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Study of Supported Heteropoly Acid Catalysts for Catalytic Oxidation Desulfurization

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Tutor: KangLiHua
School: Shihezi University
Course: Applied Chemistry
Keywords: HPW-TUD-1,[Bmim]PW/HMS,catalytic oxidation desulfurization
CLC: TE624.55
Type: Master's thesis
Year:  2013
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Abstract:
Facing the increasingly serious environmental problems and the global resources shortage, countriesall over the world for the sulfur content in fuel oil are made strict rules, thus improve the quality of the oiland how to improve the product quality problems one after another. And the thiophene compounds in theoil and its derivatives is the main form of sulfides in petroleum, such hydrodesulfurization difficult to byremoving sulfide, and hydrodesulfurization should be carried out under high temperature and high pressure.It brought many restrictions to hydrodesulfurization, so non-hydrodesulfurization caused the researchers ofgreat interest. The catalytic oxidation desulfurization because of its mild reaction condition, high activity,simple equipment and low cost of desulfurization is considered as the most potential future desulfurizationmethod.On the choice of catalytic oxidation desulfurization catalyst is the focal point. In this paper, from theaspects of environment and the cost of desulfurization, choose the present study is relatively extensivegreen environmentally friendly material, molecular sieves, heteropoly acid and ionic liquids used ascatalyst for the preparation of raw materials, synthesis of green and highly active, catalyst can be recycled,has sought to reach the purpose of deep oxidation desulfurization. This thesis mainly studies the followingseveral aspects:(1) By incorporating H3PW12O40(HPW) heteropolyacid into mesoporous TUD-1materials, a series ofHPW-TUD-1catalysts were synthesized. Nitrogen adsorption-desorption isotherm, XRD and FTIRcharacterizations showed that these catalyst exhibited mesoporous structure, and HPW presented in thecatalysts with Keggin structure. The catalytic performances of the HPW-TUD-1catalysts were testedthrough the oxidative desulfurization (ODS) process of dibenzothiophene (DBT) model oil. The resultsshowed that the obtained20HPW-TUD-1catalyst displayed excellent catalytic activity and recover abilityfor ODS. The desulfurization rate of DBT reached up to98.1%, and almost no catalytic activity loss wasobserved after three recycles of the catalyst.(2)[Bmim]PW/HMS catalyst was synthesized through impregnating the hexagonal mesoporous silica(HMS) support by phosphotungstic acid (HPW) and ionic liquid [Bmim]HSO4. At the same time, thephysical structure and chemical composition of the catalysts were characterizated by a series of analyticalinstruments. Physical structure characterizations of the catalysts showed that HMS retained mesoporousstructure, and [Bmim]PW was well dispersed on the support of HMS. The activities of catalysts, theoptimum reaction conditions and recycling of the catalysts were investigated by catalytic oxidationdesulfurization for model oil. Results showed that the optimal reaction conditions is loading of catalyst=20%, O/S molar ratio=3, catalyst=0.06g/10mL, temperature at60℃. Under the optimal reactionconditions, the conversion of benzothiophene (BT), dibenzothiophene (DBT) and4,6-dimethyldibenzothiophene (4,6-DMDBT) could reach79%,98%,88%, respectively. And catalyticactivity loss was observed after three recycles of the catalyst. At different aging temperatures preparationcarrier Hx (x for aging temperature), get [Bmim] PW/Hx series catalyst used in the catalytic oxidationdesulfurization reaction system, and its physical structure were characterized by BET. Results showed thatcatalyst pore size increased with aging temperature, active with the decrease of pore size increases.
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