响应面法优化邻苯二甲酰亚胺微波合成工艺

Optimization of microwave synthesis process for phthalimide by response surface method

采用响应面法优化邻苯二甲酰亚胺的微波合成工艺条件。以邻苯二甲酸酐和尿素为原料,N,N-二甲基甲酰胺(DMF)为反应溶剂,通过Box-Behnken中心组合实验,考察微波辐射温度、原料摩尔配比和反应溶剂量(相对于原料邻苯二甲酸酐的摩尔比例)三个因素对邻苯二甲酰亚胺收率的影响,得出其最佳微波合成条件参数组合并建立多元回归数学模型。结果表明:微波合成最佳反应条件为n(邻苯二甲酸酐)/n(尿素)/n(DMF)=1∶1.25∶1,微波144℃下搅拌回流反应1min得到的产物收率最高(96.28%)。

Response surface method（ RSM） was used to optimize the synthesis process for phthalimide with microwave heating meth-od. Phthalimide was synthesized with phthalic anhydride and urea as raw materials in DMF. Box-Behnken central composite design was adopted to investigate the influences of reaction temperature,molar ratio of raw material and solvent dosage on the yield. Then the optimal conditions for the microwave synthesis were obtained by RSM,and a quadric polynomial regression model was estab-lished. The results showed that the optimal conditions were as follows：reaction temperature 144℃,n（ phthalic anhydride）/n（ ure-a）/n（ DMF）=1∶1. 25∶1 and reaction time 1 min. Under the optimal conditions,the yield of phthalimide was 96. 28%.