CN102995417B - 一种无助剂的棉织物整理剂及其制备方法 - Google Patents

一种无助剂的棉织物整理剂及其制备方法 Download PDF

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CN102995417B
CN102995417B CN201210479724.XA CN201210479724A CN102995417B CN 102995417 B CN102995417 B CN 102995417B CN 201210479724 A CN201210479724 A CN 201210479724A CN 102995417 B CN102995417 B CN 102995417B
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苏建丽
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Abstract

一种无助剂的棉织物整理剂，包含封端型水性聚氨酯乳液，其预聚体的原料为IPDI、PPG、 BDO、DMPA，其中IPDI与PPG、DMPA、BDO的摩尔比为1.3:1-1.4:1，BDO占预聚体总质量的2%-3%，DMPA占预聚体总质量的5%-6%。其制备方法为预聚体反应完成后，加入EMAO进行封端，再经过三乙胺中和成盐及加水乳化，得到微蓝色封端型水性聚氨酯乳液，用作棉织物整理剂。应用时加热解封便可与纤维素反应起到整理剂的作用。经过该方法制备的棉织物整理剂不添加助剂，缩短了制备流程，提高了效率，降低了成本，是一种新型棉织物整理剂。

Description

一种无助剂的棉织物整理剂及其制备方法
技术领域
本发明涉及一种无助剂的棉织物整理剂及其制备方法，属化工领域。
技术背景        
水性聚氨酯是一种绿色环保、应用前景较好的新型聚氨酯材料。在实际应用中，为了对聚氨酯进行改性或使聚氨酯更好地与作用对象发生反应，可以对端-NCO基团的预聚体进行封端改性。首先将聚合阶段的异氰酸酯基保护起来，在应用时，通过加热而解封，从而与交联剂或基体反应，形成交联或分子量更大的产物，该类聚氨酯在织物整理方面表现出较好的性能。
传统的棉织物整理剂往往需要添加渗透剂、有机硅柔软剂等助剂来提高棉织物的折痕回复角，添加助剂增加了制备成本，降低了生产效率。本专利发明了一种无助剂的棉织物整理剂制备方法，在制备过程中不添加任何助剂，降低了制备成本，提高了生产效率。
发明内容
本发明的目的是提供一种以异佛尔酮二异氰酸酯(IPDI)及聚氧化丙烯二醇(PPG)为原料的无助剂棉织物整理剂及其制备方法。
为实现以上目的，本发明的无助剂的棉织物整理剂，包含封端型水性聚氨酯乳液，其预聚体的原料为异佛尔酮二异氰酸酯(IPDI)、聚氧化丙烯二醇(PPG)、1,4-丁二醇(BDO)、二羟甲基丙酸(DMPA)，封端剂为甲乙酮肟(EMAO)，其中IPDI与PPG、DMPA、BDO的摩尔比为1.3:1-1.4:1，BDO占预聚体质量的2%-3%，DMPA占预聚体质量的5%-6%，EMAO的物质的量与过量IPDI中-NCO的物质的量相等。
该无助剂的棉织物整理剂的制造方法为：
原料的预处理：经实验发现，用未经过脱水处理的原料进行反应，会使得反应后期的粘度增大，得到的乳液稳定性差，所以制备水性聚氨酯乳液的原料在前期都要进行脱水处理，即将IPDI、PPG及N-甲基吡咯烷酮进行脱水处理。
水性聚氨酯乳液的制备：容器中加入PPG、DMPA，升温至75℃，加入IPDI及适量二月桂酸二丁基锡催化剂，反应120min；在反应过程中，加入N-甲基吡咯烷酮以降低粘度；反应后加入小分子扩链剂BDO，反应90min。
封端型水性聚氨酯的制备：降温至40℃，加入MEAO进行封端，反应30min，加入三乙胺进行中和反应生成盐，反应3-5min；加水乳化60min，得到封端型水性聚氨酯乳液，用作棉织物整理剂。
如上所述，加入N-甲基吡咯烷酮的量为预聚体总质量的10%-15%，加入水的量为预聚体总质量的2-2.5倍，加入三乙胺的物质的量与DMPA的物质的量相同。
本发明产生的有益效果为，在制备过程中，预聚体反应完成后，加入甲乙酮肟(EMAO)，对端-NCO进行封端，使其失去反应能力，得到封端型的水性聚氨酯乳液。在使用时，对其进行加热解封，分子链两端释放出活性较高的-NCO，与纤维素分子内或分子间伯-OH作用，使得在外力作用下纤维素分子内或分子间相对滑移的概率降低，起到增强或交联作用，且当分子去除后，由于整理分子的紧固作用，使得变形很快恢复，从而起到抗皱作用。本发明的棉织物整理剂不用添加渗透剂、有机硅柔软剂等助剂，能更好的起到抗皱作用，从而降低了制备成本。
实施例
实施例1：
一种无助剂的棉织物整理剂，包含封端型水性聚氨酯乳液，预聚体的原料中IPDI与PPG、 BDO、DMPA的摩尔比为1.3:1，BDO占预聚体总质量的2%，DMPA占预聚体总质量的5%。
一种无助剂的棉织物整理剂的制备方法为，首先将IPDI、PPG及N-甲基吡咯烷酮进行脱水处理。在容器中加入PPG、DMPA，升温至75℃，加入IPDI及适量二月桂酸二丁基锡催化剂，反应120min。在反应过程中，加入预聚体总质量15%的N-甲基吡咯烷酮以降低粘度。反应后加入小分子扩链剂BDO，反应90min。降温至40℃，加入EMAO进行封端，加入的EMAO的物质的量与过量IPDI中-NCO的物质的量相等，反应30min，加入三乙胺中和成盐，其中三乙胺的物质的量与DMPA的物质的量相同，反应3min。加入预聚体总质量2倍的水进行乳化60min，得到封端性水性聚氨酯乳液。
所得乳液呈半透明带蓝光，稳定性好。
实施例2：
一种无助剂的棉织物整理剂，包含封端型水性聚氨酯乳液，预聚体的原料中IPDI与PPG、 BDO、DMPA的摩尔比为1.4:1，BDO占预聚体总质量的2%，DMPA占预聚体总质量的5%。
一种无助剂的棉织物整理剂的制备方法为，首先将IPDI、PPG及N-甲基吡咯烷酮进行脱水处理。在容器中加入PPG、DMPA，升温至75℃，加入IPDI及适量二月桂酸二丁基锡催化剂，反应120min。在反应过程中，加入预聚体总质量15%的N-甲基吡咯烷酮以降低粘度。反应后加入小分子扩链剂BDO，反应90min。降温至40℃，加入EMAO进行封端，加入的EMAO的物质的量与过量IPDI中-NCO的物质的量相等，反应30min，加入三乙胺中和成盐，其中三乙胺的物质的量与DMPA的物质的量相同，反应4min。加入预聚体总质量2倍的水进行乳化60min，得到封端性水性聚氨酯乳液。
所得乳液呈半透明带蓝光，稳定性好。

