摘要
采用酯化反应无需有机溶剂为介质、以碳基固体酸作酯化反应催化剂、磺化反应不外加相转移催化剂在常压下反应的新方法合成了乙二醇双子琥珀酸2-甲基戊基酯磺酸钠,最佳工艺条件为:单酯化反应,n(乙二醇)∶n(顺酐)=1.00∶2.10,催化剂碳基固体酸用量为顺酐质量的2%,于100℃反应4.7 h,酯化率99.02%(质量分数);双酯化反应,n(2-甲基-1-戊醇)∶n(顺酐)=1.30∶1.00,于210℃反应1.2 h,酯化率95.34%(质量分数);磺化反应,n(亚硫酸氢钠)∶n(顺酐)=1.05∶1.00,于油浴120℃反应3.2 h,磺化率100.64%(质量分数).对产物结构进行了IR光谱表征,测定了产物性能:CMC为2.5×10-3 mol/L,γCMC为27.79 mN/m,乳化力为11.5 min,渗透力为6 s,耐硬水力为13.5 min.比较了碳基固体酸和无水乙酸钠、对甲苯磺酸对酯化反应的催化效果,结果表明:碳基固体酸对酯化反应的催化效果好,且易于分离.
Ethylene glycol Gemini sodium 2-methyl-l-pentanol sulfosuccinate is synthesized by the methed of using carbonyl solid acid as the catalyst without organic solvents in esterification and any extra phase transfer catalysts in sulfonation. The optimal synthetic conditions are as follows： in the single-esterification, n （ethylene glycol）：n （maleic anhydride） = 1.00：2.10, the amount of carbonyl solid acid is 2% of the amount of maleic anhydride, and reacted un- der 100 ~C for 4.7 h with the esterification rate of 99.02%（Mass fraction）. In the di-esterification, n（2-methyl-1- pentanol）：n（maleic anhydride） = 1.30：1.00, and reacted under 210 ~C for 1.2 h with the esterification rate of 95.34% （Mass fraction）. In the sulfonation, n （sodium hydrogen sulfite） ：n （maleic anhydride） = 1.05：1.00, and reacted under 120 ~C for 3.2 h with the sulfonation rate of 100.64% （Mass fraction）. The structure of the product is characterized by IR. And its properties are measured： CMC = 2.5x10mol/L, Yc = 27.79 mN/m. Emulsifying power is 11.5 rain, permeability is 6 s and the ability of hard water resistance is 13.5 min. Compared with sodium acetate anhydrous andtoluenesulfonic acid, the carbonyl solid acid is more catalytic efficiency and easily to be separated.
出处
《南通大学学报（自然科学版）》
CAS
2012年第3期11-17,共7页
Journal of Nantong University(Natural Science Edition)
基金
"十二五"国家科技支撑计划重大项目(2011BAE06A06-9)
江苏高校科研成果产业化推进项目(JHB2011-46)
南通市科技创新计划项目(AS2009006)
