CN112409910A - 一种基于聚氨酯的紫外变色涂层乳液及紫外变色面料的制备方法 - Google Patents

一种基于聚氨酯的紫外变色涂层乳液及紫外变色面料的制备方法 Download PDF

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CN112409910A
CN112409910A CN202011278289.5A CN202011278289A CN112409910A CN 112409910 A CN112409910 A CN 112409910A CN 202011278289 A CN202011278289 A CN 202011278289A CN 112409910 A CN112409910 A CN 112409910A
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戴建国
李晓强
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Abstract

本发明公开了一种基于聚氨酯的紫外变色涂层乳液的制备方法，包括步骤：(1)在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加定量的异佛尔酮二异氰酸酯，加入1～2滴二月桂酸二丁基锡，升温至60～65℃，并于水浴箱中保温；(2)在反应器中加入扩链剂，静置分钟后升温至70～75℃，并添加四氢呋喃进行反应并搅拌；(3)将步骤(2)反应得到的产物自然冷却到室温，在其内加入10,12‑二十五碳二炔酸，在搅拌下反应；而后在体系中加入二乙胺和四氢呋喃；(4)在步骤(3)产物中加入蒸馏水，得到基于聚氨酯的紫外变色涂层乳液。本发明还公开了基于聚氨酯的紫外变色面料的制备方法，本发明方法变色指示剂分散均匀可均匀显色。

