CN114737400A - 大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法 - Google Patents
大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法 Download PDFInfo
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Abstract
本发明属于纺织助剂技术领域,具体的涉及一种大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,将端环氧硅油、聚醚胺和溶剂混合均匀后进行反应,制得预聚体,将叔胺和有机酸加入预聚体中,继续反应,即得季胺改性嵌段有机硅;向反应器中加入季胺改性嵌段有机硅、脂肪醇聚氧乙烯醚和溶剂,搅拌均匀,加入去离子水,转相乳化,然后加入有机酸调节pH后,即得大粒径巨乳季胺改性嵌段有机硅柔软剂。本发明制备的大粒径巨乳季胺改性嵌段有机硅柔软剂处理后的织物手感风格为滑爽、轻微蜡感和高弹性,具有良好的白度和亲水性,相比于传统的氨基巨乳液,其稳定性大大改善。
Description
技术领域
本发明属于纺织助剂技术领域,具体的涉及一种大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法。
背景技术
有机硅乳液在各种纺织特性上具有突出的优势,而粒径的大小对织物整理的风格有显著的影响。微乳含有短链或交联的有机硅,会产生柔软、蓬松的风格,而大粒径的巨乳,附着在表面,提供滑爽、松弹的手感风格。
目前市场上的巨乳液以氨基硅油为主,白度低,亲水性差,在储存、运输和使用过程中易出现分层、沾污等问题。
发明内容
本发明要解决的技术问题是:克服现有技术的不足,提供一种大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,制备的大粒径巨乳季胺改性嵌段有机硅柔软剂处理后的织物手感风格为滑爽、轻微蜡感和高弹性,具有良好的白度和亲水性,相比于传统的氨基巨乳液,其稳定性大大改善。
本发明所述的大粒径巨乳季胺改性嵌段有机硅柔软剂制备方法,具体包括以下步骤:
(1)季胺改性嵌段有机硅的合成
将环氧硅油、聚醚胺和溶剂混合均匀,在60~80℃反应10~15h,制得预聚体,将叔胺和有机酸加入上述预聚体中,在70~100℃反应4~6h,即得季胺改性嵌段有机硅;
(2)大粒径巨乳季胺改性嵌段有机硅柔软剂的制备
向反应器中加入季胺改性嵌段有机硅、脂肪醇聚氧乙烯醚和溶剂,搅拌均匀,加入去离子水,转相乳化,然后加入有机酸将pH调节至5.0-6.0,即得大粒径巨乳季胺改性嵌段有机硅柔软剂。
其中:
端环氧硅油分子量为6000~13000,聚醚胺分子量为400~2000。
聚醚胺与端环氧硅油的物质的量比为0.3~0.9:1,叔胺与端环氧硅油的物质的量比为0.4~0.7:1。
步骤(1)所述的溶剂为异丙醇、乙二醇单丁醚、二乙二醇单丁醚、乙二醇单乙醚或二丙二醇丁醚中的一种或几种的组合,其用量占整个体系质量的20~50%。
步骤(1)所述的有机酸是乙酸、月桂酸或柠檬酸中的一种,用量与叔胺等摩尔比。
叔胺为N,N-二甲基十二烷基胺、十八烷基二甲基叔胺、十四烷基二甲基叔胺或N,N-二甲基正丁胺中的一种或多种。
季胺改性嵌段有机硅与脂肪醇聚氧乙烯醚的质量比为12.0-16.0:1;季胺改性嵌段有机硅与溶剂的质量比为11.0-19.0:1。
脂肪醇聚氧乙烯醚是C12-14醇聚氧乙烯醚、C13醇聚氧乙烯醚或C10醇聚氧乙烯醚的一种或多种。
步骤(2)所述的溶剂是异丙醇、乙二醇丁醚、二乙二醇丁醚、聚乙二醇、丙三醇或2-甲基-2,4-戊二醇中的一种。
步骤(2)所述的有机酸是乙酸、月桂酸或柠檬酸中的一种,其用量占整个体系的0.3~2%。
步骤(2)中加入的去离子水占整个体系质量的50~80%。
作为一个优选的技术方案,本发明所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,具体步骤如下:
在反应器中加入聚醚胺、端环氧硅油,其物质的量比为0.3~0.9:1和质量分数占总体系30~50%的溶剂混合均匀,在60~80℃反应10~15h,制得预聚体,将叔胺和等摩尔的有机酸加入上述预聚体中,在70~100℃反应4~6h,即得季胺改性嵌段有机硅;
向容器中加入与季胺改性嵌段有机硅质量比为12.0-16.0:1的脂肪醇聚氧乙烯醚,加入与嵌段季胺改性硅油质量比11.0-19.0:1的溶剂,中速搅拌,加入去离子水转相,加入有机酸调节pH至5.0-6.0,即得成品。
本发明具有以下有益效果:
(1)本发明与现有技术、产品相比,进行了季胺阳离子化,季胺嵌段改性硅油替代了传统的氨基硅油,提高了产物的极性、反应性和吸附性和亲水性,解决了白度低,易黄变、亲水性差问题,保证了产品的稳定性。
(2)本发明与现有技术、产品相比,解决了传统微乳液柔软剂达不到的手感风格,手感风格为滑爽、轻微蜡感和高弹性。
(3)本发明与现有技术、产品相比,不需要复杂特殊的设备如高速均质机、分散机等,简单易行。
具体实施方式
下面结合实施例对本发明做进一步的说明。
实施例1
