CN109371687A - 纺织品高柔性水性聚氨酯整理剂及其制备方法 - Google Patents

纺织品高柔性水性聚氨酯整理剂及其制备方法 Download PDF

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CN109371687A
CN109371687A CN201811178928.3A CN201811178928A CN109371687A CN 109371687 A CN109371687 A CN 109371687A CN 201811178928 A CN201811178928 A CN 201811178928A CN 109371687 A CN109371687 A CN 109371687A
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polyurethane
finishing agent
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CN109371687B (zh
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徐成书
邢建伟
任燕
达来
王海霞
郭路星
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Ningxia Zhongyin Cashmere Textile Co Ltd
Xian Polytechnic University
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Xian Polytechnic University
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Abstract

本发明公开的纺织品高柔性水性聚氨酯整理剂,由以下原料反应制成:聚醚二元醇,脂肪族二异氰酸酯,非离子扩链剂,离子型亲水扩链剂,N‑甲基‑2‑吡咯烷酮,异丙醇,线性聚醚嵌段氨基硅油,中和剂,去离子水。本发明整理剂的制备方法为:采用双端氨基聚醚与双端环氧基聚醚硅油先制备线性聚醚嵌段氨基硅油;之后采用聚醚二醇与脂肪族二异氰酸酯与扩链剂制备得到聚氨酯,并采用线性聚醚嵌段氨基硅油进行改性,得到整理剂。本发明具有优异的柔顺性能,使整理纺织品的手感提高1‑2级,在纺织品整理应用方面有更为突出的优点。

Description

纺织品高柔性水性聚氨酯整理剂及其制备方法
技术领域
本发明属于高分子材料合成及应用技术领域,具体涉及一种纺织品高柔性水性聚氨酯整理剂,本发明还涉及上述水性聚氨酯整理剂的制备方法。
背景技术
水性聚氨酯在纺织品的整理加工中,可以作为涂层剂、粘合剂、抗起毛起球整理剂、羊毛与羊绒织物防缩剂、固色剂等用途,得到了较为广泛的应用。但是由于水性聚氨酯胶膜的硬度偏大,采用水性聚氨酯乳液对纺织品进行整理之后,往往使整理织物的手感偏差,即使采用柔软剂进行柔软处理依然无法获取理想的柔软性能,即无法兼顾整理效果与织物手感,尤其是对手感有高要求的纺织品这一问题更为突出。
采用有机硅对水性聚氨酯进行改性并作为纺织品整理剂用途,除了获得聚氨酯整理效果之外,因聚硅氧烷在膜表面的富集,可在一定程度上避免纯粹水性聚氨酯整理导致织物手感的恶化。关于有机硅改性水性聚氨酯的研究报道,涉及的有机硅改性剂多数为小分子量的硅氧烷偶联剂、羟基硅油、和侧链氨基硅油,其实这一类有机硅改性水性聚氨酯胶膜的柔顺性能往往不够理想,被整理纺织品的手感依然偏差。本发明采用低氨值大分子量线性嵌段聚醚氨基硅油作为水性聚氨酯的改性剂,可获得耐水性能优良的高柔性聚合物材料,其胶膜的铅笔硬度可达到3B至5B,具有柔软而不粘手的特点,并且和基材的粘附力优良,经该高柔性水性聚氨酯整理织物具有良好的柔软性性能,而相关的研究报道及应用范例还很少。
发明内容
本发明的目的在于提供一种纺织品用高柔性水性聚氨酯整理剂,解决了现有整理剂制造的纺织品的柔软性能差,手感差的问题。
