CN108047419A - 蓬松型聚氨酯改性有机硅柔软剂的制备方法 - Google Patents

蓬松型聚氨酯改性有机硅柔软剂的制备方法 Download PDF

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CN108047419A
CN108047419A CN201711351679.9A CN201711351679A CN108047419A CN 108047419 A CN108047419 A CN 108047419A CN 201711351679 A CN201711351679 A CN 201711351679A CN 108047419 A CN108047419 A CN 108047419A
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孙莹莹
王艾德
齐鹏举
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Zibo Lurui Fine Chemical Co Ltd
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Abstract

本发明属于纺织助剂的制备技术领域，具体的涉及一种蓬松型聚氨酯改性有机硅柔软剂的制备方法。在锡类催化剂催化下，反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇在60℃～90℃，反应3～5h得到异氰酸酯封端的改性有机硅聚氨酯预聚体；改性有机硅聚氨酯预聚体中加入脂肪酸，在60℃～90℃反应1～3h，得到改性有机硅脂肪酸聚氨酯共聚物；改性有机硅脂肪酸聚氨酯共聚物中加入乳化剂、助溶剂和冰醋酸，在40℃～60℃下混合，再加入去离子水进行乳化，即得蓬松型聚氨酯改性有机硅柔软剂。本发明制备的柔软剂在储存、运输和使用过程中具有优异的稳定性，赋予织物独特的蓬松型手感风格，并且与树脂一浴时可以保持织物良好的强力，提高织物免烫级别。

