CN111978905A - 一种建筑用快速固化硅烷改性聚醚密封胶及其制备方法 - Google Patents
一种建筑用快速固化硅烷改性聚醚密封胶及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种建筑用快速固化硅烷改性聚醚密封胶及其制备方法。按重量份计算,由硅烷改性聚醚30~50重量份、无机填料25~45重量份、增塑剂5~25重量份、硅烷偶联剂0.5~2重量份混合而成。采用端烯基聚醚与氨基硅烷,通过迈克尔加成反应成功制备出硅烷封端聚醚。该合成路线的反应条件温和、工艺简便、不需要催化剂、无副产物。以该硅烷封端聚醚为基础,复配交联型硅烷偶联剂,可获得优异的粘接性能。通过调控各组分比例,可制备出综合性能优异的MS密封胶。该产品分子链中不含氨基甲酸酯键,通过Si‑O‑Si键交联,能够综合聚氨酯密封胶和硅酮胶的优点。
Description
技术领域
本发明涉及一种建筑用快速固化硅烷改性聚醚密封胶及其制备方法,属于密封胶技术领域。
背景技术
硅烷改性聚醚密封胶(MS密封胶)兼具聚氨酯密封胶和硅酮密封胶的优点,具有优良的力学强度、施工性、抗污性、粘接性,原料和生产环节中不含游离异氰酸酯和有机溶剂,具有优异的环保性,符合当今新型弹性密封材料的发展趋势。
日本钟渊化学在20世纪70年代成功开发出MS密封胶至今已40多年,中国国内的MS密封胶市场占有率却非常低,其根本原因是其上游原料硅烷封端聚醚受限,一方面硅烷封端聚醚合成技术难度高且受知识产权保护限制,另一方面是产业化投入大、市占率低导致推广难度大。MS聚醚的一般合成路线是将高分子量的聚醚与烯丙基氯在碱催化剂存在下进行威廉姆森反应,得到烯丙基封端聚醚,然后用Pt或氯铂酸作催化剂,与二甲氧基甲基硅烷反应封端得到MS聚醚。日本钟渊化学、瑞士瓦克和美国陶氏化学分别用于各自独特的技术路线和商业化产品,而国内尚无真正意义上商业化的硅烷封端聚醚,国内密封胶厂商通常采用上述三家原料生产MS密封胶,或是利用硅烷化聚醚型聚氨酯来生产SPU密封胶,其本质仍然是聚氨酯。
由此可见,MS密封胶的关键是端烯基聚醚和硅烷封端聚醚的合成路线。华普密封材料有限公司独立开发出新的合成路线,即用端烯基聚醚与氨基硅烷通过迈克尔加成反应,在温和的反应条件下成功制备出硅烷封端聚醚。利用该聚醚可制备出综合性能优异的MS密封胶。
发明内容
本为解决上述问题,本发明提供一种建筑用快速固化硅烷改性聚醚密封胶及其制备方法。
本发明涉及的建筑用快速固化硅烷改性聚醚密封胶包含以下重量份的成分:
硅烷改性聚醚30~50份;
无机填料25~45份;
增塑剂5~25份
硅烷偶联剂0.5~2份。
优选地,所述硅烷改性聚醚由端烯基聚醚多元醇与氨基硅烷由迈克尔加成反应制得。
优选地,所述硅烷改性聚醚的制备中,端烯基聚醚多元醇官能度2.0~3.0,分子量1000~20000g/mol,聚醚主链和链末端结构式如下:
优选地,所述硅烷改性聚醚的制备中,氨基硅烷为γ-氨丙基三乙氧基硅烷,γ-氨丙基三甲氧基硅烷,N-β(氨乙基)-γ-氨丙基三甲氧基硅烷,N-β(氨乙基)-γ-氨丙基三乙氧基硅烷,N-β(氨乙基)-γ-氨丙基甲基二乙氧基硅烷,苯氨基甲基三乙氧基硅烷,苯氨基甲基三甲氧基硅烷,氨乙基氨乙基氨丙基三甲氧基硅烷中的一种。
优选地,所述无机填料为重质碳酸钙、轻质碳酸钙、纳米碳酸钙、气相二氧化硅、炭黑、钛白粉中的一种或多种混合物。
优选地,所述增塑剂为邻苯二甲酸二辛酯(DOP)、邻苯二甲酸二辛壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)中的一种或多种混合物。
优选地,所述硅烷偶联剂为甲基三乙氧基硅烷、甲基三乙氧基硅烷的一种或两种混合物。
