through conversion, so that the fabric has cold-proof and warm-keeping effects; then L-lysine diisocyanate and 11-aminoundecyltrimethoxysilane react to form composite gel with tetraethoxysilane serving as a mixed silicon source, and the modified fabric is subjected to permeation treatment to form aerogel, so that the air permeability of the fabric is improved, and the temperature exchange inside and outside the fabric is prevented; then 3-aminophenyltrimethoxysilane, 2-carbomethoxyethylmethyldichlorosilane, 1, 3-tetrafluoropropene and 2,3,4,5, 6-pentafluorobenzyl alcohol are grafted on the surface of the aerogel to form an oil-proof organic film, so that the fabric has oil-proof performance. The fabric prepared by the invention has the effects of cold resistance, heat preservation, ventilation and oil resistance.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a cold-proof breathable fabric and a preparation method thereof.
Background
In the cold-proof warm-keeping fabrics sold in the market at present, the cold-proof warm-keeping effect of the down products is the best. The down feather fabric is generally directly wrapped by a simple single-layer fabric and sewn into a sheet, although the down feather fabric has warm-keeping property, the down feather fabric is not close to the skin, the daily free movement of the human body is hindered, and gaseous and liquid sweat generated by the human body in winter is not easy to pass through thick clothes and is released to the surrounding environment, and the gaseous and liquid sweat is usually gathered on the inner side of the clothes, so that the human body can feel wet and cold. In addition, in order to improve the cold-proof and warm-keeping effects of the fabric, a windproof coating is usually coated on the surface of the fabric, the coating is basically a non-porous film or a microporous film, the air permeability is almost zero, so that sweat of a human body cannot be discharged in time, pores are blocked, the wearing comfort performance is poor, and the warm-keeping effect is greatly reduced.
In addition, people often touch and are stained with oil stains in daily life, but the existing fabric is poor in oil-proof effect, is easy to adsorb oil stains, forms oil stains on the surface, and is difficult to clean, so that the attractiveness of clothes is affected, and therefore, how to invent the cold-proof, warm-keeping, breathable and oil-proof fabric is very important.
Disclosure of Invention
The invention aims to provide a cold-proof breathable fabric and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: a cold-proof air-permeable fabric is prepared through putting modified fabric in composite gel, permeating for a certain time, ageing, washing, drying to obtain aerogel layer, and modifying.
Further, the modified fabric layer is prepared by the following method, mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride, heating for reaction, and continuing heating for reaction to obtain a ring-opening compound; placing the nylon 6 fabric in an irradiation tube, adding a ring-opening compound, deionized water, methanol and nitrogen, irradiating for a period of time, taking out, soaking in acetone, and standing for a period of time.
Further, the composite gel is prepared by the following method, mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and hydrochloric acid with the mass fraction of 37%, stirring for a period of time, adding ammonia water with the mass fraction of 25%, and uniformly stirring.
Further, the modification treatment is that under the protection of nitrogen, the pretreated aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane are mixed, heated and reacted, cooled to room temperature, added with absolute ethyl alcohol and perfluorohexane, kept stand for a period of time, taken out, placed in a high-pressure reaction kettle, added with Karstedt catalyst, sealed, heated, added with 1, 3-tetrafluoropropene, continuously heated, kept warm for a period of time, and cooled to obtain a composite aerogel precursor; heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide, stirring for a period of time, adding the composite aerogel precursor, heating for reaction, cooling to a preset temperature, sequentially washing with a sodium hydroxide solution with the mass fraction of 5% and deionized water, adjusting the pH value with hydrochloric acid, pouring into cold water, cooling to room temperature, filtering, and drying.
