CN107237139A - 一种高耐久性防静电液及其加工工艺 - Google Patents

一种高耐久性防静电液及其加工工艺 Download PDF

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CN107237139A
CN107237139A CN201710594727.0A CN201710594727A CN107237139A CN 107237139 A CN107237139 A CN 107237139A CN 201710594727 A CN201710594727 A CN 201710594727A CN 107237139 A CN107237139 A CN 107237139A
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宗在建
宗小明
赵余仁
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Abstract

本发明属于织物后整理领域，公开了一种高耐久防静电液的加工工艺，其特征在于，该防静电液为改性石墨烯化学接枝改性水性聚氨酯，其中石墨烯：0.5%~5%，水性聚氨酯：95%~99.5%。本发明产品具有优异的抗静电性能，优异的耐水洗性和抗磨性，且安全无毒，丰富了防静电液的品种，拓宽了石墨烯的应用领域。

Description

一种高耐久性防静电液及其加工工艺
技术领域
本发明涉及织物后整理领域，具体涉及一种高耐久性静电剂的加工工艺。
背景技术
大多数化纤织物摩擦后会产生负电荷，因而需采用防静电液进行整理，为确保穿着的舒适性和安全性，对织物进行抗静电整理是极有必要的，防静电液是一类重要的织物后整理助剂。阳离子型表面活性剂具有优异的抗静电效果，其中以季铵盐型为主，广泛用于合成纤维，但这类防静电液的相对分子质量较低，且纤维表面反应基团较少，防静电液难以在纤维表面附着，则使得实际应用中这类防静电液具有耐洗牢度差、耐摩擦牢度较低，且对已染色织物易造成变色等缺点。目前的高分子型抗静电整理剂绝大部分为溶剂型整理剂，具有整理加工成本高、易造成环境污染的缺点。总之目前高性能新品种防静电液生产能力弱，品种较少，尚不能完全满足目前需求。
水性聚氨酯具有环保、无醛、高性能的优点，结构可调节设计，综合性能优异，水性聚氨酯作为织物整理剂，可赋予织物良好的弹性，柔软和爽滑的手感，目前水性聚氨酯在纺织印染助剂领域已有较多的应用，其中可用作防静电液。
石墨烯是 Novoselov 和 Andre Geim 发现的新型碳材料，具有优异的物理化学性能，比如具有极强的导电性能、超高的比表面积等，目前关于石墨烯已进行了较广泛的研究，而且在一些领域已实现应用，但石墨烯在纺织印染助剂方面的研究和应用仍然较少。
中国专利CN103469555A公开了一种防紫外线抗静电石墨烯涂层纺织面料的加工工艺，该方法将石墨烯溶液震荡分散后加入到水溶性聚氨酯溶液中，由于石墨烯的水溶性较差，强力震荡分散后，容易产生沉淀分层，而且石墨烯与水溶性聚氨酯仅是物理共混，耐水洗及耐久性较差。
发明内容
本发明的目的在于提供了一种新型高耐久防静电液的加工工艺，解决现有技术中防静电液品种较少，抗静电原理单一，抗静电效率较低，耐水洗、耐久性差的问题。
为实现上述目的，本发明采用如下技术方案：
一种高耐久防静电液，该防静电液为改性石墨烯化学接枝改性水性聚氨酯，其中石墨烯占0.5%~5%，水性聚氨酯占95%~99.5%。
所述高耐久防静电液，改性石墨烯为氧化石墨烯还原改性制得。
所述高耐久防静电液，水性聚氨酯为阴非离子型水性聚氨酯。
所述高耐久防静电液，水性聚氨酯为封闭型水性聚氨酯。
所述高耐久防静电液，水性聚氨酯的分子量为2万~6万。
所述的改性石墨烯化学接枝改性水性聚氨酯，其特征在于利用氧化石墨烯表面羟基与聚氨酯中异氰酸酯基反应，具体包括如下步骤：
（1）羟基多元醇脱水处理，在惰性气氛下，将二异氰酸酯和羟基多元醇反应1～4小时，然后加入亲水扩链剂反应 0.5-2小时，添加适量丙酮调节粘度，得到聚氨酯预聚体；
