CN114958285B - 低温活化单组份聚氨酯密封胶及其制备方法 - Google Patents
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Abstract
本发明公开一种低温活化单组份聚氨酯密封胶，低温活化单组份聚氨酯密封胶，其特征在于：包括如下组分进行反应制备：多元醇为20%‑45%、封闭型异氰酸酯预聚体为10%‑25%、溶剂为3%‑10%、填料为20%‑50%、颜料为2%‑10%、触变剂为1%‑3%、稳定剂为0.2%‑6%、促进剂为0.1%‑2%。此款低温活化单组份聚氨酯密封胶施工操作更方便，品质更稳定，更适合复杂环境的施工，其低温90℃活化、快速固化、耐温190℃黄变、耐气候老化性能好、耐湿热、耐水解良好。
Description
技术领域
本发明涉及一种密封胶，特别是一种低温活化单组份聚氨酯密封胶及其制备方法。
背景技术
目前的聚氨酯密封胶多为双组份结合使用，虽然，其具有优异的耐气候、耐湿气老化、耐酸碱性能，可制成坚硬、色泽稳定、抗冲击、耐磨的保护涂层，但是，使用的时候需要现场将AB组份混合，施工操作不方便。
在户外照明、LED灯饰行业中，对密封、粘接、组装的要求较高，特别是大功率、户外照明，需要耐高温、高湿、耐紫外线气候老化的场景；同时，由于户外作业需要施工方便，所以，需要研发一种新型的密封胶，以适合户外照明、LED灯饰行业的施工需要。
发明内容
本发明的目的在于提供一种制作简单、快速固化、耐高温变黄、耐气候老化等的低温活化单组份聚氨酯密封胶及其制备方法。
本发明的目的是这样实现的：
一种低温活化单组份聚氨酯密封胶，其特征在于：包括如下组分进行反应制备：多元醇为20％-45％、封闭型异氰酸酯预聚体为10％-25％、溶剂为3％-10％、填料为20％-50％、颜料为2％-10％、触变剂为1％-3％、稳定剂为0.2％-6％、促进剂为0.1％-2％。
本发明的目的还可以采用以下技术措施解决：
作为更具体的方案，多元醇包括聚己二酸3-甲基戊二醇酯二醇和端羟基聚丁二烯，聚己二酸3-甲基戊二醇酯二醇为15％-30％，端羟基聚丁二烯为5％-15％。端羟基聚丁二烯是通过链延长和交联固化反应，可将其制成有三维网络结构的弹性体，该固化物具有优异的力学性能，特别具有耐水解，耐酸碱，耐磨，耐低温和优异电绝缘性。
作为进一步的方案，溶剂为邻苯二甲酸二异癸酯，填料为纳米碳酸钙，颜料为二氧化钛，触变剂为气相二氧化硅，稳定剂为氧化钙和/或分子筛，促进剂为辛酸亚锡。
邻苯二甲酸二异癸酯(DIDP)，是邻苯二甲酸酯(即邻苯二甲酸盐)的一个品种，常温下为液体，工业上常用于树脂或塑料增塑剂(塑化剂)，特别是耐热或绝缘要求高的制品，从而提升密封胶的耐温及绝缘性能，尤其适合LED灯饰及户外照明场合的使用。
纳米碳酸钙又称超微细碳酸钙、超细碳酸钙。纳米碳酸钙可改善塑料母料的流变性，提高其成型性。用作塑料填料具有增韧补强的作用，提高塑料的弯曲强度和弯曲弹性模量，热变形温度和尺寸稳定性，同时还赋予塑料滞热性。采用纳米碳酸钙的粒度更小，与其它配料混合更加均匀，不易粉化。
二氧化钛(钛白)是一种性能较好的白色颜料，钛白的粘附力强，不易起化学变化，永远是雪白的。它的熔点很高，耐高温性能强。同时，二氧化钛有较好的紫外线掩蔽作用。采用二氧化钛作为颜料，不易变黄。
