CN107189035B - 一种无溶剂超支化有机硅柔软剂的制备方法 - Google Patents

一种无溶剂超支化有机硅柔软剂的制备方法 Download PDF

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CN107189035B
CN107189035B CN201710528859.3A CN201710528859A CN107189035B CN 107189035 B CN107189035 B CN 107189035B CN 201710528859 A CN201710528859 A CN 201710528859A CN 107189035 B CN107189035 B CN 107189035B
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高雏燕
陈焜
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Hangzhou Meigao Huayi Chemical Co Ltd
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Abstract

本发明涉及一种有机硅柔软剂，尤其是涉及一种无溶剂超支化有机硅柔软剂的制备方法。按以下步骤进行：端羟基聚二甲基硅氧烷的制备→超支化有机硅柔软剂的制备。解决了传统嵌段硅油合成过程中溶剂使用较多的问题；合成工艺简单易操作，安全环保。

Description

一种无溶剂超支化有机硅柔软剂的制备方法
技术领域
本发明涉及一种有机硅柔软剂，尤其是涉及一种无溶剂超支化有机硅柔软剂的制备方法。
背景技术
近年来，嵌段硅油的使用面越来越广，相比传统氨基硅油，其乳液稳定性好，柔软性好，亲水抗静电等优点，而且从根本上避免了一般有机硅乳液在使用过程中出现破乳漂油的现象。但市面上的嵌段硅油都普遍存在耐洗性差的问题，且在合成过程中需要使用大量的溶剂，不仅对生产过程、使用过程以及生态环境造成一定的影响，而且溶剂的存在容易造成染色织物的色光改变，色牢度下降。为了解决耐洗性差的问题，有研究者采用端环氧聚二甲基硅氧烷与二乙烯三胺、三乙烯四胺等多乙烯多胺类反应，制备超支化聚醚氨基嵌段有机硅，这种特殊的超支化网状结构赋予织物柔软、丰满及耐洗等性能，但反应过程中仍然需要加入一定量的溶剂，而且多乙烯多胺的结构会使有机硅整理剂的氨值提高，增加整理后织物黄变的可能性。
发明内容
本发明目的是客服现有技术的不足，提供一种超支化无溶剂型，柔软性和耐久性优异且无黄变的的一种无溶剂超支化有机硅柔软剂的制备方法。
为了实现上述目的，本发明采用以下技术方案：
一种无溶剂超支化有机硅柔软剂的制备方法，按以下步骤进行：
(一)、端羟基聚二甲基硅氧烷的制备：
将端环氧聚二甲基硅氧烷和二乙醇胺加入到反应容器中，加热至90～100℃，再保温3～4h后，开启真空，真空度为-0.05～-0.09Mpa下除水1～1.5h后得端羟基聚二甲基硅氧烷；
具体反应式如下：
其中：78≦n≦105；
(二)、超支化有机硅柔软剂的制备：
将端羟基聚二甲基硅氧烷加入到反应容器中，加热至90～110℃，缓慢滴加二异氰酸酯，滴加时间为0.5～1h，滴加完成后在90～110℃下保温1～2h，降温至70～80℃，加入丁酮肟再保温0.5～1h，得到超支化有机硅柔软剂；
具体反应式如下：
其中：78≦n≦105。
作为优选，所述二异氰酸酯为六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯中的一种。
由于上述技术方案的运用，本发明具有如下优点：
本发明采用二异氰酸酯为扩链剂，与端环氧聚二甲基硅氧烷反应，制备超支化有机硅柔软剂，其分子量高、粘度小、吸附性强，所形成的超支化网状结构能有效的覆盖在纤维表面及渗入纤维内部，赋予织物的柔软丰满的手感；封端后的异氰酸酯基团在高温焙烘时解封，与织物上的或自身分子结构上的活泼氢发生交联，提高整理后织物的耐水洗牢度；反应过程中不需要使用溶剂，解决了传统嵌段硅油合成过程中溶剂使用较多的问题；合成工艺简单易操作，安全环保。
附图说明
图1为本发明中实施例1的红外谱图；
图2为本发明中实施例2的红外谱图；
图3为本发明中实施例3的红外谱图。
具体实施方式
下面通过具体实施方式，结合附图，对本发明做进一步的描述。
实施例1：
将100份分子量8000的端环氧聚二甲基硅氧烷和2.7份二乙醇胺加入到反应容器中，加热至100℃，保温4h后，开启真空，真空度为-0.08Mpa下除水1h，然后加热至105℃，缓慢滴加4.2份六亚甲基二异氰酸酯，滴加时间为0.5h，滴加完成后在105℃下保温1h，降温至80℃，加入2份丁酮肟保温0.5h，得到超支化有机硅柔软剂；
