CN106498720A - A kind of temperature sensitive waterproof moisture permeable fabric and preparation method thereof - Google Patents
A kind of temperature sensitive waterproof moisture permeable fabric and preparation method thereof Download PDFInfo
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- CN106498720A CN106498720A CN201611016575.8A CN201611016575A CN106498720A CN 106498720 A CN106498720 A CN 106498720A CN 201611016575 A CN201611016575 A CN 201611016575A CN 106498720 A CN106498720 A CN 106498720A
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- 239000004744 fabric Substances 0.000 title claims abstract description 192
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000011248 coating agent Substances 0.000 claims abstract description 86
- 239000000017 hydrogel Substances 0.000 claims abstract description 43
- 238000004132 cross linking Methods 0.000 claims abstract description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000007062 hydrolysis Effects 0.000 claims abstract description 17
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 7
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 80
- 238000000576 coating method Methods 0.000 claims description 45
- 239000002270 dispersing agent Substances 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 19
- 239000003292 glue Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 13
- 229920001778 nylon Polymers 0.000 abstract description 38
- 239000004677 Nylon Substances 0.000 abstract description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 239000002904 solvent Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000463 material Substances 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 11
- 238000010526 radical polymerization reaction Methods 0.000 description 11
- 230000004584 weight gain Effects 0.000 description 11
- 235000019786 weight gain Nutrition 0.000 description 11
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 238000010345 tape casting Methods 0.000 description 9
- 230000035699 permeability Effects 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 7
- 229920001661 Chitosan Polymers 0.000 description 6
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 description 6
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 6
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000004753 textile Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 5
- 230000002706 hydrostatic effect Effects 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004034 viscosity adjusting agent Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- -1 silk Polymers 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Classifications
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- 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
- D06M13/12—Aldehydes; Ketones
- D06M13/123—Polyaldehydes; Polyketones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
- D06M15/568—Reaction products of isocyanates with polyethers
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
本发明提供了一种温敏防水透湿面料及其制备方法，将基布浸泡于盐酸中进行水解处理，所述基布为能够水解得到含有氨基和/或羟基结构的面料；将得到的水解基布浸泡于戊二醛溶液中进行预交联反应，然后将得到的预交联基布在温敏水凝胶中进行浸轧处理，得到交联基布；将得到的交联基布表面涂覆涂层剂，焙烘，得到温敏防水透湿面料。本发明提供的温敏防水透湿面料具有较好的温敏性能和防水透湿性能，温敏防水透湿尼龙面料中温敏水凝胶与尼龙面料结合性能好、牢度强，耐洗性优异。
The invention provides a temperature-sensitive waterproof and moisture-permeable fabric and a preparation method thereof. The base fabric is soaked in hydrochloric acid for hydrolysis treatment, and the base fabric can be hydrolyzed to obtain a fabric containing amino and/or hydroxyl structures; The base cloth is soaked in glutaraldehyde solution for pre-crosslinking reaction, and then the obtained pre-crosslinked base cloth is subjected to padding treatment in a temperature-sensitive hydrogel to obtain a cross-linked base cloth; the surface of the obtained cross-linked base cloth is coated with The coating agent is baked to obtain a temperature-sensitive waterproof and moisture-permeable fabric. The temperature-sensitive waterproof and moisture-permeable fabric provided by the present invention has good temperature-sensitive performance and waterproof and moisture-permeable performance. In the temperature-sensitive waterproof and moisture-permeable nylon fabric, the temperature-sensitive hydrogel and nylon fabric have good bonding performance, strong fastness, and excellent washability. .
Description
技术领域technical field
本发明属于纺织面料生产技术领域，具体涉及一种温敏防水透湿面料及其制备方法。The invention belongs to the technical field of textile fabric production, and in particular relates to a temperature-sensitive waterproof and moisture-permeable fabric and a preparation method thereof.
背景技术Background technique
随着人们生活水平的日益提高，人们对纺织面料功能的要求越来越高。将人体所产生的水汽以不显汗的方式排到服装外是服装面料所需要具有的重要性能，而在不同温度及运动条件下人体排热排汗量是不同的。因此，为了维持穿着者的舒适性，对于纺织服装的透湿气性能在不同环境下的要求是不同的，如高温下要求高的透湿性以保证良好的排热排汗性，而低温时较低的透湿气性可保证保暖性。With the improvement of people's living standards, people's requirements for the function of textile fabrics are getting higher and higher. Discharging the water vapor produced by the human body out of the clothing in a non-perspiring manner is an important performance required for clothing fabrics, and the amount of heat and sweat released by the human body is different under different temperature and exercise conditions. Therefore, in order to maintain the comfort of the wearer, the requirements for the moisture permeability of textile clothing are different in different environments. Low moisture vapor transmission ensures warmth.
现有技术中以水性聚氨酯、PNCS微凝胶及水制备得到温控透湿面料整理剂，并用该整理剂对纺织面料进行整理，得到的纺织面料虽然具有较好的防水透湿性能，但是该整理剂与纺织面料之间仅仅是粘合的作用，在后续使用过程中PNCS微凝胶容易脱落、牢度差，不能满足实际需要。In the prior art, a temperature-controlled moisture-permeable fabric finishing agent is prepared with water-based polyurethane, PNCS microgel and water, and the textile fabric is finished with the finishing agent. Although the obtained textile fabric has good waterproof and moisture-permeable performance, the The relationship between the finishing agent and the textile fabric is only for adhesion, and the PNCS microgel is easy to fall off and has poor fastness during subsequent use, which cannot meet actual needs.
发明内容Contents of the invention
本发明的目的在于提供一种温敏防水透湿面料及其制备方法，旨在能够提供一种具有优良温敏功能和防水透湿性能的面料。The purpose of the present invention is to provide a temperature-sensitive waterproof and moisture-permeable fabric and a preparation method thereof, aiming to provide a fabric with excellent temperature-sensitive function and waterproof and moisture-permeable performance.
为了实现上述发明目的，本发明提供以下技术方案：In order to achieve the above-mentioned purpose of the invention, the present invention provides the following technical solutions:
本发明提供了一种温敏防水透湿面料的制备方法，包括以下步骤：The invention provides a method for preparing a temperature-sensitive waterproof and moisture-permeable fabric, comprising the following steps:
(1)将基布浸泡于盐酸中进行水解处理，所述基布为能够水解得到含有氨基和/或羟基结构的面料；(1) Soak the base cloth in hydrochloric acid to carry out hydrolysis treatment, the base cloth is a fabric that can be hydrolyzed to obtain amino and/or hydroxyl structures;
(2)将所述步骤(1)得到的水解基布浸泡于戊二醛溶液中进行预交联反应，然后将得到的预交联基布在温敏水凝胶中进行浸轧处理，得到交联基布；(2) Soak the hydrolyzed base cloth obtained in the step (1) in a glutaraldehyde solution to carry out a pre-crosslinking reaction, and then perform a padding treatment on the obtained pre-crosslinked base cloth in a temperature-sensitive hydrogel to obtain a cross-linked fabric;
(3)在所述步骤(2)得到的交联基布表面涂覆涂层剂后焙烘，得到温敏防水透湿面料。(3) Coating the coating agent on the surface of the cross-linked base cloth obtained in the step (2) and then baking to obtain a temperature-sensitive waterproof and moisture-permeable fabric.
