Schiff碱Pd(Ⅱ)配合物催化剂的制备及其在苯酚氧化羰基化反应中的应用

Preparation of Schiff Base Pd(Ⅱ)Complex and Its Application in the Oxidative Carbonylation of Phenol to Diphenyl Carbonate

以水杨醛和对氨基苯甲酸为原料合成了水杨醛缩对氨基苯甲酸配体(SP),SP再与Pd(Ⅱ)配位得到了相应的钯配合物(Pd(SP)2).采用UV-vis、FT-IR、1 H-NMR、ICP等表征方法对配体及配合物的结构进行了表征.将Pd(SP)2用于苯酚氧化羰基化制备碳酸二苯酯反应中,讨论了助剂铜加入量、助剂铜钴锰复合氧化物加入量、反应时间、反应温度和反应压力对Pd(SP)2催化活性的影响.实验结果表明,在铜加入量0.05g、铜钴锰复合氧化物加入量0.5g、反应时间8h、反应温度110℃、反应压力4.5 MPa时,碳酸二苯酯的收率和选择性分别为51.7%和64.9%.

Salicylaldehyde-4-aminobenzoic acid schiff base palladium complex（Pd（SP）2）was synthesized through the coordination reaction of Pd（Ⅱ）with salicylaldehyde-4-aminobenzoic acid schiff base ligand（SP）which was synthesized from 4-aminobenzoic and salicylaldehyde.SP and Pd（SP）2 were characterized by means of UV-vis、FT-IR、1 H-NMR and ICP.The effects of Cu（OAc）2dosage,Cu-Co-Mn mixed oxide dosage,reaction time,reaction temperature and reaction pressure on the catalytic performance of Pd（SP）2in the oxidative carbonylation of phenol to diphenyl carbonate were studied.The results showed that the yield and selectivity of DPC reached 51.7% and 64.9%,respectively,under the reaction conditions of Cu（OAc）2dosage 0.05 g,Cu-Co-Mn mixed oxide dosage 0.5g,reaction pressure 4.5 MPa,reaction temperature 110 ℃ and reaction time 8h.