本发明的另一目的在于提供上述高柔性水性聚氨酯整理剂的制备方法。
本发明所采用的第一种技术方案是,纺织品高柔性水性聚氨酯整理剂,包括以下组分:水和线性嵌段聚醚氨基硅油改性水性聚氨酯,所述线性嵌段聚醚氨基硅油改性水性聚氨酯的化学结构式如下:
其中,R1的结构式为:
或-CH2-CH2-CH2-CH2-CH2-CH2-中的一种;
R2的结构式为:
中的一种;
R3的结构式为:-CH2-CH2-O-CH2-CH2-;
R4的结构式为:
R5的结构式为:
中的一种;
R6的结构式为:
本发明所采用的第二种技术方案是,纺织品高柔性水性聚氨酯整理剂的制备方法,具体按照以下步骤实施:
步骤1、制备线性聚醚嵌段氨基硅油
步骤1.1、按质量百分比分别称取以下原材料:双端氨基聚醚3.20%~10.00%,双端环氧基聚醚硅油60.00%~67.00%,异丙醇30.00%,以上组分的含量总和为100%;
步骤1.2、将步骤1称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇混合后,在搅拌状态下升温至80℃保温反应8h~10h,制备得到有效含量为70.00%的线性聚醚嵌段氨基硅油;
步骤2、制备高柔性水性聚氨酯整理剂
步骤2.1:按质量百分比分别称取以下原料:聚醚二元醇9.50%~20.00%,脂肪族二异氰酸酯6.30%~11.80%,非离子扩链剂0.50%~3.10%,离子型亲水扩链剂0.90%~2.10%,N-甲基-2-吡咯烷酮0~4.00%,异丙醇9.00%~15.00%,线性聚醚嵌段氨基硅油2.00%~10.00%,中和剂0.70%~4.50%,去离子水49.00%~55.00%,以上组分的含量总和为100%;
步骤2.2、将步骤2.1中称取的聚醚二元醇和脂肪族二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至85℃~90℃,保温反应90min~120min,得到聚氨酯预聚体;
步骤2.3、将经步骤2.2得到的聚氨酯预聚体的温度控制在70℃~75℃,加入步骤2.1中称取的离子型亲水扩链剂,反应90min~120min;再加入步骤2.1称取的非离子扩链剂继续保温反应60min~90min,制成聚氨酯。
步骤2.4、将步骤2.1中称取的异丙醇加入到步骤2.3制备的聚氨酯中并搅拌均匀后降温至30℃~40℃,得到预改聚氨酯;然后将步骤2.1中称取的线性聚醚嵌段氨基硅油在45min~60min内滴加到预改聚氨酯中,再保温反应90min~120min,制得改性聚氨酯;
步骤2.5、制备得到纺织品高柔性水性聚氨酯整理剂
步骤2.5.1、将步骤2.1称取的中和剂加入步骤2.4制备出的改性聚氨酯中,在30℃~40℃条件下以1800-2200r/min的速度搅拌中和处理30min~40min,得到中和后改性聚氨酯;
步骤2.5.2、将步骤2.1中称取的去离子水加入到步骤2.5.1得到的中和后改性聚氨酯中,在30℃~40℃条件下以1800-2200r/min的速度搅拌乳化分散40min~60min,即制备得到本发明纺织品高柔性水性聚氨酯整理剂。
本发明的特点还在于,
双端氨基聚醚的分子量600~1000,双端环氧基聚醚硅油的分子量8000~12000;
聚醚二元醇为聚醚二醇PPG 2000、PTMG 2000中的一种。
脂肪族二异氰酸酯为异佛尔酮二异氰酸酯、1,6-己二异氰酸酯中的一种。
非离子扩链剂为二乙二醇、异佛尔酮二胺中的一种或二乙二醇、异佛尔酮二胺的组合;
离子扩链剂为二羟甲基丙酸、N-甲基二乙醇胺中的一种。
离子扩链剂为二羟甲基丙酸时需使用所述N-甲基-2-吡咯烷酮作为溶剂溶解。
中和剂为三乙胺、醋酸中的一种。
本发明的有益效果在于:
