CN107226896A - 一种水溶性黄色聚氨酯染料的制备方法 - Google Patents

一种水溶性黄色聚氨酯染料的制备方法 Download PDF

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CN107226896A
CN107226896A CN201710584606.8A CN201710584606A CN107226896A CN 107226896 A CN107226896 A CN 107226896A CN 201710584606 A CN201710584606 A CN 201710584606A CN 107226896 A CN107226896 A CN 107226896A
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卢汉炎
余敏
胡晁旻
卢汉敏
任佳
张权
任宝东
晁国库
孙鹏
张彬彬
李少东
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WENZHOU NANLI INDUSTRY Co Ltd
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Abstract

本发明涉及一种水溶性黄色聚氨酯染料的制备方法包括以下步骤：（1）将一定比例的对硝基氯苯与二乙醇胺、溶剂投入容器中，在100‑150℃下回流反应12‑24h，待原料反应完，停止反应，反应结束将混合物倒入沸水中，充分搅拌，冷却室温，离心洗涤分离，80℃干燥，干燥后的产品磨细，再离心洗涤，干燥，得到黄色扩链剂；（2）将聚乙二醇、乙二醇、步骤一的黄色扩链剂投入容器中，加热至70‑90℃，加入异佛尔酮二异氰酸酯，反应2‑4h，测定NCO%，并使用丁酮肟进行封端，得到水性的、黄色的聚氨酯染料。这种方法获得的黄色颜色具有鲜艳、纯正，永不褪色，对环境不会造成污染。

Description

一种水溶性黄色聚氨酯染料的制备方法
技术领域
本发明涉及一种水溶性黄色聚氨酯染料的制备方法。
背景技术
目前，我们使用的染料大部分是小分子有机染料，它们耐溶剂、耐热、耐迁移等许多方面的性能较差，并且在使用过程中易造成环境严重污染，所以高分子染料由此而生。高分子染料首先在德国拜耳、德国巴斯夫、荷兰斯塔尔、瑞士山德士等公司先后开始研究，特别是水性高分子染料的研究和生产更是成为热点。
高分子染料是通过一定的化学反应将带有显色的小分子基团进入到高分子的主链或悬挂于侧链上而形成有色高分子聚合物，它既具有高分子的特性，同时又具有小分子染料的特性，对特定光具有强烈的吸收和发色。
发明内容
本发明针对上述问题，提供一种水溶性黄色聚氨酯染料的制备方法。
本发明所采取的技术方案如下：一种水溶性黄色聚氨酯染料的制备方法，包括以下步骤：
（1）将一定比例的对硝基氯苯与二乙醇胺、溶剂投入容器中，在100-150℃下回流反应12-24h，待原料反应完，停止反应，反应结束将混合物倒入沸水中，充分搅拌，冷却室温，离心洗涤分离，80℃干燥，干燥后的产品磨细，再离心洗涤，干燥，得到黄色扩链剂；
（2）将聚乙二醇、乙二醇、步骤一的黄色扩链剂投入容器中，加热至70-90℃，加入异佛尔酮二异氰酸酯，反应2-4h，测定NCO%，并使用丁酮肟进行封端，得到水性的、黄色的聚氨酯染料。
步骤（1）中，所述溶剂为异丙醇、正丁醇中的一种或多种。
步骤（1）中，氯代硝基苯与二乙醇胺的摩尔配比为1:1-5。
步骤（1）中，回流反应温度为110-130℃。
步骤（1）中，回流反应时间为15-18h。
步骤（2）中，聚乙二醇的Mn=1000。
步骤（2）中，聚乙二醇、乙二醇、黄色扩链剂的摩尔比为1:4-12:0.1-0.3。
步骤（2）中，反应温度在80-85℃。
步骤（2）中，反应时间2-3h。
上述制备水溶性黄色聚氨酯染料的反应方程式如下所示：
本发明的有益效果如下：本发明利用接枝反应，将含有活泼氢的黄色染料与异氰酸酯反应，从而使水性聚氨酯树脂分子链上具有固定的发黄光体，得到黄色的、水性的聚氨酯染料。这种方法获得的黄色颜色具有鲜艳、纯正，永不褪色，对环境不会造成污染。
具体实施方式
下面结合具体实施例对本发明进行进一步描述，但本发明的保护范围并不仅限于此：
实施例1
将15.75g（0.1mol）硝基氯苯与31.542g（0.3mol）二乙醇胺投入到含有250ml异丙醇的500ml三口瓶中，在130℃下回流反应15h，待原料反应完，停止反应，反应结束将混合物倒入100℃沸水中，充分搅拌，冷却至室温，离心分离，反复洗涤干燥后，在80℃干燥得到产物。
将聚乙二醇PEG(Mn=1000）100g（0.1mol）、24.83g乙二醇（0.4mol）、步骤一的黄色扩链剂2.27g（0.01mol）投入三口瓶中，加热至70℃，加入118.88g异佛尔酮二异氰酸酯（IPDI），反应2h，测定NCO%，并使用丁酮肟进行封端，得到水性的、黄色的聚氨酯染料。
实施例2
将15.75g（0.1mol）硝基氯苯与52.575g（0.5mol）二乙醇胺投入到含有250ml异丙醇的500ml三口瓶中，在110℃下回流反应18h，待原料反应完，停止反应，反应结束将混合物倒入100℃沸水中，充分搅拌，冷却至室温，离心分离，反复洗涤干燥后，在80℃干燥得到产物。
将聚乙二醇PEG(Mn=1000）100g（0.1mol）、49.66g乙二醇（0.8mol）、步骤一的黄色扩链剂4.54g（0.02mol）投入三口瓶中，加热至80℃，加入214.45g异佛尔酮二异氰酸酯（IPDI），反应4h，测定NCO%，并使用丁酮肟进行封端，得到水性的、黄色的聚氨酯染料。
实施例3
将15.75g（0.1mol）硝基氯苯与10.51g（1mol）二乙醇胺投入到含有250ml异丙醇的500ml三口瓶中，在150℃下回流反应24h，待原料反应完，停止反应，反应结束将混合物倒入100℃沸水中，充分搅拌，冷却至室温，离心分离，反复洗涤干燥后，在80℃干燥得到产物。
将聚乙二醇PEG(Mn=1000）100g（0.1mol）、74.48g乙二醇（1.2mol）、步骤一的黄色扩链剂6.81g（0.03mol）投入三口瓶中，加热至85℃，加入310.02g异佛尔酮二异氰酸酯（IPDI），反应3.5h，测定NCO%，并使用丁酮肟进行封端，得到水性的、黄色的聚氨酯染料。

