4,4′-联苯二甲酸合成工艺研究  

Study on the synthesis process of 4,4′-diphenyldicarboxylic acid

作　　者：成西涛[1,2] 白燕 南蓉[1,2] 黄方方 郭鹏涛 郑阿龙[1,2] CHENG Xi-tao;BAI Yan;NAN Rong;HUANG Fang-fang;GUO Peng-tao;ZHENG A-long(Shaanxi Provincial Research and Design Institute of Petroleum and Chemical Industry,Xi′an 710054,China;Shaanxi Key Laboratory of Petroleum Fine Chemicals,Xi′an 710054,China)

机构地区：[1]陕西省石油化工研究设计院,陕西西安710054 [2]陕西省石油精细化学品重点实验室,陕西西安710054

出　　处：《化学研究与应用》2019年第4期763-767,共5页Chemical Research and Application

基　　金：陕西延长石油(集团)有限责任公司科学技术发展研究计划项目(ycsy2017JCYJ-A-06)资助

摘　　要：以医药中间体合成过程中产生的副产物4,4′-二甲基联苯为原料,经氯代反应生成4,4′-双(三氯甲基)联苯,然后水解制得4,4′-联苯二甲酸;对氯代反应的历程进行了探讨,并通过正交实验考察了反应参数对4,4′-联苯二甲酸收率的影响,得到了优化工艺条件,优化工艺条件下的验证实验表明:反应总收率达到93.40%,纯度达99.20%。采用IR、~1HNMR对产物的结构进行表征,通过HPLC对生成的4,4′-联苯二甲酸的纯度进行测定。该合成工艺具有环境友好、工艺操作简单、转化率及收率高、经济性好等优点,适合工业化大规模生产。4,4′-diphenyldicarboxylic acid was synthesized by the reaction of chlorination and hydrolysis from the 4,4′-dimethylbiphenyl which was the byproducts of pharmaceutical intermediates.The mechanism of the chlorination reaction was discussed and the effects of reaction parameters on the yield of 4,4′-diphenyldicarboxylic acid were studied via orthogonal experiment.The total yield of the reaction was 93.40%and the purity was 99.20%under the optimized conditions.The structure of the product was characterized by IR and 1HNMR and the purity of the 4,4′-diphenyldicarboxylic acid was determined by HPLC.The synthetic process had the advantages of environmental friendliness,simple process operation,high conversion rate,high yield and good economic performance,and was suitable for large-scale industrial production.

关 键 词：4 4′-联苯二甲酸 4 4′-双(三氯甲基)联苯 4 4′-二甲基联苯 氯代 水解 

分 类 号：O625.29[理学—有机化学]