Further, the preparation method of the cold-proof breathable fabric comprises the following preparation steps:
(1) The gram weight is 180 to 200g/m 2 The nylon 6 fabric is placed in an irradiation tube, and a ring-opening compound, deionized water and methanol are added according to a mass ratio of 1;
(2) Placing the modified fabric in composite gel with the mass of 0.1-0.4 time of that of the modified fabric, permeating for 10-24 min, aging for 20-25 h, washing for 3-5 times by using absolute ethyl alcohol, and drying at 40 ℃ for 6-8 d to obtain an aerogel layer;
(3) Mixing a pretreatment aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane according to the mass ratio of 1: 0.09-1: 0.2 under the protection of nitrogen, reacting at 60 ℃ for 2-5 h, cooling to room temperature, adding absolute ethyl alcohol 7-12 times the mass of the pretreatment aerogel layer and perfluorohexane 5-9 times the mass of the pretreatment aerogel layer, standing for 52-64 min, taking out, placing in a high-pressure reaction kettle, adding Karstedt catalyst 0.01-0.03 time the mass of the pretreatment aerogel layer, sealing, heating to 70-80 ℃, opening a feeding valve, adding 1, 3-tetrafluoropropene 0.3-0.6 time the mass of the pretreatment aerogel layer at 10mL/min, heating to 90-110 ℃, keeping the temperature for 58-70 min, cooling to 30 ℃, and taking out to obtain a composite aerogel precursor;
(4) Heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide which is 0.3-0.5 time of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, stirring at 80rpm for 58-66 min, adding a composite aerogel precursor which is 0.5-0.8 time of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, heating to 150 ℃, cooling to 80-100 ℃ after reaction for 1-3 h, washing for 2-4 times by using a sodium hydroxide solution with the mass fraction of 5% and deionized water in sequence, adding hydrochloric acid until the pH of the solution is 6-7, pouring into cold water with the temperature of 10-20 ℃ which is 3-5 times of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, cooling to room temperature, performing suction filtration, and drying at 60 ℃ for 5-10 h to obtain the cold-proof breathable fabric.
Further, the irradiation dose in the step (1) is 8-11 kGy.
Further, the preparation method of the ring-opened compound in the step (1) comprises the following steps: mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride according to a mass ratio of 1.7-1, heating to 60 ℃, reacting for 1-3 h, heating to 80 ℃, and reacting for 3-6 h.
Further, the osmotic pressure in the step (2) is 1 × 10 5 ～3×10 5 MPa。
Further, the preparation method of the composite gel in the step (2) comprises the following steps: mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% hydrochloric acid according to a mass ratio of 1.2.
Further, the preparation method of the pre-treatment aerogel layer in the step (3) comprises the following steps: mixing 3-aminophenyltrimethoxysilane and deionized water according to a mass ratio of 1.
Compared with the prior art, the invention has the following beneficial effects:
the fabric prepared by the invention comprises the composite aerogel layer and the modified fabric layer, so that the effects of cold resistance, heat preservation, ventilation and oil stain resistance are realized.
Firstly, modifying a nylon 6 fabric, carrying out ring-opening reaction on maleic anhydride by using hydroxyl of 3- (aminomethyl) -2-hydroxypentanal to form a ring-opening compound, generating free radicals on the surface of the nylon 6 fabric under the irradiation effect, polymerizing the free radicals with double bonds of the ring-opening compound, grafting the free radicals and the double bonds of the ring-opening compound into a nylon 6 molecular chain, introducing hydrophilic groups such as carboxyl, hydroxyl, aldehyde group and amino, combining sweat on the surface of a human body through hydrogen bonds, converting the hydrophilic groups into heat energy, releasing the heat energy into the environment, and supplementing heat to the human body to ensure that the fabric realizes cold-proof and warm-keeping effects; then L-lysine diisocyanate reacts with amino of 11-aminoundecyl trimethoxy silane to form a hydrophobic silane compound, the hydrophobic silane compound and tetraethoxysilane are used as a mixed silicon source to form composite gel, then the modified fabric is subjected to permeation treatment, the composite gel is filled in gaps of the modified fabric, hydroxyl of the composite gel and oxygen-containing groups of the modified fabric are subjected to chemical crosslinking, after moisture is volatilized, capillary channels are formed at the joints of the composite gel and the modified fabric and communicated with aerogel pore channels to form ventilation channels, the air permeability of the fabric is improved, the silane compound promotes silicon dioxide to gather to play a role of supporting an aerogel network framework, the silane compound is successfully combined with the silica aerogel framework, the channels are hydrophobic surfaces, and form a one-way moisture-conducting matrix together with the modified fabric, so that sweat can pass through the channels, the ventilation effect of the fabric is improved, in addition, the silane compound and the aerogel act together to form a heat-insulating layer, the temperature exchange inside and outside the fabric is blocked, and the cold-proof and warm-keeping effects of the fabric are enhanced.
