Fe-D72树脂催化苯酚羟基化反应实验研究

摘要

Fe-D72 resin was prepared by the ion exchange process between iron ions and D72 resin.It was applied to the phenol hydroxylation with H2 O2.The effects of different reaction conditions such as the iron capacity of catalyst,reaction temperature,reaction time,catalyst dosage,molar ratio of H2O2to phenol were investigated.The orthogonal experiment was carried out to get the best optimized operating conditions.Under the conditions of iron capacity as 95.4 mg.g-1,reaction temperature as 70 ℃,reactiontime as 1 h,catalyst dosage as 0.1 g,molar ratio of H2O2 to phenol as 1:1,42.4％ phenol conversion was obtained with benzenediol selectivity being 94.1％.The reusability of prepared catalyst illustrated that it could be recovered and reused without notable loss of activity.%利用D72离子交换树脂作为载体与铁离子进行离子交换制备Fe-D72树脂催化剂,将其运用到苯酚羟基化反应中.通过单因素法研究催化剂的含铁量、反应温度、反应时间、催化剂用量、苯酚(PH)/过氧化氢(H2O2)物质的量之比对苯酚羟基化反应的影响;采用L9(34)正交表设计正交试验,结果表明:n(PH)(H2O2)和反应温度对苯二酚收率的影响最大;在考察的正交范围内,n(PH)(H2O2) =1,反应温度为70℃,反应时间为1h,催化剂量为0.1g时催化效果最好,此时苯酚转化率为42.4％,苯二酚选择性为94.1％,苯二酚收率为39.8％.Fe-D72催化剂连续重复利用4次,催化稳定性较好.