CN113276533B - 一种低湿阻防水复合面料的制备方法 - Google Patents

一种低湿阻防水复合面料的制备方法 Download PDF

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CN113276533B
CN113276533B CN202011497194.2A CN202011497194A CN113276533B CN 113276533 B CN113276533 B CN 113276533B CN 202011497194 A CN202011497194 A CN 202011497194A CN 113276533 B CN113276533 B CN 113276533B
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陈明贤
孙立新
董洪波
谢国炎
金世豪
葛烨楠
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Zhejiang Dongjin New Material Co ltd
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Abstract

本发明公开了一种低湿阻防水复合面料的制备方法，包括如下步骤：步骤1按工艺处方由防水剂与水配置成防水整理液；步骤2将外层面料浸渍于防水整理液中，轧液；步骤3预烘、焙烘；步骤4将外层面料、薄膜涂覆胶点，平整地叠加在一起，再移至压烫机中，然后进行压烫，完成热压复膜，制成低湿阻防水复合面料。面料浸轧防水整理液后，面料的表面形成一层膜，有效提高面料的防泼水性能。氨基聚硅氧烷的引入则能改善面料手感，氨基与乳液中环氧基团在高温时交联反应，提高防水剂在面料表面附着的耐久性。面料、薄膜复合时，胶在面料表面的涂覆面积为40％，降低了水汽透过复合面料的阻力，同时还保证了复合面料具有良好的耐静水压、剥离强力。