Secondly, a siloxane bond of 3-aminophenyltrimethoxysilane is grafted on the surface of the aerogel, after an amino group of the aerogel reacts with a methyl ester group of 2-carbomethoxyethylmethyldichlorosilane, a silicon-hydrogen bond and chloride ions of the 2-carbomethoxyethylmethyldichlorosilane respectively react with a double bond of 1, 3-tetrafluoropropene and a hydroxyl group of 2,3,4,5, 6-pentafluorobenzyl alcohol to form an organic film, the fluoroalkyl and the silicon-oxygen chain migrate and enrich to the surface, the surface energy of the aerogel is reduced, the fabric has an oil-proof effect, and meanwhile, the organic film and pore channels on the surface of the aerogel form a concave-convex structure, so that an air film can be formed with oil while the surface energy is further reduced, the wetting and spreading of the oil are not facilitated, and the oil-proof effect of the fabric is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used for describing the method in detail, and the method for testing each index of the cold-proof breathable fabric manufactured in the following examples is as follows:
cold-proof and warm-keeping properties: carrying out moisture absorption, heat generation and heat preservation effect tests on the embodiment and the comparative example with the same size;
and (3) heat preservation: the heat retention was measured according to the KES Heat Retention test method at Δ T =10 ℃ in a 20 ℃ RH atmosphere with a humidity of 65%;
moisture absorption and heat generation: the maximum temperature rise within 3min was measured according to ISO 18782 in a RH-adjusted atmosphere at 40% humidity of 20h after 12 h.
Air permeability: the same size of the examples and comparative examples were tested for air permeability and the air permeability was tested with reference to GB/T5453 with a pressure drop across 100Pa.
Oil repellency: the oil-proof effect test is carried out on the examples and the comparative examples with the same size, the test is carried out by referring to AATCC-118, 3 times of tests are carried out, the average value is taken, the oil-repellent degree is 8 grades, the best grade is 8 grades, and the worst grade is I grade.
Example 1
(1) Mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride according to the mass ratio of 1.7, heating to 60 ℃, reacting for 1h, heating to 80 ℃, and reacting for 3h to obtain a ring-opening compound; the gram weight is 180g/m 2 The nylon 6 fabric is placed in an irradiation tube, a ring-opening compound, deionized water and methanol are added according to a mass ratio of 1;
(2) Mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% hydrochloric acid according to a mass ratio of 1.2; placing the modified fabric in a composite gel (1 × 10) with the mass of 0.1 time of that of the modified fabric 5 Permeating under MPa for 10min, aging for 20h, washing with anhydrous ethanol for 3 times, and drying at 40 deg.C for 6d to obtain aerogel layer;
(3) Mixing 3-aminophenyltrimethoxysilane and deionized water according to a mass ratio of 1;
(4) Mixing the pretreatment aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane according to the mass ratio of 1:0.09 under the protection of nitrogen, reacting for 2 hours at 60 ℃, cooling to room temperature, adding absolute ethyl alcohol 7 times the mass of the pretreatment aerogel layer and perfluorohexane 5 times the mass of the pretreatment aerogel layer, standing for 52 minutes, taking out, placing in a high-pressure reaction kettle, adding Karstedt catalyst 0.01 times the mass of the pretreatment aerogel layer, sealing, heating to 70 ℃, opening a feeding valve, adding 1, 3-tetrafluoropropene 0.3 times the mass of the pretreatment aerogel layer at 10mL/min, heating to 90 ℃, preserving heat for 58 minutes, cooling to 30 ℃, taking out, and obtaining a composite aerogel precursor;
(5) Heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide which is 0.3 time of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, stirring at 80rpm for 58min, adding a composite aerogel precursor which is 0.5 time of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, heating to 150 ℃, reacting for lh, cooling to 80 ℃, sequentially washing with a sodium hydroxide solution with the mass fraction of 5% and deionized water for 2 times, adding hydrochloric acid until the pH of the solution is 6, pouring into cold water with the temperature of 10 ℃ which is 3 times of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, cooling to room temperature, performing suction filtration, and drying at 60 ℃ for 5h to obtain the cold-proof breathable fabric.
