CN110631950A - 一种液体硅橡胶热分解过程测定方法 - Google Patents
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Abstract
本发明公开了一种液体硅橡胶热分解过程测定方法,涉及电工材料技术领域,测定方法包括以下步骤:取液体硅橡胶作为样品;将样品加入到热重分析仪中,设置热分解升温参数,得到热分解产物;将热分解产物加入傅里叶变换红外光谱仪和质谱仪中,设置热分解产物测试参数;同步测量热分解产物的傅里叶红外光谱及质谱,得到傅里叶红外光谱图及质谱图;根据热分解产物的傅里叶红外光谱图及质谱图推导热分解产物的组成;根据热分解产物的组成推导液体硅橡胶的热分解过程。本发明的有益效果是通过本发明的评估方法,可以测定液体硅橡胶的热分解过程,为调节液体硅橡胶的热分解特性提供理论依据。
Description
技术领域
本发明涉及电工材料技术领域,具体涉及一种液体硅橡胶热分解过程测定方法。
背景技术
液体硅橡胶通过硅氢加成反应进行交联,理论上无副产物,且可以注射成型及模压成型。因此,液体硅橡胶具有更优异的综合性能,已广泛用作电子、电器灌封胶,光导纤维涂料,芯片节点保护涂料,高压电器设备外绝缘材料等。然而,在上述不同场合的使用过程中,以光、热为代表的环境应力,可能使液体硅橡胶发生老化,甚至失效。因此,具备较强的热稳定性,是液体硅橡胶保持优良性能的前提条件。
时至今日,如何提高液体硅橡胶热稳定性,仍然是研究重点。目前,引入一定质量分数的无机填料是提高液体硅橡胶热稳定性的常见方法。但是,大量引入无机填料,将削弱液体硅橡胶的可加工性及机械性能。因此,迫切需要从调节液体硅橡胶热分解特性的角度出发,提高液体硅橡胶的热稳定性。然而,准确测定液体硅橡胶的热分解过程,是研究并调节液体硅橡胶热分解特性的前提。因此,准确测定液体硅橡胶的热分解过程,对于提出一套新的液体硅橡胶热稳定性提高方法具有重要意义。
现有的液体硅橡胶热分解相关研究,基本都关注于液体硅橡胶的热分解特性,偶有关注于个别热分解产物,而鲜有系统分析液体硅橡胶热分解过程。
发明内容
本发明所要解决的技术问题是,克服以上现有技术的缺点:提供一种液体硅橡胶热分解过程测定方法。
本发明的技术解决方案如下:
一种液体硅橡胶热分解过程测定方法,包括以下步骤:
(1)取样,取液体硅橡胶作为样品;
(2)将样品加入到热重分析仪中,设置热分解升温参数,得到热分解产物;
(3)将热分解产物加入傅里叶变换红外光谱仪和质谱仪中,设置热分解产物测试参数;
(4)同步测量热分解产物的傅里叶红外光谱及质谱,得到傅里叶红外光谱图及质谱图;
(5)根据热分解产物的傅里叶红外光谱图及质谱图推导热分解产物的组成;
(6)根据热分解产物的组成推导液体硅橡胶的热分解过程。
进一步地,所述步骤(1)中,取3±1mg的液体硅橡胶作为样品。
进一步地,所述步骤(2)中,设置热分解升温参数中的升温速率为20℃/min,升温范围50-1000℃,热分解气氛为氩气。
进一步地,所述步骤(3)中,设置红外光谱测试波数范围为650–4000cm−1,测试频率1次/7秒。
进一步地,所述步骤(4)中,设置质谱质荷比测试范围为2–72,测试频率为1次/2秒。
进一步地,所述步骤(5)中,根据傅里叶红外光谱图,推导出热分解产物中含有硅氧烷。
进一步地,所述有硅氧烷为环状聚二甲基硅氧烷低聚物。
进一步地,所述步骤(6)中,热分解反应包括:
热分解反应1、生成环状聚二甲基硅氧烷低聚物:
进一步地,所述步骤(5)中,根据质谱图,推导出热分解产物中含有氢气、甲烷、乙烯。
进一步地,所述步骤(6)中,热分解反应还包括:
热分解反应2、生成甲烷:
热分解反应3、生成乙烯和氢气:
热分解反应4、生成甲烷和氢气:
本发明的有益效果是:通过本发明的评估方法,可以测定液体硅橡胶的热分解过程,为调节液体硅橡胶的热分解特性提供理论依据。
附图说明
图1为本发明液体硅橡胶热分解过程测定流程图;
图2为本发明液体硅橡胶热分解产物的傅里叶红外光谱图;
图3~图5为本发明液体硅橡胶热分解产物的热失重曲线图和质谱图;其中,曲线301、曲线401、曲线501均为热失重曲线,Y坐标对应质量%;曲线302、曲线402-406以及曲线502-505为质谱曲线,Y坐标对应离子流强度。
具体实施方式
下面用具体实施例对本发明做进一步详细说明,但本发明不仅局限于以下具体实施例。
如图1所示,本发明的液体硅橡胶热分解过程测定方法,包括以下步骤:
(1)取样,取3mg的液体硅橡胶作为样品;本实施例中的液体硅橡胶为以端乙烯基硅油为基础聚合物,以白炭黑为补强材料,以含氢硅油为交联剂,在铂催化剂的作用下,通过硅氢加成反应交联形成的具有交联网络结构的液体硅橡胶;液体硅橡胶的具体制备方法参照中国专利CN107418222A;
(2)将样品加入到热重分析仪中,设置热分解升温参数,具体设置升温速率为20℃/min,升温范围50℃-1000℃,热分解气氛为氩气,得到热分解产物,并得到热失重曲线图;
