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微通道内连续合成ε-己内酯工艺研究
马 俊,王 菊,储博钊,钟思青
中石化(上海)石油化工研究院有限公司,上海 201208
Process Study on Continuous Synthesis of ε-Caprolactone in Microchannel Reactor
MA Jun, WANG Ju, CHU Bozhao, ZHONG Siqing
SINOPEC Shanghai Research Institute of Petrochemical Technology Company Limited, Shanghai 201208, China
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摘要 在微通道反应器内,以环己酮与自制的过氧丙酸溶液为原料,经Baeyer-Villiger氧化连续合成ε-己内酯。考察了过氧丙酸溶液单股进料工艺中反应温度、停留时间、原料过氧丙酸溶液与环己酮物质的量比及微管管径对合成ε-己内酯过程的影响。结果表明,在反应温度为80 ℃、停留时间为40 min、原料物质的量比为1.17、微管管径在900~2 000 μm时,反应综合指标较好,反应转化率与选择性均超过99%,但过氧酸含量仍偏高。对过氧丙酸溶液进料方式进行优化,结果表明,采用过氧丙酸溶液分段进料工艺更有利于ε-己内酯的工业生产。与传统间歇釜反应工艺相比,微通道反应器提高了ε-己内酯的收率和选择性,缩短了反应时间,实现了连续化操作及安全生产。
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马 俊
王 菊
储博钊
钟思青
关键词 &epsilon-己内酯微通道连续合成环己酮    
Abstract:ε-Caprolactone was synthesized by Baeyer-Villiger oxidization from cyclohexanone and peroxypropionic acid in a continuous flow microchannel reactor. The effects of reaction temperature, residence time, reactants molar ratio and pipe diameter were investigated for the synthesis of ε-caprolactone. The experimental results showed that under the conditions of reaction temperature at 80 ℃, residence time of 40 min, molar ratio of peroxypropionic acid to H2O2 of 1.17, pipe diameter between 900-2 000 μm, conversion of cyclohexanone and yield of ε-caprolactone reached 99%, but the content of peroxy acid in product was still relatively high. Preliminary exploration of non-distributed feeding process of peroxypropionic acid showed better process results. Comparing with the traditional batch reaction process,the selectivities and yields of target products in this continuous microchannel reaction process were increased with shortened reaction time, and process continuity ensured higher operation safety.
Key wordsε-caprolactone    microchannel    continuous synthesis    cyclohexanone   
收稿日期: 2023-07-20     
作者简介: 马 俊(1994—),女,工程师。E-mail: maj.sshy@sinopec.com。
引用本文:   
马 俊,王 菊,储博钊等. 微通道内连续合成ε-己内酯工艺研究[J]. 化学反应工程与工艺, 2024, 40(2): 168-176.
MA Jun,WANG Ju,CHU Bozhao et al. Process Study on Continuous Synthesis of ε-Caprolactone in Microchannel Reactor[J]. Chemical Reaction Engineering and Technology, 2024, 40(2): 168-176.
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