（2）加入氧化石墨烯，在催化剂作用下反应1～2小时，加入封闭剂，反应至无NCO后，加入一定量还原剂，反应2～6小时，加入中和剂中和 10～30min，高速搅拌下加入去离子水，减压蒸馏脱除丙酮，制得石墨烯化学改性水性聚氨酯。
步骤（1）所述的二异氰酸酯选自异佛尔酮二异氰酸酯(IPDI)、甲苯二异氰酸酯(TDI)、二苯甲烷二异氰酸酯(MDI)、六亚甲基二异氰酸酯(HDI)、二环己基甲烷二异氰酸酯(HMDI) 中的一种或多种。
步骤（1）所述的羟基多元醇为聚乙二醇400、聚乙二醇600、聚乙二醇800、聚乙二醇1000、聚乙二醇1500、聚乙二醇2000、聚乙二醇3000、聚乙二醇4000中的一种或多种。
步骤（1）所述的亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸中的一种。
步骤（1）所述的羟基多元醇、二异氰酸酯、扩链剂的摩尔比为1:2～4:0.5～1。
步骤（2）所述的氧化石墨烯的细度为0.5~5um，纯度＞96%。
步骤（2）所述的催化剂为环保型有机铋催化剂。
步骤（2）所述的封闭剂为亚硫酸氢钠、丁酮肟、苯酚中的一种。
步骤（2）所述的还原剂为水合肼、硼氢化钠、乙二胺中的一种。
步骤（2）所述的还原剂与氧化石墨烯的质量比为1~3:1。
步骤（2）所述的所述的中和剂为三乙胺、氨水、氢氧化钠中的一种。
本发明的优点和有益效果在于：
1、同时利用石墨烯的优异导电性和水性聚氨酯的吸湿性导电两个抗静电原理，更易提高抗静电效率。
2、石墨烯与水性聚氨酯化学键连接，结合更牢，不易产生分层沉淀现象。
3、采用封闭型聚氨酯，提高与纤维的结合力，提高耐水洗，耐久的抗静电性能。
具体实施方式
下面结合具体实施例，对本发明作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
实施例1
将100g聚乙二醇1000脱水处理，在惰性气氛下，将34.8g甲苯二异氰酸酯和聚乙二醇1000在60℃反应4小时，然后加入6.7g亲水扩链剂二羟甲基丙酸在 60℃反应 2小时，添加适量丙酮调节粘度，得到聚氨酯预聚体，加入0.7g氧化石墨烯，加入有机铋催化剂，60℃反应1小时，加入1.4g亚硫酸氢钠，反应至无NCO后，加入2.1g还原剂水合肼，继续反应2小时，加入中和剂三乙胺中和 10min，高速搅拌下加入去离子水，减压蒸馏脱除丙酮，制得改性石墨烯化学接枝改性水性聚氨酯防静电液。
实施例2
将100g聚乙二醇1000脱水处理，在惰性气氛下，将42g六亚甲基二异氰酸酯和聚乙二醇1000在60℃反应4小时，然后加入8g亲水扩链剂二羟甲基丙酸在 40℃反应 2小时，添加适量丙酮调节粘度，得到聚氨酯预聚体，加入1.5g氧化石墨烯，加入有机铋催化剂，60℃反应1小时，加入1.5g丁酮肟反应至无NCO后，加入3g乙二胺还原剂，继续反应2小时，加入中和剂氢氧化钠中和 20min，高速搅拌下加入去离子水，减压蒸馏脱除丙酮，制得改性石墨烯化学接枝改性水性聚氨酯防静电液。
实施例3
将50g聚乙二醇2000脱水处理，在惰性气氛下，将22.3g异佛尔酮二异氰酸酯和聚乙二醇2000在90℃反应1小时，然后加入3.7g亲水扩链剂二羟甲基丁酸在 50℃反应 4小时，添加适量丙酮调节粘度，得到聚氨酯预聚体，加入3.8g氧化石墨烯，加入有机铋催化剂，50℃反应2小时，加入0.76g苯酚反应至无NCO后，加入1.52g还原剂，继续反应6小时，加入中和剂氨水中和 30min，高速搅拌下加入去离子水，减压蒸馏脱除丙酮，制得改性石墨烯化学接枝改性水性聚氨酯防静电液。
为了更好的了解抗静电效果，按GB/T12703.1检测，织物为涤纶针织布，结果见表1。
整理工艺：浸轧→烘干（100℃）→焙烘（160℃，1min）→回潮→测试→洗涤→烘干→回潮→测试。
表1 各实施例抗静电效果对比
。
从表1数据看出，实施例所得防静电液均具有优异的抗静电性能，而且洗10次之后仍然有较好的抗静电性能。

Claims (9)