优选的，所述按质量份数计，所述步骤(2)中的温敏水凝胶由包括以下组分的原料制备得到：Preferably, in terms of parts by mass, the thermosensitive hydrogel in the step (2) is prepared from raw materials comprising the following components:
优选的，所述步骤(1)中盐酸的摩尔浓度为0.4～0.6mol/L。Preferably, the molar concentration of hydrochloric acid in the step (1) is 0.4-0.6 mol/L.
优选的，所述步骤(1)中水解处理的时间为20～40min。Preferably, the time for the hydrolysis treatment in the step (1) is 20-40 minutes.
优选的，所述步骤(2)中戊二醛溶液的质量百分浓度为4～6％。Preferably, the mass percentage concentration of the glutaraldehyde solution in the step (2) is 4-6%.
优选的，所述步骤(2)中预交联反应的时间为20～40min。Preferably, the time for the pre-crosslinking reaction in the step (2) is 20-40 minutes.
优选的，步骤(2)中浸轧处理的轧余率为70～90％。Preferably, the excess rate of the padding treatment in step (2) is 70-90%.
优选的，按质量份数计，所述步骤(3)中的涂层剂由包括以下组分的原料制备得到：Preferably, in parts by mass, the coating agent in the step (3) is prepared from raw materials comprising the following components:
防水透湿涂层胶 80～100份Waterproof and moisture-permeable coating glue 80-100 parts
甲苯 16～20份Toluene 16～20 parts
消光粉 3～5份Matting powder 3~5 parts
分散剂 0.3～0.7份Dispersant 0.3～0.7 parts
交联促进剂 0.8～1.2份。Cross-linking accelerator 0.8 to 1.2 parts.
优选的，所述步骤(3)中焙烘的温度为150～170℃，焙烘的时间为1～3min。Preferably, the baking temperature in the step (3) is 150-170° C., and the baking time is 1-3 minutes.
本发明提供了上述技术方案所述制备方法制备得到的温敏防水透湿面料，包括温敏水凝胶交联基布和设置在所述交联基布表面的防水透湿涂层。The present invention provides a temperature-sensitive waterproof and moisture-permeable fabric prepared by the preparation method described in the above technical solution, comprising a temperature-sensitive hydrogel cross-linked base fabric and a waterproof and moisture-permeable coating arranged on the surface of the cross-linked base fabric.
本发明提供了一种温敏防水透湿面料及其制备方法，将基布浸泡于盐酸中进行水解处理，所述基布为能够水解得到含有氨基和/或羟基结构的面料；将得到的水解基布浸泡于戊二醛溶液中进行预交联反应，然后将得到的预交联基布在温敏水凝胶中进行浸轧处理，得到交联基布；将得到的交联基布表面涂覆涂层剂后焙烘，得到温敏防水透湿面料。本发明通过温敏水凝胶与水解基布发生交联反应，使温敏水凝胶牢固附着在基布表面，使面料具有良好的温敏性能，再通过涂覆涂层剂，在交联基布表面形成防水透湿涂层，使面料具有良好的防水透湿性能。实验结果表明，本发明制备得到的温敏防水透湿面料的静水压为45.8～49.6KPa，尤其是透湿量达4208～4072g/m2·24h，明显高于未经温敏水凝胶浸轧处理得到的尼龙面料的透湿量。The invention provides a temperature-sensitive waterproof and moisture-permeable fabric and a preparation method thereof. The base fabric is soaked in hydrochloric acid for hydrolysis treatment, and the base fabric is capable of being hydrolyzed to obtain a fabric containing amino and/or hydroxyl structures; The base cloth is soaked in glutaraldehyde solution for pre-crosslinking reaction, and then the obtained pre-crosslinked base cloth is subjected to padding treatment in a temperature-sensitive hydrogel to obtain a cross-linked base cloth; the surface of the obtained cross-linked base cloth is coated with The coating agent is then baked to obtain a temperature-sensitive waterproof and moisture-permeable fabric. In the present invention, through the cross-linking reaction between the temperature-sensitive hydrogel and the hydrolyzed base fabric, the temperature-sensitive hydrogel is firmly attached to the surface of the base fabric, so that the fabric has good temperature-sensitive performance, and then the coating agent is applied to form a The waterproof and moisture-permeable coating makes the fabric have good waterproof and moisture-permeable performance. The experimental results show that the hydrostatic pressure of the temperature-sensitive waterproof and moisture-permeable fabric prepared by the present invention is 45.8-49.6KPa, especially the moisture permeability reaches 4208-4072g/m 2 ·24h, which is significantly higher than that without temperature-sensitive hydrogel padding. The moisture permeability of the treated nylon fabric.
此外，本发明提供的温敏防水透湿尼龙面料比未经温敏水凝胶浸轧处理得到的尼龙面料的质量损失率低，并且随着洗涤次数的增加，质量损失率依然保持在5％以下，说明本发明制备得到的温敏防水透湿尼龙面料耐洗性优异，同时也说明本发明制备得到的温敏防水透湿尼龙面料中温敏水凝胶与尼龙面料结合性能好、牢度强。In addition, the temperature-sensitive waterproof and moisture-permeable nylon fabric provided by the present invention has a lower mass loss rate than the nylon fabric obtained without the temperature-sensitive hydrogel padding treatment, and as the number of washings increases, the mass loss rate remains below 5%. It shows that the temperature-sensitive waterproof and moisture-permeable nylon fabric prepared by the present invention has excellent washability, and it also shows that the temperature-sensitive waterproof and moisture-permeable nylon fabric prepared by the present invention has good bonding performance and strong fastness to the temperature-sensitive hydrogel and nylon fabric.
附图说明Description of drawings
图1为实施例4制备得到的交联基布的接触角随温度变化图；Fig. 1 is that the contact angle of the cross-linked base cloth prepared by embodiment 4 varies with temperature;
图2为实施例4制备得到的交联基布的扫描电镜图；Fig. 2 is the scanning electron micrograph of the crosslinked base cloth that embodiment 4 prepares;
图3为未经任何处理的尼龙基布的扫描电镜图。Figure 3 is a scanning electron micrograph of the nylon base cloth without any treatment.
具体实施方式detailed description
本发明提供了一种温敏防水透湿面料的制备方法，包括以下步骤：The invention provides a method for preparing a temperature-sensitive waterproof and moisture-permeable fabric, comprising the following steps:
(1)将基布浸泡于盐酸中进行水解处理，所述基布为能够水解得到含有氨基和/或羟基结构的面料；(1) Soak the base cloth in hydrochloric acid to carry out hydrolysis treatment, the base cloth is a fabric that can be hydrolyzed to obtain amino and/or hydroxyl structures;
(2)将所述步骤(1)得到的水解基布浸泡于戊二醛溶液中进行预交联反应，然后将得到的预交联基布在温敏水凝胶中进行浸轧处理，得到交联基布；(2) Soak the hydrolyzed base cloth obtained in the step (1) in a glutaraldehyde solution to carry out a pre-crosslinking reaction, and then perform a padding treatment on the obtained pre-crosslinked base cloth in a temperature-sensitive hydrogel to obtain a cross-linked fabric;
(3)在所述步骤(2)得到的交联基布表面涂覆涂层剂后焙烘，得到温敏防水透湿面料。(3) Coating the coating agent on the surface of the cross-linked base cloth obtained in the step (2) and then baking to obtain a temperature-sensitive waterproof and moisture-permeable fabric.