将聚醚胺(分子量2000)14g、环氧硅油(分子量8000)80g和异丙醇40g混合均匀,在70℃反应13h,制得预聚体,将1.0g N,N-二甲基十二烷基胺和0.5g乙酸加入上述预聚体中,在80℃反应5h,即得季胺改性嵌段有机硅。
向容器中加入2.4g的C13醇聚氧乙烯醚6EO、季胺改性嵌段有机硅30.0g和1.8g二乙二醇单丁醚,搅拌均匀,在15分钟内加入65.5g去离子水进行乳化,最后加入0.3g乙酸,即得成品。
实施例2
将聚醚胺(分子量900)3.2g、环氧硅油(分子量13000)70g和异丙醇40g混合均匀,在70℃反应13h,制得预聚体,将0.9g十八烷基二甲基叔胺和0.5g醋酸加入上述预聚体中,在80℃反应5h,即得季胺改性嵌段有机硅。
向容器中加入2.0g的C13醇聚氧乙烯醚7EO、季胺改性嵌段有机硅28.0g和2.7g 2-甲基-2,4-戊二醇,搅拌均匀,在15分钟内加入67.0g去离子水进行乳化,最后加入0.3g乙酸,即得成品。
运用上述实施例1-2得到的大粒径巨乳季胺改性嵌段有机硅柔软剂,对cm40*cm30*114*70和cpt80/2*cpt80/2*160*72两种规格面料进行处理,与市场上常规产品Solusoft WA对比的应用结果如表1所示。
表1实施例1-2大粒径巨乳季胺改性嵌段有机硅柔软剂应用效果对比表
注:整理液配制如下:树脂30g/L,中和酸0.5g/L。纯棉织物在以上整理液中二浸二轧,110℃烘干1分钟。
白度测试依据GB/T 8424.2-2001《纺织品色牢度实验相对白度的仪器评定方法》
酚黄变测试依据GB/T 29778-2013测试方法进行测试
亲水性测试依据AATC79-2010《纺织品吸水性》
断裂强力测试依据AATCC5034-2009测试方法进行测试
撕破强力测试依据ASTM D 1424-2009测试方法进行测试
手感测试采用手触摸法评定,☆表示半级,★表示一级,三人摸手感,取平均值,星级越多,手感越好。
当然,上述内容仅为本发明的较佳实施例,不能被认为用于限定对本发明的实施例范围。本发明也并不仅限于上述举例,本技术领域的普通技术人员在本发明的实质范围内所做出的均等变化与改进等,均应归属于本发明的专利涵盖范围内。
Claims (10)
1.一种大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:包括以下步骤:
(1)季胺改性嵌段有机硅的合成
将端环氧硅油、聚醚胺和溶剂混合均匀后进行反应,制得预聚体,将叔胺和有机酸加入预聚体中,继续反应,即得季胺改性嵌段有机硅;
(2)大粒径巨乳季胺改性嵌段有机硅柔软剂的制备
向反应器中加入季胺改性嵌段有机硅、脂肪醇聚氧乙烯醚和溶剂,搅拌均匀,加入去离子水,转相乳化,然后加入有机酸调节pH后,即得大粒径巨乳季胺改性嵌段有机硅柔软剂。
2.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(1)中制备预聚体的反应温度为60~80℃,反应时间为10~15h;将叔胺和有机酸加入预聚体中在70~100℃反应4~6h。
3.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(1)中端环氧硅油分子量为6000~13000,聚醚胺分子量为400~2000;聚醚胺与端环氧硅油的物质的量比为0.3~0.9:1,叔胺与端环氧硅油的物质的量比为0.4~0.7:1。
4.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(1)中所述的溶剂为异丙醇、乙二醇单丁醚、二乙二醇单丁醚、乙二醇单乙醚或二丙二醇丁醚中的一种或多种的组合,其用量占整个体系质量的20~50%;步骤(1)中所述的有机酸为乙酸、月桂酸或柠檬酸中的一种,用量与叔胺等摩尔比。
5.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(1)中叔胺为N,N-二甲基十二烷基胺、十八烷基二甲基叔胺、十四烷基二甲基叔胺或N,N-二甲基正丁胺中的一种或多种。
6.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(2)中季胺改性嵌段有机硅与脂肪醇聚氧乙烯醚的质量比为12.0-16.0:1;季胺改性嵌段有机硅与溶剂的质量比为11.0-19.0:1。
7.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(2)中所述的脂肪醇聚氧乙烯醚是C12-14醇聚氧乙烯醚、C13醇聚氧乙烯醚或C10醇聚氧乙烯醚的一种或多种。
8.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(2)中所述的溶剂为异丙醇、乙二醇丁醚、二乙二醇丁醚、聚乙二醇、丙三醇或2-甲基-2,4-戊二醇中的一种。
9.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(2)中所述的有机酸为乙酸、月桂酸或柠檬酸中的一种,其用量占整个体系的0.3~2.0%,将溶液pH调节至5.0-6.0。
10.根据权利要求1所述的大粒径巨乳季胺改性嵌段有机硅柔软剂的制备方法,其特征在于:步骤(2)中加入的去离子水占整个体系质量的50~80%。
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