(1)本发明的高柔性水性聚氨酯整理剂采用聚醚二元醇为软段单体,以脂肪族二异氰酸酯为硬段单体,以离子型亲水单体与非离子单体为扩链剂,以线性聚醚嵌段氨基硅油为改性剂,所制备出的改性水性聚氨酯乳液存储稳定性能良好。通过低氨值的线性嵌段氨基硅油与水性聚氨酯形成低密度交联结构,以及聚醚嵌段氨基硅油中的聚醚链段和水性聚氨酯软段的相容性,使聚硅氧烷链段均匀的富集在胶膜表面并固定在主体聚氨酯结构上,使该改性水性聚氨酯乳液成膜所得胶膜具有优异的柔顺性能,手感特点为软而不粘手,并具有优良的耐水性能。因此,该改性水性聚氨酯乳液在柔性基材的涂膜用途方面具有显著的优势。
(2)本发明的纺织品高柔性水性聚氨酯理整理剂,具有水性聚氨酯整理剂的共性特点,可作为纺织品的涂层剂、抗起毛起球整理剂、羊毛与羊绒织物防缩剂、固色剂等用途。其与普通结构有机硅改性水性聚氨酯相比,具有优异的柔顺性能,铅笔硬度达到3B至5B,手感特点为柔软而不粘手,可使整理织物的手感提高1-2级,在纺织品整理应用方面有更为突出的柔软性能与耐水性能。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
本发明的纺织品高柔性水性聚氨酯整理剂,纺织品高柔性水性聚氨酯整理剂,包括以下组分:水和线性嵌段聚醚氨基硅油改性水性聚氨酯,所述线性嵌段聚醚氨基硅油改性水性聚氨酯的化学结构式如下:
其中,R1的结构式为:
或-CH2-CH2-CH2-CH2-CH2-CH2-中的一种;
R2的结构式为:
中的一种;
R3的结构式为:-CH2-CH2-O-CH2-CH2-;
R4的结构式为:
R5的结构式为:
中的一种;
R6的结构式为:
纺织品高柔性水性聚氨酯整理剂的制备方法,具体按照以下步骤实施:
步骤1、制备线性聚醚嵌段氨基硅油
步骤1.1、按质量百分比分别称取以下原材料:双端氨基聚醚3.20%~10.00%,双端环氧基聚醚硅油60.00%~67.00%,异丙醇30.00%,以上组分的含量总和为100%;
步骤1.2、将步骤1称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇混合后,在搅拌状态下升温至80℃保温反应8h~10h,制备得到有效含量为70.00%的线性聚醚嵌段氨基硅油;
步骤2、制备高柔性水性聚氨酯整理剂
步骤2.1:按质量百分比分别称取以下原料:聚醚二元醇9.50%~20.00%,脂肪族二异氰酸酯6.30%~11.80%,非离子扩链剂0.50%~3.10%,离子型亲水扩链剂0.90%~2.10%,N-甲基-2-吡咯烷酮0~4.00%,异丙醇9.00%~15.00%,线性聚醚嵌段氨基硅油2.00%~10.00%,中和剂0.70%~4.50%,去离子水49.00%~55.00%,以上组分的含量总和为100%;
步骤2.2、将步骤2.1中称取的聚醚二元醇和脂肪族二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至85℃~90℃,保温反应90min~120min,得到聚氨酯预聚体;
步骤2.3、将经步骤2.2得到的聚氨酯预聚体的温度控制在70℃~75℃,加入步骤2.1中称取的离子型亲水扩链剂,反应90min~120min;再加入步骤2.1称取的非离子扩链剂继续保温反应60min~90min,制成聚氨酯。
步骤2.4、将步骤2.1中称取的异丙醇加入到步骤2.3制备的聚氨酯中并搅拌均匀后降温至30℃~40℃,得到预改聚氨酯;然后将步骤2.1中称取的线性聚醚嵌段氨基硅油在45min~60min内滴加到预改聚氨酯中,再保温反应90min~120min,制得改性聚氨酯;
步骤2.5、制备得到纺织品高柔性水性聚氨酯整理剂
步骤2.5.1、将步骤2.1称取的中和剂加入步骤2.4制备出的改性聚氨酯中,在30℃~40℃条件下以1800-2200r/min的速度搅拌中和处理30min~40min,得到中和后改性聚氨酯;
步骤2.5.2、将步骤2.1中称取的去离子水加入到步骤2.5.1得到的中和后改性聚氨酯中,在30℃~40℃条件下以1800-2200r/min的速度搅拌乳化分散40min~60min,即制备得到本发明纺织品高柔性水性聚氨酯整理剂。
双端氨基聚醚的分子量600~1000,双端环氧基聚醚硅油的分子量8000~12000;
聚醚二元醇为聚醚二醇PPG 2000、PTMG 2000中的一种。
