CN107083228A - 一种单组份透明不黄变聚氨酯密封胶及其制备方法 - Google Patents

一种单组份透明不黄变聚氨酯密封胶及其制备方法 Download PDF

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CN107083228A
CN107083228A CN201710295537.9A CN201710295537A CN107083228A CN 107083228 A CN107083228 A CN 107083228A CN 201710295537 A CN201710295537 A CN 201710295537A CN 107083228 A CN107083228 A CN 107083228A
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张毅
赵朝阳
齐文斌
董雨磊
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Shanghai He Cheng Polymer Science And Technology Ltd
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Abstract

本发明涉及一种单组份透明不黄变聚氨酯密封胶及其制备方法，按重量份数，组分包括：脲基甲酸酯聚氨酯预聚物50‑75；气相硅5‑15；增塑剂20‑40；潜固化剂0.1‑2；催化剂0.1‑0.5。制备：将脲基甲酸酯聚氨酯预聚物中加入增塑剂、气相硅、潜固化剂，在真空条件下搅拌分散2h，并控制温度低于50℃；搅拌完成后，再加入催化剂，再在真空条件下搅拌分散0.5h，即得。本发明密封胶是单组份湿气固化，具有固化时间短、透明度高、无VOC挥发成分、不易产生气泡、粘结强度高、适合粘接玻璃、透明塑料；亦可用于灯饰、灯具的粘结和密封。