Example 2
(1) Mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride according to the mass ratio of 1.0, heating to 60 ℃, reacting for 2 hours, heating to 80 ℃, and reacting for 4.5 hours to obtain a ring-opening compound; the gram weight is 190g/m 2 The nylon 6 fabric is placed in an irradiation tube, a ring-opening compound, deionized water and methanol are added according to a mass ratio of 1;
(2) Mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% hydrochloric acid according to a mass ratio of 1.3; placing the modified fabric in 2 x 10 composite gel with the mass of 0.25 times of that of the modified fabric 5 Permeating under MPa for 17min, aging for 22.5h, washing with anhydrous ethanol for 4 times, and drying at 40 deg.C for 7d to obtain aerogel layer;
(3) Mixing 3-aminophenyl trimethoxy silane and deionized water according to a mass ratio of 1;
(4) Mixing the pretreatment aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane according to the mass ratio of 1:0.15 under the protection of nitrogen, reacting for 3.5h at 60 ℃, cooling to room temperature, adding absolute ethyl alcohol 9.5 times the mass of the pretreatment aerogel layer and perfluorohexane 7 times the mass of the pretreatment aerogel layer, standing for 58min, taking out, placing in a high-pressure reaction kettle, adding Karstedt catalyst 0.02 times the mass of the pretreatment aerogel layer, sealing, heating to 75 ℃, opening a feeding valve, adding 1, 3-tetrafluoropropene 0.45 times the mass of the pretreatment aerogel layer at 10mL/min, heating to 100 ℃, preserving heat for 64min, cooling to 30 ℃, taking out, and obtaining a composite aerogel precursor;
(5) Heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide which is 0.4 times of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, stirring at 80rpm for 62min, adding a composite aerogel precursor which is 0.65 times of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, heating to 150 ℃, reacting for 2h, cooling to 90 ℃, sequentially washing with 5% sodium hydroxide solution and deionized water by mass fraction for 3 times, adding hydrochloric acid until the pH value of the solution is 6.5, pouring into 15 ℃ cold water which is 4 times of the mass of 2,3,4,5, 6-pentafluorobenzyl alcohol, cooling to room temperature, carrying out suction filtration, and drying at 60 ℃ for 7.5h to obtain the cold-proof breathable fabric.