参见附图1，它是本实施例中超支化有机硅柔软剂的红外谱图。端羟基硅油曲线中，3401.41cm-1处为-OH基团的特征吸收峰，1653.01cm-1处为C-N的特征吸收峰，在1258.22cm-1、863.61cm-1和1000cm-1～1130cm-1处出现三个吸收峰，为有机硅链段中Si-CH3、Si-OCH2CH3和Si-O-Si的特征吸收峰，超支化硅油曲线中-OH的特征吸收峰明显减弱，1717.89cm-1、1559.28cm-1两处出现的新的吸收峰为氨基甲酸酯基团的特征吸收峰，表明目标产物成功获得。
实施例2：
将100份分子量10000的端环氧聚二甲基硅氧烷和2.1份二乙醇胺加入到反应容器中，加热至100℃，保温4h后，开启真空，真空度为-0.09Mpa下除水1h，然后加热至110℃，缓慢滴加3.4份六亚甲基二异氰酸酯，滴加时间为0.5h，滴加完成后在110℃下保温2h，降温至80℃，加入1.6份丁酮肟保温0.5h，得到超支化有机硅柔软剂；
参见附图2，它是本实施例中超支化有机硅柔软剂的红外谱图。端羟基硅油曲线中，3401.41cm-1处为-OH基团的特征吸收峰，1653.01cm-1处为C-N的特征吸收峰，在1258.22cm-1、863.61cm-1和1000cm-1～1130cm-1处出现三个吸收峰，为有机硅链段中Si-CH3、Si-OCH2CH3和Si-O-Si的特征吸收峰，超支化硅油曲线中-OH的特征吸收峰明显减弱，1716.72cm-1、1558.53cm-1两处出现的新的吸收峰为氨基甲酸酯基团的特征吸收峰，表明目标产物成功获得。
实施例3：
将110份分子量8000的端环氧聚二甲基硅氧烷和2.9份二乙醇胺加入到反应容器中，加热至95℃，保温4h后，开启真空，真空度为-0.09Mpa下除水1h，然后加热至100℃，缓慢滴加6.1份异佛尔酮二异氰酸酯，滴加时间为1h，滴加完成后在105℃下保温2h，降温至70℃，加入2.4份丁酮肟保温1h，得到超支化有机硅柔软剂；
参见附图3，它是本实施例中超支化有机硅柔软剂的红外谱图。端羟基硅油曲线中，3401.41cm-1处为-OH基团的特征吸收峰，1653.01cm-1处为C-N的特征吸收峰，在1258.22cm-1、863.61cm-1和1000cm-1～1130cm-1处出现三个吸收峰，为有机硅链段中Si-CH3、Si-OCH2CH3和Si-O-Si的特征吸收峰，超支化硅油曲线中-OH的特征吸收峰明显减弱，1719.57cm-1、1532.90cm-1两处出现的新的吸收峰为氨基甲酸酯基团的特征吸收峰，表明目标产物成功获得。
无溶剂超支化有机硅柔软剂应用整理工艺：
1.超支化有机硅柔软剂乳液配制：
2.整理工艺：
所用织物：灰色涤棉梭织布。
整理工艺流程：浸轧工作液(超支化有机硅柔软剂乳液30g/L，轧余率60％)→焙烘(190℃×30s)→回潮24h→测试。
3.应用性能测试：
柔软性评价：用手触摸法评定，采用1～5分评判法，1分最差，5分最好，三人同时评定，取平均分。
色变：用电脑测色配色仪测试整理前后织物的颜色变化。
摩擦牢度：参考GB/T3920-1997《纺织品色牢度试验耐摩擦色牢度》进行测试。
水洗牢度：参考GB/T3921.1-1997《纺织品色牢度试验耐洗色牢度》进行测试。
本发明的超支化有机硅柔软剂应用性能测试结果如表1所示：
表1超支化有机硅柔软剂应用性能测试结果
由上表可以看出，经本发明超支化有机硅柔软剂整理后的织物柔软性优于市售嵌段硅油，且水洗后下降程度小；对织物干湿摩擦牢度影响较小，且色变低。

Claims (2)

1.一种无溶剂超支化有机硅柔软剂的制备方法，其特征在于按以下步骤进行：
(一)、端羟基聚二甲基硅氧烷的制备：
将端环氧聚二甲基硅氧烷和二乙醇胺加入到反应容器中，加热至90～100℃，再保温3～4h后，开启真空，真空度为-0.05～-0.09Mpa下除水1～1.5h后得端羟基聚二甲基硅氧烷；
具体反应式如下：
其中：78≦n≦105；
(二)、超支化有机硅柔软剂的制备：
将端羟基聚二甲基硅氧烷加入到反应容器中，加热至90～110℃，缓慢滴加二异氰酸酯，滴加时间为0.5～1h，滴加完成后在90～110℃下保温1～2h，降温至70～80℃，加入丁酮肟再保温0.5～1h，得到超支化有机硅柔软剂；
具体反应式如下：
其中：78≦n≦105。
2.根据权利要求1所述的一种无溶剂超支化有机硅柔软剂的制备方法，其特征在于：所述二异氰酸酯为六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯中的一种。
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