化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2014年
5期
761-765
,共5页
尤思路%成丽%朱吉琴%吴晓娟%臧志和
尤思路%成麗%硃吉琴%吳曉娟%臧誌和
우사로%성려%주길금%오효연%장지화
邻苯二甲酸酐%尿素%邻苯二甲酰亚胺%微波合成%响应面法
鄰苯二甲痠酐%尿素%鄰苯二甲酰亞胺%微波閤成%響應麵法
린분이갑산항%뇨소%린분이갑선아알%미파합성%향응면법
phthalic anhydride%urea%phthalimide%microwave synthesis%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%)。
採用響應麵法優化鄰苯二甲酰亞胺的微波閤成工藝條件。以鄰苯二甲痠酐和尿素為原料,N,N-二甲基甲酰胺( DMF)為反應溶劑,通過Box-Behnken中心組閤實驗,攷察微波輻射溫度、原料摩爾配比和反應溶劑量(相對于原料鄰苯二甲痠酐的摩爾比例)三箇因素對鄰苯二甲酰亞胺收率的影響,得齣其最佳微波閤成條件參數組閤併建立多元迴歸數學模型。結果錶明:微波閤成最佳反應條件為n(鄰苯二甲痠酐)/n(尿素)/n (DMF)=1∶1.25∶1,微波144℃下攪拌迴流反應1min得到的產物收率最高(96.28%)。
채용향응면법우화린분이갑선아알적미파합성공예조건。이린분이갑산항화뇨소위원료,N,N-이갑기갑선알( DMF)위반응용제,통과Box-Behnken중심조합실험,고찰미파복사온도、원료마이배비화반응용제량(상대우원료린분이갑산항적마이비례)삼개인소대린분이갑선아알수솔적영향,득출기최가미파합성조건삼수조합병건립다원회귀수학모형。결과표명:미파합성최가반응조건위n(린분이갑산항)/n(뇨소)/n (DMF)=1∶1.25∶1,미파144℃하교반회류반응1min득도적산물수솔최고(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%.