含酯基Gemini季铵盐柔软剂的合成工艺研究

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。

Synthesis Study of Gemini Quaternary Ammonium Salt Softener with Ester Bond

A Gemini quaternary ammonium salt fabric softener with ester group synthesized from 2-dimethylaminoethanol,stearic acid,octadecyl dimethyl amine(DMA18),hydrochloric acid and epichlorohydrin(ECH).The effects on the reaction process were investigated by the single factor and orthogonal experiment.The optimum conditions of dimethyl stearic acid ethyl tertiary amine were obtained as follows:n(2-dimethylaminoethanol):n(stearic acid)=1.15:1,reaction temperature 100～110 ℃,reaction time 7 h,m(toluene):m(2-dimethylaminoethanol)=1.3:1,w(sub-phosphoric acid)=1.0%,the yield is over 96.6%.The optimum conditions of intermediate ammonium chloride were obtained as follows:n(ECH):n(DMA18)=0.95:1,w(isopropyl alcohol)=50%,reaction temperature 40～50 ℃,reaction time 60 min,the yield is above 90.9%.The optimum conditions of ester Gemini quaternary ammonium salt fabric softener were obtained as follows:n(intermediate ammonium chloride):n(dimethyl stearic acid ethyl tertiary amine)=1:1.1;reaction temperature 100 ℃;reaction time 10 h,the yield is beyond 95.3%.The synthesis had been proved successful in Henan Titaning Chemical Co.Ltd in a 500 L pilot test.