Example 3
(1) Mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride according to a mass ratio of 1.4, heating to 60 ℃, reacting for 3 hours, heating to 80 ℃, and reacting for 6 hours to obtain a ring-opening compound; the gram weight is 200g/m 2 The nylon 6 fabric is placed in an irradiation tube, a ring-opening compound, deionized water and methanol are added according to the mass ratio of 1;
(2) Mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% hydrochloric acid according to a mass ratio of 1.4; placing the modified fabric in composite gel (3 × 10) with the mass of 0.4 times of that of the modified fabric 5 Permeating under MPa for 24min, aging for 25h, washing with anhydrous ethanol for 5 times, and drying at 40 deg.C for 8d to obtain aerogel layer;
(3) Mixing 3-aminophenyl trimethoxy silane and deionized water according to a mass ratio of 1;
(4) Mixing a pretreatment aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane according to the mass ratio of 1 to 0.2 under the protection of nitrogen, reacting for 5 hours at 60 ℃, cooling to room temperature, adding absolute ethyl alcohol which is 12 times of the mass of the pretreatment aerogel layer and perfluorohexane which is 9 times of the mass of the pretreatment aerogel layer, standing for 64 minutes, taking out, placing in a high-pressure reaction kettle, adding Karstedt catalyst which is 0.03 times of the mass of the pretreatment aerogel layer, sealing, heating to 80 ℃, opening a feeding valve, adding 1, 3-tetrafluoropropene which is 0.6 times of the mass of the pretreatment aerogel layer at 10mL/min, heating to 110 ℃, preserving heat for 70 minutes, cooling to 30 ℃, taking out, and obtaining a composite aerogel precursor;
(5) Heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide with the mass of 0.5 time of that of 2,3,4,5, 6-pentafluorobenzyl alcohol, stirring at 80rpm for 66min, adding a composite aerogel precursor with the mass of 0.8 time of that of 2,3,4,5, 6-pentafluorobenzyl alcohol, heating to 150 ℃, reacting for 3h, cooling to 100 ℃, sequentially washing with 5% sodium hydroxide solution and deionized water by mass fraction for 4 times, adding hydrochloric acid until the pH value of the solution is 7, pouring into 20 ℃ cold water with the mass of 5 times of that of 2,3,4,5, 6-pentafluorobenzyl alcohol, cooling to room temperature, performing suction filtration, and drying at 60 ℃ for 10h to obtain the cold-proof breathable fabric.
Comparative example 1
Comparative example 1 differs from example 2 in that step (1) is different, step (1) being changed to: the gram weight is 190g/m 2 The nylon 6 fabric is placed in an irradiation tube, maleic anhydride, deionized water and methanol are added according to the mass ratio of 1. The rest of the procedure was the same as in example 2.
Comparative example 2
Comparative example 2 differs from example 2 in that step (2) is different, step (2) being changed to: placing the modified fabric in silica gel (2 × 10) with the mass of 0.25 times of that of the modified fabric 5 Permeating under MPa for 17min, aging for 22.5h, washing with anhydrous ethanol for 4 times, and drying at 40 deg.C for 7d to obtain aerogel layer. The rest of the procedure was the same as in example 2.
Comparative example 3
Comparative example 3 differs from example 2 in that step (2) is different, step (2) being changed to: mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% hydrochloric acid according to a mass ratio of 1.4; and (3) placing the modified fabric into composite gel with the mass of 0.4 time of that of the modified fabric, aging for 25h, washing for 5 times by using absolute ethyl alcohol, and drying at 40 ℃ for 8d to obtain the aerogel layer. The rest of the procedure was the same as in example 2.
Comparative example 4
Comparative example 4 differs from example 2 in that step (4) is different, step (4) being changed to: placing the pretreated aerogel layer in a high-pressure reaction kettle, adding Karstedt catalyst with the mass of 0.02 time of that of the pretreated aerogel layer, sealing, heating to 75 ℃, opening a feeding valve, adding 1, 3-tetrafluoropropene with the mass of 0.45 time of that of the pretreated aerogel layer at the rate of 10mL/min, heating to 100 ℃, preserving heat for 64min, cooling to 30 ℃, and taking out to obtain the composite aerogel precursor. The rest of the procedure was the same as in example 2.
Comparative example 5
Comparative example 5 differs from example 2 in that step (5) is not present, and the rest of the procedure is the same as in example 2.
Effects of the invention
Table 1 below gives the results of the performance analysis of the cold-proof breathable fabrics according to examples 1 to 3 and comparative examples 1 to 5 of the present invention.