本发明将基布浸泡于盐酸中进行水解处理，所述基布为能够水解得到含有氨基和/或羟基结构的面料。在本发明中，所述基布优选为尼龙、真丝、棉或涤纶。在本发明的实施例中，具体采用70D×70D，260T，2/2斜纹尼龙布作为基布。在本发明中，所述盐酸的摩尔浓度优选为0.4～0.6mol/L，具体可为0.4mol/L、0.5mol/L或0.6mol/L。在本发明中，所述水解处理的时间优选为20～40min，更优选为25～35min，最优选为30min。在本发明中，所述水解处理的温度优选为38～42℃。在本发明中，所述水解处理可以使基布表面形成氨基和/或羟基。In the present invention, the base cloth is soaked in hydrochloric acid for hydrolysis treatment, and the base cloth is a fabric containing amino and/or hydroxyl structures that can be hydrolyzed. In the present invention, the base cloth is preferably nylon, silk, cotton or polyester. In the embodiment of the present invention, 70D×70D, 260T, 2/2 twill nylon fabric is specifically used as the base fabric. In the present invention, the molar concentration of the hydrochloric acid is preferably 0.4-0.6 mol/L, specifically 0.4 mol/L, 0.5 mol/L or 0.6 mol/L. In the present invention, the time for the hydrolysis treatment is preferably 20-40 minutes, more preferably 25-35 minutes, and most preferably 30 minutes. In the present invention, the temperature of the hydrolysis treatment is preferably 38-42°C. In the present invention, the hydrolysis treatment can form amino groups and/or hydroxyl groups on the surface of the base fabric.
完成水解处理后，本发明将得到的水解基布浸泡于戊二醛溶液中进行预交联反应，得到预交联基布。在本发明中，所述戊二醛溶液的质量百分浓度优选为4％～6％，具体可为4％、5％或6％。本发明对于所述戊二醛溶液中的溶剂没有特殊的限定，采用本领域技术人员熟知的能够溶解戊二醛且不影响后续处理的溶剂即可。在本发明中，所述戊二醛溶液中的溶剂优选包括水。After completing the hydrolysis treatment, the present invention soaks the obtained hydrolyzed base cloth in a glutaraldehyde solution to carry out a pre-crosslinking reaction to obtain a pre-crosslinked base cloth. In the present invention, the mass percent concentration of the glutaraldehyde solution is preferably 4% to 6%, specifically 4%, 5% or 6%. In the present invention, there is no special limitation on the solvent in the glutaraldehyde solution, and a solvent known to those skilled in the art that can dissolve glutaraldehyde without affecting the subsequent treatment can be used. In the present invention, the solvent in the glutaraldehyde solution preferably includes water.
在本发明中，所述预交联反应的时间优选为20～40min，更优选为25～35min，最优选为30min。在本发明中，所述预交联反应的温度优选为38～42℃。In the present invention, the time for the pre-crosslinking reaction is preferably 20-40 min, more preferably 25-35 min, and most preferably 30 min. In the present invention, the temperature of the pre-crosslinking reaction is preferably 38-42°C.
预交联反应后，本发明将得到的预交联基布在温敏水凝胶中进行浸轧处理，得到交联基布。在本发明中，按质量份数计，所述温敏水凝胶优选由包括以下组分的原料制备得到：After the pre-crosslinking reaction, the present invention pads the obtained pre-crosslinked base cloth in the temperature-sensitive hydrogel to obtain the cross-linked base cloth. In the present invention, in terms of parts by mass, the thermosensitive hydrogel is preferably prepared from raw materials comprising the following components:
更优选的，所述温敏水凝胶由包括以下组分的原料制备得到：More preferably, the thermosensitive hydrogel is prepared from raw materials comprising the following components:
在本发明中，所述温敏水凝胶的制备方法优选包括以下步骤：In the present invention, the preparation method of the thermosensitive hydrogel preferably includes the following steps:
将壳聚糖、N-异丙基丙烯酰胺、N,N-亚甲基双丙烯酰胺和醋酸进行第一混合，然后再与N,N,N,N-四甲基乙二胺和过硫酸铵进行第二混合，将得到的混合物料在保护气氛下进行自由基聚合反应，得到温敏水凝胶。Chitosan, N-isopropylacrylamide, N,N-methylenebisacrylamide and acetic acid are mixed first, then mixed with N,N,N,N-tetramethylethylenediamine and persulfuric acid The ammonium is mixed for the second time, and the obtained mixed material is subjected to a free radical polymerization reaction under a protective atmosphere to obtain a temperature-sensitive hydrogel.
在本发明中，所述第二混合优选在搅拌条件下进行。本发明对于所述搅拌没有特殊的限定，采用本领域技术人员熟知的能够将反应原料混合均匀的搅拌的技术方案即可。在本发明中，所述搅拌的速率优选为700～900rpm；所述搅拌的时间优选为5～10min。In the present invention, the second mixing is preferably performed under stirring conditions. In the present invention, there is no special limitation on the stirring, and a technical scheme that can uniformly mix the reaction raw materials can be adopted. In the present invention, the stirring speed is preferably 700-900 rpm; the stirring time is preferably 5-10 min.
在本发明中，所述N,N,N,N-四甲基乙二胺优选以N,N,N,N-四甲基乙二胺溶液的形式与制备温敏水凝胶所需的其它反应原料混合。在本发明中，所述N,N,N,N-四甲基乙二胺溶液的质量百分浓度优选为8％～12％，更优选为9％～11％，最优选为10％。本发明对于所述N,N,N,N-四甲基乙二胺溶液中的溶剂没有特殊的限定，采用本领域技术人员熟知的能够溶解N,N,N,N-四甲基乙二胺且不影响后续处理的溶剂即可。在本发明中，所述N,N,N,N-四甲基乙二胺溶液中的溶剂优选包括水。In the present invention, the N,N,N,N-tetramethylethylenediamine is preferably reacted in the form of N,N,N,N-tetramethylethylenediamine solution with other materials required for the preparation of thermosensitive hydrogels The ingredients are mixed. In the present invention, the mass percent concentration of the N,N,N,N-tetramethylethylenediamine solution is preferably 8%-12%, more preferably 9%-11%, and most preferably 10%. In the present invention, there is no special limitation on the solvent in the N,N,N,N-tetramethylethylenediamine solution. Amines and solvents that do not affect subsequent processing are sufficient. In the present invention, the solvent in the N,N,N,N-tetramethylethylenediamine solution preferably includes water.
本发明对于提供所述保护气氛所需要的保护气体种类没有特殊的限定，采用本领域技术人员熟知的保护气体即可。本发明优选采用氮气作为保护气体。In the present invention, there is no special limitation on the type of protective gas required to provide the protective atmosphere, and the protective gas well known to those skilled in the art can be used. In the present invention, nitrogen is preferably used as the protective gas.
在本发明中，所述自由基聚合反应的温度优选为20～40℃，更优选为25～35℃；在本发明的实施例中，所述自由基聚合反应具体在室温下进行。在本发明中，所述自由基聚合反应的时间优选为20～30h，更优选为22～26h。本发明对于进行所述自由基聚合反应所采用的反应容器没有特殊的限定，采用本领域技术人员熟知的能够用于进行自由基聚合反应的反应容器即可。In the present invention, the temperature of the radical polymerization reaction is preferably 20-40° C., more preferably 25-35° C.; in an embodiment of the present invention, the radical polymerization reaction is carried out at room temperature. In the present invention, the free radical polymerization reaction time is preferably 20-30 hours, more preferably 22-26 hours. In the present invention, there is no special limitation on the reaction vessel used for the radical polymerization reaction, and a reaction vessel known to those skilled in the art that can be used for the radical polymerization reaction can be used.