Claims (9)

1.一种水溶性黄色聚氨酯染料的制备方法，其特征在于，包括以下步骤：
（1）将一定比例的对硝基氯苯与二乙醇胺、溶剂投入容器中，在100-150℃下回流反应12-24h，待原料反应完，停止反应，反应结束将混合物倒入沸水中，充分搅拌，冷却室温，离心洗涤分离，80℃干燥，干燥后的产品磨细，再离心洗涤，干燥，得到黄色扩链剂；
（2）将聚乙二醇、乙二醇、步骤一的黄色扩链剂投入容器中，加热至70-90℃，加入异佛尔酮二异氰酸酯，反应2-4h，测定NCO%，并使用丁酮肟进行封端，得到水性的、黄色的聚氨酯染料。
2.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（1）中，所述溶剂为异丙醇、正丁醇中的一种或多种。
3.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（1）中，氯代硝基苯与二乙醇胺的摩尔配比为1:1-5。
4.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（1）中，回流反应温度为110-130℃。
5.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（1）中，回流反应时间为15-18h。
6.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（2）中，聚乙二醇的Mn=1000。
7.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（2）中，聚乙二醇、乙二醇、黄色扩链剂的摩尔比为1:4-12:0.1-0.3。
8.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（2）中，反应温度在80-85℃。
9.根据权利要求1所述的水溶性黄色聚氨酯染料的制备方法，其特征在于：步骤（2）中，反应时间2-3h。
CN201710584606.8A 2017-07-18 2017-07-18 一种水溶性黄色聚氨酯染料的制备方法 Pending CN107226896A (zh)

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CN109467673A (zh) * 2018-09-10 2019-03-15 清华大学 一种封闭型活性阴离子彩色聚氨酯乳液及其制备方法和用途

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109467673A (zh) * 2018-09-10 2019-03-15 清华大学 一种封闭型活性阴离子彩色聚氨酯乳液及其制备方法和用途

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