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以2-二甲氨基乙醇、硬脂酸为原料,合成了二甲基硬脂酸乙酯基叔胺,再与由十八烷基二甲基叔胺(DMA18)和环氧氯丙烷(ECH)为原料合成的中间体氯化铵反应,合成了一种含酯基的Gemini季铵盐柔软剂。通过单因素实验和正交实验考察了反应的影响因素。确定二甲基硬脂酸乙酯基叔胺的优化工艺条件为:n(2-二甲氨基乙醇)∶n(硬脂酸)=1.15∶1,反应温度100～110℃,m(甲苯)∶m(2-二甲氨基乙醇)=1.3∶1,反应时间7h,w(次磷酸)=1.0%,收率达96.6%以上;中间体氯化铵的优化工艺条件为:n(ECH)∶n(DMA18)=0.95:1,w(异丙醇)=50%,反应温度40～50℃,反应时间60min,收率达90.9%以上;含酯基Gemini季铵盐柔软剂的优化工艺条件为:n(中间体氯化铵)∶n(二甲基硬脂酸乙酯基叔胺)=1∶1.1;反应温度100℃;反应时间10h,收率达95.3%以上。该合成工艺已在河南省道纯化工技术有限公司成功进行了500L中试。
Using 2-dimethylaminoethanol and stearic acid as raw materials, dimethyl-stearic acid ethyl ester tertiary amine was synthesized, and then reacted with octadecyl dimethyl tertiary amine (DMA18) and epichlorohydrin (ECH ) Was used as the starting material to synthesize an ester group-containing Gemini quaternary ammonium salt softener. The influencing factors of the reaction were investigated by single factor experiment and orthogonal experiment. The optimum technological conditions for the determination of dimethyl dimethyl stearate were as follows: n (2 - dimethylaminoethanol): n (stearic acid) = 1.15:1, reaction temperature 100 ~ 110 ℃, The optimum conditions of ammonium chloride were n (ECH): m (2-dimethylaminoethanol) = 1.3:1, reaction time 7h, w (hypophosphorous acid) = 1.0% and yield of 96.6% (DMA18) = 0.95: 1, w (isopropanol) = 50%, reaction temperature 40 ~ 50 ℃, reaction time 60min, the yield of over 90.9%. The optimization process of Ester containing Gemini quaternary ammonium salt softener The conditions are as follows: n (intermediate ammonium chloride): n (dimethyl ethylstearyl tertiary amine) = 1: 1.1; reaction temperature 100 ℃; reaction time 10h, the yield is more than 95.3%. The synthesis process has been conducted in Henan Province, Purification Chemical Technology Co., Ltd. successfully 500L pilot.