Description

一种单组份透明不黄变聚氨酯密封胶及其制备方法
技术领域
本发明属于聚氨酯密封胶及其制备领域，特别涉及一种单组份透明不黄变聚氨酯密封胶及其制备方法。
背景技术
聚氨酯密封胶在汽车工业、建筑、装修都有大量应用，目前聚氨酯密封胶按照组份分为单组份和双组份，按照成分分为聚氨酯、改性聚氨酯密封胶(一般是硅酮改性、环氧改性、硫醇改性等)。其中单组份密封胶由于使用方便，无VOC挥发，粘结材料种类多，弹性好，收缩率低受到市场和施工人员青睐。
但是普通单组份聚氨酯密封胶存在易黄变、透明度差等缺点，也有厂家根据普通聚氨酯密封胶的配方调整用不黄变异氰酸酯生产聚氨酯密封胶又存在固化时间长、容易发泡、粘结强度差等缺点。
该发明利用聚醚胺及小分子扩链剂搭配不黄变异氰酸酯生产聚氨酯密封胶从配方上引入活性高的聚醚胺和小分子扩链剂，既增加了固化速度也增加了粘结强度，同时反应生成脲基甲酸酯又具有较高机械强度和任性，产品透明度和抗黄变性能也更高。
该发明适合粘接玻璃、透明塑料；亦可用于灯饰、灯具的粘结和密封。
发明内容
本发明所要解决的技术问题是提供一种单组份透明不黄变聚氨酯密封胶及其制备方法，本发明为了改善上述说明中提到的现有传统密封胶的不足，本发明在异氰酸酯，多元醇多元胺以及其他填料方面进行了优选与改良，并提供了一种单组份不黄变聚氨酯密封胶的合成方法。
本发明的一种单组份透明不黄变聚氨酯密封胶，按重量份数，组分包括：
按重量份数，所述脲基甲酸酯聚氨酯预聚物原料组分包括：
端氨基聚氧化丙烯醚 50-90份；
脂肪族二醇或二胺混合物 10-50份；
异氰酸酯 30-50份。
所述脲基甲酸酯聚氨酯预聚物是由不黄变异氰酸酯与端氨基聚氧化丙烯醚、脂肪族二醇或二胺中的一种或多种聚合而成。
所述异氰酸酯为异氰酸酯为4，4-二苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二环乙基甲烷二异氰酸酯苯二亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯、甲基环己基二异氰酸酯中的一种或几种；端氨基聚氧化丙烯醚是分子量Mn＝230～5000，官能度为2的聚醚胺中的一种或几种。
所述脂肪族二醇为乙二醇、丙二醇、丁二醇、戊二醇、新戊二醇、甲基丙二醇、己二醇、一缩二乙二醇、二缩三乙二醇中的一种或几种；脂肪族二胺为六亚甲基二胺、异佛尔酮二胺、三甲基己二胺、二甲基二氨基二环己基甲烷中的一种或几种。
所述气相硅为气相二氧化硅；增塑剂为邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、己二酸二辛酯、己二酸二丁酯、环己烷1，2-二甲酸二异壬基酯、苯甲酸二醇酯、磷酸三苯酯中的一种或几种。
所述潜固化剂为ALT-101、ALT-102、ALT-201、ALT-401、ALT-402、ALT-403中的一种或几种；催化剂为三亚乙基二胺、双(二甲氨基乙基)醚、二月桂酸二丁基锡、辛酸亚锡、异辛酸锌、异辛酸铋中的一种或几种。
本发明的一种单组份透明不黄变聚氨酯密封胶的制备方法，包括：
(1)将脲基甲酸酯聚氨酯预聚物中加入增塑剂、气相硅、潜固化剂，在真空条件下搅拌分散2h，并控制温度低于50℃；
(2)搅拌完成后，再加入催化剂，再在真空条件下搅拌分散0.5h，即得单组份透明不黄变聚氨酯密封胶。
所述脲基甲酸酯聚氨酯预聚物的制备具体为：将端氨基聚氧化丙烯醚、脂肪族二醇或二胺混合物进行混合均匀后备用，称取不黄变异氰酸酯，置于反应容器中，将混合完成的聚醚胺与脂肪族二醇或二胺缓慢滴加到不黄变异氰酸酯中，并持续搅拌，内部通入N2保护，外部用冰水降温，保持内部反应温度不高于50℃，滴加完成后继续搅拌反应0.5～2h，反应完成后测试NCO含量，NCO含量合格后即得脲基甲酸酯预聚物。
所述NCO含量合格为NCO含量为2-10％。
有益效果
(1)本发明在异氰酸酯，多元醇多元胺以及其他填料方面进行了优选与改良，并提供了一种单组份不黄变聚氨酯密封胶的合成方法，改善了现有传统密封胶的不足；
(2)本发明的密封胶是单组份湿气固化，具有固化时间短、透明度高、无VOC挥发成分、不易产生气泡、粘结强度高、适合粘接玻璃、透明塑料；亦可用于灯饰、灯具的粘结和密封。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
取581.2gHMDI置于反应容器中，加热至完全澄清透明后，冷却至室温；
取366.5g聚醚胺D230与二氨基二环己基甲烷(PACM)混合后搅拌均匀；
向反应容器中通入N2，并将反应容器置于冰水中，将混合好的D230与PACM缓慢滴加到HMDI中，并持续真空搅拌；
控制反应温度于40-50℃，滴加完成后，保温2h；
保温完成后，对产物进行NCO检测，测得实际NCO为3％；
取反应完成聚脲基甲酸酯预聚物650g置于反应容器中；
向反应容器内加入气相二氧化硅100g，邻苯二甲酸二甲基乙二醇酯(DMEP)250g，潜固化剂ALT-401 2g，在真空条件下开始搅拌，控制温度40-50℃；
搅拌2h后，向反应容器内加入催化剂三亚乙基二胺0.2g，再次搅拌0.5h；
搅拌完成后，即制得单组份不黄变聚氨酯密封胶样品1。
实施例2
取436.9gIPDI置于反应容器中，加热至完全澄清透明后，冷却至室温；
取242.7g聚醚胺D400与异佛尔酮二胺(IPDA)混合后搅拌均匀；
向反应容器中通入N2，并将反应容器置于冰水中，将混合好的D400与IPDA缓慢滴加到IPDI中，并持续真空搅拌；
控制反应温度于40-50℃，滴加完成后，保温2h；
保温完成后，对产物进行NCO检测，测得实际NCO为3.5％；
取反应完成聚脲基甲酸酯预聚物550g置于反应容器中；
向反应容器内加入气相二氧化硅100g，邻苯二甲酸二甲基乙二醇酯(DMEP)350g，潜固化剂ALT-101 1g，在真空条件下开始搅拌，控制温度40-50℃；
搅拌2h后，向反应容器内加入催化剂三亚乙基二胺0.5g，再次搅拌0.5h；
搅拌完成后，即制得单组份不黄变聚氨酯密封胶样品2。
测试结果如下表所示：
产品型号 样品1 样品2
产品外观 无色透明 无色透明
表干时间/min 12 10
制品外观 无色透明 无色透明
制品外观/90天日光照射 无色透明 无色透明
制品硬度/邵A 46 50
抗拉强度/Mpa 8.2 7.6
抗拉伸长率/％ 623 597
撕裂强度/N/mm 32 36
粘接强度/Mpa 7.5 7.1
本发明所涉及部分测试标准如下：
GB/T 12009.4-2016塑料聚氨酯生产用芳香族异氰酸酯第4部分：异氰酸根含量的测定
GB/T 528-2009硫化橡胶或热塑性橡胶拉伸应力应变性能的测定
GB/T 529-2008硫化橡胶或热塑性橡胶撕裂强度的测定
GB/T 531-2008硫化橡胶或热塑性橡胶压入硬度试验方法
GB/T 13936-1992硫化橡胶与金属粘接拉伸剪切强度测定方法

