摘要
以副产物4,4’-双(三氯甲基)联苯为原料,经碱性水解一步反应合成出4,4’-联苯二甲酸。考察反应物料摩尔比、反应温度、反应时间对4,4’-联苯二甲酸产品收率的影响,得到优化工艺条件:氯苯为溶剂,4,4’-双(三氯甲基)联苯与10%氢氧化钠溶液的摩尔比为1∶9,反应温度为105℃,反应时间为14 h。在上述条件下,4,4’-联苯二甲酸的收率为95.25%,纯度可达99.20%,通过红外光谱、核磁共振氢谱及高效液相色谱等对产物进行了表征。
Taking 4,4’-bis(trichloromethyl) biphenyl as raw material, 4,4’-biphenyl dicarboxylic acid was synthesized via alkaline hydrolysis.The effects of raw material ratio, reaction temperature and reaction time on product yield were investigated.The optimized process conditions were obtained as follows: in a chlorobenzene solvent, the molar ratio of 4,4’-bis(trichloromethyl) biphenylto sodium hydroxide is 1∶9, the reaction temperature is 105 ℃and the reaction time is 14 h.Under the above condition, the yield of 4,4’-biphenyl dicarboxylic acid is 95.25%,and the purity can reach 99.20%.The products were characterized by IR,1H NMR and HPLC.
作者
成西涛
南蓉
郭鹏涛
蒋靖波
孙群宁
雷珂
CHENG Xi-tao;NAN Rong;GUO Peng-tao;JIANG Jing-bo;SUN Qun-ning;LEI Ke(Shaanxi Research Design Institute of Petroleum and Chemical Industry,Xi’an 710054,China;Shaanxi Key Laboratory of Petroleum Fine Chemicals,Xi’an 710054,China)
出处
《应用化工》
CAS
CSCD
北大核心
2021年第6期1582-1584,共3页
Applied Chemical Industry
基金
陕西省重点研发计划项目资助(2019SF-263)
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资助(ycsy2017JCYJ-A-06)。
