Epoxidation of methyl oleate in a TiO2 coated-wall capillary microreactor
Epoxidation of methyl oleate in a TiO2 coated-wall capillary microreactor
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DOI：
10.1016/j.cej.2016.12.017
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发表时间：
2017-04
影响因子：
15.1
通讯作者：
Songphon Phimsen;H. Yamada;T. Tagawa;W. Kiatkittipong;K. Kiatkittipong;N. Laosiripojana;S. Assabumrungrat
中科院分区：
文献类型：
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作者：
Songphon Phimsen;H. Yamada;T. Tagawa;W. Kiatkittipong;K. Kiatkittipong;N. Laosiripojana;S. Assabumrungrat
在本工作中，开发了一种用于在无溶剂体系中生产环氧化油酸甲酯的催化涂层壁式微反应器并进行了测试。采用静态方法在微毛细管反应器内壁涂覆二氧化钛，氧化剂为过氧化氢，稳定剂为乙二胺四乙酸乙酯。根据ASTM D1652确定了环氧乙烷的质量分数，并以环氧乙烷的产率和选择性作为反应性能的评价指标。在没有二氧化钛包覆催化剂和甲酸的情况下，得到了痕量环氧乙烷的产率。在没有EDTA作为稳定剂的情况下，过氧化氢的分解以气泡的形式发生，导致系统运行失败。结果表明，二氧化钛负载催化剂以及EDTA和甲酸的存在对环氧化反应是至关重要的，在最佳反应温度为60℃、停留时间为2.7min时，环氧乙烷的产率可达43.1%。并将计算结果与间歇反应器的实验数据进行了比较。微毛细管反应器提供连续操作，环氧化物生产的反应速度是间歇式反应器的23倍。然而，3h后，TiO2涂层部分剥落，导致环氧化物产率下降。
In the present work, a catalytic coated-wall microreactor was developed and tested for producing epoxidized methyl oleate in a solvent-free system. TiO2was coated inside the microcapillary reactor wall by a static method, while H2O2and ethylenediaminetetraacetic acid (EDTA) were used as oxidant and stabilizer, respectively. The weight percent of oxirane oxygen was determined according to ASTM D1652 and the reaction performance was evaluated as oxirane oxygen yield and selectivity. Without TiO2coated catalyst or formic acid, trace oxirane yield were obtained. Without EDTA as stabilizer, decomposition of H2O2occurred as bubbles formation causing system operation failure. The results indicated that TiO2coated catalyst as well as the presences of EDTA and formic acid were crucial for epoxidation reaction, and oxirane yield of 43.1% could be achieved at the optimal reaction temperature of 60 °C and residence time of 2.7 min. The results were compared with the data obtained from a batch reactor. Microcapillary reactor offers continuous operation with 23 times higher reaction rate of epoxide production than batch reactor. However, TiO2coated layer was partially peeled off over 3 h lead to decrease in epoxide yield.