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用马来酸酐(MA)与三羟甲基丙烷(TMP)经酯化反应制备系列三羟甲基丙烷马来酸单酯(TMPMs)。重点考察投料比、反应温度、时间、催化剂等对酯化反应的影响。结果表明,90℃下,n(MA)∶n(TMP)低于2.5∶1时,在240 min内MA单酯化率可达99%以上;n(MA)∶n(TMP)=3∶1时,需添加占单体总质量0.2%的对甲苯磺酸催化剂,MA酯化率方可达99%以上。采用NMR对产物的结构和组成进行表征和分析,通过酯化率计算其平均双键官能度。
A series of trimethylolpropane maleate monoesters (TMPMs) were prepared by esterification of maleic anhydride (MA) with trimethylolpropane (TMP). Focus on the feed ratio, reaction temperature, time, catalyst on the esterification reaction. The results showed that the MA esterification rate could reach more than 99% within 240 min when n (MA): n (TMP) was lower than 2.5:1 at 90 ℃; n (MA): n 1, the need to add 0.2% of the total monomer mass p-toluenesulfonic acid catalyst, MA esterification rate of up to 99% or more. The structure and composition of the product were characterized and analyzed by NMR, and its average double bond functionality was calculated by esterification rate.