气相法二氧化硅是一种无定形二氧化硅产品，表面未处理的气相二氧化硅聚集体是含有多种硅羟基。一是孤立的、未受干扰的自由羟基；二是连生、彼此形成氢键的键合硅羟基。表面未处理的气相法白炭黑聚集体是含有多个-OH的集合体，它们在液体体系中极易形成均匀的三维网状结构(氢键)。
氧化钙是一种无机化合物，化学式是CaO。物理性质是表面白色粉末，具有吸湿性，可以去除体系里的水份。
分子筛在结构上有许多孔径均匀的孔道和排列整齐的孔穴，不同孔径的分子筛把不同大小和形状分子分开。它的吸附能力高、选择性强、耐高温。
作为进一步的方案，聚己二酸3-甲基戊二醇酯二醇和端羟基聚丁二烯的分子量均为3000g/mol；其中，聚己二酸3-甲基戊二醇酯二醇为30％、端羟基聚丁二烯为9％、封闭型异氰酸酯预聚体为16％、邻苯二甲酸二异癸酯为7％、二氧化钛为8％、气相二氧化硅为2.3％、氧化钙为4％、分子筛为1.2％、辛酸亚锡为0.7％、余量为纳米碳酸钙。
一种低温活化单组份聚氨酯密封胶的制备方法，首先将多元醇、溶剂、填料、颜料、触变剂分批加入到行星混合反应釜中，混合搅拌30-60min，升温110-120℃，抽真空至-0.1MPa脱水2.5h；然后降温至50℃以下，投入封闭型异氰酸酯预聚体、促进剂、稳定剂，抽真空至-0.1Mpa，搅拌20-30min，降温至40℃，包装出料。
一种封闭型异氰酸酯预聚体的制备方法,将摩尔比1:1异佛尔酮二异氰酸酯与马来酰亚胺在70-80℃反应得到部分封闭的中间产物；该部分封闭的IPDI低聚物与等量的聚碳酸酯二醇在100-130℃反应，得到封闭型异氰酸酯预聚体。
本发明的有益效果如下：
(1)此款低温活化单组份聚氨酯密封胶施工操作更方便，品质更稳定，更适合复杂环境的施工，其低温90℃活化、快速固化、耐温190℃黄变、耐气候老化性能好、耐湿热、耐水解良好。
(2)此款低温活化单组份聚氨酯密封胶可用于LED灯饰、照明行业密封、粘接、组装，特别是大功率、户外照明，需要耐高温、高湿、耐紫外线气候老化的场景。
(3)此款低温活化单组份聚氨酯密封胶的制作工艺简单。
具体实施方式
下面结合实施例对本发明作进一步描述：
一种低温活化单组份聚氨酯密封胶，包括如下组分进行反应制备：多元醇为20％-45％、封闭型异氰酸酯预聚体为10％-25％、溶剂为3％-10％、填料为20％-50％、颜料为2％-10％、触变剂为1％-3％、稳定剂为0.2％-6％、促进剂为0.1％-2％。
其中，多元醇包括聚己二酸3-甲基戊二醇酯二醇和端羟基聚丁二烯，聚己二酸3-甲基戊二醇酯二醇为15％-30％，端羟基聚丁二烯为5％-15％。溶剂为邻苯二甲酸二异癸酯，填料为纳米碳酸钙，颜料为二氧化钛，触变剂为气相二氧化硅，稳定剂为氧化钙和/或分子筛，促进剂为辛酸亚锡。
实施例1：聚己二酸3-甲基戊二醇酯二醇和端羟基聚丁二烯的分子量均为3000g/mol；其中，聚己二酸3-甲基戊二醇酯二醇为30％、端羟基聚丁二烯为9％、封闭型异氰酸酯预聚体为16％、邻苯二甲酸二异癸酯为7％、二氧化钛为8％、气相二氧化硅为2.3％、氧化钙为4％、分子筛为1.2％、辛酸亚锡为0.7％、余量为纳米碳酸钙(21.8％)。
