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以硬脂酸和N-甲基二乙醇胺(MDEA)为原料进行酯化反应得到中间体硬脂酸甲基二乙醇胺酯,再与γ-氯丙基甲基二甲氧基硅烷季铵化反应制备二烷基酯基甲基二甲氧基硅烷季铵盐。通过单因素和正交实验,考察了反应温度、反应时间、反应物摩尔比及催化剂用量等对酯化反应的影响。酯化反应优化工艺条件:反应温度为180℃,反应时间为8 h,反应物摩尔比n(硬脂酸)∶n(MDEA)=1.6∶1.0,次磷酸催化剂质量分数为0.9%,转化率达98%;二甲基亚砜作为季铵化反应的溶剂。通过溴酚蓝显色反应以及红外光谱、1HNMR、ESI-MS分析中间体和产物的结构。测定了目标产物在298 K下的表面活性以及柔软性能,临界胶束质量浓度CMC为0.197 g/L,γCMC为24.25 mN/m,柔软性能优于同类市售产品。
Esterification reaction with stearic acid and N-methyldiethanolamine (MDEA) as raw materials to obtain intermediate stearic acid methyldiethanolamine ester, followed by quaternization with γ-chloropropylmethyldimethoxysilane Preparation of Dialkyl Ester Methyldimethoxysilane Quaternary Ammonium Salt. The effects of reaction temperature, reaction time, molar ratio of reactants and the amount of catalyst on the esterification reaction were investigated by single factor and orthogonal experiments. The optimized reaction conditions were: reaction temperature 180 ℃, reaction time 8 h, reaction molar ratio n (stearic acid): n (stearic acid): 1.6:1.0, hypophosphorous acid catalyst mass fraction 0.9%, conversion rate Up to 98%; dimethyl sulfoxide as a solvent for the quaternization reaction. The structures of intermediates and products were analyzed by bromophenol blue color reaction as well as IR, 1HNMR, ESI-MS. The surface activity and softness properties of the target product at 298 K were determined. The CMC of the critical micelle was 0.197 g / L, and the γCMC was 24.25 mN / m. The softening properties were better than that of similar commercial products.