A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H ...A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H 3PW 12 O 40 /SiO 2 was characterized by IR,XRD and TEM.The following optimum condition were that the mole ratio of alcohol to carboxylic acid is 27∶1,the temperature is 75℃,the reaction time is 5 hours,and the catalyst is 2 5% of feedstock.Under the optimum conditions,the yield of esters was above 94%.展开更多
A bimodal mesoporous silica(BMMS) modified with amphiphilic compound(C_(19)H_(42)N)_3(PMo_(12)O_(40))(CTA-PMO) was prepared by the two-step impregnation method. Firstly, H3PMo12O40 was introduced into the bimodal meso...A bimodal mesoporous silica(BMMS) modified with amphiphilic compound(C_(19)H_(42)N)_3(PMo_(12)O_(40))(CTA-PMO) was prepared by the two-step impregnation method. Firstly, H3PMo12O40 was introduced into the bimodal mesoporous silica via impregnation, then C_(19)H_(42)NBr(CTAB) was grafted on the surface of BMMS containing H3PMo12O40 based on the chemical reaction between quaternary ammonium compound and the phosphomolybdic acid, and then the catalyst CTAPMO/BMMS was obtained. The samples were characterized by XRD, N_2 adsorption and desorption, FTIR, 31P-NMR, 29Si-NMR and TEM analyses. It is shown that the catalyst has a typical bimodal mesoporous structure, in which the small mesopore diameter is about 3.0 nm and the large mesopore diameter is about 5.0 nm. The chemical interaction happens between the Keggin structure and silica group of BMMS. Compared with the mono-modal porous Hβ and SBA-15 zeolites modified with CTA-PMO, CTA-PMO/BMMS showed better catalytic activity in the oxidative conversion of dibenzothiophene(DBT), and the desulfurization rate can reach about 94% with the help of extraction, and the catalyst can be separated by filtration and reused directly. The catalytic oxidative desulfurization mechanism on CTA-PMO/BMMS was proposed and verified.展开更多
文摘A nanosolid heteropoly acid of H 3PW 12 O 40 /SiO 2 was prepared with the sol-gel method and used to catalyze sythesis of methyl 5-amino-1,2,4,-trazolylformate sulfate.The structure of the nanosolid heteropoly acid H 3PW 12 O 40 /SiO 2 was characterized by IR,XRD and TEM.The following optimum condition were that the mole ratio of alcohol to carboxylic acid is 27∶1,the temperature is 75℃,the reaction time is 5 hours,and the catalyst is 2 5% of feedstock.Under the optimum conditions,the yield of esters was above 94%.
基金financially supported by the Program for Liaoning Excellent Talents in Universities(LJQ2015062)the Fushun Science Project(FSKJHT201376)
文摘A bimodal mesoporous silica(BMMS) modified with amphiphilic compound(C_(19)H_(42)N)_3(PMo_(12)O_(40))(CTA-PMO) was prepared by the two-step impregnation method. Firstly, H3PMo12O40 was introduced into the bimodal mesoporous silica via impregnation, then C_(19)H_(42)NBr(CTAB) was grafted on the surface of BMMS containing H3PMo12O40 based on the chemical reaction between quaternary ammonium compound and the phosphomolybdic acid, and then the catalyst CTAPMO/BMMS was obtained. The samples were characterized by XRD, N_2 adsorption and desorption, FTIR, 31P-NMR, 29Si-NMR and TEM analyses. It is shown that the catalyst has a typical bimodal mesoporous structure, in which the small mesopore diameter is about 3.0 nm and the large mesopore diameter is about 5.0 nm. The chemical interaction happens between the Keggin structure and silica group of BMMS. Compared with the mono-modal porous Hβ and SBA-15 zeolites modified with CTA-PMO, CTA-PMO/BMMS showed better catalytic activity in the oxidative conversion of dibenzothiophene(DBT), and the desulfurization rate can reach about 94% with the help of extraction, and the catalyst can be separated by filtration and reused directly. The catalytic oxidative desulfurization mechanism on CTA-PMO/BMMS was proposed and verified.