一种封闭型异氰酸酯预聚体的制备方法,将摩尔比1:1异佛尔酮二异氰酸酯与马来酰亚胺在70-80℃反应得到部分封闭的中间产物；该部分封闭的IPDI低聚物与等量的聚碳酸酯二醇在100-130℃反应，得到封闭型异氰酸酯预聚体。
其中，封闭型异氰酸酯的封闭与解封反应式:
一种低温活化单组份聚氨酯密封胶的制备方法，首先将多元醇、溶剂、填料、颜料、触变剂分批加入到行星混合反应釜中，混合搅拌30-60min，升温110-120℃，抽真空至-0.1MPa脱水2.5h；然后降温至50℃以下，投入封闭型异氰酸酯预聚体、促进剂、稳定剂，抽真空至-0.1Mpa，搅拌20-30min，降温至40℃，包装出料。
比较例：聚氧化丙烯二醇(分子量2000)27％、聚己二酸乙二醇酯二醇(分子量2000)12％、BL1100封闭型异氰酸酯(科思创)16％、邻苯二甲酸二异癸酯7％、纳米碳酸钙21.8％、二氧化钛8％、气相二氧化硅2.3％、氧化钙4％、分子筛1.2％、辛酸亚锡0.7。
通过将实施例1和比较例做项目测试，具体情况如下表所示：
由此可见，实施例1固化速度明显较快，耐温190℃黄变、耐湿热、耐水解良好、耐气候老化性能好。
上述为本发明的优选方案，显示和描述了本发明的基本原理、主要特征和本发明的优点。本领域的技术人员应该了解本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内，本发明要求保护范围由所附的权利要求书及其等同物界定。
Claims (3)
1.一种低温活化单组份聚氨酯密封胶，其特征在于：包括如下组分进行反应制备：多元醇为20%-45%、封闭型异氰酸酯预聚体为10%-25%、溶剂为3%-10%、填料为20%-50%、颜料为2%-10%、触变剂为1%-3%、稳定剂为0.2%-6%、促进剂为0.1%-2%；
多元醇包括聚己二酸3-甲基戊二醇酯二醇和端羟基聚丁二烯，聚己二酸3-甲基戊二醇酯二醇为15%-30%，端羟基聚丁二烯为5%-15%；
溶剂为邻苯二甲酸二异癸酯，填料为纳米碳酸钙，颜料为二氧化钛，触变剂为气相二氧化硅，稳定剂为氧化钙和/或分子筛，促进剂为辛酸亚锡；
聚己二酸3-甲基戊二醇酯二醇和端羟基聚丁二烯的分子量均为3000g/mol；
封闭型异氰酸酯预聚体的制备：将摩尔比1:1 异佛尔酮二异氰酸酯与马来酰亚胺在70-80℃反应得到部分封闭的中间产物；该部分封闭的IPDI低聚物与等量的聚碳酸酯二醇在100-130℃反应，得到封闭型异氰酸酯预聚体。
2.根据权利要求1所述的低温活化单组份聚氨酯密封胶，其特征在于：聚己二酸3-甲基戊二醇酯二醇为30%、端羟基聚丁二烯为9%、封闭型异氰酸酯预聚体为16%、邻苯二甲酸二异癸酯为7%、二氧化钛为8%、气相二氧化硅为2.3%、氧化钙为4%、分子筛为1.2%、辛酸亚锡为0.7%、余量为纳米碳酸钙。
3.一种根据权利要求1所述低温活化单组份聚氨酯密封胶的制备方法，其特征是：首先将多元醇、溶剂、填料、颜料、触变剂分批加入到行星混合反应釜中，混合搅拌30-60min，升温110-120℃，抽真空至-0.1 MPa脱水2.5h；然后降温至50℃以下，投入封闭型异氰酸酯预聚体、促进剂、稳定剂，抽真空至-0.1 Mpa，搅拌20-30 min，降温至40℃，包装出料。
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