4-氯代邻苯二甲酸酐合成的中试研究  

Pilot study on synthesis of 4-chlorophthalic anhydride

作　　者：周兆良[1] 许青青[1] 阳永荣[2] 

机构地区：[1]浙江工业大学浙西分校化学与制药工程系,浙江衢州324000 [2]浙江大学化学工程与生物工程学系,浙江杭州310027

出　　处：《现代化工》2010年第2期81-84,86,共5页Modern Chemical Industry

摘　　要：以苯酐为原料,水为介质,先用氢氧化钠中和生成邻苯二甲酸单钠盐,再向混合体系通氯气,亲电取代得纯度大于72%(HPLC)的4-氯邻苯二甲酸单钠盐。然后经酸化、脱水、精馏。中试规模制备了纯度大于98.5%(HPLC)的4-氯邻苯二甲酸酐。探索了反应条件对转化率和选择性的影响。结果表明,最佳反应条件为:体系的pH4.5～5.5、水/苯酐质量比2.0～2.2、反应温度55～65℃、通氯速度30～50L/min,反应时间180～220min。苯酐转化率84.4%,总收率50%～60%。The sodium salt of phthalic anhydride is prepared by neutralization of sodium hydroxide with phthalic anhydride and an aqueous medium, subsequently the sodium salt of 4-chloro phthalic anhydride is synthesized by electrophilic substitution of chlorine gas, and the purity is more than 72% （HPLC）. Then after acidification, dehydration and rectification, 4-chloro phthalic anhydride are gained with purity more than 98.5% （HPLC） in the pilot-plant-scale. The effect of various reaction conditions on selectivity and conversion is investigated. The experimental results indicate that the production yield can reach 50% - 60% and the conversion of phthalic anhydride is 84.4% under the optimum reaction conditions： the system pH value of 4.5 - 5.5; the mass ratio of water to phthalic anhydride of 2.0 - 2.2; reaction temperature of 55 - 65 ℃ ; reaction time of 180 - 220 min.

关 键 词：4-氯邻苯二甲酸酐 氯气 中试 

分 类 号：TQ031.7[化学工程]