本发明将所述预交联基布在温敏水凝胶中进行浸轧处理，得到交联基布。在本发明中，所述浸轧处理优选为二浸二轧，具体是将预交联基布浸没在温敏水凝胶中后经轧辊轧过，共计重复两次。在本发明中，所述浸轧处理过程中的轧制压力优选为1～3kgf/cm2，具体可为1kgf/cm2、2kgf/cm2或3kgf/cm2；轧余率优选为70％～90％，更优选为75％～85％。在本发明中，所述温敏水凝胶与预交联基布在浸轧处理过程中发生交联反应，牢固附着在基布表面。In the invention, the pre-crosslinked base cloth is subjected to padding treatment in a temperature-sensitive hydrogel to obtain a cross-linked base cloth. In the present invention, the padding treatment is preferably two dipping and two padding, specifically, the pre-crosslinked base fabric is immersed in the temperature-sensitive hydrogel and then rolled by a roll, and is repeated twice in total. In the present invention, the rolling pressure during the padding process is preferably 1 to 3kgf/cm 2 , specifically 1kgf/cm 2 , 2kgf/cm 2 or 3kgf/cm 2 ; the rolling ratio is preferably 70% ~ 90%, more preferably 75% to 85%. In the present invention, the temperature-sensitive hydrogel and the pre-crosslinked base fabric undergo a crosslinking reaction during the padding process, and are firmly attached to the surface of the base fabric.
完成所述浸轧处理后，本发明优选对得到的基布进行干燥，得到交联基布。在本发明中，所述干燥优选采用烘干。在本发明中，所述烘干优选包括预烘干和二次烘干。在本发明中，所述预烘干的温度优选为60～70℃；所述预烘干的时间优选为3～5min。在本发明中，所述二次烘干的温度优选为85～95℃；所述二次烘干的时间优选为3～5min。After the padding treatment is completed, the present invention preferably dries the obtained base cloth to obtain a crosslinked base cloth. In the present invention, the drying is preferably drying. In the present invention, the drying preferably includes pre-drying and secondary drying. In the present invention, the temperature of the pre-drying is preferably 60-70° C.; the time of the pre-drying is preferably 3-5 minutes. In the present invention, the temperature of the secondary drying is preferably 85-95°C; the time of the secondary drying is preferably 3-5 minutes.
得到交联基布后，本发明将所述交联基布表面涂覆涂层剂后焙烘，得到温敏防水透湿面料。在本发明中，按质量份数计，所述涂层剂优选由包括以下组分的原料制备得到：After obtaining the cross-linked base fabric, the present invention coats the surface of the cross-linked base fabric with a coating agent and then bakes to obtain a temperature-sensitive waterproof and moisture-permeable fabric. In the present invention, in terms of parts by mass, the coating agent is preferably prepared from raw materials comprising the following components:
防水透湿涂层胶 80～100份Waterproof and moisture-permeable coating glue 80-100 parts
甲苯 16～20份Toluene 16～20 parts
消光粉 3～5份Matting powder 3~5 parts
分散剂 0.3～0.7份Dispersant 0.3～0.7 parts
交联促进剂 0.8～1.2份。Cross-linking accelerator 0.8 to 1.2 parts.
在本发明中，按质量份数计，制备所述涂层剂的原料优选包括防水透湿涂层胶80～100份，更优选为85～95份，最优选为88～92份。在本发明中，所述防水透湿涂层胶优选为聚醚型聚氨酯。本发明对于所述防水透湿涂层胶的来源没有特殊的限定，采用本领域技术人员熟知的防水透湿涂层胶的市售商品即可。在本发明的实施例中，具体采用辽宁恒星精细化工有限公司生产的防水透湿涂层胶FS-5600。In the present invention, in terms of parts by mass, the raw materials for preparing the coating agent preferably include 80-100 parts of waterproof and moisture-permeable coating glue, more preferably 85-95 parts, and most preferably 88-92 parts. In the present invention, the waterproof and moisture-permeable coating adhesive is preferably polyether polyurethane. The present invention has no special limitation on the source of the waterproof and moisture-permeable coating glue, and commercially available waterproof and moisture-permeable coating glue well known to those skilled in the art can be used. In the embodiment of the present invention, the waterproof and moisture-permeable coating adhesive FS-5600 produced by Liaoning Xingxing Fine Chemical Co., Ltd. is specifically used.
在本发明中，按质量份数计，制备所述涂层剂的原料优选包括甲苯16～20份，更优选为18～19份。In the present invention, in terms of parts by mass, the raw materials for preparing the coating agent preferably include 16-20 parts of toluene, more preferably 18-19 parts.
在本发明中，按质量份数计，制备所述涂层剂的原料优选包括消光粉3～5份，具体可为3份、4份或5份。本发明对于所述消光粉的种类或来源没有特殊的限定，采用本领域技术人员熟知的消光粉的市售商品即可。在本发明的实施例中，具体采用上海凯茵化工化工有限公司生产的德固赛消光粉TS-100。In the present invention, in terms of parts by mass, the raw materials for preparing the coating agent preferably include 3-5 parts of matting powder, specifically 3 parts, 4 parts or 5 parts. The present invention has no special limitation on the type or source of the matting powder, and commercially available matting powders well known to those skilled in the art can be used. In the embodiment of the present invention, Degussa matting powder TS-100 produced by Shanghai Kaiyin Chemical Co., Ltd. is specifically used.
在本发明中，按质量份数计，制备所述涂层剂的原料优选包括分散剂0.3～0.7份，更优选为0.4～0.6份。在本发明中，所述分散剂优选为溶剂型分散剂。在本发明的实施例中，具体采用德谦(上海)化学有限公司生产的溶剂型分散剂9850。In the present invention, the raw materials for preparing the coating agent preferably include 0.3-0.7 parts of dispersant, more preferably 0.4-0.6 parts by mass parts. In the present invention, the dispersant is preferably a solvent-based dispersant. In the embodiment of the present invention, solvent-based dispersant 9850 produced by Deqian (Shanghai) Chemical Co., Ltd. is specifically used.
在本发明中，按质量份数计，制备所述涂层剂的原料优选包括交联促进剂0.8～1.2份，更优选为0.9～1.1份。本发明对于所述交联促进剂的种类或来源没有特殊的限定，采用本领域技术人员熟知的交联促进剂即可。在本发明的实施例中，具体采用辽宁恒星精细化工有限公司生产的交联促进剂DF-899。In the present invention, the raw materials for preparing the coating agent preferably include 0.8-1.2 parts, more preferably 0.9-1.1 parts, of a crosslinking accelerator in terms of parts by mass. The present invention has no special limitation on the type or source of the cross-linking accelerator, and the cross-linking accelerator well-known to those skilled in the art can be used. In the embodiment of the present invention, the cross-linking accelerator DF-899 produced by Liaoning Xingxing Fine Chemical Co., Ltd. is specifically used.
