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采用以碳基固体酸为双酯化反应催化剂,中间产物不需提纯分离等环境友好的合成工艺路线,在常压下合成了乙二醇双子琥珀酸2-甲基戊基双酯磺酸钠。对各步反应条件进行了考察,得到的最佳工艺条件为:单酯化反应:n(顺酐)∶n(2-甲基-1-戊醇)=1.05∶1.00,w(对甲苯磺酸)=1%,反应温度80℃,单酯化反应时间1 h,在该条件下得到产率为98.88%的单酯化产物;磺化反应:n(顺酐)∶n(亚硫酸氢钠)=1.00∶1.05,反应温度70℃,磺化反应时间2.0 h,在该条件下得到产率为98.71%的磺化产物;双酯化反应:n(顺酐)∶n(乙二醇)=1.00∶2.20,w(碳基固体酸)=3%,加热介质温度180℃,双酯化反应时间3.5 h,在该条件下得到产率为85.03%的双酯化产物。测定了目标产物的表面张力为27.79 mN/m;临界胶束浓度为2.5×10-3 mol/L。
The carbon-based solid acid as a double esterification catalyst, intermediate without purification and separation of environmentally friendly synthetic route, at normal pressure ethylene glycol monosuccinic acid 2-methyl pentyl ester sodium . The optimum reaction conditions were as follows: Monoesterification reaction: n (maleic anhydride): n (2-methyl-1-pentanol) = 1.05:1.00, w (Maleic acid) = 1%, reaction temperature 80 ℃, monoesterification reaction time 1 h under the conditions to give a monoesterified product with a yield of 98.88%; sulfonation reaction: n (maleic anhydride): n Sodium = 1.00: 1.05, the reaction temperature was 70 ℃, the sulfonation reaction time was 2.0 h, the yield of sulfonated product was 98.71% ) = 1.00: 2.20, w (carbon-based solid acid) = 3%, the temperature of heating medium is 180 ℃ and the reaction time of dioester is 3.5 h. Under these conditions, the yield of double esterification product is 85.03%. The surface tension of target product was determined to be 27.79 mN / m and the critical micelle concentration was 2.5 × 10-3 mol / L.