模板法制备催化剂PW12@Fe-TiO2及其催化氧化脱硫性能  

Preparation of PW12@Fe-TiO2 catalyst by template method and its catalytic oxidative desulfurization performances

作　　者：高洪成[1] 高爽 吴效楠[1] 薛伟[1] 于雅潇[1] 马丽雅[1] GAO Hong-cheng;GAO Shuang;WU Xiao-nan;XUE Wei;YU Ya-xiao;MA Li-ya(Department of Chemical Engineering,Chengde Petroleum College,Chengde 067000,China;Department of Chemical and Environmental Engineering,Yingkou Institute of Technology,Yingkou 115000,China)

机构地区：[1]承德石油高等专科学校化学工程系,河北承德067000 [2]营口理工学院化学与环境工程系,辽宁营口115000

出　　处：《化学研究与应用》2020年第6期963-970,共8页Chemical Research and Application

基　　金：河北省自然科学青年基金(B2017411009)资助。

摘　　要：采用模板法一步合成了一类多酸基PW12@Fe-TiO2材料,利用Raman、XRD、XPS和SEM表征手段对材料进行了结构表征。结果表明,磷钨酸(PW12)被包埋到Fe-TiO2中,形成球形结构。N2吸附-脱附测试显示,PW12@Fe-TiO2为介孔材料:孔径尺寸为4.1nm,比表面积为30.3m^2·g^-1。所合成材料作为催化剂,以H2O2为氧化剂,乙腈为溶剂,在模拟油的氧化脱硫反应体系中表现出较好的催化性能。当PW12@Fe-TiO2的加入量为40mg,反应底物为5.0mL,反应温度60℃,反应到40min时,DBT的去除率到达了99.9%。中断和循环实验结果表明,催化剂PW12@Fe-TiO2具有良好的稳定性,在相似的反应条件下,循环使用5次,催化剂的催化活性依然保持不变。A polyoxometalate-based material has been synthesized by the one-step template,denoted as PW [e-mail] characterization methods namely Raman,XRD,XPS and SEM were used to characterize the resultant materials,and results indicated that phosphotungstic acid(PW12)is introduced into Fe-TiO2,forming spherical structure.N2 adsorption-desorption test showed that PW 12@Fe-TiO2 was mesoporous material with pore size of 4.1 nm and specific surface area of 30.3 m^2·g^-1.The resultant material was used as catalyst for the oxidative desulfurization of model oil,and exhibited good catalytic activity with H2O2 as oxidant and acetonitrile as solvent.The S-removal of DBT reached 99.9%after 40 min reaction at a temperature of 60℃ when dosage of catalyst PW12@Fe-TiO2 was 40 mg and reaction substrate was 5.0 mL.Leaching and recycling experiments revealed that catalyst PW12@Fe-TiO2 has excellent stability,and catalytic activities of the catalyst remain unchanged after five cycles under identical reaction conditions.

关 键 词：模板法 多金属氧酸盐 过渡金属 多相催化 氧化脱硫 

分 类 号：O643.3[理学—物理化学]