化工进展 ›› 2020, Vol. 39 ›› Issue (12): 5228-5233.DOI: 10.16085/j.issn.1000-6613.2020-0292

• 精细化工 • 上一篇    下一篇

循环微反应系统内间甲基苯甲醚的合成

王德强1(), 王金婷1, 王凯2(), 骆广生2   

  1. 1.潍坊科技学院,山东半岛卤水资源高值化绿色化综合利用工程技术研发中心,山东 潍坊 262700
    2.清华大学化工系,化学工程联合国家重点实验室,北京 100084
  • 出版日期:2020-12-05 发布日期:2020-12-02
  • 通讯作者: 王凯
  • 作者简介:王德强(1973—),男,博士,讲师,研究方向为有机合成。E-mail:ciacwdq@163.com
  • 基金资助:
    国家自然科学基金(21991104);山东省重大科技创新工程(2019JZZY020401)

Synthesis of m-methylanisole in a cycled microreactor system

Deqiang WANG1(), Jinting WANG1, Kai WANG2(), Guangsheng LUO2   

  1. 1.Shandong Peninsula Engineering Research Center of Comprehensive Brine Utilization, Weifang University of Science and Technology, Weifang 262700, Shandong, China
    2.State Key Lab of Chemical Engineering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
  • Online:2020-12-05 Published:2020-12-02
  • Contact: Kai WANG

摘要:

间甲基苯甲醚是一种染料中间体,其传统合成方法是通过低温控制反应物混合,生产效率低下,通过微反应器改善反应物混合具有重要的研究价值。本文系统研究了微反应器辅助下的间甲基苯甲醚合成过程,发现体系内间甲酚与氢氧化钠可快速发生反应,形成间甲酚钠,进而发现间甲酚钠与硫酸二甲酯间的氧烷基化反应随着反应温度的提升而获得强化,60~80℃的高温更有利于氧烷基化反应与硫酸二甲酯水解反应的竞争。通过实验考察了反应物流量比、计量比、浓度等因素对间甲基苯甲醚收率的影响,发现微反应器保证两相反应物的快速均匀混合是成功实施高温快反应的关键。相对优化的实验结果表明:当硫酸二甲酯/间甲酚摩尔比大于1.05时,使用质量分数为30%的氢氧化钠溶液实施间甲基苯甲醚的合成反应的产率可达99%以上。

关键词: 微反应器, 微通道, 间甲基苯甲醚

Abstract:

M-methylanisole is a dye intermediate. Its traditional synthesis method controls the mixing of reactants by low temperature, and the production efficiency is low. Improving the mixing of reactants through microreactors has important research value. The synthesis process of m-methylanisole with the aid of a microreactor was systematically studied, and it was found that m-cresol and sodium hydroxide reacted quickly to form sodium m-cresol in the reaction system. The oxyalkylation reaction between sodium m-cresol and dimethyl sulfate could be enhanced with the increase of the reaction temperature, and therefore the high temperature of 60—80℃ was more beneficial for the oxyalkylation reaction to compete with the hydrolysis of dimethyl sulfate. The effects of reactant flow ratio, metering ratio, concentration and other factors on the yield of m-methylanisole were investigated, and it was found that the microreactor to ensure the rapid and uniform mixing of the two-phase reactants was crucial for the success of fast and high temperature reaction. The relatively optimized experimental results showed that the yield of m-methylanisole reached more than 99% as the molar ratio of dimethyl sulfate to m-cresol was greater than 1.05 and 30% sodium hydroxide solution was used during the reaction.

Key words: microreactor, microchannel, m-methylanisole

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