Description

一种低湿阻防水复合面料的制备方法
技术领域
本发明属于功能纺织品面料领域，具体涉及一种低湿阻防水复合面料的制备方法。
背景技术
防水透湿纺织品作为一种集防水、防风、透气、透湿于一体的功能型织物，它很好地解决了防水和透湿的矛盾，使人体微气候和外界能够保持良好的热湿传递性能。
防水透湿织物的优势主要体现在其防水及透湿性能达到了和谐的统一，即防水透湿织物优异的防水性使织物外侧的水不能穿透织物浸到内侧，其优异的透湿性又能把人体本身散发的汗液蒸汽通过织物扩散或传导到外界。
通常把织物对水蒸气的透过有一定的阻力称作，湿阻。湿阻越大，则对水蒸气透过织物的阻力越大；反之，湿阻越小。湿阻大，水蒸气难以透过织物，也即汗液难以由织物里侧扩散至外侧，不利于排出汗液；若湿阻小，则汗液易于排出。
常规的防水透湿服装，主要强调其表面的不沾水性以及水滴的易滚动性，但激烈运动时，穿着的服装必须具备防水及优异的透湿功能，即一方面要防止水的渗透，另一方面又要让人体散发的大量汗液以蒸汽的形式通过面料排出以使人感到舒适。因为大量汗液若无法以蒸汽的形式排出，在衣服内部形成冷凝水，使人感觉粘湿而不舒适，遇到天气寒冷时非常容易造成冻伤。仅仅透湿，或仅仅防水，难以达到服用需求，只有防水、透湿协调，才能实现织物防护性能与舒适性的统一。
发明内容
本发明目的是提供一种低湿阻防水复合面料的制备方法，通过对外层面料浸轧防水剂、复膜的方法实现。
一种低湿阻防水复合面料的制备方法，包括如下步骤：
步骤1按工艺处方由防水剂与水配置成防水整理液；
步骤2将外层面料浸渍于防水整理液中，轧液；
步骤3预烘、焙烘；
步骤4将外层面料、薄膜涂覆胶点，平整地叠加在一起，再移至压烫机中，然后设定热压时间和热压温度，待温度达到后，进行压烫，完成热压复膜，制成低湿阻防水复合面料。
所述的防水剂，制备方法为：
1)乳化剂十二烷基硫酸钠、OS-15、TX-30以及去离子水于乳化釜中，搅拌、溶解，形成乳化剂溶液；另取BA、MMA、St及正十六烷搅拌混匀成混合单体；将混合单体加入乳化剂溶液中，搅拌乳化30min，超声处理15min，得乳化液；
2)在装有电动搅拌器、恒压滴液漏斗、回流冷凝管的反应器中加入十二烷基硫酸钠、乳化剂OS-15、去离子水，搅拌溶解，加入经表面改性的纳米SiO2，分散均匀，升温加热至78℃时，加入1/2体积乳化液及1/3体积引发剂水溶液，待反应温度稳定，乳液呈明显蓝光后，保温反应30min，然后升温至82℃，滴加剩余乳化液和1/3体积引发剂水溶液，2h内滴完；
3)滴加正十六烷和MMA、BA、GMA(甲基丙烯酸缩水甘油醚)及如式1所示的有机硅单体混合液，滴加时间为1h左右，补加1/3体积引发剂水溶液，加料完毕后，升温到86℃，保温45min，停止加热，得纳米改性丙烯酸酯乳液，当反应体系温度降为40℃以下，加入适量氨基聚硅氧烷乳液，再搅拌30min，得防水剂乳液。
Figure BDA0002842529750000031
所述的面料为100D平纹四面弹，94％涤纶/6％氨纶。
所述的薄膜为TPE膜。
本发明有益效果：
防水透湿复合面料通常由面层面料及薄膜、或者由面层面料、里层面料及薄膜组成，复合面料表面的防泼水性能与施加在面层面料的防水整理剂有关，复合面料的透湿性能则与用于贴合薄膜与面料的热熔胶涂覆面积、薄膜的透湿量有关。热熔胶涂覆面积越大，水汽的透湿量越小、耐静水压性能越好、复合面料的剥离强度越大。
面料与薄膜复合时，热熔胶在熔融状态下，以圆形、方形或其他形状的胶点散布式地施加在面料表面，高温、压力条件下使面料与薄膜贴合。热熔胶涂覆面积、薄膜直接与复合面料的耐静水压性能相关。
在选定薄膜的情况下，降低热熔胶的涂覆面积，可直接降低复合面料的湿阻，提高复合面料的透湿性能。但另一方面，若热熔胶的涂覆面积过小，会降低复合面料的剥离强度，影响后期面料的服用。
显然，低湿阻防水复合面料的性能与防水整理、面料与薄膜的复合相关。
本发明的防水整理采用了有机硅、纳米材料复合聚丙烯酸酯乳液，面料浸轧防水整理液后，面料的表面形成一层膜，有机硅、纳米材料可有效提高面料的防泼水性能。面料经常规的丙烯酸酯乳液浸轧、焙烘成膜后，手感略微变硬；氨基聚硅氧烷的引入则能改善面料手感，并且氨基与乳液中环氧基团在高温时交联反应，提高防水剂在面料表面附着的耐久性。
面料、薄膜复合时，胶在面料表面的涂覆面积为40％，降低了水汽透过复合面料的阻力，同时还保证了复合面料具有良好的耐静水压、剥离强力。
具体实施方式
以下通过具体实施方式对本发明作进一步说明。如无特殊说明，本发明涉及的原料质量单位“份”为质量份。
本发明公开了一种低湿阻防水复合面料的制备方法，包括如下步骤：
步骤1按工艺处方由防水剂乳液与水配置成防水整理液；
工艺处方：
防水整理液 240g/L
浴比 1:20
步骤2将外层面料浸渍于防水整理液中，轧液；
步骤3预烘、焙烘；
步骤4将外层面料、薄膜涂覆胶点，平整地叠加在一起，再移至压烫机中，然后设定热压时间和热压温度，待温度达到后，进行压烫，完成热压复膜，制成低湿阻防水复合面料。
所述的外层面料为100D平纹四面弹，94％涤纶/6％氨纶。
所述的薄膜为TPE膜。
所述的防水剂，制备方法为：
1)乳化剂十二烷基硫酸钠、OS-15、TX-30以及去离子水于乳化釜中，搅拌、溶解，形成乳化剂溶液；另取BA、MMA、St及正十六烷搅拌混匀成混合单体；将混合单体加入乳化剂溶液中，搅拌乳化30min，超声处理15min，得乳化液；
2)在装有电动搅拌器、恒压滴液漏斗、回流冷凝管的反应器中加入十二烷基硫酸钠、乳化剂OS-15、去离子水，搅拌溶解，加入经表面改性的纳米SiO2，分散均匀，升温加热至78℃时，加入1/2体积乳化液及1/3体积引发剂水溶液，待反应温度稳定，乳液呈明显蓝光后，保温反应30min，然后升温至82℃，滴加剩余乳化液和1/3体积引发剂水溶液，2h内滴完；
3)滴加正十六烷和MMA、BA、GMA(甲基丙烯酸缩水甘油醚)及如式1所示的有机硅单体混合液，滴加时间为1h左右，补加1/3体积引发剂水溶液，加料完毕后，升温到86℃，保温45min，停止加热，得纳米改性丙烯酸酯乳液，当反应体系温度降为40℃以下，加入适量氨基聚硅氧烷乳液，再搅拌30min，得防水剂乳液。