Description

一种基于聚氨酯的紫外变色涂层乳液及紫外变色面料的制备 方法
技术领域
本发明涉及一种紫外变色涂层乳液及面临的制备方法，特别是涉及一种基于聚氨酯的紫外变色涂层乳液及紫外变色面料的制备方法。
背景技术
紫外变色面料是利用小分子或大分子变色性能实现织物面料在紫外光刺激下产生变色行为，从而体现面料提示或者防伪功能的一类功能面料。紫外变色面料因其变色直观性，在防伪和指示方面具有显著优势，因而被广泛地应用于现有的服装产业。
二炔是一种无色单体，在254nm紫外光的诱导下会发生聚合，形成蓝色聚二炔(PDA)。聚氨酯(PU)是由软硬段交替组成的嵌段共聚物，具有一定的弹性，采用PU可赋予面料涂层良好的力学性能。此外，聚氨酯是一种可对其分子结构进行设计的有机高分子材料，因其卓越的性能被广泛应用于涂料、胶粘剂、泡沫、弹性体、纤维等领域。而水性聚氨酯以水为溶剂，具有无污染、安全可靠、易于改性等优点。因此，将二炔与聚氨酯的性能相结合，则可以得到性能优异的紫外变色涂层材料。但是，仅仅通过简单的混合，二炔在聚氨酯体系中存在分散不均匀的缺点。应用于面料时，也造成了面料变色不匀均的问题。
发明内容
针对上述现有技术缺陷，本发明的任务在于提供一种基于聚氨酯的紫外变色涂层乳液的制备方法，改善变色指示剂在乳液中的分散性，以达到显示均匀的目的。本发明的任务在于提供一种基于聚氨酯的紫外变色面料的制备方法。
本发明技术方案是这样的：一种基于聚氨酯的紫外变色涂层乳液的制备方法，包括以下步骤：(1)配制聚氨酯反应溶液：在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加定量的异佛尔酮二异氰酸酯，加入1～2滴二月桂酸二丁基锡，升温至60～65℃，并于水浴箱中保温；(2)聚氨酯的合成：在反应器中加入扩链剂，静置10～15分钟后，将反应体系温度升至70～75℃，并添加四氢呋喃进行反应并搅拌；(3)指示剂的引入：将步骤(2)反应得到的产物自然冷却到室温，在其内加入10,12-二十五碳二炔酸，在搅拌下反应；而后在体系中加入二乙胺和四氢呋喃；(4)变色涂层的分散，在步骤(3)产物中加入蒸馏水，得到基于聚氨酯的紫外变色涂层乳液。
优选地，所述步骤(1)中异佛尔酮二异氰酸酯的加入量以异佛尔酮二异氰酸酯和聚四氢呋喃的总质量计为20～30％。
优选地，所述基于聚氨酯的紫外变色涂层乳液的固含量为30～40％。
优选地，所述步骤(2)反应时间2～3h。
优选地，所述步骤(3)反应时间10～12h。
一种基于聚氨酯的紫外变色面料的制备方法，包括步骤将上述发明得到的基于聚氨酯的紫外变色涂层乳液涂覆于织物面料上烘干后即可得到基于聚氨酯的紫外变色面料。
优选地，所述烘干时的烘干温度为90～95℃，烘干时间4～6h。
本发明与现有技术相比的优点在于：在聚氨酯体系中加入10,12-二十五碳二炔酸后加入二乙胺和四氢呋喃持续反应，使变色指示剂与聚氨酯基体材料结合，避免了指示剂的团聚，显色均匀。本发明方法简便、易控、成本低。
附图说明
图1为基于聚氨酯的紫外变色面料的紫外变色性能数据图。
具体实施方式
下面结合实施例对本发明作进一步说明，但不作为对本发明的限定。
实施例1，本实施例涉及的基于聚氨酯的紫外变色面料的制备方法如下：
(1)配制聚氨酯反应溶液：称取70.0g聚四氢呋喃，30.0g异佛尔酮二异氰酸酯，在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加异佛尔酮二异氰酸酯，最后加入1～2滴(0.05ml左右)二月桂酸二丁基锡，升温至60℃，并于水浴箱中保温；
(2)聚氨酯的合成：在上述反应物中加入扩链剂(如：乙二醇、丙三醇等多元醇，氢化双酚A等酯环醇类，二乙醇胺等醇胺类，等)，静置10分钟后，将反应体系温度升至70℃，并添加四氢呋喃20g，反应一段时间并在反应过程中搅拌以避免产物凝聚；
(3)指示剂的引入：将上步反应得到的产物自然冷却到室温，在其内加入0.5g 10,12-二十五碳二炔酸，在搅拌下反应；而后在体系中加入10.0g二乙胺和20.0g四氢呋喃；
(4)变色涂层的分散，在上述产物中加入250ml蒸馏水，得到基于聚氨酯的紫外变色涂层乳液。
(5)将基于聚氨酯的紫外变色涂层乳液通过浸渍法涂覆于涤纶机织织物面料上，并在90℃左右烘干4h。
实施例2，本实施例涉及的基于聚氨酯的紫外变色面料的制备方法如下：
(1)配制聚氨酯反应溶液：称取80.0g聚四氢呋喃，20.0g异佛尔酮二异氰酸酯，在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加异佛尔酮二异氰酸酯，最后加入1～2滴(0.05ml左右)二月桂酸二丁基锡，升温至65℃，并于水浴箱中保温；
(2)聚氨酯的合成：在上述反应物中加入扩链剂(如：乙二醇、丙三醇等多元醇，氢化双酚A等酯环醇类，二乙醇胺等醇胺类，等)，静置15分钟后，将反应体系温度升至70℃，并添加四氢呋喃20g，反应一段时间并在反应过程中搅拌以避免产物凝聚；
(3)指示剂的引入：将上步反应得到的产物自然冷却到室温，在其内加入0.5g 10,12-二十五碳二炔酸，在搅拌下反应；而后在体系中加入10.0g二乙胺和20.0g四氢呋喃；
(4)变色涂层的分散，在上述产物中加入250ml蒸馏水，得到基于聚氨酯的紫外变色涂层乳液。
(5)将基于聚氨酯的紫外变色涂层乳液通过浸渍法涂覆于涤纶机织织物面料上，并在95℃左右烘干5h。
实施例3，本实施例涉及的基于聚氨酯的紫外变色面料的制备方法如下：
(1)配制聚氨酯反应溶液：称取75.0g聚四氢呋喃，25.0g异佛尔酮二异氰酸酯，在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加异佛尔酮二异氰酸酯，最后加入1～2滴(0.05ml左右)二月桂酸二丁基锡，升温至65℃，并于水浴箱中保温；
(2)聚氨酯的合成：在上述反应物中加入扩链剂(如：乙二醇、丙三醇等多元醇，氢化双酚A等酯环醇类，二乙醇胺等醇胺类，等)，静置10分钟后，将反应体系温度升至70℃，并添加四氢呋喃20g，反应一段时间并在反应过程中搅拌以避免产物凝聚；
(3)指示剂的引入：将上步反应得到的产物自然冷却到室温，在其内加入0.5g 10,12-二十五碳二炔酸，在搅拌下反应；而后在体系中加入10.0g二乙胺和20.0g四氢呋喃；
(4)变色涂层的分散，在上述产物中加入250ml蒸馏水，得到基于聚氨酯的紫外变色涂层乳液。
(5)将基于聚氨酯的紫外变色涂层乳液通过浸渍法涂覆于涤纶机织织物面料上，并在90℃左右烘干6h。
对比例，紫外变色面料的制备方法如下：
(1)配制聚氨酯反应溶液：称取75.0g聚四氢呋喃，25.0g异佛尔酮二异氰酸酯，在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加异佛尔酮二异氰酸酯，最后加入1～2滴(0.05ml左右)二月桂酸二丁基锡，升温至65℃，并于水浴箱中保温；
(2)聚氨酯的合成：在上述反应物中加入扩链剂(如：乙二醇、丙三醇等多元醇，氢化双酚A等酯环醇类，二乙醇胺等醇胺类，等)，静置10分钟后，将反应体系温度升至70℃，并添加四氢呋喃20g，反应一段时间并在反应过程中搅拌以避免产物凝聚；
(3)将上述产物自然冷却至室温中加入250ml蒸馏水，得到聚氨酯涂层乳液；
(4)指示剂的引入：在聚氨酯涂层乳液中加入0.5g 10,12-二十五碳二炔酸，得到紫外变色涂层乳液；
(5)将紫外变色涂层乳液通过浸渍法涂覆于涤纶机织织物面料上，并在90℃左右烘干4h。
各实施例与对比例的紫外变色性能比较如下
紫外变色能力 变色时间 颜色均匀性(肉眼观测)
实施例1 有变色能力 30s 均匀
实施例2 有变色能力 31s 均匀
实施例3 有变色能力 28s 均匀
对比例 有变色能力 120s 不均匀