Description

蓬松型聚氨酯改性有机硅柔软剂的制备方法
技术领域
本发明属于纺织助剂的制备技术领域，具体的涉及一种蓬松型聚氨酯改性有机硅柔软剂的制备方法。
背景技术
纺织品柔软剂是一种能赋予织物特殊手感的纺织助剂，目前以改性有机硅柔软剂或三元嵌段有机硅柔软剂为主，这类结构的硅油具有良好的分子柔软性，能有效降低纤维之间的动静摩擦系数，具有优异的手感和亲水性，随着客户越来越多的要求，单一风格的柔软剂已经不能满足客户需求，根据风格要求出现脂肪酸类、聚氨酯类和改性硅油中的一种或者几种组合的复配产品，来达到客户对柔软性、亲水性、蓬松性、抗皱性等综合性能的要求，但是由于混合复配的产品稳定性较差，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
本发明的目的是克服现有技术的不足，提供一种蓬松型聚氨酯改性有机硅柔软剂的制备方法。使其柔软剂在储存、运输和使用过程中具有优异的稳定性，赋予织物独特的蓬松型手感风格，并且与树脂一浴时可以保持织物良好的强力，提高织物免烫级别。
本发明所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，具体包括以下步骤：
(1)在锡类催化剂催化下，反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇在60℃～90℃，搅拌反应3～5h得到异氰酸酯封端的改性有机硅聚氨酯预聚体；
(2)在改性有机硅聚氨酯预聚体中加入脂肪酸，在60℃～90℃搅拌反应1～3h，得到改性有机硅脂肪酸聚氨酯共聚物；
(3)在改性有机硅脂肪酸聚氨酯共聚物中加入乳化剂、助溶剂和冰醋酸，在40℃～60℃下混合搅拌，再加入去离子水进行乳化，30-90分钟内滴加完毕，即得蓬松型聚氨酯改性有机硅柔软剂。
其中：
反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇的摩尔比例0.5～1.5:1～3:0.5～2；锡类催化剂的质量分数占反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇总质量的0.01％～0.1％。
脂肪酸为C12～C18脂肪酸，优选月桂酸或硬脂酸中的一种或两种的混合物；脂肪酸加入量占改性有机硅聚氨酯预聚体质量分数的10％～25％。
乳化剂为5EO异构C12～C13脂肪醇聚氧乙烯醚、7EO异构C12～C13脂肪醇聚氧乙烯醚或12EO异构C12～C13脂肪醇聚氧乙烯醚中的一种或多种的组合；乳化剂用量为改性有机硅脂肪酸聚氨酯共聚物质量的10％～50％。
反应性聚硅氧烷线性体为数均分子量在1000～3000的羟乙基聚硅氧烷或羟丙基聚硅氧烷中的一种或两种的化合物的混合物。
二异氰酸酯为六亚甲基二异氰酸酯；锡类催化剂为辛酸亚锡或二月桂酸二丁基锡中的一种。
聚醚多元醇为聚氧化乙烯二元醇或聚氧化丙烯二元醇中的一种，数均分子量在800～2000。
助溶剂为乙二醇单丁醚、二乙二醇单丁醚、异丙醇或丙二醇中的一种或多种；助溶剂用量为改性有机硅脂肪酸聚氨酯共聚物质量的5％～10％。
冰醋酸用量为步骤(3)整个体系质量的0.3～1％。
去离子水用量为步骤(3)整个体系质量的50～80％。
作为一个优选的技术方案，本发明所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，具体包括以下步骤：
(1)由反应性聚硅氧烷线性体、二异氰酸酯、聚醚多元醇，摩尔比例为0.5～1.5:1～3:0.5～2，加入占反应体系的0.01％～0.1％的锡类催化剂，在60℃～90℃，氮气保护状态下，搅拌反应3～5h得到异氰酸酯封端的改性有机硅聚氨酯预聚体；
(2)在改性有机硅聚氨酯预聚体中加入C12-C18脂肪酸，其加入量占预聚体质量分数的10％-25％，在60℃～90℃搅拌反应1～3h，得到改性有机硅脂肪酸聚氨酯共聚物；
(3)脂肪酸聚氨酯有机硅共聚物的乳化
在步骤(2)所得到的有机硅共聚物中加入乳化剂、助溶剂和冰醋酸，在40℃～60℃下混合搅拌均匀，乳化剂用量为共聚物质量的10％～50％，助溶剂用量为共聚物的5％-10％，再加入去离子水进行乳化，去离子水用量为整个体系质量的60～80％，30分钟内均匀滴加完毕，即得蓬松型聚氨酯改性有机硅共聚物柔软剂。
本发明具有以下有益效果：
(1)通过反应性聚硅氧烷线性体、二异氰酸酯、聚醚多元醇、脂肪酸共聚制得共聚物，含有一定刚度和极性的氨基甲酸酯链节，可以赋予织物独特的柔软手感风格；由于脂肪酸结构的存在，赋予织物蓬松的手感；而且由于聚氨酯的交联作用，在树脂一浴的工艺使用中，增加了织物的强力和免烫级别，同时改变原来混合复配的物理模式。
(2)经过共聚物乳化后制备的柔软剂不但保持了优异的柔软蓬松应用效果，而且其储存、运输和使用的稳定性好，不易出现分层、沾污等现象。
具体实施方式
以下结合实施例对本发明作进一步描述。
实施例1
(1)在干净的烧瓶中加入80g羟乙基聚硅氧烷(分子量1500)、23.5g六亚甲基二异氰酸酯(HDI分子量168)，96.5g聚氧化丙烯二元醇(分子量1600)、加入催化剂二月桂酸二丁基锡0.15g，在65℃搅拌反应3.5h得到异氰酸酯封端的聚氨酯改性有机硅预聚体。
(2)继续加入26.5g月桂酸，70℃搅拌反应1.5h，得到有机硅脂肪酸聚氨酯共聚物。
(3)取制备的共聚物25g，加入3g异构C12～C13脂肪醇聚氧乙烯醚(5EO)、3g异构C12～C13脂肪醇聚氧乙烯醚(7EO)、1g二乙二醇单丁醚、1g异丙醇，0.5g冰醋酸，混合均匀，在30分钟内均匀滴加66.5g去离子水进行乳化，得到蓬松型聚氨酯改性有机硅共聚物柔软剂。
实施例2
(1)在干净的烧瓶中加入115g羟丙基聚硅氧烷(分子量2100)、21g六亚甲基二异氰酸酯(HDI分子量168)、164g聚氧化乙烯二元醇(分子量2000)，加入催化剂辛酸亚锡0.25g，在85℃搅拌反应4.5h得到异氰酸酯封端的聚氨酯改性有机硅预聚体。
(2)继续加入42g硬脂酸，90℃搅拌反应3h，得到有机硅脂肪酸聚氨酯共聚物。
(3)取制备的共聚物28g，加入5g异构C12～C13脂肪醇聚氧乙烯醚(7EO)、3g异构C12～C13脂肪醇聚氧乙烯醚(12EO)、1g乙二醇单丁醚、1g丙二醇，1.0g冰醋酸，混合均匀，在30分钟内均匀滴加61g去离子水进行乳化，得到蓬松型聚氨酯改性有机硅共聚物柔软剂。
柔软剂应用测试效果参见表1：
表1实施例1-2与市售混拼复配硅油柔软剂对织物柔软整理的效果对比表
从表1的数据可以看出，本发明柔软剂在柔软度和蓬松度上均能与混拼复配的脂肪酸聚氨酯硅油柔软剂抗衡，综合柔软蓬松的手感风格，几乎不影响织物的亲水性，并且与树脂一浴时，可以保持织物的强力，一定程度增加织物的免烫级别，同时储存放置稳定性得到明显的改进，使其可适用的工艺条件更广泛。
备注：柔软级别和蓬松级别均使用Handle-O-Meter柔软度测试仪进行测试；亲水性测试依据AATCC79-2010《纺织品吸水性》；白度测试依据GB/T 8424.2-2001《纺织品色牢度试验相对白度的仪器评定方法》；撕破强力测试依据ASTM D 1424-2009测试方法进行测试，断裂强力测试依据AATCC5034-2009方法进行测试；免烫级别测试依据AATCC124-2010测试方法进行测试；高温稳定性的测试方法如下：配置20g/L的试样溶液，加热到100℃，冷却后看表面是否有漂油现象；剪切稳定性的测试方法如下：配制40g/L的溶液500mL，用乙酸或氢氧化钠调节pH值在4和10，用搅拌器在1500rpm搅拌30分钟，维持溶液温度在50℃，看表面是否有漂油现象。

