CN111057377A - 一种阳离子光固化有机硅组合物的制备方法 - Google Patents
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Abstract
本发明涉及一种阳离子光固化有机硅组合物的制备方法,制备方法包括:(1)小分子预聚物GTM的制备(2)组分A‑脂环族环氧改性聚二甲基硅氧烷的制备,(3)组分B‑脂环族环氧改性MQ硅树脂的制备,(4)阳离子光固化有机硅组合物:取50~80份脂肪族环氧改性的聚二甲基硅氧烷,20~50份脂环族环氧改性的乙烯基MQ硅树脂,加入1~3份阳离子光固化剂,混合均匀,然后真空脱除气泡既得可阳离子光固化有机硅组合物。本发明合成步骤中不需要去除催化剂的步骤;以乙烯基封端硅油为原料,具有来源广范,黏度可控的特点,此外光固化后表面干爽,解决一般UV有机硅光照后,表面发粘的问题。
Description
技术领域
本发明涉及一种阳离子光固化有机硅组合物的制备方法,属于有机合成领域。
背景技术
传统有机硅固化体系主要为3种。1.经典的如借助烷氧基基团与空气中水分水解形成硅羟基,硅羟基之间脱水缩合的缩合型固化体系。根据组成分为单组份和双组份,单组份又可以分为以107胶体系和末端为烷氧基体系的单组份室温缩合型硅橡胶。而根据缩合基团的不同又可以分为脱醇型,脱酸型,脱丙酮等。但是该体系具有一个较大的缺点,即严重依赖空气中水分含量及胶层的厚度,因此固化速度较慢,往往需要几天甚至几周才能完全固化,影响了在部分领域的工作效率。2.借助硅氢基团和乙烯基在铂催化剂作用下加成反应形成的交联网状结构的有机硅体系则大大避免了固化速度慢这个问题,其固化速度非常快,通过调整催化剂含量,最快可以得到几分钟的固化速度,且不受固化厚度的影响。加成型硅橡胶同样可以分为单组份和双组分。单组份固化胶往往需要储存在低温条件下,而双组份硅胶则增加了重新搅拌的步骤,降低生产效率,且双组份硅胶固化速度不宜过快,否则混合不均则已固化。且若要达到较快的固化速度,加入较多价格昂贵的铂金催化剂无疑也会增加成本。3.相比之下,以过氧化物固化的硅橡胶所使用的催化剂价格就便宜多了,但是由于过氧化物分解会受到氧气的影响,所以这种固化方式往往受到氧气的干预,而出现表面发黏的状况。传统硅橡胶固化速度均比较慢,难以满足在特定领域的速度要求。
为了满足生产速度要求,有人以丙烯酸酯改性有机硅制备了一系列产品,固化速度得到了大大提升,但是丙烯酸酯体系的有机硅体系,往往存在表干差的问题,固化后往往有些粘手,若是做涂层材料则容易吸附灰尘,有时需要二段的湿气固化以解决。且丙烯酸酯改性有机硅往往还存在气味问题,即未完全除尽的单体。这些也会限制它在实践中的应用。
而以脂环族环氧接枝到有机硅主链上,则可避免表面发黏的问题,且与丙烯酸酯体系相比,阳离子光固化体系还具有有优异的粘接强度、无氧阻聚、薄膜固化性好(<1um)、固化收缩性小、树脂储存性好、对基材粘附性好,刺激性气味少等优点。适宜制备胶粘剂,三防胶等对粘接气味固化速度有要求的固化领域。
发明内容
本发明的目的在于针对目前技术的不足,提供一种阳离子光固化有机硅组合物,及主要原料的合成方式。
本发明是通过以下技术方案实现的:
(1)小分子预聚物GTM:
将124份1,2-环氧-4-乙烯基环己烷与0.5~1g铂金催化剂混合均匀,逐滴滴加至装有150g~250g四甲基二甲氧基硅烷的四口烧瓶中,四口烧瓶安装有温度计、搅拌器、回流冷凝管,当四口烧瓶内温度达到70℃,开始滴加,滴加时间控制在3-8h,然后保持60-80℃反应3-5h,旋蒸除去低沸物,即得到目标产物GTM;
(2)组分A-脂环族环氧改性聚二甲基硅氧烷:
将5~15份小分子预聚物GTM,100份乙烯基封端的聚二甲基硅氧烷及0.5~1g铂金催化剂混合均匀,升温至80-120℃,保持温度反应3-8h,降温即得到脂环族环氧改性聚二甲基硅氧烷;
(3)组分B-脂环族环氧改性MQ硅树脂:
