工艺条件对环丁烷四甲酸二酐连续化合成收率的影响  

Effect of process conditions on the yield of continuous synthesis of cyclobutane-1,2,3,4-tetracarboxylic dianhydrid

作　　者：杜友兴 何立 Du Youxing;He Li(Shanghai Chemspec Corporation, Shanghai 200331, China)

机构地区：[1]上海康鹏科技股份有限公司,上海200331

出　　处：《合成技术及应用》2020年第2期30-34,52,共6页Synthetic Technology & Application

摘　　要：以顺丁烯二酸酐(MA)为原料,碳酸二甲酯作溶剂,在连续化光反应器中紫外光照射下连续高效地制备了环丁烷四羧酸二酐(CBDA)。通过单因素实验和正交实验优化了环丁烷四甲酸二酐的合成工艺。结果表明,制备环丁烷四甲酸二酐的最佳工艺条件为:诱导光源为500 W,反应溶剂为碳酸二甲酯,管道内径2.0 mm,反应温度10℃,反应时间80 min,顺丁烯二酸酐浓度0.15 g/mL。经优化后,反应收率达到83.1%,产品纯度99.2%。Cyclobutane-1,2,3,4-tetracarboxylic dianhydride(CBDA)was continuously and efficiently synthesized by photoreaction of maleic anhydride(MA)using dimethyl carbonate as solvent in a continuous UV irradiation photoreactor.The synthesis process of cyclobutane tetracarboxylic dianhydride was optimized by single factor experiment and orthogonal experiment.The results showed that the optimum conditions for the preparation of Cyclobutane-1,2,3,4-tetracarboxylic dianhydride were as follows:light intensity at 500 W,the reaction solvent dimethyl carbonate,the inner diameter of the pipe at 2.0 mm,the reaction temperature at 10℃,the reaction time at 80 min,the concentration of maleic anhydride at 0.15 g/ml.After optimization,the yield was 83.1%with the purity of 99.2%.

关 键 词：环丁烷四甲酸二酐 顺丁烯二酸酐 光反应 连续化 合成 

分 类 号：TQ235[化学工程—有机化工]