SiO2负载磷钨酸催化合成1,4-丁二醇双琥珀酸十八醇双酯磺酸钠

化工进展

SiO2负载磷钨酸催化合成1,4-丁二醇双琥珀酸十八醇双酯磺酸钠

刘士荣，张雪梅，龚雁，倪忠斌，陈明清

江南大学化学与材料工程学院

出版日期:2010-02-05 发布日期:2010-02-05

Synthesis of sodium 1,4-butanediol bisulfosuccinate diester catalyzed with PW12/SiO2

LIU Shirong，ZHANG Xuemei，GONG Yan，NI Zhongbin，CHEN Mingqing

School of Chemical & Material Engineering，Jiangnan University

Online:2010-02-05 Published:2010-02-05

摘要/Abstract

摘要： 采用1,4-丁二醇、马来酸酐、十八醇为主要原料，合成出一种双子表面活性剂1,4-丁二醇双琥珀酸十八醇双酯磺酸钠。此化合物的合成由两步酯化以及一步磺化反应组成，双酯化反应采用SiO2负载磷钨酸（PW12/SiO2）为催化剂。通过正交实验确定了1,4-丁二醇双马来酸十八醇双酯合成的优化反应条件为：n（1,4-丁二醇双马来酸单酯）: n（十八醇）=1.00 : 2.20，催化剂用量1.5%，反应温度150 ℃，反应8 h，酯化率达到97.2%，产率为84.9%。磺化反应的条件为 : n（1,4-丁二醇双马来酸双酯）: n（NaHSO3）= 1.00 : 3.00；反应4 h；反应温度90 ℃；催化剂（CTAB）用量1.5%，磺化率达到92.7%，产率为74.9%。在25 ℃水溶液中测得该表面活性剂的表面张力γcmc为41.9 mN/m，CMC为7.2×10-5 mol/L。表明该表面活性剂具有很低的临界胶束浓度。

Abstract: Sodium 1,4-butanediol bisulfosuccinate diester was synthesized from 1,4-butanediod, maleic anhydride and 1-octadecanol. The diesterfication reaction was catalyzed with phosphotungstic acid supported on silica (PW12/SiO2). The optimized conditions for the esterification were determined with orthogonal experiments as：molar ratio of 1,4-butanediol bismaleic acid monoester to 1-octadecanol was 1.00 : 2.20, amount of catalyst was ω=1.5%, reaction temperature was 150℃，reaction time was 8h，the esterification rate could reach to 97.2 % and the yield was up to 84.9%. The sulfonation reaction was carried out with the molar ratio of 1,4-butanediol bismaleic acid diester to NaHSO3 of 1.00 : 3.00 and 1.5% catalyst (cetyltrimethylammonium bromide) at 90℃ for 4h，the sulphonation rate could reach to 92.7 % and the yield was up to 74.9%. The obtained sodium 1,4-butanediol bisulfosuccinate diester has a surface tension γcmc of 41.9mN/m，a CMC of 7.2×10-5 mol/L in aqueous solution at 25 ℃，indicating that the surfactant has a low CMC.

刘士荣，张雪梅，龚雁，倪忠斌，陈明清. SiO2负载磷钨酸催化合成1,4-丁二醇双琥珀酸十八醇双酯磺酸钠 [J]. 化工进展.

LIU Shirong，ZHANG Xuemei，GONG Yan，NI Zhongbin，CHEN Mingqing. Synthesis of sodium 1,4-butanediol bisulfosuccinate diester catalyzed with PW12/SiO2[J]. Chemical Industry and Engineering Progree.