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 The 2,4-dichlorobenzonitrile was prepared by the ammoxidation of 2,4-dichlorotoluene in one step. After the catalyst comparison and screening were completed on the “micro-reverse-chromatography” unit, experiments were carried out on a quartz tube fixed bed reactor with an inner diameter of 30 mm and the process conditions were tested. The effects of reaction temperature, ammonia ratio, air ratio and space velocity on the reaction conversion, molar yield and selectivity were investigated. The determination of the process is simple, under the proper conditions using DT124 catalyst, the conversion rate of up to 98.1%, the molar yield of 89.5%, resulting in 2,4-dichlorobenzonitrile white needle-like or flaky crystals, Purity higher than 99%. At the same time, combined with 2,6-dichlorotoluene ammoxidation reaction of the work, the 2,4-dichlorobenzene and 2,6-position of two chlorine atoms on the reaction were discussed