CN106543408A - 二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法 - Google Patents
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Abstract
本发明二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,涉及聚氨酯工业领域,具体涉及二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,包括以下步骤:在装有搅拌器、回流冷凝管、热电偶的500mL四口烧瓶中,加入二环己基甲烷二异氰酸酯、聚醚或聚酯多元醇及催化剂二丁基锡二月桂酸,并在80度下反应约1 h,测定NCO含量,当达到质量分数9.43%,预聚反应结束;将预聚物降温至70度,加入溶解于N‑甲基吡咯烷酮的二羟甲基丙酸、1,4‑丁二醇及丙酮,进行扩链反应,当NCO质量分数达到2.30%,扩链反应结束,本发明操作简单,方便加工,且能保证产品质量,提高产品性能,节约成本,降低能耗。
Description
技术领域
本发明涉及聚氨酯工业领域,具体涉及二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法。
背景技术
二环己基甲烷二异氰酸酯由于分子结构不含苯环,故生产的制品不易氧化变色,常用于制备浇注型弹性体和其它具有良好弹性、光学透明性和光稳定性的涂料⋯。水性聚氨酯(WPU)涂料由于具有不易燃、无毒、环境友好等优点,近年来备受关注。将二环己基甲烷二异氰酸酯用于制备WPU涂料,其产品除具有上述优点外,还有优良的力学性能、化学稳定性和耐候性。但鲜有关于二环己基甲烷二异氰酸酯型WPU胶膜的报道。
发明内容
本发明目的在于提供一种操作简单,方便加工,且能保证产品质量,提高产品性能,节约成本,降低能耗的二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法。
本发明二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,包括以下步骤:
第一步,在装有搅拌器、回流冷凝管、热电偶的500mL四口烧瓶中,加入二环己基甲烷二异氰酸酯、聚醚或聚酯多元醇及催化剂二丁基锡二月桂酸,并在80度下反应约1 h,测定NCO含量,当达到质量分数9.43%,预聚反应结束;
第二步,将预聚物降温至70度,加入溶解于N-甲基吡咯烷酮的二羟甲基丙酸、1,4-丁二醇及丙酮,进行扩链反应,当NCO质量分数达到2.30%,扩链反应结束, 将上述反应物降温至40度,加入三乙胺中和0.5h降至室温,用去离子水乳化后加入乙二胺,最后在10000 r/min条件下高速搅拌,将乳液置于水平的玻璃板自然干燥24 h,70度烘箱干燥4 h,得到二环己基甲烷二异氰酸酯型水性聚氨酯胶膜。
优选地,第二步中二羟甲基丙酸与1,4-丁二醇及丙酮投料方式为分步投料,即扩链过程中先加入二羟甲基丙酸,待其反应完全后加入1,4-丁二醇及丙酮。
优选地,第二步中二羟甲基丙酸与1,4-丁二醇及丙酮投料方式为一步投料,即扩链过程中直接加入二羟甲基丙酸与1,4-丁二醇及丙酮的混合物,同时参与扩链反应。
本发明操作简单,方便加工,且能保证产品质量,提高产品性能,节约成本,降低能耗。
具体实施方式
实施例一:
本发明二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,包括以下步骤:
第一步,在装有搅拌器、回流冷凝管、热电偶的500mL四口烧瓶中,加入二环己基甲烷二异氰酸酯、聚醚或聚酯多元醇及催化剂二丁基锡二月桂酸,并在80度下反应约1 h,测定NCO含量,当达到质量分数9.43%,预聚反应结束;
第二步,将预聚物降温至70度,加入溶解于N-甲基吡咯烷酮的二羟甲基丙酸、1,4-丁二醇及丙酮,进行扩链反应,当NCO质量分数达到2.30%,扩链反应结束, 将上述反应物降温至40度,加入三乙胺中和0.5h降至室温,用去离子水乳化后加入乙二胺,最后在10000 r/min条件下高速搅拌,将乳液置于水平的玻璃板自然干燥24 h,70度烘箱干燥4 h,得到二环己基甲烷二异氰酸酯型水性聚氨酯胶膜。
