马来酸酐与三羟甲基丙烷酯化反应

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。

Esterification of Maleic Anhydride with Trimethylpropane

Trimethylolpropane maleates(TMPMs) were prepared by esterification of trimethylolpropane(TMP) with maleic anhydride(MA).The effect of feed ratio,temperature,reaction time and catalyst on the esterification reaction was studied,and the results indicate that the esterification rate of MA could reach more than 99% with n(MA)∶n(TMP) lower than 2.5∶1 under 90 ℃ for 240 min,while the esterification rate of MA could reach more than 99% with n(MA)∶n(TMP)=3∶1 under 90 ℃ for 240 min only when toluene-p-sulfonic acid was used as catalyst which accounted for 0.2% of the total mass of the monomer.Catalyst addition was conducive to the increase of esterification rate of MA,which could reach over 99% without diesterification of MA.The structure and composition of TMPMs were characterized and analyzed by means of NMR,and the average double bond functionality(ADF) of TMPMs were calculated by esterification rate.