CN102424704B - 改性的水分散多异氰酸酯 - Google Patents
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
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- IEDVJHCEMCRBQM-UHFFFAOYSA-N trimethoprim Chemical compound COC1=C(OC)C(OC)=CC(CC=2C(=NC(N)=NC=2)N)=C1 IEDVJHCEMCRBQM-UHFFFAOYSA-N 0.000 abstract 2
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Abstract
本发明公开了一种改性的水分散多异氰酸酯，通过以下步骤制备：a、将TMP和二羟基特戊酸溶于甲基异丁基酮，并加热到40℃，搅拌溶解；b、在反应釜中加入计量的MDI、甲基异丁基酮及复合催化剂，升温至40℃，完全溶解；c、然后缓慢加入步骤a获得的溶液，该添加过程时间为0.5h～5h，并加热到50～90℃下保温反应0.5h～5h；d、然后降低温度到30℃以下，缓慢加入N,N-二甲基乙醇胺进行中和反应，并搅拌0.5h，e、最后加入计量的去离子水，冷却至室温，得到淡黄色透明液体产物。本发明更加环保，对人体健康伤害更小。
Description
技术领域
本发明涉及一种稳定的水性多异氰酸酯及其制备方法。
背景技术
带有NCO端基的预聚体是聚氨酯合成中非常重要的中间体，因为NCO预聚体可用带代各种活波氢的化合的羟基、羧基、氨基等基团反应形成交联结构物而作为交联架桥剂使用，传统的交联剂很难直接乳化或分散于水中，通过引入亲水性基团来改善聚异氰酸酯的亲水性，使其易于在水中乳化或分散，从而保持一定的稳定性。如美国专利No.4,433,095和CN101316874A。
发明内容
本发明的目的在于，提供一种低游离TDI含量，水分散性好的新型架桥剂，该架桥剂存储稳定，热处理性能卓越，适于工业化生产。
为实现上述发明的目的，本发明中新型架桥剂采用以下技术方案制备：一种改性的水分散多异氰酸酯，通过以下步骤制备：
a、将TMP和二羟基特戊酸溶于甲基异丁基酮，并加热到40℃，搅拌溶解；
b、在反应釜中加入计量的MDI、甲基异丁基酮及复合催化剂，升温至40℃，完全溶解；所述复合催化剂由二辛酸锡以及苯胺基亚胺镍复配而成；
c、然后缓慢加入步骤a获得的溶液，该添加过程时间为0.5h～5h，并加热到50～90℃下保温反应0.5h～5h ；
d、然后降低温度到30℃以下，缓慢加入N,N-二甲基乙醇胺进行中和反应，并搅拌0.5h，
e、最后加入计量的去离子水，冷却至室温，得到淡黄色透明液体产物。
MDI与TMP的摩尔配比为1～2:1。
所述TMP与二羟基特戊酸的摩尔比为1:0.2～1。
所述复合催化剂浓度为800～2000ppm。
有益效果：本发明相对于现有技术，具有以下优点：
我们通过实验，在 对MDI-TMP型架桥剂进行改性的基础上，通过引入另一种亲水试剂羟基羧酸化合物，调整各工艺参数，欲寻求一种水分散体型粘合强度增进剂、固色剂、接着剂、颜料耐染摩擦洗涤坚牢度向上剂，对被处理物均有架桥增强之效果，经干燥，热处理就能发挥卓越的性能，并能广泛适用于水性涂料、染料的交联架桥剂由于采用MDI、 TMP等作为原料，使得获得的改性的水分散多异氰酸酯更加环保，对人体健康伤害更小；本发明采用复合催化剂进行预聚反应，可以提高合成效率，降低聚合难度。
具体实施方式
下面结合实施例对本发明做进一步地详细说明，但是本发明要求保护的范围并不局限于实施例表示的范围。
实施例：
在清洁干燥并装有冷凝器的容器中，加入TMP(1.00kmol)，二羟基特戊酸（0.5kmol）及甲基异丁基酮溶剂，配制成75%左右的溶液，升温至40℃-50℃，充分搅拌溶解，待混合物完全溶解后，停止搅拌，体系温度保持40℃-50℃待用。
在清洁干燥的反应釜中，安装冷凝器，真空计量加入MDI（5.5kmol）、甲基异丁基酮及复合催化剂3.00kg，配制成75%左右的溶液，完毕后关好入孔大盖，开动搅拌并慢慢升温至60℃，待其完全溶解，在60℃温度的条件下，慢慢滴加TMP和二羟基特戊酸的混合液，滴加温度控制在60℃-85℃，滴加时间控制在1h-2.5h,滴加结束后，在85℃-95℃反应1.5h,在低于80℃下滴加计量的N,N-二甲基乙醇胺（0.55kmol）进行中和，搅拌0.5h，加入去离子水(687kg)，冷却至室温，得到淡黄色透明分散液体产物,固体含量39.50%，粘度≥1570mPa.s，pH值：约9.0。所述复合催化剂由二辛酸锡以及苯胺基亚胺镍按照摩尔比为2:0.5的比例复配而成。
Claims (2)
1.一种改性的水分散多异氰酸酯，其特征在于：通过以下步骤制备：a、将TMP和二羟基特戊酸溶于甲基异丁基酮，并加热到40℃，搅拌溶解；b、在反应釜中加入计量的MDI、甲基异丁基酮及复合催化剂，升温至40℃，完全溶解；所述复合催化剂由二辛酸锡以及苯胺基亚胺镍复配而成；c、然后缓慢加入步骤a获得的溶液，该添加过程时间为0.5h～5h，并加热到50～90℃下保温反应0.5h～5h；d、然后降低温度到30℃以下，缓慢加入N,N-二甲基乙醇胺进行中和反应，并搅拌0.5h，e、最后加入计量的去离子水，冷却至室温，得到淡黄色透明液体产物；MDI与TMP的摩尔配比为1～2:1；所述TMP与二羟基特戊酸的摩尔比为1:0.2～1。
2.根据权利要求1所述改性的水分散多异氰酸酯，其特征在于：复合催化剂浓度为800～2000ppm。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4801644A (en) * | 1985-10-04 | 1989-01-31 | Polyvinyl Chemicals Inc. | Coating compositions |
| CN1611522A (zh) * | 2003-10-29 | 2005-05-04 | 深圳彩虹环保建材科技有限公司 | 水性聚氨酯的制备方法 |
| CN101456942A (zh) * | 2008-12-30 | 2009-06-17 | 南京工业大学 | 一种水性聚氨酯和含水性聚氨酯胶粘剂及其应用 |
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| WO2010095665A1 (ja) * | 2009-02-18 | 2010-08-26 | 東ソー株式会社 | 水性ポリウレタン樹脂組成物およびこれを用いたフィルム成型体 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4801644A (en) * | 1985-10-04 | 1989-01-31 | Polyvinyl Chemicals Inc. | Coating compositions |
| CN1611522A (zh) * | 2003-10-29 | 2005-05-04 | 深圳彩虹环保建材科技有限公司 | 水性聚氨酯的制备方法 |
| CN101456942A (zh) * | 2008-12-30 | 2009-06-17 | 南京工业大学 | 一种水性聚氨酯和含水性聚氨酯胶粘剂及其应用 |
Non-Patent Citations (2)
| Title |
|---|
| MDI基水性聚氨酯胶粘剂的合成与性能研究;刘都宝等;《印染助剂》;20081031;第25卷(第10期);25-27 * |
| 刘都宝等.MDI基水性聚氨酯胶粘剂的合成与性能研究.《印染助剂》.2008,第25卷(第10期),25-27. |
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