Claims (7)

1.一种基于聚氨酯的紫外变色涂层乳液的制备方法，其特征在于，包括以下步骤：(1)配制聚氨酯反应溶液：在装有电动搅拌器、回流冷凝器的反应器中，加入聚四氢呋喃，然后向其中滴加定量的异佛尔酮二异氰酸酯，加入1～2滴二月桂酸二丁基锡，升温至60～65℃，并于水浴箱中保温；(2)聚氨酯的合成：在反应器中加入扩链剂，静置10～15分钟后，将反应体系温度升至70～75℃，并添加四氢呋喃进行反应并搅拌；(3)指示剂的引入：将步骤(2)反应得到的产物自然冷却到室温，在其内加入10,12-二十五碳二炔酸，在搅拌下反应；而后在体系中加入二乙胺和四氢呋喃；(4)变色涂层的分散，在步骤(3)产物中加入蒸馏水，得到基于聚氨酯的紫外变色涂层乳液。
2.根据权利要求1所述的基于聚氨酯的紫外变色涂层乳液的制备方法，其特征在于，所述步骤(1)中异佛尔酮二异氰酸酯的加入量以异佛尔酮二异氰酸酯和聚四氢呋喃的总质量计为20～30％。
3.根据权利要求1所述的基于聚氨酯的紫外变色涂层乳液的制备方法，其特征在于，所述基于聚氨酯的紫外变色涂层乳液的固含量为30～40％。
4.根据权利要求1所述的基于聚氨酯的紫外变色涂层乳液的制备方法，其特征在于，所述步骤(2)反应时间2～3h。
5.根据权利要求1所述的基于聚氨酯的紫外变色涂层乳液的制备方法，其特征在于，所述步骤(3)反应时间10～12h。
6.一种基于聚氨酯的紫外变色面料的制备方法，其特征在于，包括步骤：将如权利要求1所述的基于聚氨酯的紫外变色涂层乳液的制备方法得到的基于聚氨酯的紫外变色涂层乳液涂覆于织物面料上烘干后即可得到基于聚氨酯的紫外变色面料。
7.根据权利要求6所述的基于聚氨酯的紫外变色面料的制备方法，其特征在于，所述烘干时的烘干温度为90～95℃，烘干时间4～6h。
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