CN108867069A - 一种聚氨酯-有机硅共聚型柔软剂及其制备方法 - Google Patents
一种聚氨酯-有机硅共聚型柔软剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种聚氨酯‑有机硅共聚型柔软剂及其制备方法,包括以下步骤:以蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂等为原料制得聚氨酯‑有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯‑有机硅共聚型柔软剂。织物经本申请的柔软剂整理后,手感柔软,服用效果显著提高,经长时间使用,以及多次洗涤过后仍能保持良好的柔软度,并且不易泛黄。
Description
技术领域
本发明涉及纺织助剂领域,特别是一种聚氨酯-有机硅共聚型柔软剂及其制备方法。
背景技术
随着人们生活水平的提高,对纺织品的要求也越来越多,不仅要求织物吸湿、透气、穿着舒服,并且希望织物具有柔软,滑爽的手感,因此对纺织品的后整理受到人们越来越多的关注。尤其是对织物进行柔软整理,使织物手感柔软,提高穿着的舒适度,改善织物的外观风格。已经被广泛使用的柔软剂品种有多种,可以分为非表面活性剂类柔软剂、表面活性类柔软剂、反应型柔软剂和有机硅类柔软剂。其中有机硅是一种性能优越的织物柔软剂,由于其良好的分子柔顺性和较多的甲基,使得其可以在纤维表面形成甲基覆盖层,从而降低了纤维之间的动静摩擦系数,从而达到柔软效果。有机硅类柔软剂整理后的织物具有良好的平滑效果,获得温暖丰满的手感,能够提高织物的撕破强力和耐磨强度。
但是,由于有机硅没有与纤维形成结合力,仅仅是通过有限的范德华力和氢键与纤维进行结合,牢固性较差。聚氨酯改性的有机硅可以有效的解决这一问题,由于在有机硅中氨基的存在,使其能够与纤维上的负电荷基团形成静电引力结合的较为牢固的键合,牢固度大大优于普通有机硅油。同时,由于这种静电引力的作用,使得有更多的甲基可以外露,因此柔软效果更佳。但是聚氨酯改性的有机硅柔软剂存在易泛黄的缺点,不适宜用于浅色织物的柔软整理,因此仍需对其进行改性研究。
中国专利CN201610826047.2公开了一种有机硅改性聚氨酯共聚物织物柔软剂的制备方法,包括以下步骤:a)由聚醚多元醇、端羟基聚硅氧烷线性体、二异氰酸酯,在锡类催化剂作用下,在75℃~85℃搅拌反应2~3h得到异氰酸酯封端的有机硅改性聚氨酯预聚体;b)在有机硅改性聚氨酯预聚体中加入小分子胺类扩链剂,在50℃~60℃搅拌反应1~2h,得到有机硅改性聚氨酯共聚体;c、将步骤b)获得的有机硅改性聚氨酯共聚物在50℃~70℃与乳化剂混合均匀并缓慢加入去离子水进行乳化,即可得有机硅改性聚氨酯共聚物织物柔软剂。本发明方法制备的柔软剂稳定性好,并赋予织物优异的柔软和滑爽特性以及亲水性,且具有优异的耐黄变性,能保持浅色织物的鲜艳度和白色织物的白度。
发明内容
本发明涉及一种聚氨酯-有机硅共聚型柔软剂及其制备方法,织物经本申请的柔软剂整理后,手感柔软,服用效果显著提高,经长时间使用,以及多次洗涤过后仍能保持良好的柔软度,并且不易泛黄。
为实现上述目的,本发明采用以下技术方案:
一种聚氨酯-有机硅共聚型柔软剂的制备方法,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在110-120℃,以40-60转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应90-120min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为80-90℃,进行反应2-3h;
(2)降低温度至40-55℃,放入乳化器中,向其中加入水,搅拌乳化3-4h,蒸除丙酮,制得聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
优选的,所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物。
优选的,所述扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
优选的,所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油50-60份,聚四氢呋喃二醇22-34份,乙二胺聚氧化丙烯四醇33-45份,聚己内酯三醇24-35份,羟丙基硅油22-38份,扩链剂10-17份;二羟甲基丁酸15-22份。
优选的,所述步骤(1)中环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5。
优选的,所述步骤(1)中异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1-1.5。
优选的,所述二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
优选的,所述聚氨酯-有机硅共聚乳液的固含量为40%。
优选的,所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
本发明具有以下有益效果:
本申请采用聚醚多元醇、聚酯多元醇和羟丙基共混的形式,合成聚氨酯-有机硅共聚型乳液,即改善了聚氨酯型柔软剂的水渍问题,又使其可以具有有机硅类柔软剂的高柔软度。此外由于聚氨酯组分具有良好的交联性,可以与织物形成较为稳定的键合,使得所制备的柔软剂具有良好的附着力,织物经其整理后,在多次水洗后仍能保持良好柔软度。同时本申请选择具有良好耐候性,耐黄变性能的组分进行聚合反应,使得所制备的柔软剂可以具有良好的耐候性和耐黄变性能,长时间使用不会发黄变色。
具体实施方式
为了更好的理解本发明,下面通过实施例对本发明进一步说明,实施例只用于解释本发明,不会对本发明构成任何的限定。
实施例1