脂肪族二异氰酸酯为异佛尔酮二异氰酸酯、1,6-己二异氰酸酯中的一种。
非离子扩链剂为二乙二醇、异佛尔酮二胺中的一种或二乙二醇、异佛尔酮二胺的组合;
离子扩链剂为二羟甲基丙酸、N-甲基二乙醇胺中的一种。
中和剂为三乙胺、醋酸中的一种。
双端氨基聚醚化学结构式如下所示:
双端环氧基聚醚硅油化学结构式如下所示:
线性聚醚嵌段氨基硅油化学结构式如下所示:
实施例1
纺织品高柔性水性聚氨酯整理剂,按质量百分比由以下原料反应而成:
步骤1、制备线性聚醚嵌段氨基硅油
线性聚醚嵌段氨基硅油按质量百分比由以下原料制成:双端氨基聚醚(分子量600)3.30%,双端环氧基聚醚硅油(分子量12000)66.70%,异丙醇30.00%。
将称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇混合后,在搅拌状态下升温至80℃保温反应8小时,制备得到有效含量为70.00%的线性聚醚嵌段氨基硅油。
步骤2、制备高柔性水性聚氨酯整理剂
按质量百分比分别称取以下原料:聚醚二醇PPG 2000 12.00%,异佛尔酮二异氰酸酯6.8%,异佛尔酮二胺0.60%,二羟甲基丙酸1.3%,N-甲基-2-吡咯烷酮4%,异丙醇10.00%,线性聚醚嵌段氨基硅油9.85%,三乙胺1.37%,去离子水54.38%;
将称取的聚醚二醇PPG 2000与异佛尔酮二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至85℃,保温反应90min,得到聚氨酯预聚体;
将预聚体的温度控制在70℃时加入称取的二羟甲基丙酸(事先将二羟甲基丙酸充分溶解于N-甲基-2-吡咯烷酮)反应90min,之后加入异佛尔酮二胺继续反应60min,制成聚氨酯;
先将称取的异丙醇加入到上述制备的聚氨酯中并搅拌均匀,并降温至30℃;再将线性聚醚嵌段氨基硅油于60min内滴加到上述聚氨酯中,保温反应120min,制得改性聚氨酯;
将称取的三乙胺加入到制备出的改性聚氨酯中,在30℃下以2000r/min的速度搅拌中和反应30min,得到中和后的改性聚氨酯;
将称取的去离子水加入上述已经中和的改性聚氨酯中,在40℃条件下以2100r/min的速度搅拌乳化分散60min,即制备得到本发明的纺织品高柔性水性聚氨酯整理剂乳液。
实施例2
纺织品高柔性水性聚氨酯整理剂,按质量百分比由以下原料反应而成:
步骤1、制备线性聚醚嵌段氨基硅油
线性聚醚嵌段氨基硅油按质量百分比由以下原料制成:双端氨基聚醚(分子量1000)9.88%,双端环氧基聚醚硅油(分子量8000)60.12%,异丙醇30.00%,以上组分的含量总和为100%。
将称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇加入反应装置,在搅拌状态下升温至80℃保温反应10小时,制备得到线性聚醚嵌段氨基硅油,有效含量为70.00%。
步骤2、制备高柔性水性聚氨酯整理剂
按质量百分比分别称取以下原料:聚醚二醇PTMG 2000 19.00%,异佛尔酮二异氰酸酯7.50%,二乙二醇0.5%,二羟甲基丙酸1.00%,N-甲基-2-吡咯烷酮2.29%,异丙醇15.00%,线性聚醚嵌段氨基硅油2.30%,三乙胺0.85%,去离子水51.56%。
将称取的聚醚二醇PTMG 2000与异佛尔酮二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至90℃,保温反应120min,得到聚氨酯预聚体;将预聚体的温度控制在75℃时加入称取的二羟甲基丙酸(事先将二羟甲基丙酸充分溶解于N-甲基-2-吡咯烷酮)反应120min,之后加入二乙二醇继续反应90min,制成聚氨酯;
将称取的异丙醇加入到上述制备的聚氨酯中并搅拌均匀,并降温至40℃;再将线性聚醚嵌段氨基硅油于45min内滴加到上述聚氨酯中,保温反应90min,制得改性聚氨酯;
将称取的三乙胺加入到制备出的改性聚氨酯中,在40℃下以2100r/min的速度搅拌中和反应40min,得到中和后的改性聚氨酯;
