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以十二烷基二甲基叔胺(12DMA)为主原料,在酸性条件下,合成了一种羟丙基双子型阳离子季铵盐1,3-二(烷基二甲基氯化铵)异丙醇(ADAC)。利用亚甲基蓝逆向滴定法测得产物纯度为98.63%,熔点为70.7~71.2℃。用FT-IR和~1H NMR对产物进行了结构表征。以单因素试验为基础,采用响应面法优化的ADAC合成工艺条件为:反应温度91℃、反应时间11 h、溶剂为异丙醇、n(12DMA):n(盐酸)=2.03:1、转速250 r/min。在此条件下,ADAC产率约为93.37%。15℃下对目标产物表面性能测定可知,cmc为4.5×10~(-5)mol/L,γ_(cmc)为27.07 mN/m,有效性(π_(cmc))为45.99 mN/m,效率(pc_(20))为5.301。
A kind of hydroxyl propyl Gemini ammonium chloride cationic surfactant, 1,3-bis(alkyldimethylammonium chloride) isopropanol (ADAC) was synthesized with dodecyl dimethyl amine (12DMA) as main starting material under acidic condition. The purity of ADAC in the product reaches 98.63%, which was determinated by methylene blue back titration method, and its melting point is 70.7~71.2 ℃. The chemical structure of the product was characterized by means of FT-IR and 1HNMR. Based on single factor experiments, the optimum conditions were obtained using response surface methodology as: reaction temperature, 91.02 ℃; reaction time, 11 h; solvent, isopropanol; n(12DMA)∶n(hydrochloric acid)=2.03∶1; stirrer rotation speed, 250 r/min. Under the aforesaid conditions, the reaction yield of ADAC achieves 93.37%. Surface performance of the target product at 15 ℃ was measured as: cmc, 4.5×10-5 mol/L; γcmc, 27.07 mN/m; effectiveness (πcmc), 45.99 mN/m; efficiency (pc20), 5.301.