Claims (10)

1.一种蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：具体包括以下步骤：
(1)在锡类催化剂催化下，反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇在60℃～90℃，搅拌反应3～5h得到异氰酸酯封端的改性有机硅聚氨酯预聚体；
(2)在改性有机硅聚氨酯预聚体中加入脂肪酸，在60℃～90℃搅拌反应1～3h，得到改性有机硅脂肪酸聚氨酯共聚物；
(3)在改性有机硅脂肪酸聚氨酯共聚物中加入乳化剂、助溶剂和冰醋酸，在40℃～60℃下混合搅拌，再加入去离子水进行乳化，30-90分钟内滴加完毕，即得蓬松型聚氨酯改性有机硅柔软剂。
2.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇的摩尔比例为0.5～1.5:1～3:0.5～2；锡类催化剂的质量分数占反应性聚硅氧烷线性体、二异氰酸酯和聚醚多元醇总质量的0.01％～0.1％。
3.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：脂肪酸为C12～C18脂肪酸；脂肪酸加入量占改性有机硅聚氨酯预聚体质量分数的10％～25％。
4.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：乳化剂为5EO异构C12～C13脂肪醇聚氧乙烯醚、7EO异构C12～C13脂肪醇聚氧乙烯醚或12EO异构C12～C13脂肪醇聚氧乙烯醚中的一种或多种的组合；乳化剂用量为改性有机硅脂肪酸聚氨酯共聚物质量的10％～50％。
5.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：反应性聚硅氧烷线性体为数均分子量在1000～3000的羟乙基聚硅氧烷或羟丙基聚硅氧烷中的一种或两种的化合物的混合物。
6.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：二异氰酸酯为六亚甲基二异氰酸酯；锡类催化剂为辛酸亚锡或二月桂酸二丁基锡中的一种。
7.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：聚醚多元醇为聚氧化乙烯二元醇或聚氧化丙烯二元醇中的一种，数均分子量在800～2000。
8.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：助溶剂为乙二醇单丁醚、二乙二醇单丁醚、异丙醇或丙二醇中的一种或多种；助溶剂用量为改性有机硅脂肪酸聚氨酯共聚物质量的5％～10％。
9.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：冰醋酸用量为步骤(3)整个体系质量的0.3～1％。
10.根据权利要求1所述的蓬松型聚氨酯改性有机硅柔软剂的制备方法，其特征在于：去离子水用量为步骤(3)整个体系质量的60～80％。
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