Claims (4)

1.一种无助剂的棉织物整理剂，包含封端型水性聚氨酯乳液，其特征在于：其预聚体的原料为异佛尔酮二异氰酸酯(IPDI)、聚氧化丙烯二醇(PPG)、1,4-丁二醇(BDO)、二羟甲基丙酸(DMPA)，封端剂为甲乙酮肟，其中 IPDI与PPG、DMPA、BDO的摩尔比为1.3:1-1.4:1，BDO占预聚体质量的2%-3%，DMPA占预聚体质量的5%-6%，甲乙酮肟的物质的量与过量IPDI中 -NCO的物质的量相等；
制备方法如下：
步骤(1)原料的预处理：将IPDI、PPG及N-甲基吡咯烷酮进行脱水处理；
步骤(2)水性聚氨酯乳液的制备：容器中加入PPG、DMPA，升温至75℃，加入IPDI及适量二月桂酸二丁基锡催化剂，反应120min；在反应过程中，加入N-甲基吡咯烷酮以降低粘度；反应后加入小分子扩链剂BDO，反应90min；
步骤(3)封端型水性聚氨酯的制备：降温至40℃，加入甲乙酮肟进行封端，反应30min，加入三乙胺进行中和反应生成盐，反应3-5min；加水乳化60min，得到封端型水性聚氨酯乳液，用作棉织物整理剂。
2.如权利要求1所述的一种无助剂的棉织物整理剂，其特征在于：步骤(2)中所述N-甲基吡咯烷酮的量为预聚体总质量的10%-15%。
3.如权利要求1所述的一种无助剂的棉织物整理剂，其特征在于：步骤(3)中所述水的量为预聚体总质量的2-2.5倍。
4.如权利要求1所述的一种无助剂的棉织物整理剂，其特征在于：步骤(3)中所述三乙胺的物质的量与DMPA的物质的量相同。
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CN106243313B (zh) * 2016-08-26 2019-04-12 山东天庆科技发展有限公司 一种水性聚氨酯消光树脂及其制备方法
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