将称取的去离子水加入上述已经中和后的改性聚氨酯中,在30℃条件下以1900r/min的速度搅拌乳化分散40min,即制备得到本发明的纺织品高柔性水性聚氨酯整理剂乳液。
实施例3
步骤1、制备线性聚醚嵌段氨基硅油
线性聚醚嵌段氨基硅油按质量百分比由以下原料制成:双端氨基聚醚(分子量950)3.2%,双端环氧基聚醚硅油(分子量10000)66.8%,异丙醇30.00%,以上组分的含量总和为100%。
将称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇加入反应装置,在搅拌状态下升温至80℃保温反应9小时,制备得到线性聚醚嵌段氨基硅油,有效含量为70.00%。
步骤2、制备高柔性水性聚氨酯整理剂
按质量百分比分别称取以下原料:聚醚二醇PPG 2000 20%,异佛尔酮二异氰酸酯7.5%,异佛尔酮二胺1.5%,二乙二醇1.6%,二羟甲基丙酸2.1%,N-甲基-2-吡咯烷酮0.6%,异丙醇15.00%,线性聚醚嵌段氨基硅油2%,三乙胺0.7%,去离子水49%,以上组分的含量总和为100%。
将称取的聚醚二醇PPG 2000与异佛尔酮二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至88℃,保温反应100min,得到聚氨酯预聚体;将预聚体的温度控制在72℃时加入称取的二羟甲基丙酸(事先将二羟甲基丙酸充分溶解于N-甲基-2-吡咯烷酮)反应110min,之后加入二乙二醇与异佛尔酮二胺继续反应70min,制成聚氨酯;
先将称取的异丙醇加入到上述制备的聚氨酯中并搅拌均匀,并降温至35℃;再将线性聚醚嵌段氨基硅油于50min内滴加到上述聚氨酯中,保温反应110min,制得改性聚氨酯;
将称取的三乙胺加入到制备出的改性聚氨酯中,在35℃下以2200r/min的速度搅拌中和反应35min,得到中和后的改性聚氨酯;
将称取的去离子水加入上述已经中和的改性聚氨酯中,在30℃条件下以2000r/min的速度搅拌乳化分散50min,即制备得到本发明的纺织品高柔性水性聚氨酯整理剂乳液。
实施例4
步骤1、制备线性聚醚嵌段氨基硅油
线性聚醚嵌段氨基硅油按质量百分比由以下原料制成:双端氨基聚醚(分子量800)5.20%,双端环氧基聚醚硅油(分子量10000)64.80%,异丙醇30.00%,以上组分的含量总和为100%。
将称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇加入反应装置,在搅拌状态下升温至80℃保温反应8小时,制备得到线性聚醚嵌段氨基硅油,有效含量为70.00%。
步骤2、制备高柔性水性聚氨酯整理剂
按质量百分比分别称取以下原料:聚醚二醇PTMG 2000 10.00%,1,6-己二异氰酸酯10%,异佛尔酮二胺0.70%,二乙二醇1.00%,N-甲基二乙醇胺1.80%,异丙醇15.00%,线性聚醚嵌段氨基硅油2.50%,醋酸4.00%,去离子水55%,以上组分的含量总和为100%。
将称取的聚醚二醇PTMG 2000与异佛尔酮二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至90℃,保温反应110min,得到聚氨酯预聚体;将预聚体的温度控制在70℃时加入称取的N-甲基二乙醇胺(事先将N-甲基二乙醇胺充分溶解于N-甲基-2-吡咯烷酮)反应100min,之后加入二乙二醇与异佛尔酮二胺继续反应80min,制成聚氨酯;
先将称取的异丙醇加入到上述制备的聚氨酯中并搅拌均匀,并降温至40℃;再将线性聚醚嵌段氨基硅油于60min内滴加到上述聚氨酯中,保温反应110min,制得改性聚氨酯;
将称取的醋酸加入到制备出的改性聚氨酯中,在30℃下以1800r/min的速度搅拌中和反应30min,得到中和后的改性聚氨酯;
将称取的去离子水加入上述已经中和的改性聚氨酯中,在35℃条件下以1800r/min的速度搅拌乳化分散55min,即制备得到本发明的纺织品高柔性水性聚氨酯整理剂乳液。
实施例5
步骤1、制备线性聚醚嵌段氨基硅油
