Mozo Mulero Cristina, Sáez Alfonso, Iniesta Jesús, Montiel Vicente
Instituto de Electroquímica, Universidad de Alicante, Apartado 99, 03080 Alicante, Spain.
Beilstein J Org Chem. 2018 Mar 1;14:537-546. doi: 10.3762/bjoc.14.40. eCollection 2018.
The electrocatalytic hydrogenation of benzophenone was performed at room temperature and atmospheric pressure using a polymer electrolyte membrane electrochemical reactor (PEMER). Palladium (Pd) nanoparticles were synthesised and supported on a carbonaceous matrix (Pd/C) with a 28 wt % of Pd with respect to carbon material. Pd/C was characterised by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). Cathodes were prepared using Pd electrocatalytic loadings (L) of 0.2 and 0.02 mg cm. The anode consisted of hydrogen gas diffusion for the electrooxidation of hydrogen gas, and a 117 Nafion exchange membrane acted as a cationic polymer electrolyte membrane. Benzophenone solution was electrochemically hydrogenated in EtOH/water (90/10 v/v) plus 0.1 M HSO. Current densities of 10, 15 and 20 mA cm were analysed for the preparative electrochemical hydrogenation of benzophenone and such results led to the highest fractional conversion (X) of around 30% and a selectivity over 90% for the synthesis of diphenylmethanol upon the lowest current density. With regards to an increase by ten times the Pd electrocatalytic loading the electrocatalytic hydrogenation led neither to an increase in fractional conversion nor to a change in selectivity.
使用聚合物电解质膜电化学反应器(PEMER)在室温和大气压下进行二苯甲酮的电催化氢化反应。合成了钯(Pd)纳米颗粒,并将其负载在含碳基质(Pd/C)上,相对于碳材料,Pd的含量为28 wt%。通过透射电子显微镜(TEM)和热重分析(TGA)对Pd/C进行了表征。使用0.2和0.02 mg cm的Pd电催化负载量(L)制备阴极。阳极由用于氢气电氧化的氢气扩散组成,117 Nafion交换膜用作阳离子聚合物电解质膜。二苯甲酮溶液在乙醇/水(90/10 v/v)加0.1 M HSO中进行电化学氢化。分析了10、15和20 mA cm的电流密度用于二苯甲酮的制备性电化学氢化,结果表明,在最低电流密度下,二苯甲醇合成的最高分数转化率(X)约为30%,选择性超过90%。关于将Pd电催化负载量增加十倍,电催化氢化既未导致分数转化率增加,也未导致选择性改变。