2,4-二氯甲苯氨氧化法制备2,4-二氯苯腈研究

2,4-二氯甲苯氨氧化法制备2,4-二氯苯腈研究 Research on Preparation of 2,4 Dichlorobenzonitrile by Ammoxidation of 2,4 Dichlorotoluene 黄驰 HUANG Chi 1 first-author 郑穹 ZHENG Qiong 1 谢光勇 XIE Guang yong 1 许崇文 XU Chong wen 1 陈高清 CHEN Gao qing 1 陈远荫 CHEN Yuan yin 1 武汉大学化学学院 武汉大学化学学院 College of Chemistry, Wuhan University College of Chemistry, Wuhan University 对２，４－二氯甲苯经氨氧化法，一步制备有机中间体２，４－二氯苯腈进行了研究．在“微反－色谱”联用装置上完成催化剂的评比和筛选后，在内径３０ｍｍ的石英管固定床反应器上印证并进行工艺条件实验．考察了反应温度、氨比、空气比和空速对反应的转化率、摩尔收率和选择性的影响．所确定的工艺简捷，在合适的条件下使用ＤＴ１２４号催化剂，转化率高达９８．１％、摩尔收率８９．５％，生成２，４－二氯苯腈为白色针状或片状结晶，纯度高于９９％．同时，结合２，６－二氯甲苯氨氧化反应研究工作，对二氯甲苯的２、４位和２、６位的两个氯原子对反应的影响进行了初步的讨论 A process for ammoxidation of 2,4 dichlorotoluene to prepare 2,4 dichlorobenzonitrile which is a key intermediate of organic synthesis was studied. Having appraised and screened catalysts on an apparatus of “microreactor chromatograghy”, the further experiments confirming the catalyst and finding the optimum technological conditions were carried out by using a fixed bed reactor made of quartz （30 mm inside diameter）. The influence of temperature, the ratio of ammonia, the ratio of air and the space velocity of catalyst upon the conversion, molar yield and selectivity of the reaction were observed, respectively. Using catalyst of DC124, on the suitable conditions, the highest conversion is 98.1%, molar yield is 89.5%. The 2,4 dichlorobenzonitrile obtained is white sheet or needle crystal with the purity higher than 99%. The effect of two chlorine atoms at 2,6 or 2,4 position on the reaction is discussed based on the research of the ammoxidation of 2,6 dichlorotoluene and 2,4 dichlorotoluene. 氨氧化 2.4－二氯甲苯 2.4－二氯苯腈 ammoxidation 2,4 dichlorotoluene 2,4 dichlorobenzonitrile O625.67 1999-02-01 2021-04-01 2