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首次将具有“温控相转移催化”功能的非离子表面活性水溶性膦/铑配合物用于以CO为还原剂的水/有机两相芳香硝基物选择还原反应.以邻氯硝基苯为底物考察了反应温度、CO压力、底物浓度、催化剂浓度和水/有机两相体积比等对反应转化率和选择性的影响.结果表明,当反应条件为 150℃和4 MPa,反应32 h时,邻氯硝基苯的转化率为 98%,邻氯苯胺的选择性接近 100%.动力学研究表明,底物浓度和催化剂浓度分别对反应速率呈一级,反应的表观活化能Ea=131.13 kJ/mol.
For the first time, a non-ionic surface-active water-soluble phosphine / rhodium complex with the function of “temperature controlled phase transfer catalysis” was used for the selective reduction of water / organic two phase aromatic nitroxides with CO as the reducing agent. The effects of reaction temperature, CO pressure, substrate concentration, catalyst concentration and volume ratio of water to organic phase on the reaction conversion and selectivity were investigated using o-chloronitrobenzene as a substrate. The results showed that when the reaction conditions were 150 ℃ and 4 MPa, the conversion of o-chloronitrobenzene was 98% and the selectivity of o-chloroaniline was nearly 100%. Kinetic studies show that the substrate concentration and catalyst concentration, respectively, for the reaction rate was one level, the apparent activation energy Ea = 131.13 kJ / mol.