CN106479189A - 一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶 - Google Patents
一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶 Download PDFInfo
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- C08L83/04—Polysiloxanes
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Abstract
一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,涉及一种硅橡胶,所述硅橡胶,由以下组分按重量份计组成:甲基苯基乙烯基硅油100份;苯基含氢交联剂10‑80份;金属氧化物1~20份;催化剂0.1~5份。甲基苯基乙烯基硅油,粘度为15000 mPa·s~50000 mPa·s,苯基质量分数为5%~55%,乙烯基质量分数为0.1%~5%。本发明将含有苯环及硅氢键的分子引入POSS结构上,使其作为甲基苯基乙烯基硅橡胶的交联剂。含苯基三硅烷基笼型倍半硅氧烷的硅橡胶和传统的苯基硅橡胶类产品相比,具有更高的耐热性及力学性能,加入耐热助剂后热分解温度在400℃以上。
Description
技术领域
本发明涉及一种硅橡胶,特别是涉及一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶。
背景技术
甲基苯基乙烯基硅橡胶是指主链上的一部分硅原子连有二甲基而另一部分连有一个甲基和一个苯基,其特殊的化学结构赋予其一系列优异性能,已广泛应用于LED封装材料、耐高温涂层、导热胶、电子电器、轻工纺织、建筑建材等各个领域。随其应用领域的不断拓展,传统意义上的苯基硅油已经无法满足日渐苛刻的使用要求。因此迫切需要开发出一种耐高温、剪切强度高的硅橡胶。
本发明通过添加新型交联剂苯基三硅烷基笼型倍半硅氧烷得到了一种高性能苯基硅橡胶。目前常用的甲基苯基乙烯基硅橡胶交联剂为苯基含氢硅油,多为直链型结构,固化后所得胶体力学性能较低。与传统苯基硅橡胶类产品的交联剂相比,苯基三硅烷基笼型倍半硅氧烷有机硅交联剂由于POSS结构的引入可使得交联后的硅橡胶类产品有更高的耐热性及力学性能;而目前较为热门的POSS-笼型倍半硅氧烷立体网状结构,研究其作为含苯基的高性能硅胶的交联剂时由于相容性低而使其发展受到阻碍。本发明利用同时含有硅氢键与苯环的POSS结构作为苯基硅胶的交联剂使用,成功的提高了苯基硅橡胶的综合性能。
发明内容
本发明的目的在于提供一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,本发明将含有苯环及硅氢键的分子引入POSS结构上,使其作为甲基苯基乙烯基硅橡胶的交联剂。含苯基三硅烷基笼型倍半硅氧烷的硅橡胶和传统的苯基硅橡胶类产品相比,具有更高的耐热性及力学性能,加入耐热助剂后热分解温度在400℃以上。
本发明的目的是通过以下技术方案实现的:
一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,由以下组分按重量份计组成:
甲基苯基乙烯基硅油100份;
苯基含氢交联剂10-80份;
金属氧化物1~20份;
催化剂0.1~5份。
所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,所述甲基苯基乙烯基硅油,粘度为15000 mPa·s ~50000 mPa·s,苯基质量分数为5%~55%,乙烯基质量分数为0.1%~5%。
所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,苯基含氢交联剂结构如下所示:
。
所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,所述金属氧化物为氧化铁,氧化锡,氧化钛,氧化锌,氧化铈中的一种或多种,粒度为20nm~30um。
所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,所述催化剂为Karstedt铂金催化剂,含量为3000~5000ppm。
所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,上述所有实验药品均经过低压脱水处理,之后放入分子筛保存。
本发明的优点与效果是:
本发明将含有苯环及硅氢键的分子引入POSS结构上,使其作为甲基苯基乙烯基硅橡胶的交联剂。含苯基三硅烷基笼型倍半硅氧烷的硅橡胶和传统的苯基硅橡胶类产品相比,具有更高的耐热性及力学性能,加入耐热助剂后热分解温度在400℃以上。
具体实施方式
下面结合实施例对本发明进行详细说明。
含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,由以下组分按重量份计组成:
甲基苯基乙烯基硅油100份;
苯基含氢交联剂 10-30份;
金属氧化物1~20份;
催化剂 0.1~5份;
上述苯基含氢交联剂合成方法如下所示:
(1)在氯铂酸存在的情况下,将82mL苯基三硅烷与10mL乙烯基三甲氧基硅烷进行硅氢加成反应,反应完成后低压除去未反应的苯基三硅烷(可重复利用)及副产物;
(2)将步骤一所得产物和丙酮、甲苯体积比1:3混合溶液加入到三口瓶中,并在55℃的恒温水浴锅中搅拌10分钟,使之混合均匀,然后缓慢滴加3mol/L浓度的盐酸,继续搅拌,使之聚合60h,等反应结束后,对其进行抽滤,得到粗产物,将产物用无水乙醇清洗三次,并在60℃的条件下进行烘干,然后用二氯甲烷、四氢呋喃、甲苯进行重结晶,重结晶后得到的产物放入真空干燥箱中,并在60℃的条件下进行烘干,得到苯基三硅烷基笼型倍半硅氧烷硅橡胶交联剂的产率如下:
上述甲基苯基乙烯基硅油,粘度为15000 mPa·s ~50000 mPa·s,苯基质量分数为5%~55%,乙烯基质量分数为0.1%~5%。
