化工进展 ›› 2019, Vol. 38 ›› Issue (04): 1978-1983.DOI: 10.16085/j.issn.1000-6613.2018-1581

• 精细化工 • 上一篇    下一篇

直接氧化法制备2,5-二氯苯酚

廖阳群1,2(),张跃2(),严生虎1,2,刘建武1,马晓明1,2,辜顺林1,沈介发1,2,陈代祥1,2   

  1. 1. 常州大学制药与生命科学学院,江苏 常州 213164
    2. 石油和化工行业连续流技术工程实验室,江苏 常州 213164
  • 收稿日期:2018-08-02 修回日期:2018-12-20 出版日期:2019-04-05 发布日期:2019-04-05
  • 通讯作者: 张跃
  • 作者简介:<named-content content-type="corresp-name">廖阳群</named-content>(1994—),女,硕士研究生,研究方向为流动化学和过程工程。E-mail:<email>1428542103@qq.com</email>。|张跃,研究员,工学博士,主要从事制药工程工艺学、化学工艺的优化研究工作。E-mail:<email>zyjs@cczu.edu.cn</email>

Preparation of 2,5-dichlorophenol by direct oxidation

Yangqun LIAO1,2(),Yue ZHANG2(),Shenghu YAN1,2,Jianwu LIU1,Xiaoming MA1,2,Shunlin GU1,Jiefa SHEN1,2,Daixiang CHEN1,2   

  1. 1. School of Pharmaceutical and Life Sciences, Changzhou University, Changzhou 213164, Jiangsu, China
    2. Continuous Flow Engineering Laboratory of National Petroleum and Chemical Industry, Changzhou 213164, Jiangsu, China
  • Received:2018-08-02 Revised:2018-12-20 Online:2019-04-05 Published:2019-04-05
  • Contact: Yue ZHANG

摘要:

2,5-二氯苯酚是重要的酚类化合物,工业上常用的2,5-二氯苯酚的制备方法大多存在生产流程长、污染严重等问题。针对这些问题,本文提出了以对二氯苯为原料、H2O2为氧化剂的直接氧化制备2,5-二氯苯酚的工艺,并对催化剂和溶剂进行初步筛选,探讨了不同催化体系对反应的影响,确定以铁粉作催化剂、乙酸为溶剂的反应体系下,通过对氧化剂用量、反应温度、反应时间、催化剂用量等工艺条件的考察,获得最佳工艺条件。实验结果表明,当工艺条件为n(对二氯苯)∶n(50%H2O2)∶n(Fe)=1∶3∶0.10、反应温度60℃、反应时间2.5h时,反应效果最佳;产物经GC-MS和1HNMR分析确定为2,5-二氯苯酚,经气相色谱分析,2,5-二氯苯酚选择性达83.4%,收率达42.6%。

关键词: 直接氧化法, 过氧化氢, 对二氯苯, 2,5-二氯苯酚, 选择性

Abstract:

2,5-Dichlorophenol is an important phenolic compound. Regarding the preparation of 2,5-dichlorophenol, most of the preparation methods commonly used in the industry have problems such as long production process and serious pollution. The process of preparing 2,5-dichlorophenol by direct oxidation of dichlorobenzene as raw material and H2O2 as oxidant. The catalysts and solvents were initially screened to investigate the effects of different catalytic systems on the reaction. The process conditions of oxidant dosage, reaction temperature, reaction time and catalyst dosage were determined by using iron powder as catalyst and acetic acid as solvent. The experimental results showed that the best process conditions were n(p-dichlorobenzene)∶n(50% H2O2)∶n(Fe) = 1∶3∶0.10, the reaction temperature was 60℃ and the reaction time was 2.5h. The product was identified as 2,5-dichlorophenol by GC-MS and 1H NMR analysis. The gas chromatographic analysis showed that the selectivity of 2,5-dichlorophenol was 83.4% and the yield of 2,5-dichlorophenol was 42.6%.

Key words: direct oxidation, hydrogen peroxide, p-dichlorobenzene, 2,5-dichlorophenol, selectivity

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