Figure BDA0002842529750000051
防水剂制备方法中，所述的表面改性的纳米SiO2，制备方法为：
取20份硅烷偶联剂乙烯基三乙氧基硅烷于烧杯中并加20份水于烧杯中，用0.1mol/L的盐酸调pH值到3-4，磁力搅拌水解1h，形成偶联剂水解溶液；往接有冷凝管的反应器中，加入10份干燥后的纳米SiO2，50份无水乙醇溶剂，设置反应温度为70℃，在反应釜中磁力搅拌30分钟，再滴入20份的水解后的偶联剂溶液反应3h，制得表面改性纳米SiO2。
防水剂制备方法中，所述的氨基聚硅氧烷乳液，制备方法为：
在装有温度计、搅拌器的干燥四口烧瓶中，加入摩尔比为1:20的1,3-双(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷、八甲基环四硅氧烷，边搅拌边升温至反应温度，并加入一定量的三氟甲基磺酸，保温反应一定时间；反应结束后加入无水Na2CO3搅拌中和至pH为6-7，过滤并将产物进行减压蒸馏(90℃，真空度-0.1Mpa以下)，脱除未反应单体，得无色透明的液体产物，为端氨基聚硅氧烷。反应过程如反应式1所示。
称取端氨基聚硅氧烷、乳化剂于乳化器中，再取适量去离子水，边搅拌边将去离子水慢慢加入乳化器中，制得氨基聚硅氧烷乳液。端氨基聚硅氧烷、乳化剂、去离子水的质量比为5:1:20。乳化剂由XP-70、AEO-9组成。
Figure BDA0002842529750000061
实施例1：
一种防水剂，制备方法为：
(1)纳米SiO2表面改性
取20份硅烷偶联剂乙烯基三乙氧基硅烷于烧杯中并加20份水于烧杯中，用0.1mol/L的盐酸调pH值到3-4，磁力搅拌水解1h，形成偶联剂水解溶液；往接有冷凝管的反应器中，加入10份干燥后的纳米SiO2，50份无水乙醇溶剂，设置反应温度为70℃，在反应釜中磁力搅拌30分钟，再滴入20份水解后的偶联剂溶液，反应3h，制得表面改性纳米SiO2；
(2)乳液的合成
1)乳化剂十二烷基硫酸钠2.5份、OS-15 2份、TX-30 4份以及去离子水100份置于乳化釜中，搅拌、溶解，形成乳化剂溶液；另取丙烯酸丁酯(BA)42份、甲基丙烯酸甲酯(MMA)9份、苯乙烯(St)6份及正十六烷2份搅拌混匀成混合单体；将混合单体加入乳化剂溶液中，搅拌乳化30min，超声处理15min，得乳化液；
2)在装有电动搅拌器、恒压滴液漏斗、回流冷凝管的反应器中加入2份十二烷基硫酸钠、1.6份OS-15、3.2份TX-30、80份去离子水，搅拌溶解；加入16份经表面改性的纳米SiO2，分散均匀，升温加热至78℃时，加入1/2体积的乳化液及1/3体积的引发剂水溶液，待反应温度稳定，乳液呈明显蓝光后，保温反应30min，然后升温至82℃，滴加剩余乳化液和1/3体积的引发剂水溶液，2h内滴完；
3)滴加3份正十六烷和6份甲基丙烯酸甲酯(MMA)、14份丙烯酸丁酯(BA)、4份甲基丙烯酸缩水甘油醚(GMA)及9份如式1所示有机硅单体的混合液，滴加时间为1h左右，补加剩余1/3体积的引发剂水溶液，加料完毕后，升温到86℃，保温45min，停止加热，得纳米改性丙烯酸酯乳液，当反应体系温度降为40℃以下，加入适量氨基聚硅氧烷乳液，再搅拌30min，得防水剂乳液。所述的引发剂水溶液由0.24份过硫酸钠溶于30份水中形成。纳米改性丙烯酸酯乳液与氨基聚硅氧烷乳液的质量比为5:1。
Figure BDA0002842529750000071
其中，氨基聚硅氧烷乳液由下述方法制成：
在装有温度计、搅拌器的干燥四口烧瓶中，加入摩尔比为1:20的1,3-双(3-氨基丙基)-1,1,3,3-四甲基二硅氧烷、八甲基环四硅氧烷，边搅拌边升温至反应温度，并加入一定量的三氟甲基磺酸，保温反应一定时间；反应结束后加入无水Na2CO3搅拌中和至pH为6-7，过滤并将产物进行减压蒸馏(90℃，真空度-0.1Mpa以下)，脱除未反应单体，得无色透明的液体产物，为端氨基聚硅氧烷。
称取端氨基聚硅氧烷、乳化剂于乳化器中，再取适量去离子水，边搅拌边将去离子水慢慢加入乳化器中，制得氨基聚硅氧烷乳液。端氨基聚硅氧烷、乳化剂、去离子水的质量比为5:1:20，乳化剂由XP-70、AEO-9组成。
所述的有机硅单体，由2-(三甲基硅氧基)乙醇胺与甲基丙烯酸异氰酸酯乙酯反应制成，其方法如下：
在装有搅拌器、温度计、冷凝管的反应器中，加入经脱水处理的2-(三甲基硅氧基)乙醇胺、甲基丙烯酸异氰酸酯乙酯、二月桂酸二丁基锡，100℃搅拌反应5h，得到含C＝C键的功能性有机硅单体；2-(三甲基硅氧基)乙醇胺、甲基丙烯酸异氰酸酯乙酯的摩尔比1:1，二月桂酸二丁基锡的质量占反应单体总质量的0.4％。
应用例1：
取实施例1制得的防水剂240g，与水配成1L溶液，为防水整理液；按浴比1:20，将面料浸渍于防水整理液中，二浸二轧，轧余率80％；经100℃、预烘3min，180℃、焙烘90s，面料完成防水整理。
面料为100D平纹四面弹，94％涤纶/6％氨纶。
经防水整理后，面料的防泼水评分(洗前)100分。
实施例2：
一种低湿阻防水复合面料的制备方法，包括如下步骤：
步骤1按工艺处方由防水剂与水配置成防水整理液；
工艺处方：
防水整理液 240g/L
浴比 1:20
步骤2将外层面料浸渍于防水整理液中，二浸二轧，轧余率80％；
步骤3 100℃、预烘3min，180℃、焙烘90s；
步骤4复膜：先将外层面料、薄膜涂覆胶点，胶在面料表面的涂覆面积为40％，平整地叠加在一起，再移至压烫机中，然后设定热压温度105℃和热压时间30s，待温度达到后，进行压烫，收卷压力8kg、贴合速度12m/min，完成热压复膜，制成低湿阻防水复合面料。胶为聚氨酯热熔胶。防水剂按实施例1方法制备。
外层面料为100D平纹四面弹，94％涤纶/6％氨纶。
薄膜为TPE膜，膜的厚度为0.02mm。
低湿阻防水复合面料的性能：防泼水(洗前)100分、5次洗后80分；耐静水压13275mmH2O；湿阻RET值9；剥离强度：经向6.18N/cm，纬向4.37N/cm。
防泼水性能测试方法参照AATCC 22。
耐静水压参照JIS L 1092-1998测试。
湿阻参照ISO 11092-2014方法测试。
剥离强度参照ISO 2411-2017方法测试。