在本发明中，所述涂层剂的制备方法优选包括以下步骤：In the present invention, the preparation method of the coating agent preferably comprises the following steps:
将防水透湿涂层胶、甲苯、消光粉、分散剂和交联促进剂混合、分散，得到涂层剂。The coating agent is obtained by mixing and dispersing waterproof and moisture-permeable coating glue, toluene, matting powder, dispersant and crosslinking accelerator.
本发明对于所述分散没有特殊的限定，采用本领域技术人员熟知的分散的技术方案即可。本发明优选采用分散机进行所述分散。在本发明中，进行所述分散时的转速优选为900～1100rpm。在本发明中，所述分散的时间优选为4～6min。The present invention has no special limitation on the dispersion, and the technical solution of dispersion well known to those skilled in the art can be adopted. In the present invention, it is preferred to use a disperser to carry out the dispersing. In the present invention, the rotation speed when performing the dispersion is preferably 900 to 1100 rpm. In the present invention, the dispersion time is preferably 4-6 minutes.
在本发明中，制备得到的涂层剂的黏度优选为8000～10000CPS，更优选为8500～9500CPS。在本发明中，可通过加入黏度调节剂调节涂层剂的黏度，具体是将防水透湿涂层胶、甲苯、消光粉、分散剂和交联促进剂混合、分散后，向得到的混合物料中加入黏度调节剂，继续分散至所得物料的黏度为8000～10000CPS。本发明对所述黏度调节剂的种类和用量没有特殊的限定，将涂层剂调整至所需黏度即可。在本发明中，所述黏度调节剂优选为甲苯；所述黏度调节剂的用量优选为17～20份。In the present invention, the viscosity of the prepared coating agent is preferably 8000-10000 CPS, more preferably 8500-9500 CPS. In the present invention, the viscosity of the coating agent can be adjusted by adding a viscosity modifier, specifically, after mixing and dispersing the waterproof and moisture-permeable coating glue, toluene, matting powder, dispersant and crosslinking accelerator, to the obtained mixed material Add a viscosity modifier to the mixture and continue to disperse until the viscosity of the obtained material is 8000-10000CPS. In the present invention, there is no special limitation on the type and amount of the viscosity regulator, and the coating agent can be adjusted to the required viscosity. In the present invention, the viscosity modifier is preferably toluene; the amount of the viscosity modifier is preferably 17-20 parts.
本发明对于所述涂覆的方式没有特殊的限定，采用本领域技术人员熟知的涂覆的技术方案即可。本发明优选采用干法直接涂覆。本发明对于进行所述涂覆所采用的设备没有特殊的限定，采用本领域技术人员熟知的用于涂覆的设备即可。本发明优选采用浮刀式涂层机进行所述涂覆。在本发明中，所述涂层剂的涂敷量优选使基布在焙烘后的干增重为16～20g/m2，更优选为17～19g/m2，最优选为18g/m2。在本发明中，所述涂层剂在基布表面形成防水透湿涂层，使面料具有良好的防水透湿性能。In the present invention, there is no special limitation on the coating method, and a coating technical solution well known to those skilled in the art can be used. The present invention preferably employs dry direct coating. In the present invention, there is no special limitation on the equipment used for the coating, and the coating equipment well known to those skilled in the art can be used. In the present invention, a floating knife coater is preferably used for the coating. In the present invention, the coating amount of the coating agent is preferably such that the dry weight gain of the base fabric after baking is 16-20 g/m 2 , more preferably 17-19 g/m 2 , most preferably 18 g/m 2 . In the present invention, the coating agent forms a waterproof and moisture-permeable coating on the surface of the base fabric, so that the fabric has good waterproof and moisture-permeable performance.
在本发明中，所述焙烘的温度优选为150～170℃，更优选为155～165℃；所述焙烘的时间优选为1～3min，具体可为1min、2min或3min。In the present invention, the baking temperature is preferably 150-170° C., more preferably 155-165° C.; the baking time is preferably 1-3 minutes, specifically 1 minute, 2 minutes or 3 minutes.
本发明提供了上述技术方案制备得到的温敏防水透湿面料，包括温敏水凝胶交联基布和设置在所述交联基布表面的防水透湿涂层。本发明提供的温敏防水透湿面料中，所述温敏水凝胶通过与基布发生交联反应牢固附着其表面；所述防水透湿涂层具有防水透湿特性，使面料具有温敏防水透湿功能。The present invention provides a temperature-sensitive waterproof and moisture-permeable fabric prepared by the above-mentioned technical solution, including a temperature-sensitive hydrogel cross-linked base fabric and a waterproof and moisture-permeable coating arranged on the surface of the cross-linked base fabric. In the temperature-sensitive waterproof and moisture-permeable fabric provided by the present invention, the temperature-sensitive hydrogel is firmly attached to the surface through a cross-linking reaction with the base fabric; wet function.
下面将结合本发明中的实施例，对本发明中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions in the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Apparently, the described embodiments are only some of the embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
将70D×70D，260T，2/2斜纹尼龙布浸泡在0.5mol/L的盐酸中，进行水解处理30min，得到水解基布；Soak 70D×70D, 260T, 2/2 twill nylon fabric in 0.5mol/L hydrochloric acid, and perform hydrolysis treatment for 30 minutes to obtain hydrolyzed base fabric;
按质量份数计，将壳聚糖15份、N-异丙基丙烯酰胺20份、N、N-亚甲基双丙烯酰胺1份在室温下用醋酸2份溶解；然后加入质量百分含量为10％的N、N、N、N-四甲基乙二胺溶液1份和过硫酸铵1份，800r/min搅拌5min后装三口圆底烧瓶，在氮气保护下室温进行自由基聚合反应24h，得到温敏水凝胶；In terms of parts by mass, 15 parts of chitosan, 20 parts of N-isopropylacrylamide, and 1 part of N, N-methylenebisacrylamide were dissolved with 2 parts of acetic acid at room temperature; It is 1 part of 10% N, N, N, N-tetramethylethylenediamine solution and 1 part of ammonium persulfate, stirred at 800r/min for 5min, then filled into a three-necked round bottom flask, and carried out free radical polymerization at room temperature under the protection of nitrogen 24h, obtain thermosensitive hydrogel;
将水解基布浸泡于质量百分含量为5％的戊二醛溶液中，进行预交联反应30min，然后将得到的预交联基布在温敏水凝胶中二浸二轧，其中轧制压力为1kgf/cm2，轧余率为70％，将得到的基布在65℃预烘干3min，在90℃二次烘干3min，得到交联基布；Soak the hydrolyzed base cloth in a glutaraldehyde solution with a mass percentage of 5%, perform a pre-crosslinking reaction for 30 minutes, and then dip the obtained pre-crosslinked base cloth in the temperature-sensitive hydrogel for two dips and two rolls, wherein the rolling pressure 1kgf/cm 2 , the scrap rate is 70%, pre-dry the obtained base fabric at 65°C for 3 minutes, and dry it again at 90°C for 3 minutes to obtain a cross-linked base fabric;
将防水透湿涂层胶80份、甲苯16份、消光粉3份、溶剂型分散剂0.3份和交联促进剂0.8份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为8000CPS，得到涂层剂；Mix 80 parts of waterproof and moisture-permeable coating glue, 16 parts of toluene, 3 parts of matting powder, 0.3 parts of solvent-based dispersant and 0.8 parts of crosslinking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing To the viscosity of gained material is 8000CPS, obtains coating agent;
采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，150℃焙烘1min，干增重16g/m2，得到温敏防水透湿面料。Direct coating by dry method, coating the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, baking at 150°C for 1 minute, and dry weight gain of 16g/m 2 to obtain a temperature-sensitive waterproof and moisture-permeable fabric .
