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采用椰壳活性炭为载体,通过20%HNO3氧化处理,Boehm滴定表明活性炭表面羟基含量达0.376 mmol/g.之后分别接枝(MeO)3Si(CH2)3NH2和(MeO)3Si(CH2)3Cl,并成功合成了两种不同类型的含氮双齿配体用来配合钯离子,以FT-IR、XPS、1H NMR、ICP及N2吸附-脱附等手段表征了催化剂制备过程中的各种中间体.在高压反应釜中以苯酚氧化羰基化反应考察了所制催化剂的催化性能.结果表明,在100℃,7.0 MPa及p(CO)/p(O2)=10/1下,二氯甲烷为溶剂,以环庚二胺配体配合的钯离子为催化剂,苯酚转化率及产物碳酸二苯酯(DPC)选择性分别为11.91%、86.82%,对于双氰基配体配合的催化剂,苯酚转化率及产物DPC选择性分别为6.22%及81.02%.
Using coconut shell activated carbon as carrier, Boehm titration showed that the hydroxyl content of the activated carbon reached 0.376 mmol / g by 20% HNO3 oxidation and then grafted with (MeO) 3Si (CH2) 3NH2 and (MeO) 3Si Two different types of nitrogen-containing bidentate ligands were successfully synthesized for the coordination with palladium ions. Various intermediates in the preparation of catalysts were characterized by FT-IR, XPS, 1H NMR, ICP and N2 adsorption-desorption The catalytic performance of the prepared catalyst was investigated by oxidative carbonylation of phenol in high pressure autoclave.The results showed that at 100 ℃, 7.0 MPa and p (CO) / p (O2) = 10/1, Solvent and palladium ion with cycloheptamethylenediamine ligand as catalyst, the conversion of phenol and the selectivity of DPC were 11.91% and 86.82%, respectively. For the catalyst with dicyano ligand, the conversion of phenol The DPC selectivity and product selectivity were 6.22% and 81.02%, respectively.