高品质间苯二甲酰氯的合成工艺研究
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摘要
利用间苯二甲酸与光气在催化剂N,N-二甲基甲酰胺的作用下进行反应,合成了间苯二甲酰氯。探讨了反应物配比、反应温度、催化剂用量、脱色剂的量和溶剂种类等对反应的影响。并针对间苯二甲酰氯易变色的问题,采用活性炭作为脱色剂处理,得无色稳定的产品。精馏后产品收率98%,产品含量大于99.95%。
Isophthaloyl dichloride was synthesized from the reaction between isophthalic acid and phosgene using dimethylformamide as catalyst. Factors influencing the reaction including the ratio of reagents, reaction temperature, the amount of catalyst, decoloration reagent, and the type of solvent were studied. A colorless and stable product was obtained by using activated carbon as decoloration reagent to avoid the discoloration of isophthaloyl chloride. Under the optimum reaction conditions, the yield and purity of isophthaloyl chloride was up to98% and 99.95%, respectively.
Isophthaloyl dichloride was synthesized from the reaction between isophthalic acid and phosgene using dimethylformamide as catalyst. Factors influencing the reaction including the ratio of reagents, reaction temperature, the amount of catalyst, decoloration reagent, and the type of solvent were studied. A colorless and stable product was obtained by using activated carbon as decoloration reagent to avoid the discoloration of isophthaloyl chloride. Under the optimum reaction conditions, the yield and purity of isophthaloyl chloride was up to98% and 99.95%, respectively.
引文
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[7]钱定权,曹如珍,刘纶祖,等.Vilsmeier试剂近年来在有机合成中的应用[J].有机化学,2000,120(1):30-43.
[8]Seagraves R L.Manufacture of phthaloyl chlorides:US,5113016[P].1992-05-12.
[9]王鲁敏,崔丙存,纪建业,等.间苯二甲酰氯的合成研究[J].通化师范学院学报,2005,26(4):46-47.
[10]徐海全,杨万宏,杜永顺,等.一种高纯度间苯二甲酰氯的制备方法:中国,200410023804.X[P].2005-01-12.
[11]盛庆全,肖鉴谋,奕伟丽,等.对苯二甲酰氯合成研究进展[J].江西化工,2007,23(4):15-18.
[12]Charles F H.Process for producing acidchlorides:US,3180940[P].1974-05-14.
[13]林卓然.对(间)苯二甲酰氯的制备与提纯[J].广州化工,1978,6(3):30-32.
[2]Stuan H.Preparation of cabroxylic acid chlorides:US,3184506[P].1965-05-18.
[3]Roben L.Manufacture of phthaloyl chlorides:US,5113016[P].1992-08-12.
[4]王登奎.一种制备对苯二甲酰氯的方法:中国,01139192.8[P].2003-07-09.
[5]陈敏析.联体法生产对苯二甲酰氯、间苯二甲酰氯和苯乙酮:中国,91111452.1[P].1993-06-09.
[6]让-克劳德.德斯考普斯.酸和/或酸酐在压力下光气化制备酰氯:中国,97104714.6[P].1997-11-05.
[7]钱定权,曹如珍,刘纶祖,等.Vilsmeier试剂近年来在有机合成中的应用[J].有机化学,2000,120(1):30-43.
[8]Seagraves R L.Manufacture of phthaloyl chlorides:US,5113016[P].1992-05-12.
[9]王鲁敏,崔丙存,纪建业,等.间苯二甲酰氯的合成研究[J].通化师范学院学报,2005,26(4):46-47.
[10]徐海全,杨万宏,杜永顺,等.一种高纯度间苯二甲酰氯的制备方法:中国,200410023804.X[P].2005-01-12.
[11]盛庆全,肖鉴谋,奕伟丽,等.对苯二甲酰氯合成研究进展[J].江西化工,2007,23(4):15-18.
[12]Charles F H.Process for producing acidchlorides:US,3180940[P].1974-05-14.
[13]林卓然.对(间)苯二甲酰氯的制备与提纯[J].广州化工,1978,6(3):30-32.