线性聚醚嵌段氨基硅油按质量百分比由以下原料制成:双端氨基聚醚(分子量950)7.20%,双端环氧基聚醚硅油(分子量12000)62.80%,异丙醇30.00%,以上组分的含量总和为100%。
将称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇加入反应装置,在搅拌状态下升温至80℃保温反应9小时,制备得到线性聚醚嵌段氨基硅油,有效含量为70.00%。
步骤2、制备高柔性水性聚氨酯整理剂
按质量百分比分别称取以下原料:聚醚二醇PTMG 2000 9.70%,六亚甲基二异氰酸酯11.60%,二乙二醇1.13%,异佛尔酮二胺1.87%,N-甲基二乙醇胺2.00%,异丙醇15.00%,线性聚醚嵌段氨基硅油5.00%,醋酸4.40%,去离子水49.30%。
将称取的聚醚二醇PTMG 2000与六亚甲基二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至90℃,保温反应100min,得到聚氨酯预聚体;将预聚体的温度控制在70℃时加入称取的N-甲基二乙醇胺反应100min,之后加入二乙二醇与异佛尔酮二胺继续反应90min,制成聚氨酯;
先将称取的异丙醇加入到上述制备的聚氨酯中并搅拌均匀,并降温至40℃;再将线性聚醚嵌段氨基硅油于50min内滴加到上述聚氨酯中,保温反应110min,制得改性聚氨酯;
将称取的醋酸加入到制备出的改性聚氨酯中,在35℃条件下以2000r/min的速度搅拌中和处理40min,得到中和后的改性聚氨酯;
将称取的去离子水加入上述已经中和的改性聚氨酯中,在32℃条件下以1900r/min的速度搅拌乳化分散50min,即制备得到本发明的纺织品高柔性水性聚氨酯整理剂乳液。
实施例6
步骤1、制备线性聚醚嵌段氨基硅油
线性聚醚嵌段氨基硅油按质量百分比由以下原料制成:双端氨基聚醚(分子量950)10.00%,双端环氧基聚醚硅油(分子量10000)60.00%,异丙醇30.00%,以上组分的含量总和为100%。
将称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇混合后,在搅拌状态下升温至80℃保温反应10小时,制备得到线性聚醚嵌段氨基硅油。
步骤2、制备高柔性水性聚氨酯整理剂
按质量百分比分别称取以下原料:聚醚二醇PPG2000 9.5%,1,6-己二异氰酸酯6.30%,异佛尔酮二胺0.5%,二乙二醇0.9%,二羟甲基丙酸1.50%,N-甲基-2-吡咯烷酮4%,异丙醇9.00%,线性聚醚嵌段氨基硅油10%,三乙胺4.5%,去离子水53.8%,以上组分的含量总和为100%。
将称取的聚醚二醇PPG 2000与异佛尔酮二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至85℃,保温反应100min,得到聚氨酯预聚体;将预聚体的温度控制在72℃时加入称取的二羟甲基丙酸(事先将二羟甲基丙酸充分溶解于N-甲基-2-吡咯烷酮)反应110min,之后加入二乙二醇与异佛尔酮二胺继续反应70min,制成聚氨酯;
先将称取的异丙醇加入到上述制备的聚氨酯中并搅拌均匀,并降温至35℃;再将线性聚醚嵌段氨基硅油于50min内滴加到上述聚氨酯中,保温反应110min,制得改性聚氨酯;
将称取的三乙胺加入到制备出的改性聚氨酯中,在35℃下以2200r/min的速度搅拌中和反应35min,得到中和后的改性聚氨酯;
将称取的去离子水加入上述已经中和的改性聚氨酯中,在30℃条件下以2000r/min的速度搅拌乳化分散50min,即制备得到本发明的纺织品高柔性水性聚氨酯整理剂乳液。
本发明方法制备的产品用途:
采用本发明的方法制备出的纺织品高柔性水性聚氨酯整理剂,具有水性聚氨酯整理剂的共性特点,可作为纺织品的涂层剂、抗起毛起球整理剂、羊毛与羊绒织物防缩剂、固色剂等用途。其与普通结构有机硅改性水性聚氨酯相比,具有优异的柔顺性能,其胶膜铅笔硬度达到3B至5B,手感特点为柔软而不粘手,可使整理纺织品的手感提高1-2级,在纺织品整理应用方面有更为突出的柔软性能与耐水性能。

