CN105732944A - 一种透明聚氨酯的制备方法 - Google Patents

一种透明聚氨酯的制备方法 Download PDF

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CN105732944A
CN105732944A CN201610239745.2A CN201610239745A CN105732944A CN 105732944 A CN105732944 A CN 105732944A CN 201610239745 A CN201610239745 A CN 201610239745A CN 105732944 A CN105732944 A CN 105732944A
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陈瑶
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WENZHOU DENGDA CHEMICAL CO Ltd
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Abstract

本发明涉及化工领域，特别涉及一种透明聚氨酯的制备方法。将聚己二酸丁二醇酯、对甲苯磺酸、脂肪族二胺与碳酸丙烯酯为原料制备反应，加入二月桂酸二丁基锡及三羟甲基丙烷(TMP)交联改性聚氨酯预聚体，降温至40℃，加入三乙胺中和，反应3min；加入水强力搅拌乳化1h，得到透明聚氨酯，本发明提供了一种透明聚氨酯的制备方法，得到的聚氨酯具有优异的高透明性、粘结性和耐黄变性。

Description

一种透明聚氨酯的制备方法
技术领域
本发明涉及化工领域，特别涉及一种透明聚氨酯的制备方法。
背景技术
在高透明复合材料中，基材之间的粘结是制备这类复合材料的关键，不仅要求粘结剂具有优良的光学透明性，同时要求抗剥离强度高，具有耐黄变性能，因此技术要求较高，聚氨酯胶黏剂是一类用途广泛、性能优良的胶黏剂。近年来基于产业政策的导向及对环境保护的要求，水性聚氨酯因其不燃、无毒以及好的粘合性、成膜性、机械性能优良成为聚氨酯领域的研究方向，其应用也越来越广泛，但要求其具有高透明光学性的同时有高的粘结强度是聚氨酯胶黏剂的难点。
发明内容
为了克服背景技术的不足，本发明提供了一种透明聚氨酯的制备方法，得到的聚氨酯具有优异的高透明性、粘结性和耐黄变性。
本发明所提供的一种透明聚氨酯的制备方法，其具体步骤如下：(1)将聚己二酸丁二醇酯(PBA)、对甲苯磺酸、脂肪族二胺H2NCnH2nNH2(n＝2～6)与碳酸丙烯酯为原料制备130℃搅拌反应2-4h；四种反应物摩尔比＝1∶1∶1∶2～12，反应温度80～130℃，反应时间2～12小时，产物为浅黄色粘稠状液体，放置数天后为白色固体，生成含氨基甲酸酯的小分子量二元醇；
(2)将开环产物含氨基甲酸酯的小分子量二元醇与异佛尔酮二异氰酸酯(IPDI)、芳香族聚酯二元醇(PAD)、1，4-丁二醇(BDO)、二羟甲基丙酸(DPMA)为原料制备预聚体，78℃搅拌反应2h，过程中视体系黏度添加N-甲级吡咯烷酮(NMP)；
(3)加入催化剂，催化剂为三乙烯二胺和70％双(二甲氨基乙基)醚溶液，用量为总质量的2～3％，温度75～80℃，预聚1～2小时，放入烘箱，再保温20～24小时；
(4)加入三羟甲基丙烷(TMP)交联改性聚氨酯预聚体，反应1h；
(5)降温至40℃，加入三乙胺中和，反应3min；
(6)加入水强力搅拌乳化1h，得到透明聚氨酯。
步骤(1)中搅拌转速为500r/min。
步骤(2)中NMP的用量以使得搅拌得以顺利进行为准。
步骤(4)中三羟甲基丙烷(TMP)的用量为预聚体质量的2％。
在本发明中，所述的多元醇为聚酯多元醇或聚醚多元醇。
本发明的有益效果是：本专利采用聚己二酸丁二醇酯(PBA)、对甲苯磺酸、脂肪族二胺H2NCnH2nNH2(n＝2～6)与碳酸丙烯酯为原料制备芳香族聚酯多元醇(PAD)，然后以异佛尔酮二异氰酸酯(IPDI)、芳香族聚酯二元醇(PAD)、1，4-丁二醇(BDO)、二羟甲基丙酸(DPMA)为原料制备预聚体，加入催化剂二月桂酸二丁基锡，并采用三羟甲基丙烷(TMP)对预聚体交联扩链，经中和乳化反应制得透明聚氨酯。首先PAD为芳香族聚酯二元醇，主链中含有刚性苯环，分子链的规整化排列受到限制，链段的空间运动受阻，因此制备的聚氨酯透明度高。其次，由于使用IPDI作为多异氰酸酯原料，使得制备的聚氨酯具有优异的耐黄变性能。最后，TMP的使用使得聚氨酯形成网络交联结构，具有优异的粘结性。
具体实施方式
本发明所提供的一种透明聚氨酯的制备方法，具体实施例一：将聚己二酸丁二醇酯(PBA)、对甲苯磺酸、脂肪族二胺H2NCnH2nNH2(n＝2～6)与碳酸丙烯酯为原料放置反应釜中反应3小时，反应时的温度为90℃，得出浅黄色粘稠状液体，将反应出的液体放置3-5天后，液体变为固体，生成含氨基甲酸酯的小分子量二元醇，将含氨基甲酸酯的小分子量二元醇与异佛尔酮二异氰酸酯(IPDI)、芳香族聚酯二元醇(PAD)、1，4-丁二醇(BDO)、二羟甲基丙酸(DPMA)为原料制备预聚体，放置反应釜内反应2h，反应温度为78℃，在反应过程中视体系黏度添加N-甲级吡咯烷酮(NMP)；然后加入催化剂，预聚1.5小时，放入烘箱，再保温22小时，然后加入三羟甲基丙烷(TMP)交联改性聚氨酯预聚体，反应1h，然后降温至40℃，加入三乙胺中和，反应3min；加入水强力搅拌乳化1h，得到透明聚氨酯，采用此方法得出的聚氨酯，聚氨酯胶膜T剥离强度为5.17N/25mm，透光率为85％。
具体实施例二：将聚己二酸丁二醇酯(PBA)、对甲苯磺酸、脂肪族二胺H2NCnH2nNH2(n＝2～6)与碳酸丙烯酯为原料放置反应釜中反应4小时，反应时的温度为90℃，得出浅黄色粘稠状液体，将反应出的液体放置7-10天后，液体变为固体，生成含氨基甲酸酯的小分子量二元醇，将含氨基甲酸酯的小分子量二元醇与异佛尔酮二异氰酸酯(IPDI)、芳香族聚酯二元醇(PAD)、1，4-丁二醇(BDO)、二羟甲基丙酸(DPMA)为原料制备预聚体，放置反应釜内反应2h，反应温度为100℃，在反应过程中视体系黏度添加N-甲级吡咯烷酮(NMP)；然后加入催化剂，预聚2小时，放入烘箱，再保温22小时，然后加入三羟甲基丙烷(TMP)交联改性聚氨酯预聚体，反应1h，然后降温至40℃，加入三乙胺中和，反应2min；得到透明聚氨酯，采用此方法得出的聚氨酯，聚氨酯胶膜T剥离强度为5.35N/25mm，透光率为87％。