(3)将热分解产物加入并列的傅里叶变换红外光谱仪和质谱仪中,即从热重分析仪出来的分解气体分为两路,分别进入傅里叶变换红外光谱仪和质谱仪中;设置热分解产物测试参数;具体设置红外光谱测试波数范围为650–4000cm−1,测试频率1次/7秒;质谱质荷比测试范围为2-72,测试频率为1次/2秒;
(4)同步测量热分解产物的傅里叶红外光谱及质谱,得到热分解产物的傅里叶红外光谱图及质谱图,如图2~图5所示,傅里叶红外光谱图为图2,质谱图为图3-图5;
(5)根据热分解产物的傅里叶红外光谱图及质谱图推导热分解产物的组成;
由如图2可知,热分解产物在波数1303cm-1以及3015cm-1处显示出强吸收峰,分别对应于Si-C和Si-O键,在波数813cm-1、1026cm-1以及1084cm-1处也有较强吸收峰,由此可推测出,液体硅橡胶热分解产物中含有大量硅氧烷,即环状聚二甲基硅氧烷低聚物。
如图3-图5可知,热分解产物在质荷比为2(图3曲线302)、12-16(图4曲线402-406)以及25-28(图5曲线502-505)时存在明显离子流强度,分别对应氢气(H2)、甲烷(CH4)、以及乙烯(CH2=CH2),由此可推测出,液体硅橡胶热分解产物中含有氢气(H2)、甲烷(CH4)、以及乙烯(CH2=CH2)。
由于环状聚二甲基硅氧烷低聚物经过质谱仪能够生成的最小的碎片离子的质荷比是73,对应分子量也是73左右,因此本发明选用的质谱质荷比测试范围为2-72,本实施例中分子量高于72的热分解产物是通过测试氩气氛围下的热分解产物的傅里叶红外光谱得到;为确保悉数得到各分解产物,故设置傅里叶红外光谱测试频率为1次/7秒。本实施例中分子量低于72的热分解产物是通过测试氩气氛围下的热分解产物的质谱得到;为确保悉数得到各热分解产物,故设置质谱测试频率为1次/2秒。
综上,本发明中,分子量低于72的热分解产物有且只有氢气(H2)、甲烷(CH4)、乙烯(CH2=CH2),分子量高于72的热分解产物为环状聚二甲基硅氧烷低聚物。
(6)根据热分解产物的组成推导液体硅橡胶的热分解过程;根据热分解的产物包括环状聚二甲基硅氧烷低聚物、氢气、甲烷、乙烯,再结合液体硅橡胶的交联网络结构及配方,可唯一性推导液体硅橡胶的热分解反应下:
热分解反应1、生成环状聚二甲基硅氧烷低聚物:
热分解反应2、生成甲烷:
热分解反应3、生成乙烯和氢气:
热分解反应4、生成甲烷和氢气:
本发明方法适用于通过硅氢加成反应硫化形成的液体硅橡胶热反应过程的测定。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的技术人员来说,在不脱离本发明构思的前提下,还可以做出若干等同替代或明显变型,而且性能或用途相同,都应当视为属于本发明的保护范围。
Claims (10)
1.一种液体硅橡胶热分解过程测定方法,其特征在于:包括以下步骤:
S1、取液体硅橡胶作为样品;
S2、将样品加入到热重分析仪中,设置热分解升温参数,得到热分解产物;
S3、将热分解产物加入傅里叶变换红外光谱仪和质谱仪中,设置热分解产物测试参数;
S4、同步测量热分解产物的傅里叶红外光谱及质谱,得到傅里叶红外光谱图及质谱图;
S5、根据热分解产物的傅里叶红外光谱图及质谱图推导热分解产物的组成;
S6、根据热分解产物的组成推导液体硅橡胶的热分解过程。
2.根据权利要求1所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述步骤S1中,取3±1mg的液体硅橡胶作为样品。
3.根据权利要求1所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述步骤S2中,设置热分解升温参数中的升温速率为20℃/min,升温范围50-1000℃,热分解气氛为氩气。
4.根据权利要求3所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述步骤S3中,设置红外光谱测试波数范围为650-4000cm−1,测试频率1次/7秒。
5.根据权利要求4所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述步骤S4中,设置质谱质荷比测试范围为2-72,测试频率为1次/2秒。
6.根据权利要求5所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述步骤S5中,根据傅里叶红外光谱图,推导出热分解产物中含有硅氧烷。
7.根据权利要求6所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述有硅氧烷为环状聚二甲基硅氧烷低聚物。
9.根据权利要求8所述的一种液体硅橡胶热分解过程测定方法,其特征在于:所述步骤S5中,根据质谱图,推导出热分解产物中含有氢气、甲烷、乙烯。
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