十二烷基正丁基琥珀酸混合双酯磺酸钠的合成

Synthesis of Sodium Dodecyl n -Butyl Sulfosuccinate

以十二醇、马来酸酐、正丁醇和亚硫酸氢钠为原料,通过单酯化、双酯化和磺化反应合成了十二烷基正丁基琥珀酸混合双酯磺酸钠,通过傅里叶变换红外光谱表征了产物的结构。对单酯化、双酯化和磺化反应的条件进行了考察。十二醇与马来酸酐的单酯化反应的适宜条件为:n(马来酸酐):n(十二醇)=1.05,反应温度90℃,反应时间180 min;十二烷基马来酸单酯与正丁醇双酯化反应的适宜条件为:n(正丁醇):n(十二烷基马来酸单酯)=1.5,催化剂对甲苯磺酸的用量(基于总反应物的质量)为0.50%,反应温度130℃,反应时间90 min;十二烷基正丁基马来酸混合双酯与亚硫酸氢钠磺化反应的适宜条件为:n(亚硫酸氨钠):n(十二烷基正丁基马米酸混合双酯)=1.25,反应时间4 h,反应温度95℃。在此优化反应条件下,十二烷基正丁基琥珀酸混合双酯磺酸钠的总收率为88.55%。

Sodium dodecyl n-butyl sulfosuccinate was synthesized by monoesterification, diesterification and sulfonation from dodecanol, maleic anhydride, n-butanol and sodium bisulfite. Its structure was characterized by means of FTIR. The effects of reaction conditions on monoesterification, diesterification and sulfonation were studied. The optimal monoesterification conditions are： dodecanol and maleic anhydride as materials, mole ratio of maleic anhydride to dodecanol 1.05, reaction temperature 90 ℃ and reaction time 180 min. The optimal diesterification conditions are ： dodecyl maleic monoester and n-butanol as starting materials, mole ratio of n-butanol to dodecyl maleic monoester 1.5, toluene-p-sulfonic acid as catalyst mass fraction 0.50% （ base on total mass of reaction materials ）, reaction temperature 130 ℃ and reaction time 90 min. The optimal sulfonation conditions for NaHSO3 and dodecyl n-butyl maleic bisester are：mole ratio of NaHSO3 to dodecyl n-butyl maleic bisester 1.25, reaction temperature 95 ℃ and reaction time 4 h. The overall yield to sodium dodecyl n-butyl sulfosuccinate is 88.55%.