Claims (5)

1.一种透明聚氨酯的制备方法，其特征在于：其步骤如下：
(1)将聚己二酸丁二醇酯(PBA)、对甲苯磺酸、脂肪族二胺H2NCnH2nNH2(n＝2～6)与碳酸丙烯酯为原料制备130℃搅拌反应2-4h；四种反应物摩尔比＝1∶1∶1∶2～12，反应温度80～130℃，反应时间2～12小时，生成含氨基甲酸酯的小分子量二元醇；
(2)将含氨基甲酸酯的小分子量二元醇与异佛尔酮二异氰酸酯(IPDI)、芳香族聚酯二元醇(PAD)、1，4-丁二醇(BDO)、二羟甲基丙酸(DPMA)为原料制备预聚体，78℃搅拌反应2h，过程中视体系黏度添加N-甲级吡咯烷酮(NMP)；
(3)加入催化剂，催化剂为三乙烯二胺和70％双(二甲氨基乙基)醚溶液，用量为总质量的2～3％，温度75～80℃，预聚1～2小时，放入烘箱，再保温20～24小时；
(4)加入三羟甲基丙烷(TMP)交联改性聚氨酯预聚体，反应1h；
(5)降温至40℃，加入三乙胺中和，反应3min；
(6)加入水强力搅拌乳化1h，得到透明聚氨酯。
2.根据权利要求1所述的一种透明聚氨酯的制备方法，其特征在于：所述的步骤(1)中搅拌转速为500r/min。
3.根据权利要求1中所述的一种透明聚氨酯的制备方法，其特征在于：所述的步骤(2)中NMP的用量以使得搅拌得以顺利进行为准。
4.根据权利要求1中所述的一种透明聚氨酯的制备方法，其特征在于：所述的步骤(4)中三羟甲基丙烷(TMP)的用量为预聚体质量的2％。
5.根据权利要求1所述的一种透明聚氨酯的制备方法，其特征在于：所述的多元醇为聚酯多元醇或聚醚多元醇。
CN201610239745.2A 2016-04-12 2016-04-12 一种透明聚氨酯的制备方法 Pending CN105732944A (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604526A (zh) * 2012-03-16 2012-07-25 广州有色金属研究院 一种透明聚氨酯涂料组合物及其制备方法
CN102993397A (zh) * 2012-09-13 2013-03-27 太原理工大学 一种制备透明可降解聚氨酯的方法
CN103030771A (zh) * 2012-12-19 2013-04-10 青岛海尔软件有限公司 一种高透明水性聚氨酯乳液制备方法
CN103073876A (zh) * 2013-01-24 2013-05-01 浙江德美博士达高分子材料有限公司 一种芳香族高固含水基聚氨酯的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604526A (zh) * 2012-03-16 2012-07-25 广州有色金属研究院 一种透明聚氨酯涂料组合物及其制备方法
CN102993397A (zh) * 2012-09-13 2013-03-27 太原理工大学 一种制备透明可降解聚氨酯的方法
CN103030771A (zh) * 2012-12-19 2013-04-10 青岛海尔软件有限公司 一种高透明水性聚氨酯乳液制备方法
CN103073876A (zh) * 2013-01-24 2013-05-01 浙江德美博士达高分子材料有限公司 一种芳香族高固含水基聚氨酯的制备方法

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Application publication date: 20160706