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《Chinese Journal of Catalysis》 2003-06
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Hydrothermal Deactivation of USY/ZnO/Al_2O_3 Additive for Sulfur Removal of FCC Gasoline

LI Chunyi 1* , YUAN Qimin 1, PANG Xinmei 2, YANG Hongyan 1, SHAN Honghong 1, YANG Chaohe 1, ZHANG Jianfang 1(1 State Key Laboratory of Heavy Oil Processing, College of Chemistry and Chemical Engineering, University of Petroleum, Dongying 257061, Shandong, China; 2 Petrochemical Research Institure, Lanzhou Petrochemical Company, PetroChina Company Limited, Lanzhou 730060, Gansu, China)  
Using additives for sulfur removal to reduce sulfur content of FCC (fluid catalytic cracking) gasoline during the in situ FCC process is the cheapest route to desulfurization. The USY/ZnO/Al 2O 3 additive we developed can reduce more than 30% of sulfur (400 μg/g ) in gasoline. However, the hydrothermal treatment at high temperature may cause deactivation of the additive. After the fresh additive is aged at 800 ℃ with 100% steam, the micro activity and sulfur removal activity drop significantly. In this paper, the reasons for the hydrothermal deactivation of the additive were investigated by FT IR and XRD techniques. The experiments show that hydrothermal aging at 800 ℃ with 100% steam leads to a decrease in the surface area of the additive by about 50%, the framework collapse of the cracking component USY, the disappearance of ZnO, and a drop of the Lewis and Brnsted acid amounts by 91% and 96%, respectively. These changes may be caused by the strong interactions between USY and ZnO. The experiments that USY/ZnO samples were calcined at various temperatures and then analyzed by XRD show that the destruction of USY by ZnO becomes more and more serious with increasing temperature over 650 ℃. ZnO can capture the framework Al of USY to form inert ZnAl 2O 4 spinel and cause the collapse of the framework. When the content of ZnO in the samples is enough, ZnO can react with the Si in the collapsed framework to form Zn 2SiO 4 willemite. Here, the interactions between ZnO and USY depend on temperature and seemingly have nothing to do with steam. For the USY/ZnO/Al 2O 3 additive, high temperature alone cannot cause the serious destruction of the additive. With the participation of steam, however, both USY and ZnO disappear after aging. The reason is that there is a thin layer spinel film between the ZnO particles and the support Al 2O 3, and the film can fix the ZnO particles and isolate them from the USY particles. At high temperature steam can promote the ZnO particles to break away from the bondage of the film to contact and destroy USY. Therefore, the deactivation of USY/ZnO/Al 2O 3 is caused by the solid phase reactions between USY and ZnO, which can be promoted by steam, to form inert ZnAl 2O 4 spinel and Zn 2SiO 4 willemite. How to depress these reactions is the key to improve the stability of the additive.
【Fund】: 中国石油天然气股份有限公司资助项目 ( 0 10 3 0 2 0 6)
【CateGory Index】: TE624.9
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