对氯甲苯氨氧化法制备对氯苯腈实验综合性实验研究

设计了对氯甲苯氨氧化制备对氯苯腈的综合研究性实验,采用浸渍法制备了VPO/SiO2催化剂,并用XRD、FTIR和SEM对催化剂进行表征,在内径30 mm的石英管固定床反应器上采用正交设计进行工艺条件实验,考察了反应温度、氨比以及空气比对反应的转化率、摩尔产率和选择性的影响。在经过筛选的最佳反应条件下,使用VPO/SiO2催化剂,PCT转化率92.24%、PCBN摩尔产率86.01%,生成的对氯苯腈为白色针状结晶,纯度高于99%。

Research on preparation of p-chlorobenzonitrile by ammoxidation of p-chlorotoluene

A comprehensive research experiment of preparing p-chlorobenzonitrile by ammoxidation of p-chlorotoluene has been designed. The VPO/SiO2 catalyst is prepared by impregnation method and char-acterized by XRD, FTIR and SEM. The orthogonal experiment to find the optimum technological condi-tions are carried out by a fixed-bed reactor made of quartz with a tube 30mm in inside diameter. The in-fluence of temperature, the ratio of ammonia and the ratio of air upon the conversion, molar yield and selectivity of the reaction are observed, respectively. Using VPO/SiO2 catalyst, on the screened optimal reaction conditions, the conversion of PCT is 92. 24%, molar yield of PCBN is 86. 01%. The p-chloro-benzonitrile obtained is white needle crystal with the purity higher than 99%.