TABLE 1
| Heat insulation Rate (%) | Maximum rise in temperature (. Degree. C.) | Air permeability (mm/s) | Oil repellency rating | |
| Example 1 | 33.8 | 6.9 | 409.4 | 8 |
| Example 2 | 34.5 | 7.1 | 420.6 | 8 |
| Example 3 | 33.7 | 6.7 | 399.1 | 8 |
| Comparative example 1 | 33.5 | 3.3 | 289.1 | 7 |
| Comparative example 2 | 20.6 | 6.6 | 279.0 | 7 |
| Comparative example 3 | 28.5 | 6.5 | 283.5 | 6 |
| Comparative example 4 | 33.3 | 6.6 | 397.1 | 1 |
| Comparative example 5 | 33.6 | 6.4 | 398.0 | 2 |
Compared with the experimental data of the heat preservation rate, the air permeability and the highest temperature rise value of the comparative example, the experimental data show that the nylon 6 fabric is modified by using the hydroxyl and the maleic anhydride of the 3- (aminomethyl) -2-hydroxypentanal, hydrophilic groups are introduced, sweat on the surface of a human body is combined, and heat energy is generated through conversion, so that the cold-proof and warm-keeping effects are realized; then L-lysine diisocyanate reacts with 11-aminoundecyltrimethoxysilane to form composite gel with tetraethoxysilane serving as a mixed silicon source, then the modified fabric is subjected to permeation treatment, after moisture is volatilized, a capillary channel is formed at the joint of the composite gel and the modified fabric and communicated with an aerogel pore channel, and a silane compound is successfully combined with a silicon dioxide aerogel framework, so that the channel is a hydrophobic surface and forms a one-way moisture-conducting matrix together with the modified fabric, sweat can pass through the channel, the breathable effect of the fabric is improved, in addition, the silane compound and the aerogel act together to form a heat-insulating layer, the heat exchange inside and outside the fabric is prevented, and the cold-proof and warm-keeping effects of the fabric are enhanced; from the comparison of the experimental data of the oil repellency grades in the examples and the comparative examples, it can be found that the surface energy of the aerogel is reduced by grafting 3-aminophenyltrimethoxysilane, 2-carbomethoxyethylmethyldichlorosilane, 1, 3-tetrafluoropropene and 2,3,4,5, 6-pentafluorobenzyl alcohol on the surface of the aerogel to form an organic film, so that the fabric has an oil-proof effect, and meanwhile, the organic film and pores on the surface of the aerogel form a concave-convex structure, so that the surface energy is further reduced, and simultaneously, the organic film and the oil can form an air film, which is not beneficial to wetting and spreading of the oil, and the oil-proof effect of the fabric is enhanced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. A cold-proof air-permeable fabric is prepared through putting modified fabric in composite gel, immersing for a certain time, ageing, washing, drying to obtain aerogel layer, and modifying.
2. The cold-proof breathable fabric according to claim 1, wherein the modified fabric layer is prepared by mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride, heating for reaction, and continuing heating for reaction to obtain a ring-opening compound; placing the nylon 6 fabric in an irradiation tube, adding a ring-opening compound, deionized water, methanol and nitrogen, irradiating for a period of time, taking out, soaking in acetone, and standing for a period of time.
3. The cold-proof breathable fabric according to claim 1, wherein the composite gel is prepared by mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% by weight of hydrochloric acid, stirring for a period of time, adding 25% by weight of ammonia water, and uniformly stirring.
4. The cold-proof breathable fabric according to claim 1, wherein the modification treatment is mixing the pre-treated aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane under the protection of nitrogen, heating to react, cooling to room temperature, adding absolute ethyl alcohol and perfluorohexane, standing for a period of time, taking out, placing in a high-pressure reaction kettle, adding Karstedt catalyst, sealing, heating, adding 1, 3-tetrafluoropropene, continuing to heat, keeping the temperature for a period of time, and cooling to obtain a composite aerogel precursor; heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide, stirring for a period of time, adding the composite aerogel precursor, heating for reaction, cooling to a preset temperature, sequentially washing with a sodium hydroxide solution with the mass fraction of 5% and deionized water, adjusting the pH value with hydrochloric acid, pouring into cold water, cooling to room temperature, filtering, and drying.
