一种有机硅产物热稳定性实验分析

Experimental Analysis of Thermal Stability of MEKOH

利用烧瓶法、热分析仪法和气相色谱法对有机硅生产企业制备甲基三丁酮肟基硅烷(MOS)所生成的丁酮肟盐酸盐(MEKOH)进行热稳定性实验分析,然后通过扫描量热仪绘制温度(T)-TG-DSC和温度(T)-TG-DTG曲线确定MEKOH热稳定性。结果表明:烧瓶法对SP-001样品与去离子水混溶后无明显温升,两次充分溶解实验后样品的温升均为5℃左右(溶解前28℃,溶解后33℃)。热分析仪分析得出SP-001样品在51~57℃开始失重,经图解积分求得样品在50~90℃之间失重放热在29.65~45.86 J/g之间。气相色谱法对SP-顶-002,SP-顶-003,SP-底-004样品进行MEKOH定性分析。检测相对分子质量范围为5~450。三个样品中均检出丁酮肟(MEKO),未能检出MEKOH,表明MEKOH易分解且分解为反应物MEKO,这为MOS合成工艺的优化提供了依据。

Using flask method,thermal analyzer method and gas chromatography method,the product of Methyltris(methyl ethyl ketone oxime)silane(MOS)produced by silicone production enterprises was analyzed for thermal stability experiments of Methyl ethyl ketone oxime hydrochloride(MEKOH),and then the temperature(T)-TG-DSC and temperature(T)-TG-DTG curve was drawn by scanning the volume heater to determine MEKOH thermal stability.The results showed that there was no significant temperature rise after mixing the SP-001 sample with deionized water,and the temperature rise of the sample after the two fully dissolved experiments was 5℃(28℃before dissolution and 33℃after dissolution).The thermal analyzer found that the SP-001 sample began to lose weight at 51~57℃,and the resulting sample weight loss between 50℃and 90℃was between 29.65~45.86 J/g.The gas chromatography method performs a qualitative analysis of the hydrochloric acid of the SP-top-002,SP-top-003,SP-bottom-004 samples.The detection molecular weight range is 5~450.MEKO was detected in all three samples,and MEKOH was not detected.It is stated that MEKOH is easy to decompose and decompose into reactant MEKO.This provides a basis for the optimization of MOS synthesis process.