一种聚氨酯-有机硅共聚型柔软剂的制备方法,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在110℃,以40转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应90min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为80℃,进行反应2h;
(2)降低温度至40℃,放入乳化器中,向其中加入水,搅拌乳化3h,蒸除丙酮,制得固含量为40%的聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物;扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油50份,聚四氢呋喃二醇22份,乙二胺聚氧化丙烯四醇33份,聚己内酯三醇24份,羟丙基硅油22份,扩链剂10份;二羟甲基丁酸15份。
环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5;异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1。
二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
织物经制备的柔软剂进行柔软整理后,手感柔软,爽滑,并且经过多次水洗后仍能保持良好的柔软度,且不会出现黄变现象。
实施例2
一种聚氨酯-有机硅共聚型柔软剂的制备方法,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在120℃,以60转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应120min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为90℃,进行反应3h;
(2)降低温度至55℃,放入乳化器中,向其中加入水,搅拌乳化4h,蒸除丙酮,制得固含量为40%的聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物;扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油60份,聚四氢呋喃二醇34份,乙二胺聚氧化丙烯四醇45份,聚己内酯三醇35份,羟丙基硅油38份,扩链剂17份;二羟甲基丁酸22份。
环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5;异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1.5。
二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
织物经制备的柔软剂进行柔软整理后,手感柔软,爽滑,并且经过多次水洗后仍能保持良好的柔软度,且不会出现黄变现象。
实施例3
一种聚氨酯-有机硅共聚型柔软剂的制备方法,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在110℃,以60转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应90min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为90℃,进行反应2h;
(2)降低温度至55℃,放入乳化器中,向其中加入水,搅拌乳化3h,蒸除丙酮,制得固含量为40%的聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物;扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油50份,聚四氢呋喃二醇34份,乙二胺聚氧化丙烯四醇33份,聚己内酯三醇35份,羟丙基硅油22份,扩链剂17份;二羟甲基丁酸15份。
环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5;异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1.5。
二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
织物经制备的柔软剂进行柔软整理后,手感柔软,爽滑,并且经过多次水洗后仍能保持良好的柔软度,且不会出现黄变现象。
实施例4
一种聚氨酯-有机硅共聚型柔软剂的制备方法,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在120℃,以40转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应120min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为80℃,进行反应3h;
(2)降低温度至40℃,放入乳化器中,向其中加入水,搅拌乳化4h,蒸除丙酮,制得固含量为40%的聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物;扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油60份,聚四氢呋喃二醇22份,乙二胺聚氧化丙烯四醇45份,聚己内酯三醇24份,羟丙基硅油38份,扩链剂10份;二羟甲基丁酸22份。
环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5;异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1。
二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