上述金属氧化物为氧化铁,氧化锡,氧化钛,氧化锌,氧化铈中的一种或多种,粒度为20nm~30um。
上述催化剂为Karstedt铂金催化剂,含量为3000~5000ppm。
上述所有实验药品均经过低压脱水处理,之后放入分子筛保存
实施例 1
100份甲基苯基乙烯基硅油(粘度为30200mPa·s,苯基质量分数为55%,乙烯基质量分数为3.6%),4份纳米氧化锡,0.5份Karstedt 铂金催化剂(5000ppm),机械搅拌混合均匀,再用行星搅拌机搅拌2h,最后100℃真空除水5h。再加入37.8份苯基三硅烷基笼型倍半硅氧烷有机硅交联剂(溶于等质量的甲苯溶液中),混合均匀后低压除去体系中的甲苯;再于100℃下热处理4h后即可完全固化。按照GB/T 13477.6-2002测试所得固化后胶体的性能:断裂伸长率为231%,拉升强度为3.9Mpa。初始分解温度为451. 2℃。
实施例 2
100份甲基苯基乙烯基硅油(粘度为30200mPa·s,苯基质量分数为55%,乙烯基质量分数为3.6%),4份纳米氧化锡,5份纳米氧化铈,0.5份Karstedt 铂金催化剂(5000ppm), 机械搅拌混合均匀,再用行星搅拌机搅拌3h,最后100℃真空除水5h。再加入37.8份苯基三硅烷基笼型倍半硅氧烷有机硅交联剂(溶于等质量的甲苯溶液中),混合均匀后低压除去体系中的甲苯;再于100℃下热处理4h后即可完全固化。按照GB/T 13477.6-2002测试所得固化后胶体的性能:断裂伸长率为214%,拉升强度为3.5Mpa。初始分解温度为477. 4℃。
实施例 3
100份甲基苯基乙烯基硅油(粘度为15000mPa·s,苯基质量分数为25%,乙烯基质量分数为1.8%),4份纳米氧化锡,0.5份Karstedt 铂金催化剂(5000ppm), 机械搅拌混合均匀,再用行星搅拌机搅拌2h,最后100℃真空除水5h。再加入18.5份苯基三硅烷基笼型倍半硅氧烷有机硅交联剂(溶于等质量的甲苯溶液中),混合均匀后低压除去体系中的甲苯;再于80℃下热处理2h后即可完全固化。按照GB/T 13477.6-2002测试所得固化后胶体的性能:断裂伸长率为234%,拉升强度为2.8Mpa。初始分解温度为415.9℃。
实施例 4
100份甲基苯基乙烯基硅油(粘度为38000mPa·s,苯基质量分数为10%,乙烯基质量分数为0.3%),4份纳米氧化锡,0.5份Karstedt 铂金催化剂(5000ppm), 机械搅拌混合均匀,再用行星搅拌机搅拌2h,最后100℃真空除水5h。再加入3.15份苯基三硅烷基笼型倍半硅氧烷有机硅交联剂(溶于等质量的甲苯溶液中),混合均匀后低压除去体系中的甲苯;再于100℃下热处理4h后即可完全固化。按照GB/T 13477.6-2002测试所得固化后胶体的性能:断裂伸长率为374%,拉升强度为2.9Mpa。初始分解温度为429. 1℃。
实施例5
85份苯基乙烯基硅树脂(粘度为12000mPa·s,苯基质量分数为45%,乙烯基质量分数为5%),15份乙烯基封端甲基苯基硅油(粘度为1000mPa·s,苯基质量分数为45%,乙烯基质量分数为0.45%),4份纳米氧化锡,0.5份Karstedt铂金催化剂(5000ppm),机械搅拌混合均匀,用行星搅拌机搅拌2h后100℃真空除水5h。再加入0.06份抑制剂PC-610(市售),50份二苯基三硅氧烷基笼型倍半硅氧烷有机硅交联剂(溶于等质量的甲苯溶液中),混合均匀后低压除去体系中的甲苯;室温下10h后即可完全固化。按照GB/T 13477.6-2002测试所得固化后胶体的性能:断裂伸长率为175%,拉升强度为3.9Mpa。初始分解温度为435. 8℃。
由5个实施例对比可得,随着金属氧化物加入量的提高,胶黏剂的耐热性有所提高,但是力学性能随之下降;甲基苯基乙烯基硅油粘度的变化会影响胶体的可加工性,粘度大即分子量大,力学性相对较好,但使用工艺逐渐复杂;不同的胶体可适用于对硅橡胶有特殊耐热要求的不同场合,根据实际应用条件的不同,可选择相应的配方。上述的具体实施方式只是示例性的,是为了更好地使本领域技术人员能够理解本发明,不能理解为是对本发明包括范围的限制;只要是根据本发明所揭示精神的所作的任何等同变更或修饰,均落入本发明包括的范围。
Claims (6)
1.一种含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,其特征在于由以下组分按重量份计组成:
甲基苯基乙烯基硅油100份;
苯基含氢交联剂10-80份;
金属氧化物1~20份;
催化剂0.1~5份。
2.根据权利要求1所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,其特征在于所述甲基苯基乙烯基硅油,粘度为15000 mPa·s ~50000 mPa·s,苯基质量分数为5%~55%,乙烯基质量分数为0.1%~5%。
3.根据权利要求1所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,其特征在于苯基含氢交联剂结构如下所示:
。
4.根据权利要求1所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,其特征在于所述金属氧化物为氧化铁,氧化锡,氧化钛,氧化锌,氧化铈中的一种或多种,粒度为20nm~30um。
5.根据权利要求1所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,其特征在于所述催化剂为Karstedt铂金催化剂,含量为3000~5000ppm。
6.根据权利要求1所述的含苯基三硅烷基笼型倍半硅氧烷的硅橡胶,其特征在于上述所有实验药品均经过低压脱水处理,之后放入分子筛保存。
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CN113777702A (zh) * | 2021-09-06 | 2021-12-10 | 中国建筑材料科学研究总院有限公司 | 对排板后的光学纤维丝进行捆绑的方法和装置 |
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