对硝基苯甲酸的制备新工艺  

New process for preparation of p-nitrobenzoic acid

作　　者：王松林 李永祥 任君 WANG Songlin;LI Yongxiang;REN Jun(College of Chemical Engineering and Technology,North University of China,Taiyuan Shanxi 030051,China)

机构地区：[1]中北大学化学工程与技术学院,山西太原030051

出　　处：《山西化工》2020年第1期1-4,共4页Shanxi Chemical Industry

基　　金：基于密度泛函理论和机器学习法预测钙钛矿化合物的光电特性,国家自然科学基金(2197020820)。

摘　　要：以对硝基甲苯为主要原料,氯酸钠为氧化剂.通过一步反应制得对硝基苯甲酸,并详细研究了制备对硝基苯甲酸的工艺,得出最佳工艺条件为:对硝基甲苯与氯酸钠的摩尔比1:2.5,反应时间4.1 h,反应温度80℃~85℃,得率81.37%;该工艺反应条件温和,得率较高,产生的废液中ClO-3可以被还原为Cl-,再通过电解或者阴离子交换树脂降低Cl-浓度.通过熔点测定、薄层色谱分析、红外光谱分析,对制得的对硝基苯甲酸进行了检测分析,其熔点为235.9℃,且纯度较高.P-nitrobenzoic acid was prepared by one-step reaction with p-nitrotoluene as main raw materials and sodium chlorate as oxidizer.The process of preparing p-nitrobenzoic acid was studied in detail.The optimum conditions were obtained as follows:the molar ratio of p-nitrotoluene to sodium chlorate was 1:2.5,the reaction time was 4.1 h,the reaction temperature was 80℃~85℃,and the yield was 81.37%;the reaction conditions are mild and the yield is high.ClO-3 in the waste liquid can be reduced to Cl-,and then the concentration of Cl-can be reduced by electrolysis or anion exchange resin.The product was detected,analyzed by melting point determinatio,thin layer chromatography and infrared spectroscopy.The melting point of p-nitrobenzoic acid was 235.9℃and it’s purity was high.

关 键 词：对硝基甲苯 对硝基苯甲酸 氯酸钠 氧化反应 

分 类 号：O625.53[理学—有机化学]