实施例2Example 2
将70D×70D，260T，2/2斜纹尼龙布浸泡在0.4mol/L的盐酸中，进行水解处理40min，得到水解基布；Soak 70D×70D, 260T, 2/2 twill nylon fabric in 0.4mol/L hydrochloric acid, and perform hydrolysis treatment for 40min to obtain hydrolyzed base fabric;
按质量份数计，将壳聚糖25份、N-异丙基丙烯酰胺40份、N、N-亚甲基双丙烯酰胺1.5份在室温下用醋酸4份溶解；然后加入质量百分含量为8％的N、N、N、N-四甲基乙二胺溶液2份和过硫酸铵1.5份，900r/min搅拌5min后装三口圆底烧瓶，在氮气保护下室温进行自由基聚合反应30h，得到温敏水凝胶；In terms of parts by mass, 25 parts of chitosan, 40 parts of N-isopropylacrylamide, 1.5 parts of N, N-methylenebisacrylamide were dissolved with 4 parts of acetic acid at room temperature; It is 2 parts of 8% N, N, N, N-tetramethylethylenediamine solution and 1.5 parts of ammonium persulfate, stirred at 900r/min for 5min, then filled into a three-neck round bottom flask, and carried out free radical polymerization at room temperature under the protection of nitrogen 30h, obtain thermosensitive hydrogel;
将水解基布浸泡于质量百分含量为4％的戊二醛溶液中，进行预交联反应40min，然后将得到的预交联基布在温敏水凝胶中二浸二轧，其中轧制压力为2kgf/cm2，轧余率为80％，将得到的基布在60℃预烘干5min，在85℃二次烘干4min，得到交联基布；Soak the hydrolyzed base fabric in a glutaraldehyde solution with a mass percentage of 4%, perform a pre-crosslinking reaction for 40 minutes, and then dip the obtained pre-crosslinked base fabric in the temperature-sensitive hydrogel for two dips and two rolls, wherein the rolling pressure 2kgf/cm 2 , the scrap rate is 80%, pre-dry the obtained base fabric at 60°C for 5 minutes, and dry it again at 85°C for 4 minutes to obtain a cross-linked base fabric;
将防水透湿涂层胶85份、甲苯17份、消光粉3.5份、溶剂型分散剂0.4份和交联促进剂0.9份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为8500CPS，得到涂层剂；Mix 85 parts of waterproof and moisture-permeable coating glue, 17 parts of toluene, 3.5 parts of matting powder, 0.4 parts of solvent-based dispersant and 0.9 part of crosslinking accelerator, and disperse with a disperser for 5 minutes at 1000 rpm, then add toluene to continue dispersing The viscosity to gained material is 8500CPS, obtains coating agent;
采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，155℃焙烘1.5min，干增重17g/m2，得到温敏防水透湿面料。Direct coating by dry method, coating the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, baking at 155°C for 1.5min, and dry weight gain of 17g/m 2 to obtain temperature-sensitive waterproof and moisture-permeable fabric.
实施例3Example 3
将70D×70D，260T，2/2斜纹尼龙布浸泡在0.6mol/L的盐酸中，进行水解处理20min，得到水解基布；Soak 70D×70D, 260T, 2/2 twill nylon fabric in 0.6mol/L hydrochloric acid, and perform hydrolysis treatment for 20 minutes to obtain hydrolyzed base fabric;
按质量份数计，将壳聚糖35份、N-异丙基丙烯酰胺60份、N、N-亚甲基双丙烯酰胺2份在室温下用醋酸6份溶解；然后加入质量百分含量为12％的N、N、N、N-四甲基乙二胺溶液1.5份和过硫酸铵2份，700r/min搅拌10min后装三口圆底烧瓶，在氮气保护下室温进行自由基聚合反应20h，得到温敏水凝胶；In terms of parts by mass, 35 parts of chitosan, 60 parts of N-isopropylacrylamide, and 2 parts of N, N-methylenebisacrylamide were dissolved with 6 parts of acetic acid at room temperature; 1.5 parts of 12% N, N, N, N-tetramethylethylenediamine solution and 2 parts of ammonium persulfate, stirred at 700r/min for 10min, then filled into a three-necked round bottom flask, and carried out free radical polymerization at room temperature under the protection of nitrogen 20h, obtain thermosensitive hydrogel;
将水解基布浸泡于质量百分含量为6％的戊二醛溶液中，进行预交联反应20min，然后将得到的预交联基布在温敏水凝胶中二浸二轧，其中轧制压力为3kgf/cm2，轧余率为80％，将得到的基布在70℃预烘干3min，在95℃二次烘干3min，得到交联基布；Soak the hydrolyzed base fabric in a glutaraldehyde solution with a mass percentage of 6%, perform a pre-crosslinking reaction for 20 minutes, and then dip the obtained pre-crosslinked base fabric in the temperature-sensitive hydrogel for two dips and two rolls, wherein the rolling pressure 3kgf/cm 2 , the excess reduction rate is 80%, pre-dry the obtained base fabric at 70°C for 3 minutes, and dry it again at 95°C for 3 minutes to obtain a cross-linked base fabric;
将防水透湿涂层胶90份、甲苯18份、消光粉4份、溶剂型分散剂0.5份和交联促进剂1份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为9000CPS，得到涂层剂；Mix 90 parts of waterproof and moisture-permeable coating glue, 18 parts of toluene, 4 parts of matting powder, 0.5 parts of solvent-based dispersant and 1 part of crosslinking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing The viscosity to gained material is 9000CPS, obtains coating agent;
采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，160℃焙烘2min，干增重18g/m2，得到温敏防水透湿面料。Direct coating by dry method, coating the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, baking at 160°C for 2 minutes, and dry weight gain of 18g/m 2 to obtain a temperature-sensitive waterproof and moisture-permeable fabric .