Claims (7)

1.纺织品高柔性水性聚氨酯整理剂,其特征在于,包括以下组分:水和线性嵌段聚醚氨基硅油改性水性聚氨酯,所述线性嵌段聚醚氨基硅油改性水性聚氨酯的化学结构式如下:
其中,R1的结构式为:
或-CH2-CH2-CH2-CH2-CH2-CH2-中的一种;
R2的结构式为:
中的一种;
R3的结构式为:-CH2-CH2-O-CH2-CH2-;
R4的结构式为:
R5的结构式为:
中的一种;
R6的结构式为:
2.纺织品高柔性水性聚氨酯整理剂的制备方法,其特征在于,具体按照以下步骤实施:
步骤1、制备线性聚醚嵌段氨基硅油
步骤1.1、按质量百分比分别称取以下原材料:双端氨基聚醚3.20%~10.00%,双端环氧基聚醚硅油60.00%~67.00%,异丙醇30.00%,以上组分的含量总和为100%;
步骤1.2、将步骤1称取的双端氨基聚醚、双端环氧基聚醚硅油与异丙醇混合后,在搅拌状态下升温至80℃保温反应8h~10h,制备得到有效含量为70.00%的线性聚醚嵌段氨基硅油;
步骤2、制备高柔性水性聚氨酯整理剂
步骤2.1:按质量百分比分别称取以下原料:聚醚二元醇9.50%~20.00%,脂肪族二异氰酸酯6.30%~11.80%,非离子扩链剂0.50%~3.10%,离子型亲水扩链剂0.90%~2.10%,N-甲基-2-吡咯烷酮0~4.00%,异丙醇9.00%~15.00%,线性聚醚嵌段氨基硅油2.00%~10.00%,中和剂0.70%~4.50%,去离子水49.00%~55.00%,以上组分的含量总和为100%;
步骤2.2、将步骤2.1中称取的聚醚二元醇和脂肪族二异氰酸酯加入到连接有搅拌装置的反应容器中,搅拌、升温至85℃~90℃,保温反应90min~120min,得到聚氨酯预聚体;
步骤2.3、将离子型亲水扩链剂将经步骤2.2得到的聚氨酯预聚体的温度控制在70℃~75℃,加入步骤2.1中称取的离子型亲水扩链剂,反应90min~120min;再加入步骤2.1称取的非离子扩链剂继续保温反应60min~90min,制成聚氨酯。
步骤2.4、将步骤2.1中称取的异丙醇加入到步骤2.3制备的聚氨酯中并搅拌均匀后降温至30℃~40℃,得到预改聚氨酯;然后将步骤2.1中称取的线性聚醚嵌段氨基硅油在45min~60min内滴加到预改聚氨酯中,再保温反应90min~120min,制得改性聚氨酯;
步骤2.5、制备得到纺织品高柔性水性聚氨酯整理剂
步骤2.5.1、将步骤2.1称取的中和剂加入步骤2.4制备出的改性聚氨酯中,在30℃~40℃条件下以1800-2200r/min的速度搅拌中和处理30min~40min,得到中和后改性聚氨酯;
步骤2.5.2、将步骤2.1中称取的去离子水加入到步骤2.5.1得到的中和后改性聚氨酯中,在30℃~40℃条件下以1800-2200r/min的速度搅拌乳化分散40min~60min,即制备得到本发明纺织品高柔性水性聚氨酯整理剂。
3.根据权利要求2所述的纺织品高柔性水性聚氨酯整理剂的制备方法,其特征在于:所述双端氨基聚醚的分子量600~1000,双端环氧基聚醚硅油的分子量8000~12000;
所述聚醚二元醇为聚醚二醇PPG 2000、PTMG 2000中的一种。
4.根据权利要求2所述的纺织品高柔性水性聚氨酯整理剂的制备方法,其特征在于:所述脂肪族二异氰酸酯为异佛尔酮二异氰酸酯、1,6-己二异氰酸酯中的一种。
5.根据权利要求2所述的纺织品高柔性水性聚氨酯整理剂的制备方法,其特征在于:所述非离子扩链剂为二乙二醇、异佛尔酮二胺中的一种或二乙二醇、异佛尔酮二胺的组合;
所述离子扩链剂为二羟甲基丙酸、N-甲基二乙醇胺中的一种。
6.根据权利要求2所述的纺织品高柔性水性聚氨酯整理剂的制备方法,其特征在于:所述中和剂为三乙胺、醋酸中的一种。
7.根据权利要求5所述的纺织品高柔性水性聚氨酯整理剂的制备方法,其特征在于:所述离子扩链剂为二羟甲基丙酸时需使用所述N-甲基-2-吡咯烷酮作为溶剂溶解。
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