Claims (5)

1.一种低湿阻防水复合面料的制备方法，包括如下步骤：
步骤1按工艺处方由防水剂与水配置成防水整理液；
步骤2将外层面料浸渍于防水整理液中，轧液；
步骤3预烘、焙烘；
步骤4将外层面料、薄膜涂覆胶点，平整地叠加在一起，再移至压烫机中，然后设定热压时间和热压温度，待温度达到后，进行压烫，完成热压复膜，制成低湿阻防水复合面料；
所述的防水剂，制备方法为：
1)乳化剂十二烷基硫酸钠、OS-15、TX-30以及去离子水于乳化釜中，搅拌、溶解，形成乳化剂溶液；另取BA、MMA、St及正十六烷搅拌混匀成混合单体；将混合单体加入乳化剂溶液中，搅拌乳化30min，超声处理15min，得乳化液；
2)在装有电动搅拌器、恒压滴液漏斗、回流冷凝管的反应器中加入十二烷基硫酸钠、乳化剂OS-15、去离子水，搅拌溶解，加入经表面改性的纳米SiO2，分散均匀，升温加热至78℃时，加入1/2体积乳化液及1/3体积引发剂水溶液，待反应温度稳定，乳液呈明显蓝光后，保温反应30min，然后升温至82℃，滴加剩余乳化液和1/3体积引发剂水溶液，2h内滴完；
3)滴加正十六烷和MMA、BA、GMA及如式1所示的有机硅单体混合液，滴加时间为1h左右，补加1/3体积引发剂水溶液，加料完毕后，升温到86℃，保温45min，停止加热，得纳米改性丙烯酸酯乳液，当反应体系温度降为40℃以下，加入适量氨基聚硅氧烷乳液，再搅拌30min，得防水剂乳液。
Figure FDA0002842529740000011
2.根据权利要求1所述的一种低湿阻防水复合面料的制备方法，其特征在于：所述的面料为100D平纹四面弹，94％涤纶/6％氨纶。
3.根据权利要求1所述的一种低湿阻防水复合面料的制备方法，其特征在于：所述的薄膜为TPE膜。
4.根据权利要求1所述的一种低湿阻防水复合面料的制备方法，其特征在于：步骤1中工艺处方为防水整理液240g/L、浴比1:20。
5.根据权利要求1所述的一种低湿阻防水复合面料的制备方法，其特征在于：步骤3中预烘温度100℃、时间3min，焙烘温度180℃、时间90s。
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