取乙烯基封端的MQ硅树脂(M/Q=1,乙烯基含量1%)100-300g,100-150g甲苯,5-15g上述制备的小分子预聚体GTM,0.1-0.5g铂金催化剂至带有搅拌和温度计的四口烧瓶中,室温搅拌10-50min混合均匀;升温至80~110℃,维持温度反应3~8h,然后接通真空蒸馏装置抽真空2~4h,将溶剂甲苯与未反应单体除去,通入氮气,静置室温后,密封保存,即得脂环族环氧改性的MQ硅树脂;
(4)阳离子光固化有机硅组合物:取50~80份脂肪族环氧改性聚二甲基硅氧烷,20~50份脂环族环氧改性MQ硅树脂,加入1~3份阳离子光固化剂,混合均匀,然后真空脱除气泡既得可阳离子光固化有机硅组合物。
所述阳离子光引发剂是一种暴露在紫外光下发生光分解的化学物质,发生这种分解时,会产生超强酸,能够引发环氧的开环聚合反应,从而形成交联网络。所述阳离子光引发剂可包括二芳基碘鎓盐,三芳基碘鎓盐,四芳基碘鎓盐。
所述铂金催化剂可包括卡斯特催化剂,氯铂酸,及以上催化剂的稀释物,其在反应中占的比例,以铂金属含量为3~10ppm。
本发明的优点是:合成步骤中不需要去除催化剂的步骤;以乙烯基封端硅油为原料,具有来源广范,黏度可控的特点。此外光固化后表面干爽,解决一般UV有机硅光照后,表面发粘的问题。
具体实施方式
1小分子预聚体GTM的合成:
GTM-1
取124g 1,2-环氧-4-乙烯基环己烷与0.66g 5000ppm的卡斯特催化剂硅油稀释物50℃混合30min,将150g四甲基二硅氧烷加入到带有搅拌和温度计的四口烧瓶中,升温至70℃,将1,2-环氧-4-乙烯基环己烷与铂金催化剂的混合物,通过恒压滴液漏斗逐渐滴加到反应瓶中,控制滴加速度,将其在6h内均匀的滴加至四口烧瓶中,控制反应温度不超过72℃,滴加结束后,控制温度在75℃继续反应5h,反应结束,待料温降至50℃,加入5g活性炭继续搅拌2-4h,然后使用带有滤纸的布氏漏斗过滤,得到滤液密封保存。
GTM-2
取124g 1,2-环氧-4-乙烯基环己烷与0.66g 5000ppm的卡斯特催化剂硅油稀释物50℃混合30min,将250g四甲基二硅氧烷加入到带有搅拌和温度计的四口烧瓶中,升温至70℃,将1,2-环氧-4-乙烯基环己烷与铂金催化剂的混合物,通过恒压滴液漏斗逐渐滴加到反应瓶中,控制滴加速度,将其在6h内均匀的滴加至四口烧瓶中,控制反应温度不超过72℃,滴加结束后,控制温度在75℃继续反应5h,反应结束,待料温降至50℃,加入5g活性炭继续搅拌2-4h,然后使用带有滤纸的布氏漏斗过滤,得到滤液密封保存。
聚合物A-1:
取粘度500mpas的乙烯基封端的聚二甲基硅氧烷200g,5.1g上述制备的小分子预聚体GTM-2,0.208g 5000ppm卡斯特催化剂硅油稀释物至带有搅拌和温度计的四口烧瓶中,室温搅拌30min混合均匀,设置油温110℃,并开始升温,待温度升至110℃,维持温度反应3h,然后接真空蒸馏装置,抽真空1h左右,通入氮气,静置室温后,密封保存。
聚合物A-2:
取粘度500mpas的乙烯基封端的聚二甲基硅氧烷200g,13.8g上述制备的小分子预聚体GTM-2,0.208g 5000ppm卡斯特催化剂硅油稀释物至带有搅拌和温度计的四口烧瓶中,室温搅拌30min混合均匀,设置油温110℃,并开始升温,待温度升至110℃,维持温度反应3h,然后接真空蒸馏装置,抽真空1h左右,通入氮气,静置室温后,密封保存。
聚合物B-1:
取乙烯基封端的MQ硅树脂(M/Q=1,乙烯基含量1%)200g,100g甲苯,6g上述制备的GTM-2,0.31g 5000ppm卡斯特催化剂硅油稀释物至带有搅拌和温度计的四口烧瓶中,室温搅拌30min混合均匀,设置油温110℃,并开始升温,待温度升至110℃,维持温度反应3h,通过旋蒸抽真空1h左右,将溶剂甲苯与未反应单体除去,通入氮气,静置室温后,密封保存。
聚合物B-2:
