| 4-氯代邻苯二甲酸酐合成的中试研究 |
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| 引用本文： | 周兆良,许青青,阳永荣.4-氯代邻苯二甲酸酐合成的中试研究[J].现代化工,2010,30(2). |
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| 作者姓名： | 周兆良 许青青 阳永荣 |
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| 作者单位： | 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 |
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| 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pH 4.5～5.5、水/苯酐质量比2.0～2.2、反应温度55～65℃、通氯速度30～50 L/min,反应时间180～220 min.苯酐转化率84.4%,总收率50%～60%.
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| 关 键 词： | 4-氯邻苯二甲酸酐 氯气 中试 |
Pilot study on synthesis of 4-chlorophthalic anhydride |
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| ZHOU Zhao-liang,XU Qing-qing,YANG Yong-rong.Pilot study on synthesis of 4-chlorophthalic anhydride[J].Modern Chemical Industry,2010,30(2). |
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| Authors: | ZHOU Zhao-liang XU Qing-qing YANG Yong-rong |
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| Affiliation: | ZHOU Zhao-liang1,XU Qing-qing1,YANG Yong-rong2(1.Department of Chemistry , Pharmaceutical,West Branch of Zhejiang Industry University,Quzhou 324000,China,2.Department of Chemical , Bio Engineering,Zhejiang University,Hangzhou 310027,China) |
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| Abstract: | 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 conv... |
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| Keywords: | 4-Chlorophthalic anhydride chlorine scale-up synthesis |
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