所述硅烷改性聚醚的制备方法如下:控制反应体系端烯基与(氨基+亚氨基)摩尔比为1.0~1.2,按照设定配方往反应器中投入端烯基聚醚多元醇,升温至120℃,控制真空度不大于-0.095MPa,在该条件下除水1~2小时;降温至30~60℃,投入氨基硅烷,氮气保护下搅拌12~36小时,得到硅烷改性聚醚,密封保存备用。
所述建筑用快速固化硅烷改性聚醚密封胶的制备方法如下:反应器内温度控制在25~30℃,按设定配方投入硅烷改性聚醚、无机填料、增塑剂和硅烷偶联剂,控制真空度不大于-0.095MPa,搅拌混合0.5~1小时,计量出料,密封包装得产品。
本发明的建筑用快速固化硅烷改性聚醚密封胶的有益效果:(1)采用多官能度端烯基聚氧化丙烯醚与氨基硅烷经迈克尔加成反应制备硅烷改性聚醚,反应条件温和,产物不含氨基甲酸酯键,耐候性、热稳定性与传统硅烷改性聚醚相当;(2)硅烷改性聚醚搭配交联型硅烷偶联剂,能够实现湿气条件下的快速固化。
具体实施实例
为更好的说明本发明的目的、技术方案和优点,下面将结合具体实施例对本发明作进一步说明。
本发明实施例及对比例中实验所用的原料如下,但是不限于以下原料,本发明只是以下原料为具体例子来进一步具体说明本申请中所述长效低气味低VOC单组份聚氨酯密封胶的效果:
端烯基聚醚多元醇:官能度2.0,数均分子量2000g/mol,链末端R2为CH3,郑州华普密封材料有限公司自制。
氨基硅烷:γ-氨丙基三乙氧基硅烷,KH550。
无机填料:NAK-2108纳米碳酸钙和NC-60A重质碳酸钙混合物,质量比1:4,旭丰粉体。
增塑剂:南京荣基化工DOP。
硅烷偶联剂:甲基三甲氧基硅烷,CG-8030。
综合性能依据GB/T 14683-2017中关于MS-I-F-20HM规定的方法进行测试,技术指标参考该标准规定。
表干时间:参考GB/T 13477.5-2002规定的A法进行测试,GB/T 14683-2017规定表干时间≤24小时。
下垂度:参考GB/T 13477.6-2002规定的方法进行测试,GB/T 14683-2017规定垂直方向≤3mm,水平方向不变形。
挤出性:参考B/T 13477.3-2017规定的方法进行测试,GB/T 14683-2017规定挤出性≥150mL/min。
弹性恢复率:参考GB/T 13477.17-2017规定的A法进行测试,伸长百分率100%,拉伸速率5mm/min,GB/T 14683-2017规定弹性恢复率≥60%。
拉伸模量:参考GB/T 13477.8-2017规定的A法进行测试,GB/T 14683-2017规定23℃拉伸模量≥0.4MPa,-20℃拉伸模量≥0.6MPa。
定伸粘结性:参考GB/T 13477.10-2017规定的方法进行测试,GB/T 14683-2017规定定伸粘结性应为无破坏。
浸水后定伸粘结性:参考GB/T 13477.11-2017规定的方法进行测试,GB/T 14683-2017规定定伸粘结性应为无破坏。
冷拉-热压后定伸粘结性:参考GB/T 13477.13-2017规定的方法进行测试,GB/T14683-2017规定定伸粘结性应为无破坏。
质量损失:参考GB/T 13477.19-2017方法进行测试,GB/T 14683-2017规定质量损失≤5%。
实施例和对比例制备方法如下:
本发明设置实施例1~8及对比例1~3,实验步骤和方法相同,获得一系列单组份透明高粘接强度硅烷改性聚氨酯组角胶,其制备方法如下:
步骤(1):控制反应体系端烯基与氨基摩尔比为1.0~1.2,按照设定配方往反应器中投入端烯基聚醚多元醇,升温至120℃,控制真空度不大于-0.095MPa,在该条件下除水1~2小时;降温至30~60℃,投入γ-氨丙基三乙氧基硅烷(KH550),氮气保护下搅拌12~36小时,得到硅烷改性聚醚,密封保存备用。
步骤(2):上述反应器内温度控制在25~30℃,按设定配方投入NAK-2108纳米碳酸钙和NC-60A重质碳酸钙混合物、增塑剂DOP和甲基三甲氧基硅烷(CG-8030),控制真空度不大于-0.095MPa,搅拌混合0.5~1小时,计量出料,密封包装得产品。
