马来酰化端基聚乙二醇合成工艺的优化

Optimization for the Synthesis of Polyethylene Glycol-maleimide

以PEG4000为起始原料,通过对甲苯磺酸酯法生成AT-PEG4000,然后与马来酸酐反应,经过缩合反应合成PEG4000-MAL.旨在采用正交实验设计考察相关因素对其最终产物PEG4000-MAL收率的影响,结果表明对其收率影响最大的因素为AT-PEG4000的氨基与马来酸酐摩尔比,最佳工艺条件是AT-PEG4000的氨基与马来酸酐摩尔比为1∶4,反应温度为100℃,反应时间为3h.经验证实验知此路线全程收率为87.2%.用红外光谱对产物结构进行了表征,证实最终合成产物即为PEG4000-MAL.

Using Polyethylene Glycol 4000（PEG4000）as initial ingredient,AT-PEG4000 is produced via Tosylate method,which will then be reacted with maleic anhydride through condensation reaction,yielding PEG4000-MAL.The aim of this research is to evaluate the influence of other factors upon the productivity of PEG4000-MAL by using orthogonal design.The results indicate that the mol ratio of amino-group of AT-PEG4000 and maleic anhydride contribute the most to the PEG4000-MAL productivity.The optimal conditions were identified as follows：1∶4 for the mol ratio of amino-group of AT-PEG4000 and maleic anhydride;100 ℃ for the reaction temperature;3 hours for reaction time.The full yield of the whole process was proved to be 87.2%.The final synthetic product was identified as PEG4000-MAL by infrared spectrum.