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Three step synthesis of benzylacetone and 4-(4-methoxyphenyl)butan-2-one in flow using micropacked bed reactors
Chemical Engineering Journal ( IF 13.3 ) Pub Date : 2018-09-18 , DOI: 10.1016/j.cej.2018.09.137
Conor Waldron , Enhong Cao , Stefano Cattaneo , Gemma L. Brett , Peter J. Miedziak , Gaowei Wu , Meenakshisundaram Sankar , Graham J. Hutchings , Asterios Gavriilidis

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.



中文翻译:

使用微填充床反应器三步合成苄基丙酮和4-(4-甲氧基苯基)丁-2-

由苯甲醇合成苄基丙酮和由4-甲氧基苄醇合成4-(4-甲氧基苯基)丁-2-酮(以前以间歇式级联方式进行)在由三个微填充床反应器组成的伸缩式流动系统中成功进行了合成以及用于除去氧气的管中膜。该系统由大约10 mg的1 wt%AuPd / TiO 2催化剂用于氧化,150–250 mg的锐钛矿TiO 2用于C–C偶联和10 mg的1 wt%Pt / TiO 2用于还原的温度分别在115°C,130°C和120°C下运行。氧气和氢气的流速分别为2和1.5 NmL / min,酒精溶液的入口流速为10-80 µL / min,而系统的背压为5 barg。与分批级联反应相比,该系统的苄丙酮收率显着提高(56%比8%),4-(4-甲氧基苯基)丁烷-2-酮的收率略有提高(48%,相比使用相同催化剂时为41%)。支持)。伸缩式流动系统的主要优点是能够分离三个反应,因此每个反应都可以有自己的催化剂和操作条件,从而导致工艺强度的显着提高。

更新日期:2018-09-18
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