Claims (10)

1.一种单组份透明不黄变聚氨酯密封胶，其特征在于：按重量份数，组分包括：
2.根据权利要求1所述的一种单组份透明不黄变聚氨酯密封胶，其特征在于：按重量份数，所述脲基甲酸酯聚氨酯预聚物原料组分包括：
端氨基聚氧化丙烯醚 50-90份；
脂肪族二醇或二胺混合物 10-50份；
异氰酸酯 30-50份。
3.根据权利要求1所述的一种单组份透明不黄变聚氨酯密封胶，其特征在于：所述脲基甲酸酯聚氨酯预聚物是由不黄变异氰酸酯与端氨基聚氧化丙烯醚、脂肪族二醇或二胺中的一种或多种聚合而成。
4.根据权利要求2所述的一种单组份透明不黄变聚氨酯密封胶，其特征在于：所述异氰酸酯为异氰酸酯为4，4-二苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二环乙基甲烷二异氰酸酯苯二亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯、甲基环己基二异氰酸酯中的一种或几种；端氨基聚氧化丙烯醚是分子量Mn＝230～5000，官能度为2的聚醚胺中的一种或几种。
5.根据权利要求2所述的一种单组份透明不黄变聚氨酯密封胶，其特征在于：所述脂肪族二醇为乙二醇、丙二醇、丁二醇、戊二醇、新戊二醇、甲基丙二醇、己二醇、一缩二乙二醇、二缩三乙二醇中的一种或几种；脂肪族二胺为六亚甲基二胺、异佛尔酮二胺、三甲基己二胺、二甲基二氨基二环己基甲烷中的一种或几种。
6.根据权利要求1所述的一种单组份透明不黄变聚氨酯密封胶，其特征在于：所述气相硅为气相二氧化硅；增塑剂为邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、己二酸二辛酯、己二酸二丁酯、环己烷1，2-二甲酸二异壬基酯、苯甲酸二醇酯、磷酸三苯酯中的一种或几种。
7.根据权利要求1所述的一种单组份透明不黄变聚氨酯密封胶，其特征在于：所述潜固化剂为ALT-101、ALT-102、ALT-201、ALT-401、ALT-402、ALT-403中的一种或几种；催化剂为三亚乙基二胺、双(二甲氨基乙基)醚、二月桂酸二丁基锡、辛酸亚锡、异辛酸锌、异辛酸铋中的一种或几种。
8.一种如权利要求1所述的一种单组份透明不黄变聚氨酯密封胶的制备方法，包括：
(1)将脲基甲酸酯聚氨酯预聚物中加入增塑剂、气相硅、潜固化剂，在真空条件下搅拌分散0.5～2h，并控制温度低于50℃；
(2)搅拌完成后，再加入催化剂，再在真空条件下搅拌分散0.5～2h，即得单组份透明不黄变聚氨酯密封胶。
9.根据权利要求8所述的一种单组份透明不黄变聚氨酯密封胶的制备方法，其特征在于：所述脲基甲酸酯聚氨酯预聚物的制备具体为：将端氨基聚氧化丙烯醚、脂肪族二醇或二胺混合物进行混合均匀后，滴加到不黄变异氰酸酯中，并持续搅拌，内部通入N2保护，外部用冰水降温，保持内部反应温度不高于50℃，滴加完成后继续搅拌反应0.5～2h，反应完成后测试NCO含量，NCO含量合格后即得脲基甲酸酯预聚物。
10.根据权利要求9所述的一种单组份透明不黄变聚氨酯密封胶的制备方法，其特征在于：所述NCO含量合格为NCO含量为2～10％。
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