甲基二乙氧基硅烷季铵盐的合成

为制备线性聚硅氧烷季铵盐高分子,以3-氯丙基甲基二乙氧基硅烷和叔胺为原料,合成了甲基二乙氧基硅烷季铵盐(QAD IES)单体,考察了溶剂、反应时间对产品中QAD IES质量分数的影响,并用红外光谱、电喷雾离子化质谱(ESI-MS)、1HNRM和13CNMR对其结构进行了分析。以异丙醇为溶剂,3-氯丙基甲基二乙氧基硅烷和癸基二甲基叔胺为反应原料时,产物的正模式ESI-MS谱图中,m/Z:374.5、388.5、755.5、769.5、783.5和797.5处出现准分子离子峰,表明异丙醇在反应过程中与乙氧基硅烷发生了酯交换反应。通过实验得出该反应较优的反应条件为:在N2氛围中,以乙醇为溶剂回流反应40 h左右。产品色泽较好,季铵盐质量分数可达80%以上。

Synthesis of Quaternary Ammonium Functional Methyldiethoxysilane

Quaternary ammonium functional methyldiethoxysilane(QADIES) monomers were synthesized to prepare linear quaternary ammonium functional silicone by reacting 3-chloropropylmethyldiethoxysilane with a tertiary amine.The dependence of quaternary ammonium salt content in the product on solvent and reaction time was also investigated.The structural characteristics of QADIES were indicated by IR,electrospray ionization-mass spectrometry(ESI-MS),~1HNMR and ~(13)CNMR.Quasi-molecular ions at m/Z:374.5,388.5,755.5,769.5,783.5 and 797.5 in ESI-MS spectra of the product,obtained by using 3-chloropropylmethyldiethoxysilane and decyldiethylamine as reactants and isopropanol as solvent,means the occurrence of transesterification between ethoxysilane and isopropanol during the reaction.The better reaction conditions determined by experiments was reflux for about 40 h under N_2 with ethanol as solvent.Product with more than 80% quaternary ammonium salt content and better coloration can be obtained.