实施例4Example 4
将70D×70D，260T，2/2斜纹尼龙布浸泡在0.5mol/L的盐酸中，进行水解处理25min，得到水解基布；Soak 70D×70D, 260T, 2/2 twill nylon fabric in 0.5mol/L hydrochloric acid, and perform hydrolysis treatment for 25min to obtain hydrolyzed base fabric;
按质量份数计，将壳聚糖45份、N-异丙基丙烯酰胺80份、N、N-亚甲基双丙烯酰胺2.5份在室温下用醋酸8份溶解；然后加入质量百分含量为9％的N、N、N、N-四甲基乙二胺溶液2.5份和过硫酸铵2.5份，800r/min搅拌5min后装三口圆底烧瓶，在氮气保护下室温进行自由基聚合反应22h，得到温敏水凝胶；In terms of parts by mass, 45 parts of chitosan, 80 parts of N-isopropylacrylamide, and 2.5 parts of N, N-methylenebisacrylamide were dissolved with 8 parts of acetic acid at room temperature; It is 2.5 parts of 9% N, N, N, N-tetramethylethylenediamine solution and 2.5 parts of ammonium persulfate, stirred at 800r/min for 5min, then filled into a three-neck round bottom flask, and carried out free radical polymerization at room temperature under the protection of nitrogen 22h, obtain thermosensitive hydrogel;
将水解基布浸泡于质量百分含量为5％的戊二醛溶液中，进行预交联反应25min，然后将得到的预交联基布在温敏水凝胶中二浸二轧，其中轧制压力为2kgf/cm2，轧余率为85％，将得到的基布在65℃预烘干4.5min，在90℃二次烘干4.5min，得到交联基布；Soak the hydrolyzed base cloth in a glutaraldehyde solution with a mass percentage of 5%, perform a pre-crosslinking reaction for 25 minutes, and then dip the obtained pre-crosslinked base cloth in the temperature-sensitive hydrogel for two dips and two rolls, wherein the rolling pressure 2kgf/cm 2 , the scrap rate is 85%, the obtained base fabric is pre-dried at 65°C for 4.5 minutes, and then dried at 90°C for 4.5 minutes to obtain a cross-linked base fabric;
将防水透湿涂层胶95份、甲苯19份、消光粉4.5份、溶剂型分散剂0.6份和交联促进剂1.1份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为9500CPS，得到涂层剂；Mix 95 parts of waterproof and moisture-permeable coating glue, 19 parts of toluene, 4.5 parts of matting powder, 0.6 parts of solvent-based dispersant and 1.1 parts of cross-linking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing The viscosity to gained material is 9500CPS, obtains coating agent;
采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，165℃焙烘2.5min，干增重19g/m2，得到温敏防水透湿面料。Direct coating by dry method, coating the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, baking at 165°C for 2.5min, and dry weight gain of 19g/m 2 to obtain temperature-sensitive waterproof and moisture-permeable fabric.
实施例5Example 5
将70D×70D，260T，2/2斜纹尼龙布浸泡在0.5mol/L的盐酸中，进行水解处理35min，得到水解基布；Soak 70D×70D, 260T, 2/2 twill nylon fabric in 0.5mol/L hydrochloric acid, and perform hydrolysis treatment for 35min to obtain hydrolyzed base fabric;
按质量份数计，将壳聚糖55份、N-异丙基丙烯酰胺100份、N、N-亚甲基双丙烯酰胺3份在室温下用醋酸10份溶解；然后加入质量百分含量为11％的N、N、N、N-四甲基乙二胺溶液3份和过硫酸铵3份，800r/min搅拌5min后装三口圆底烧瓶，在氮气保护下室温进行自由基聚合反应26h，得到温敏水凝胶；In terms of parts by mass, 55 parts of chitosan, 100 parts of N-isopropylacrylamide, and 3 parts of N, N-methylenebisacrylamide were dissolved with 10 parts of acetic acid at room temperature; 3 parts of 11% N, N, N, N-tetramethylethylenediamine solution and 3 parts of ammonium persulfate, stirred at 800r/min for 5min, then filled into a three-necked round-bottomed flask, and carried out free radical polymerization at room temperature under the protection of nitrogen 26h, obtain thermosensitive hydrogel;
将水解基布浸泡于质量百分含量为5％的戊二醛溶液中，进行预交联反应35min，然后将得到的预交联基布在温敏水凝胶中二浸二轧，其中轧制压力为3kgf/cm2，轧余率为90％，将得到的基布在70℃预烘干3min，在95℃二次烘干3min，得到交联基布；Soak the hydrolyzed base cloth in a glutaraldehyde solution with a mass percentage of 5%, perform a pre-crosslinking reaction for 35 minutes, and then dip the obtained pre-crosslinked base cloth in the temperature-sensitive hydrogel for two dips and two rolls, wherein the rolling pressure 3kgf/cm 2 , the scrap rate is 90%, pre-dry the obtained base fabric at 70°C for 3 minutes, and dry it again at 95°C for 3 minutes to obtain a cross-linked base fabric;
将防水透湿涂层胶100份、甲苯20份、消光粉5份、溶剂型分散剂0.7份和交联促进剂1.2份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为10000CPS，得到涂层剂；Mix 100 parts of waterproof and moisture-permeable coating glue, 20 parts of toluene, 5 parts of matting powder, 0.7 parts of solvent-based dispersant and 1.2 parts of cross-linking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing Until the viscosity of the obtained material is 10000CPS, the coating agent is obtained;
采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，170℃焙烘3min，干增重20g/m2，得到温敏防水透湿面料。Direct coating by dry method, coating the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, baking at 170°C for 3 minutes, and dry weight gain of 20g/m 2 to obtain a temperature-sensitive waterproof and moisture-permeable fabric .
对比例1Comparative example 1
将防水透湿涂层胶80份、甲苯16份、消光粉3份、溶剂型分散剂0.3份和交联促进剂0.8份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为8000CPS，得到涂层剂；Mix 80 parts of waterproof and moisture-permeable coating glue, 16 parts of toluene, 3 parts of matting powder, 0.3 parts of solvent-based dispersant and 0.8 parts of crosslinking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing To the viscosity of gained material is 8000CPS, obtains coating agent;
以70D×70D，260T，2/2斜纹尼龙布为基布，采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，150℃焙烘1min，干增重16g/m2。Use 70D×70D, 260T, 2/2 twill nylon fabric as the base fabric, and use the dry method to directly coat the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, and bake at 150°C 1min, dry weight gain 16g/m 2 .
对比例2Comparative example 2
将防水透湿涂层胶85份、甲苯17份、消光粉3.5份、溶剂型分散剂0.4份和交联促进剂0.9份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为8500CPS，得到涂层剂；Mix 85 parts of waterproof and moisture-permeable coating glue, 17 parts of toluene, 3.5 parts of matting powder, 0.4 parts of solvent-based dispersant and 0.9 part of crosslinking accelerator, and disperse with a disperser for 5 minutes at 1000 rpm, then add toluene to continue dispersing The viscosity to gained material is 8500CPS, obtains coating agent;
以70D×70D，260T，2/2斜纹尼龙布为基布，采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，155℃焙烘1.5min，干增重17g/m2。Use 70D×70D, 260T, 2/2 twill nylon fabric as the base fabric, and use the dry method to directly coat the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, and bake at 155°C After 1.5 minutes, the dry weight gain was 17g/m 2 .
对比例3Comparative example 3
将防水透湿涂层胶90份、甲苯18份、消光粉4份、溶剂型分散剂0.5份和交联促进剂1份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为9000CPS，得到涂层剂；Mix 90 parts of waterproof and moisture-permeable coating glue, 18 parts of toluene, 4 parts of matting powder, 0.5 parts of solvent-based dispersant and 1 part of crosslinking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing The viscosity to gained material is 9000CPS, obtains coating agent;
以70D×70D，260T，2/2斜纹尼龙布为基布，采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，160℃焙烘2min，干增重18g/m2。Use 70D×70D, 260T, 2/2 twill nylon fabric as the base fabric, use dry method to directly coat, apply the obtained coating agent on the cross-linked base fabric with a floating knife coater, and bake at 160°C After 2 minutes, the dry weight gain was 18g/m 2 .
