1,4-丁二醇双琥珀酸八氟戊醇双酯磺酸钠的合成工艺研究

Study on Synthesis of Sodium 1,4- Butanediol Bis- octafluoropentyl Sulfo Succinate

采用八氟戊醇、马来酸酐、1,4-丁二醇为原料,合成了一种新型的双子表面活性剂—1,4-丁二醇双琥珀酸八氟戊醇双酯磺酸钠。通过实验得到各步反应的最优工艺条件,单酯化反应:马来酸酐与八氟戊醇摩尔比为1.2∶1.0,加入占马来酸酐质量1%的无水乙酸钠,反应时间为4h,反应温度为80℃;双酯化反应:八氟戊醇马来酸单酯与1,4-丁二醇的摩尔比为2.1∶1.0,占八氟戊醇马来酸单酯质量1.5%的对甲苯磺酸催化剂,反应温度为160℃,反应时间为7h;磺化反应:Na HSO3与1,4-丁二醇双马来酸八氟戊醇双酯摩尔比为1.0∶2.2,反应温度为100℃,反应时间为6h。对终产物的性能进行测定,表面张力为:28.6 m N·m-1,CMC为0.005 g/L。

With eight fluorine amyl alcohol,maleic anhydride and 1,4 -butanediol as raw material,a new Gemini surfactants of sodium glycol bis-octafluoropentyl sulfo succinate was synthesized. The optimal reac-tion conditions were obtained through experiments as follow,for single esterification reaction,the molar ratio of maleic anhydride to eight fluorine amyl alcohol was 1. 2：1. 0 ,with anhydrous sodium acetate accounted for 1% of the mass of maleic anhydride as catalyst,reaction temperature e was 90℃ and reaction time was 4h;for the double-esterification reaction,the molar ratio of eight fluorine amyl alcohol maleic acid monoester to 1, 4-butanediol was 2. 1：1. 0 ,with p-toluenesulfonic acid accounted for 1. 5% of the mass of octafluoropenta-nol maleic acid monoester as catalyst,reaction temperature was 160℃ and reaction time was 7h;for sulfona-tion reaction：the molar ratio of NaHSO3 to 1 ,4-butanediol bis-maleic acid octafluoropentanol diester molar ratio was 1. 0：2. 2,the reaction temperature was 100℃ and the reaction time was 6h. Determination of the fi-nal product performance,surface tension：29. 6 mN m^-1 ,CMC：0. 005 g/L.