1.一种高耐久防静电液，其特征在于，防静电液为改性石墨烯化学接枝改性水性聚氨酯，其中改性石墨烯所占的质量百分比是：0.5%~5%；改性石墨烯为氧化石墨烯还原改性制得；水性聚氨酯为阴非离子型水性聚氨酯。
2.根据权利要求1所述高耐久防静电液，其特征在于，水性聚氨酯为封闭型水性聚氨酯，水性聚氨酯的分子量为2万~6万。
3.根据权利要求1所述高耐久防静电液的加工工艺，利用氧化石墨烯表面羟基与聚氨酯中异氰酸酯基反应，其特征在于包括如下步骤：
（1）羟基多元醇脱水处理，在惰性气氛下，将二异氰酸酯和羟基多元醇反应1～4小时，然后加入亲水扩链剂反应 0.5-2小时，添加适量丙酮调节粘度，得到聚氨酯预聚体；
（2）加入氧化石墨烯，在催化剂作用下反应1～2小时，加入封闭剂，反应至无NCO后，加入一定量还原剂，反应2～6小时，加入中和剂中和 10～30min，高速搅拌下加入去离子水，减压蒸馏脱除丙酮，制得石墨烯化学改性水性聚氨酯。
4.根据权利要求3所述加工工艺，其特征在于，步骤（1）所述的二异氰酸酯选自异佛尔酮二异氰酸酯(IPDI)、甲苯二异氰酸酯(TDI)、二苯甲烷二异氰酸酯(MDI)、六亚甲基二异氰酸酯(HDI)、二环己基甲烷二异氰酸酯(HMDI) 中的一种或多种。
5.根据权利要求4所述的改性石墨烯化学接枝改性水性聚氨酯，其特征在于：步骤（1）所述的羟基多元醇为聚乙二醇400、聚乙二醇600、聚乙二醇800、聚乙二醇1000、聚乙二醇1500、聚乙二醇2000、聚乙二醇3000、聚乙二醇4000中的一种或多种；步骤（1）所述的亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸中的一种。
6.根据权利要求3所述的改性石墨烯化学接枝改性水性聚氨酯，其特征在于：羟基多元醇、二异氰酸酯、扩链剂的摩尔比为 1:2～4:0.5～1；氧化石墨烯的细度为0.5~5um，纯度＞96%。
7.根据权利要求3所述的改性石墨烯化学接枝改性水性聚氨酯，其特征在于：催化剂为环保型有机铋催化剂，封闭剂为亚硫酸氢钠、丁酮肟、苯酚中的一种，还原剂为水合肼、硼氢化钠、乙二胺中的一种。
8.根据权利要求6所述的改性石墨烯化学接枝改性水性聚氨酯，其特征在于：还原剂与氧化石墨烯的质量比为1~3:1。
9.根据权利要求6所述的改性石墨烯化学接枝改性水性聚氨酯，其特征在于：所述的中和剂为三乙胺、氨水、氢氧化钠中的一种。
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CN108642691A (zh) * 2018-07-05 2018-10-12 刘群英 抗静电面料及其制备方法
CN108659199A (zh) * 2018-04-13 2018-10-16 中国皮革和制鞋工业研究院（晋江）有限公司 改性水性聚氨酯分散体及其制备方法和鞋面整理剂
CN109944066A (zh) * 2019-04-08 2019-06-28 福建华彩新材料有限公司 一种石墨烯抗静电织物及其制备方法
CN110643274A (zh) * 2019-08-28 2020-01-03 武汉纺织大学 无机-聚合物复合导电水性聚氨酯乳液涂层剂及其制备方法与应用

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CN108659199A (zh) * 2018-04-13 2018-10-16 中国皮革和制鞋工业研究院（晋江）有限公司 改性水性聚氨酯分散体及其制备方法和鞋面整理剂
CN108642691A (zh) * 2018-07-05 2018-10-12 刘群英 抗静电面料及其制备方法
CN108642691B (zh) * 2018-07-05 2020-04-24 珠海鑫康源新材料科技有限公司 抗静电面料及其制备方法
CN109944066A (zh) * 2019-04-08 2019-06-28 福建华彩新材料有限公司 一种石墨烯抗静电织物及其制备方法
CN109944066B (zh) * 2019-04-08 2021-06-18 福建华彩新材料有限公司 一种石墨烯抗静电织物及其制备方法
CN110643274A (zh) * 2019-08-28 2020-01-03 武汉纺织大学 无机-聚合物复合导电水性聚氨酯乳液涂层剂及其制备方法与应用

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