实施例二:
本发明二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,包括以下步骤:
第一步,在装有搅拌器、回流冷凝管、热电偶的500mL四口烧瓶中,加入二环己基甲烷二异氰酸酯、聚醚或聚酯多元醇及催化剂二丁基锡二月桂酸,并在80度下反应约1 h,测定NCO含量,当达到质量分数9.43%,预聚反应结束;
第二步,将预聚物降温至70度,加入溶解于N-甲基吡咯烷酮的二羟甲基丙酸、1,4-丁二醇及丙酮,进行扩链反应,当NCO质量分数达到2.30%,扩链反应结束, 将上述反应物降温至40度,加入三乙胺中和0.5h降至室温,用去离子水乳化后加入乙二胺,最后在10000 r/min条件下高速搅拌,将乳液置于水平的玻璃板自然干燥24 h,70度烘箱干燥4 h,得到二环己基甲烷二异氰酸酯型水性聚氨酯胶膜。
第二步中二羟甲基丙酸与1,4-丁二醇及丙酮投料方式为分步投料,即扩链过程中先加入二羟甲基丙酸,待其反应完全后加入1,4-丁二醇及丙酮。
实施例三:
本发明二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,包括以下步骤:
第一步,在装有搅拌器、回流冷凝管、热电偶的500mL四口烧瓶中,加入二环己基甲烷二异氰酸酯、聚醚或聚酯多元醇及催化剂二丁基锡二月桂酸,并在80度下反应约1 h,测定NCO含量,当达到质量分数9.43%,预聚反应结束;
第二步,将预聚物降温至70度,加入溶解于N-甲基吡咯烷酮的二羟甲基丙酸、1,4-丁二醇及丙酮,进行扩链反应,当NCO质量分数达到2.30%,扩链反应结束, 将上述反应物降温至40度,加入三乙胺中和0.5h降至室温,用去离子水乳化后加入乙二胺,最后在10000 r/min条件下高速搅拌,将乳液置于水平的玻璃板自然干燥24 h,70度烘箱干燥4 h,得到二环己基甲烷二异氰酸酯型水性聚氨酯胶膜。
第二步中二羟甲基丙酸与1,4-丁二醇及丙酮投料方式为一步投料,即扩链过程中直接加入二羟甲基丙酸与1,4-丁二醇及丙酮的混合物,同时参与扩链反应。
本发明操作简单,方便加工,且能保证产品质量,提高产品性能,节约成本,降低能耗。
Claims (3)
1.一种二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,其特征在于,包括以下步骤:
第一步,在装有搅拌器、回流冷凝管、热电偶的500mL四口烧瓶中,加入二环己基甲烷二异氰酸酯、聚醚或聚酯多元醇及催化剂二丁基锡二月桂酸,并在80度下反应约1 h,测定NCO含量,当达到质量分数9.43%,预聚反应结束;
第二步,将预聚物降温至70度,加入溶解于N-甲基吡咯烷酮的二羟甲基丙酸、1,4-丁二醇及丙酮,进行扩链反应,当NCO质量分数达到2.30%,扩链反应结束, 将上述反应物降温至40度,加入三乙胺中和0.5h降至室温,用去离子水乳化后加入乙二胺,最后在10000 r/min条件下高速搅拌,将乳液置于水平的玻璃板自然干燥24 h,70度烘箱干燥4 h,得到二环己基甲烷二异氰酸酯型水性聚氨酯胶膜。
2.如权利要求1所述二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,其特征在于,第二步中二羟甲基丙酸与1,4-丁二醇及丙酮投料方式为分步投料,即扩链过程中先加入二羟甲基丙酸,待其反应完全后加入1,4-丁二醇及丙酮。
3.如权利要求1所述二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法,其特征在于,第二步中二羟甲基丙酸与1,4-丁二醇及丙酮投料方式为一步投料,即扩链过程中直接加入二羟甲基丙酸与1,4-丁二醇及丙酮的混合物,同时参与扩链反应。
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CN114395320B (zh) * | 2021-12-31 | 2023-02-17 | 唐山东方雨虹防水技术有限责任公司 | 一种化学抗流挂外露型单组分聚氨酯防水涂料及制备方法 |
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