Solid acid catalyst plays a crucial role in the petroleum refinery industry and bio-refinery technology.In this work,p-phenolsulfonic acid(PSA)was successfully grafted onto the surface of KH560-modified zirconium phos...Solid acid catalyst plays a crucial role in the petroleum refinery industry and bio-refinery technology.In this work,p-phenolsulfonic acid(PSA)was successfully grafted onto the surface of KH560-modified zirconium phosphate(K-ZrP)in a facile routine.The structure and property of this organic-inorganic combined solid acid PSA/K-ZrP-x were characterized via XRD,FTIR,^(13)C solid-state NMR,TG,N_(2) adsorption-desorption,SEM,pyridine-adsorption FTIR and XPS technologies.The characterization results showed that KH560 can bond with ZrP and promote the grafting of PSA on the surface of K-ZrP via the condensation reaction between its epoxy ring and the phenolic hydroxyl group in PSA.Consequently,PSA/K-ZrP-2 exhibited excellent performance and stability in the transesterification between glycerol and methyl acetate among the tested H_(3)PW_(12)O_(40),Amber-lyst-45,HBEA,HZSM-5,ZrP,AlCl_(3) and FeCl_(3) catalysts.The calculated conversion of glycerol reached 81.3%with a 97.9%selectivity for monoacetin(MAG)and diacetin(DAG)with a 2.2%dosage of[H^(+)]at 100℃ for 4 h.The highest specific activity of PSA/K-ZrP-2 reached 24028.2 mg-glycerol/g-cat/h in a short reaction time(at 0.17 h),and it could be recycled five times without obvious deactivation.展开更多
文摘Solid acid catalyst plays a crucial role in the petroleum refinery industry and bio-refinery technology.In this work,p-phenolsulfonic acid(PSA)was successfully grafted onto the surface of KH560-modified zirconium phosphate(K-ZrP)in a facile routine.The structure and property of this organic-inorganic combined solid acid PSA/K-ZrP-x were characterized via XRD,FTIR,^(13)C solid-state NMR,TG,N_(2) adsorption-desorption,SEM,pyridine-adsorption FTIR and XPS technologies.The characterization results showed that KH560 can bond with ZrP and promote the grafting of PSA on the surface of K-ZrP via the condensation reaction between its epoxy ring and the phenolic hydroxyl group in PSA.Consequently,PSA/K-ZrP-2 exhibited excellent performance and stability in the transesterification between glycerol and methyl acetate among the tested H_(3)PW_(12)O_(40),Amber-lyst-45,HBEA,HZSM-5,ZrP,AlCl_(3) and FeCl_(3) catalysts.The calculated conversion of glycerol reached 81.3%with a 97.9%selectivity for monoacetin(MAG)and diacetin(DAG)with a 2.2%dosage of[H^(+)]at 100℃ for 4 h.The highest specific activity of PSA/K-ZrP-2 reached 24028.2 mg-glycerol/g-cat/h in a short reaction time(at 0.17 h),and it could be recycled five times without obvious deactivation.