织物经制备的柔软剂进行柔软整理后,手感柔软,爽滑,并且经过多次水洗后仍能保持良好的柔软度,且不会出现黄变现象。
实施例5
一种聚氨酯-有机硅共聚型柔软剂的制备方法,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在120℃,以50转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应100min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为80℃,进行反应3h;
(2)降低温度至50℃,放入乳化器中,向其中加入水,搅拌乳化4h,蒸除丙酮,制得固含量为40%的聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物;扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油55份,聚四氢呋喃二醇28份,乙二胺聚氧化丙烯四醇38份,聚己内酯三醇29份,羟丙基硅油30份,扩链剂14份;二羟甲基丁酸17份。
环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5;异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1.2。
二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
织物经制备的柔软剂进行柔软整理后,手感柔软,爽滑,并且经过多次水洗后仍能保持良好的柔软度,且不会出现黄变现象。
Claims (10)
1.一种聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于,包括以下步骤:
(1)将蓖麻油,聚四氢呋喃二醇,乙二胺聚氧化丙烯四醇,聚己内酯三醇,羟丙基硅油,环己烷二亚甲基二异氰酸酯,降冰片烷二异氰酸酯,催化剂加入反应釜中,加热使温度维持在110-120℃,以40-60转/min的速度搅拌,加入丙酮搅拌均匀后,加入扩链剂,二羟甲基丁酸持续搅拌反应90-120min,向反应釜中加入二乙醇胺混合搅拌均匀,控制温度为80-90℃,进行反应2-3h;
(2)降低温度至40-55℃,放入乳化器中,向其中加入水,搅拌乳化3-4h,蒸除丙酮,制得聚氨酯-有机硅共聚乳液,向其中加入月桂醇醚琥珀酸单酯磺酸钠,混合搅拌均匀,去除气泡,即得聚氨酯-有机硅共聚型柔软剂。
2.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述催化剂为二甲基乙醇胺和二醋酸二丁基锡的摩尔比为7:4的混合物。
3.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述扩链剂为新戊二醇和甘露醇的摩尔比为5:1的混合物。
4.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于,所述步骤(1)中原料的使用量为,以质量份数计:
蓖麻油50-60份,聚四氢呋喃二醇22-34份,乙二胺聚氧化丙烯四醇33-45份,聚己内酯三醇24-35份,羟丙基硅油22-38份,扩链剂10-17份;二羟甲基丁酸15-22份。
5.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述步骤(1)中环己烷二亚甲基二异氰酸酯和降冰片烷二异氰酸酯的使用量摩尔比为8:5。
6.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述步骤(1)中异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1-1.5。
7.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述二乙醇胺和二羟甲基丁酸的使用量摩尔比为1:1。
8.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述聚氨酯-有机硅共聚乳液的固含量为40%。
9.根据权利要求1所述的聚氨酯-有机硅共聚型柔软剂的制备方法,其特征在于:所述步骤(2)中聚氨酯-有机硅共聚乳液和月桂醇醚琥珀酸单酯磺酸钠的使用量质量比为20:1。
10.一种聚氨酯-有机硅共聚型柔软剂,其特征在于:以权利要求1-9任一项所述的方法制备而成。
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CN110684171A (zh) * | 2019-10-29 | 2020-01-14 | 兰州科天水性高分子材料有限公司 | 一种水性聚氨酯乳液及其制备方法和用途 |
CN112341597A (zh) * | 2020-10-30 | 2021-02-09 | 西安工程大学 | 一种水性聚氨酯湿摩擦牢度提升剂的制备方法 |
CN115612055A (zh) * | 2022-10-11 | 2023-01-17 | 江苏富淼科技股份有限公司 | 一种无溶剂自乳化的耐水洗型柔软剂、其制备方法和应用 |
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CN110684171A (zh) * | 2019-10-29 | 2020-01-14 | 兰州科天水性高分子材料有限公司 | 一种水性聚氨酯乳液及其制备方法和用途 |
CN112341597A (zh) * | 2020-10-30 | 2021-02-09 | 西安工程大学 | 一种水性聚氨酯湿摩擦牢度提升剂的制备方法 |
CN115612055A (zh) * | 2022-10-11 | 2023-01-17 | 江苏富淼科技股份有限公司 | 一种无溶剂自乳化的耐水洗型柔软剂、其制备方法和应用 |
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