Fe-D72树脂催化苯酚羟基化反应实验研究

摘要

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）/n（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）/n（H₂O₂）=1，反应温度为70 ℃，反应时间为1 h，催化剂量为0.1 g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。

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	冯惠生
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关键词：离子交换 D72树脂苯酚羟基化重复利用

Abstract：

Fe-D72 resin was prepared by the ion exchange process between iron ions and D72 resin. It was applied to the phenol hydroxylation with H₂O₂. 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 ℃, reaction time 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.

Keywords： ion exchange； D72 resin； phenol hydroxylation； reusability

Received 2016-03-18;

Corresponding Authors: 冯惠生,E-mail:hshfengtju@163.com. Email: hshfengtju@163.com

About author: 冯惠生(1962-),男,副教授,主要研究精细化工,传质与分离.

引用本文:

冯惠生, 钟鑫, 何丽娟, 孙德章, 罗彬彬.Fe-D72树脂催化苯酚羟基化反应实验研究[J]. 化学工业与工程, 2017,34(5): 49-54,60

Feng Huisheng, Zhong Xin, He Lijuan, Sun Dezhang, Luo Binbin.Experimental Study on Phenol Hydroxylation with Fe-D72 Resin Catalyst[J]. Chemcial Industry and Engineering, 2017,34(5): 49-54,60

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