实施例1~8及对比例1~3的建筑用快速固化硅烷改性聚醚密封胶配方和性能如表1所示
实施例1~8性能如表1所示
对比例1~3性能如表2所示
表1实施例1~8均具有较优异施工性(挤出性、下垂性、表干时间)、力学强度和粘接性。对比例1~2的施工性和力学强度虽然能要求,但是粘接性出现失效,这是因为硅烷偶联剂缺失导致粘接表面的化学粘接减少,说明本发明的硅烷改性聚醚与硅烷偶联剂能协同提升粘接能力对比例3施工性和粘接性均能满足要求,仅有拉伸模量一项低于指标,这表明适量硅烷改性聚醚对调控力学性能至关重要。
以上所述仅为本发明的实施例而已,并不用于限制本发明。本发明可以有各种合适的更改和变化。凡在本发明的精神和原则之内所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述的建筑用快速固化硅烷改性聚醚密封胶,由硅烷改性聚醚30~50重量份、无机填料25~45重量份、增塑剂5~25重量份、硅烷偶联剂0.5~2重量份混合而成。根据权利要求1所述的单组份透明高粘接强度硅烷改性聚氨酯组角胶及其制备方法,其特征在于,所述硅烷改性聚氨酯预聚物由聚醚二元醇、生物基多元醇分别与二异氰酸酯和氨基硅烷偶联剂在催化剂作用下反应制得。
2.根据权利要求1所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述硅烷改性聚醚由端烯基聚醚多元醇与氨基硅烷由迈克尔加成反应制得。
4.根据权利要求1~3所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述硅烷改性聚醚的制备中,氨基硅烷为γ-氨丙基三乙氧基硅烷,γ-氨丙基三甲氧基硅烷,N-β(氨乙基)-γ-氨丙基三甲氧基硅烷,N-β(氨乙基)-γ-氨丙基三乙氧基硅烷,N-β(氨乙基)-γ-氨丙基甲基二乙氧基硅烷,苯氨基甲基三乙氧基硅烷,苯氨基甲基三甲氧基硅烷,氨乙基氨乙基氨丙基三甲氧基硅烷中的一种。
5.根据权利要求1~4所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述无机填料为重质碳酸钙、轻质碳酸钙、纳米碳酸钙、气相二氧化硅、炭黑、钛白粉中的一种或多种混合物。
6.根据权利要求1~5所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述增塑剂为邻苯二甲酸二辛酯(DOP)、邻苯二甲酸二辛壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)中的一种或多种混合物。
7.根据权利要求1~6所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述硅烷偶联剂为甲基三乙氧基硅烷、甲基三乙氧基硅烷的一种或两种混合物。
8.根据权利要求1~7所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述硅烷改性聚醚的制备方法如下:控制反应体系端烯基与(氨基+亚氨基)摩尔比为1.0~1.2,按照设定配方往反应器中投入端烯基聚醚多元醇,升温至120℃,控制真空度不大于-0.095MPa,在该条件下除水1~2小时;降温至30~60℃,投入氨基硅烷,氮气保护下搅拌12~36小时,得到硅烷改性聚醚,密封保存备用。
9.根据权利要求1~8所述的建筑用快速固化硅烷改性聚醚密封胶及其制备方法,其特征在于,所述建筑用快速固化硅烷改性聚醚密封胶的制备方法如下:反应器内温度控制在25~30℃,按设定配方投入硅烷改性聚醚、无机填料、增塑剂和硅烷偶联剂,控制真空度不大于-0.095MPa,搅拌混合0.5~1小时,计量出料,密封包装得产品。
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