Three step synthesis of benzylacetone and 4-(4-methoxyphenyl)butan-2-one in flow using micropacked bed reactors
Three step synthesis of benzylacetone and 4-(4-methoxyphenyl)butan-2-one in flow using micropacked bed reactors
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使用微填充床反应器连续三步合成苄基丙酮和4-(4-甲氧基苯基)丁-2-酮
DOI：
10.1016/j.cej.2018.09.137
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发表时间：
2019
影响因子：
15.1
通讯作者：
Waldron C
中科院分区：
文献类型：
--
作者：
Waldron C
在由3个微填充床反应器和一个管中膜组成的伸缩流系统中，成功地完成了由苯甲醇合成苯丙酮和由4-甲氧基苯甲醇合成4-（4-甲氧基苯基）丁烷-2- 1的过程。该系统由约10 mg 1 wt%的AuPd/TiO2催化剂组成，用于氧化，150-250 mg锐钛矿TiO2用于C - C偶联，10 mg 1 wt%的Pt/TiO2用于还原，分别在115°C， 130°C和120°C下工作。氧气和氢气流量分别为2和1.5 NmL/min，酒精溶液进口流量为10-80µL/min，系统在5 bar的背压下工作。与间歇级联相比，该系统显著提高了苯丙酮的收率（56%比8%），并略微提高了4-（4-甲氧基苯基）丁烷-2- 1的收率（48%比41%，使用相同的催化剂载体）。伸缩流系统的主要优点是能够将三种反应分离开来，这样每个反应都可以有自己的催化剂和操作条件，这导致了显著的过程强化。
The synthesis of benzylacetone from benzyl alcohol and of 4-(4-methoxyphenyl)butan-2-one from 4-methoxybenzyl alcohol, which were previously performed in a batch cascade, were successfully performed in a telescoped flow system consisting of three micropacked bed reactors and a tube-in-tube membrane to remove oxygen. The system consisted of approximately 10 mg of 1 wt% AuPd/TiO2 catalyst for oxidation, 150–250 mg of anatase TiO2 for C–C coupling and 10 mg of 1 wt% Pt/TiO2 for reduction, operating at 115 °C, 130 °C and 120 °C respectively. Oxygen and hydrogen flowrates were 2 and 1.5 NmL/min and alcohol solution inlet flowrates were 10–80 µL/min, while the system operated at a back pressure of 5 barg. This system achieved significantly increased yields of benzylacetone compared to the batch cascade (56% compared to 8%) and slightly increased yields of 4-(4-methoxyphenyl)butan-2-one (48% compared to 41% when using the same catalyst supports). The major advantage of the telescoped flow system was the ability to separate the three reactions, so that each reaction could have its own catalyst and operating conditions, which led to significant process intensification.
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