对比例4Comparative example 4
将防水透湿涂层胶95份、甲苯19份、消光粉4.5份、溶剂型分散剂0.6份和交联促进剂1.1份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为9500CPS，得到涂层剂；Mix 95 parts of waterproof and moisture-permeable coating glue, 19 parts of toluene, 4.5 parts of matting powder, 0.6 parts of solvent-based dispersant and 1.1 parts of cross-linking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing The viscosity to gained material is 9500CPS, obtains coating agent;
以70D×70D，260T，2/2斜纹尼龙布为基布，采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，165℃焙烘2.5min，干增重19g/m2。Use 70D×70D, 260T, 2/2 twill nylon fabric as the base fabric, use dry method to directly coat, use the floating knife coating machine to coat the obtained coating agent on the cross-linked base fabric, and bake at 165°C After 2.5 minutes, the dry weight gain was 19g/m 2 .
对比例5Comparative example 5
将防水透湿涂层胶100份、甲苯20份、消光粉5份、溶剂型分散剂0.7份和交联促进剂1.2份混合，在1000rpm条件下，用分散机分散5min，然后加入甲苯继续分散至所得物料的黏度为10000CPS，得到涂层剂；Mix 100 parts of waterproof and moisture-permeable coating glue, 20 parts of toluene, 5 parts of matting powder, 0.7 parts of solvent-based dispersant and 1.2 parts of cross-linking accelerator, disperse with a disperser for 5 minutes at 1000 rpm, and then add toluene to continue dispersing Until the viscosity of the obtained material is 10000CPS, the coating agent is obtained;
以70D×70D，260T，2/2斜纹尼龙布为基布，采用干法直接涂层，用浮刀式涂层机将得到的涂层剂涂覆在交联基布上，170℃焙烘3min，干增重20g/m2。Use 70D×70D, 260T, 2/2 twill nylon fabric as the base fabric, and use the dry method to directly coat the obtained coating agent on the cross-linked base fabric with a floating knife coating machine, and bake at 170°C 3min, dry weight gain 20g/m 2 .
对实施例4制备得到的交联基布进行温敏性能测试，具体是测试交联基布的接触角，得到所述接触角与温度变化图，如图1所示，随着温度升高，交联基布的水接触角逐渐增大，由亲水向疏水转变，这说明基布经温敏水凝胶浸轧处理后，具有较好的温敏性能。The cross-linked base cloth prepared in Example 4 was tested for temperature-sensitive properties, specifically the contact angle of the cross-linked base cloth was tested, and the contact angle and temperature change diagram were obtained. As shown in Figure 1, as the temperature increased, The water contact angle of the cross-linked base fabric increases gradually, and changes from hydrophilic to hydrophobic, which shows that the base fabric has better temperature-sensitive properties after being treated with temperature-sensitive hydrogel padding.
对实施例4制备得到的交联基布进行表征，并与未交联整理的尼龙面料进行对照，结果见图2和图3。由图2和图3可知，基布经经温敏水凝胶浸轧处理后，尼龙纤维由原来的光滑平整变的粗糙，并且水凝胶在基布表面分布均匀，这说明温敏水凝胶已经牢固附着在尼龙纤维表面。The cross-linked base fabric prepared in Example 4 was characterized, and compared with the non-cross-linked nylon fabric, the results are shown in Figures 2 and 3. It can be seen from Figure 2 and Figure 3 that after the base fabric is treated by thermosensitive hydrogel padding, the nylon fiber becomes rough from the original smoothness, and the hydrogel is evenly distributed on the surface of the base fabric, which shows that the thermosensitive hydrogel has been firmly attached on the surface of nylon fibers.
对实施例1～5和对比例1～5制备的面料进行性能测试，并设置纯尼龙面料作为对照，其中，按照GB/T4744-1997规定的方法检测面料的静水压，按照GB/T12704.1-2009规定的方法检测面料的透湿量，结果见表1和表2。The fabrics prepared in Examples 1 to 5 and Comparative Examples 1 to 5 were tested for performance, and pure nylon fabric was set as a contrast, wherein the hydrostatic pressure of the fabric was detected according to the method specified in GB/T4744-1997, and the fabric was tested according to GB/T12704. 1-2009 to test the moisture permeability of fabrics, the results are shown in Table 1 and Table 2.
表1实施例1～5制备的温敏防水透湿尼龙面料与纯尼龙面料的性能检测结果Table 1 Performance testing results of temperature-sensitive waterproof and moisture-permeable nylon fabrics prepared in Examples 1-5 and pure nylon fabrics
表2对比例1～5制备的防水透湿尼龙面料与纯尼龙面料的性能检测结果Table 2 Performance testing results of waterproof and moisture-permeable nylon fabrics prepared in comparative examples 1 to 5 and pure nylon fabrics
由表1和表2可以看出，本发明实施例1～5制备的温敏防水透湿尼龙面料具有较好的防水透湿综合性能，与对比例1～5中未经温敏水凝胶浸轧处理得到的尼龙面料相比，静水压几乎没有变化，防水性能相当；但是渗透量显著增加，说明本发明实施例1～5制备的温敏防水透湿尼龙面料经温敏水凝胶浸轧处理后，具有优异的透湿性能。It can be seen from Table 1 and Table 2 that the temperature-sensitive waterproof and moisture-permeable nylon fabrics prepared in Examples 1-5 of the present invention have better waterproof and moisture-permeable comprehensive properties, compared with those in Comparative Examples 1-5 without padding with temperature-sensitive hydrogel Compared with the nylon fabrics obtained by treatment, the hydrostatic pressure hardly changes, and the waterproof performance is equivalent; but the penetration rate increases significantly, indicating that the temperature-sensitive waterproof and moisture-permeable nylon fabrics prepared in Examples 1 to 5 of the present invention are treated by temperature-sensitive hydrogel padding. , has excellent moisture permeability.
对本发明实施例1～5和对比例1～5制备的面料的耐洗性进行测试，其中，按照GB/T 8629-2001规定的方法对面料进行洗涤，结果见表3。The washing durability of the fabrics prepared in Examples 1-5 and Comparative Examples 1-5 of the present invention were tested, wherein the fabrics were washed according to the method specified in GB/T 8629-2001, and the results are shown in Table 3.
表3实施例1～5和对比例1～5制备的面料洗涤后的质量损失率The mass loss rate of the fabrics prepared in Table 3 Examples 1 to 5 and Comparative Examples 1 to 5 after washing
由表3可以看出，本发明实施例1～5制备得到的温敏防水透湿尼龙面料比对比例1～5制备的面料的质量损失率低，并且随着洗涤次数的增加，质量损失率依然保持在5％以下，说明本发明制备得到的温敏防水透湿尼龙面料耐洗性优异，同时也说明本发明制备得到的温敏防水透湿尼龙面料中温敏水凝胶与尼龙面料结合性能好、牢度强。It can be seen from Table 3 that the mass loss rate of the temperature-sensitive waterproof and moisture-permeable nylon fabrics prepared in Examples 1 to 5 of the present invention is lower than that of the fabrics prepared in Comparative Examples 1 to 5, and the mass loss rate decreases as the number of washings increases. It is still kept below 5%, indicating that the temperature-sensitive waterproof and moisture-permeable nylon fabric prepared by the present invention has excellent washability, and it also shows that the temperature-sensitive waterproof and moisture-permeable nylon fabric prepared by the present invention has the bonding performance between the temperature-sensitive hydrogel and the nylon fabric Good, strong fastness.
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, and it should be pointed out that for those of ordinary skill in the art, some improvements and modifications can be made without departing from the principle of the present invention. It should be regarded as the protection scope of the present invention.
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