微反应器中双氧水氧化丙烯酸制备乙醛酸的研究

周林利, 张跃, 娄喜营, 严生虎, 辜顺林, 刘建武

现代化工 ›› 2021, Vol. 41 ›› Issue (12) : 165 -169.

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现代化工 ›› 2021, Vol. 41 ›› Issue (12) : 165-169. DOI: 10.16606/j.cnki.issn0253-4320.2021.12.033
科研与开发

微反应器中双氧水氧化丙烯酸制备乙醛酸的研究

    周林利, 张跃, 娄喜营, 严生虎, 辜顺林, 刘建武
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Preparation of glyoxylic acid via oxidation of acrylic acid by hydrogen peroxide in microreactor

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摘要

以丙烯酸(C3H4O2)为原料、H2O2为氧化剂、V2O5和H3PW12O40为组合催化剂,设计了在微反应器中液相氧化合成乙醛酸的连续流工艺。分别考察了物料摩尔比、催化剂种类、催化剂物质的量、反应停留时间、反应温度、H2O2质量分数等对反应的影响。结果表明,在管式反应器中,n(C3H4O2):n(H2O2):n(V2O5):n(H3PW12O40)=1:6:0.025:0.012 5、反应温度为55℃、反应停留时间为6.5 min、H2O2质量分数为35%时,丙烯酸转化率达97.1%,乙醛酸选择性达91.4%。与间歇氧化反应相比,连续流反应具有反应效率高、时间短、安全性高以及容易控制流态等优点,消除了氧化过程中双氧水分解带来的安全隐患,实现了乙醛酸的绿色安全生产。

Abstract

A continuous flow process is designed for the synthesis of glyoxylic acid through liquid phase oxidation process in a microreactor with acrylic acid as raw material, H2O2 as oxidant, V2O5 and H3PW12O40 as a combined catalyst.The effects of material ratio, catalyst type, catalyst dosage, reaction residence time, reaction temperature and H2O2 concentration on the reaction are investigated.It is shown that the conversion rate of acrylic acid reaches 97.1% and the selectivity of glyoxylic acid reaches 91.4% in a tubular microreactor when n(acrylic acid):n(35%H2O2):n(V2O5):n(H3PW12O40)=1:6:0.025:0.012 5, reaction temperature is at 55℃, reaction residence time is 6.5 min, and H2O2 concentration (mass fraction) is 35%.Compared with a batch oxidation process, the continuous flow process has the advantages of high reaction efficiency, short time, high safety and easy to control the flow state, which eliminates the potential safety hazard caused by the decomposition of hydrogen peroxide in the oxidation process, and realizes the green and safe production of glyoxylic acid.

关键词

丙烯酸 / 连续流 / 氧化 / 乙醛酸

Key words

acrylic acid / continuous flow / oxidation / glyoxylic acid

Author summay

周林利(1995-),女,硕士研究生,研究方向为流动化学和过程工程,1790841301@qq.com

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微反应器中双氧水氧化丙烯酸制备乙醛酸的研究[J]. 现代化工, 2021, 41(12): 165-169 DOI:10.16606/j.cnki.issn0253-4320.2021.12.033

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