对氯甲苯氨氧化法制备对氯苯腈研究

Research on Preparation of p-chlorobenzonitrile by Ammoxidation of p-chlorotoluene

在“微反 -色谱”联用装置上完成对氯甲苯氨氧化制备对氯苯腈的催化剂评比和筛选后 ,在内径 30 mm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、空气比和空间速度对反应的转化率、摩尔产率和选择性的影响 .所确定的工艺简捷 ,在合适的条件下使用 PC97催化剂 ,对氯甲苯转化率高达 10 0 % ,对氯苯腈摩尔产率 90 .9% ,生成的对氯苯腈为白色针状结晶 ,纯度高于 99%

p \|Chlorobenzonitrile is a key intermediate of organic synthesis. Having appraised and screened ammoxidation catalysts of p \|chlorotoluene 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 with a tube 30 mm in 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 PC97, on the suitable conditions, the highest conversion is 100%, molar yield is 90.9%. The p \|chlorobenzonitrile obtained is white needle crystal with the purity higher than 99%.