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

二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法 Download PDF

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CN106543408A
CN106543408A CN201611139190.0A CN201611139190A CN106543408A CN 106543408 A CN106543408 A CN 106543408A CN 201611139190 A CN201611139190 A CN 201611139190A CN 106543408 A CN106543408 A CN 106543408A
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王耀斌
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Shaanxi Gaoxin Industry Co Ltd
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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

二环己基甲烷二异氰酸酯型水性聚氨酯胶膜的制备方法
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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CN114395320A (zh) * 2021-12-31 2022-04-26 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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114395320A (zh) * 2021-12-31 2022-04-26 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
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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