取乙烯基封端的MQ硅树脂(M/Q=1,乙烯基含量1%)200g,100g甲苯,14g上述制备的GTM-2,0.31g 5000ppm卡斯特催化剂硅油稀释物至带有搅拌和温度计的四口烧瓶中,室温搅拌30min混合均匀,设置油温110℃,并开始升温,待温度升至110℃,维持温度反应3h,通过旋蒸抽真空1h左右,将溶剂甲苯与未反应单体除去,通入氮气,静置室温后,密封保存。
配方混合方式:
将制备的材料按照配方表依次加入小罐中,加入阳离子光引发剂PAG(含有45%wt左右的双(4-十二烷基苯基)碘鎓六氟锑酸盐-UV 9390C从克雷格粘合剂和涂料公司商购),然后加入均泡机中混合均匀;将所述材料涂覆至四氟板上,以深圳市久来电子有限公司制造的仪器进行紫外照射,照射功率为300mw,涂层在紫外线照射下10s;照射后放置10min,以指触涂层表面判断表干情况,不产生指纹则表干可。
结果分析:
从表中可以看出,使用本方案制备的可紫外照射UV涂层,表干可。且可以通过所选取乙烯基封端的聚二甲基硅氧烷和乙烯基硅树脂自由调整配方粘度,且制备的有机硅光固化材料具有柔软的特点。
以上所述仅为本发明的较佳实施例,并不是用于限制本发明范围,凡是在本发明的精神和原则之内,所做出的任何修改、等同替换、改进,均已包含在本发明的保护范围内。
Claims (2)
1.一种阳离子光固化有机硅组合物的制备方法,其特征在于,制备方法包括:
(1)小分子预聚物GTM:
将124份1,2-环氧-4-乙烯基环己烷与0.5~1g铂金催化剂混合均匀,逐滴滴加至装有150g~250g四甲基二甲氧基硅烷的四口烧瓶中,四口烧瓶安装有温度计、搅拌器、回流冷凝管,当四口烧瓶内温度达到70℃,开始滴加,滴加时间控制在3-8h,然后保持60-80℃反应3-5h,旋蒸除去低沸物,即得到目标产物GTM;
(2)组分A-脂环族环氧改性聚二甲基硅氧烷:
将5~15份小分子预聚物GTM,100份乙烯基封端的聚二甲基硅氧烷及0.5~1g铂金催化剂混合均匀,升温至80-120℃,保持温度反应3-8h,降温即得到脂环族环氧改性聚二甲基硅氧烷;
(3)组分B-脂环族环氧改性MQ硅树脂:
取乙烯基封端的MQ硅树脂(M/Q=1,乙烯基含量1%)100-300g,100-150g甲苯,5-15g上述制备的小分子预聚体GTM,0.1-0.5g铂金催化剂至带有搅拌和温度计的四口烧瓶中,室温搅拌10-50min混合均匀;升温至80~110℃,维持温度反应3~8h,然后接通真空蒸馏装置抽真空2~4h,将溶剂甲苯与未反应单体除去,通入氮气,静置室温后,密封保存,即得脂环族环氧改性的MQ硅树脂;
(4)阳离子光固化有机硅组合物:取50~80份脂肪族环氧改性聚二甲基硅氧烷,20~50份脂环族环氧改性MQ硅树脂,加入1~3份阳离子光固化剂,混合均匀,然后真空脱除气泡既得可阳离子光固化有机硅组合物。
2.根据权利要求1所述的阳离子光固化有机硅组合物的制备方法,其特征在于,所述阳离子光引发剂包括二芳基碘鎓盐,三芳基碘鎓盐,四芳基碘鎓盐;所述铂金催化剂包括卡斯特催化剂,氯铂酸,及以上催化剂的稀释物,其在反应中占的比例,以铂金属含量为3~10ppm。
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CN115926170A (zh) * | 2022-12-12 | 2023-04-07 | 宁波润禾高新材料科技股份有限公司 | 硅树脂、制备方法及其应用 |
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CN109233626A (zh) * | 2018-07-30 | 2019-01-18 | 江苏科琪高分子材料研究院有限公司 | 光固化环氧改性有机硅涂层组合物及其制备方法 |
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CN115873254A (zh) * | 2022-12-12 | 2023-03-31 | 杭州师范大学 | 硅树脂、制备方法以及应用 |
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