5. A preparation method of a cold-proof breathable fabric is characterized by comprising the following preparation steps:
(1) The gram weight is 180 to 200g/m 2 The nylon 6 fabric is placed in an irradiation tube, and a ring-opening compound, deionized water and methanol are added according to a mass ratio of 1;
(2) Placing the modified fabric in composite gel with the mass of 0.1-0.4 time of that of the modified fabric, permeating for 10-24 min, aging for 20-25 h, washing for 3-5 times by using absolute ethyl alcohol, and drying at 40 ℃ for 6-8 d to obtain an aerogel layer;
(3) Mixing the pretreated aerogel layer and 2-carbomethoxyethyl methyl dichlorosilane according to the mass ratio of 1: 0.09-1: 0.2 under the protection of nitrogen, reacting at 60 ℃ for 2-5 h, cooling to room temperature, adding absolute ethyl alcohol which is 7-12 times of the mass of the pretreated aerogel layer and perfluorohexane which is 5-9 times of the mass of the pretreated aerogel layer, standing for 52-64 min, taking out, placing in a high-pressure reaction kettle, adding Karstedt catalyst which is 0.01-0.03 times of the mass of the pretreated aerogel layer, sealing, heating to 70-80 ℃, opening a feeding valve, adding 1, 3-tetrafluoropropene which is 0.3-0.6 times of the mass of the pretreated aerogel layer at 10mL/min, heating to 90-110 ℃, preserving heat for 58-70 min, cooling to 30 ℃, and taking out to obtain a composite aerogel precursor;
(4) Heating 2,3,4,5, 6-pentafluorobenzyl alcohol to be molten, adding potassium hydroxide with the mass of 0.3-0.5 time of that of the 2,3,4,5, 6-pentafluorobenzyl alcohol, stirring at 80rpm for 58-66 min, adding a composite aerogel precursor with the mass of 0.5-0.8 time of that of the 2,3,4,5, 6-pentafluorobenzyl alcohol, heating to 150 ℃, reacting for l-3 h, cooling to 80-100 ℃, washing with 5% sodium hydroxide solution and deionized water for 2-4 times in sequence, adding hydrochloric acid until the pH value of the solution is 6-7, pouring into cold water with the mass of 3-5 times of that of the 2,3,4,5, 6-pentafluorobenzyl alcohol and the temperature of 10-20 ℃, cooling to room temperature, performing suction filtration, and drying at 60 ℃ for 5-10 h to obtain the cold-proof breathable fabric.
6. The method for preparing cold-proof breathable fabric according to claim 5, wherein the irradiation dose in the step (1) is 8-11 kGy.
7. The method for preparing cold-proof breathable fabric according to claim 5, wherein the ring-opening compound in the step (1) is prepared by: mixing 3- (aminomethyl) -2-hydroxypentanal and maleic anhydride according to a mass ratio of 1.7-1, heating to 60 ℃, reacting for 1-3 h, heating to 80 ℃, and reacting for 3-6 h.
8. The method for preparing cold-proof breathable fabric according to claim 5, wherein the infiltration pressure in the step (2) is 1 x 10 5 ～3×10 5 MPa。
9. The method for preparing the cold-proof breathable fabric according to claim 5, wherein the preparation method of the composite gel in the step (2) comprises the following steps: mixing ethyl orthosilicate, 11-aminoundecyltrimethoxysilane, N-dimethylformyl, L-lysine diisocyanate, deionized water and 37% hydrochloric acid according to a mass ratio of 1.2.
10. The method for preparing the cold-proof breathable fabric according to claim 5, wherein the method for preparing the pre-treatment aerogel layer in the step (3) comprises the following steps: mixing 3-aminophenyltrimethoxysilane and deionized water according to a mass ratio of 1.
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