缩合型甲基苯基硅树脂取代度的测试方法研究  

Study on Measurement of R/Si Ratio of Condensed Methylphenyl Silicone Resin

作　　者：李川阳 李霞 朱良波 孙挚 宋祖杰 唐小斗 王芳 钱杉杉[3] LI Chuanyang;LI Xia;ZHU Liangbo;SUN Zhi;SONG Zujie;TANG Xiaodou;WANG Fang;QIAN Shanshan(Chengrand Research Institute of Chemical Industry Co.Ltd.,China Bluestar,Chengdu 610041,Sichuan;China Bluestar Chengrand Co.,Ltd.,Chengdu 610041,Sichuan;National Institute of Measurement and Testing Technology,Chengdu 610021,Sichuan)

机构地区：[1]中蓝晨光化工研究设计院有限公司,成都610041 [2]中蓝晨光化工有限公司,成都610041 [3]中国测试技术研究院,成都610021

出　　处：《有机硅材料》2023年第3期47-53,共7页Silicone Material

摘　　要：取代度(R/Si比)作为有机硅聚合物重要的结构参数,尚无可靠的测试方法报道。根据缩合型硅树脂主链硅氧原子交替排列的结构特点,建立了其中硅原子、氧原子及取代基数量关系,并推导出取代度的计算公式。通过核磁共振波谱法测定取代基团物质的量之比,并与电感耦合等离子光谱法测定的硅质量分数相结合,建立了缩合型甲基苯基硅树脂取代度的定量测试方法,经验证具有可行性和良好重复性,规避了核磁硅谱测试中背景信号干扰、耗时长以及难以精确定量等难题。As an important structural parameter of silicone polymers,no reliable test methods of the degree of substitution(R/Si ratio)have been reported yet.According to the Si-O alternating arrangement structural characteristics of condensed silicone resin,the quantitative relationship between Si,O and substituent R groups could be established,and the calculation formula of degree of substitution could be deduced.A quantitative test method for the R/Si ratio of condensed methylphenyl silicone resin was established by determining the molar ratio of the substituent groups by nuclear magnetic resonance spectroscopy combined with the silicon content determination by inductively coupled plasma spectrometry.This method proved to be feasible and repeatable,avoiding signal interference in background,long time,and imprecise quantification in 29 Si NMR test.

关 键 词：有机硅 甲基苯基硅树脂 取代度 测试 

分 类 号：TQ324.2+1[化学工程—合成树脂塑料工业]