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柠檬酸对Ni2P/TiO2-Al2O3催化剂加氢脱硫性能的影响
引用本文:宋华,张永江,宋华林,代敏.柠檬酸对Ni2P/TiO2-Al2O3催化剂加氢脱硫性能的影响[J].物理化学学报,2012,28(3):661-666.
作者姓名:宋华  张永江  宋华林  代敏
作者单位:1. College of Chemistry & Chemical Engineering, Northeast Petroleum University, Daqing 163318, Heilongjiang Province, P. R. China; 2. Provincial Key Laboratory of Oil & Gas Chemical Technology, Northeast Petroleum University, Daqing 163318, Heilongjiang Province, P. R. China; 3. Department of Image School, Mudanjiang Medical University, Mudanjiang 157011, Heilongjiang Province, P. R. China
基金项目:黑龙江省科技厅(2009G0947-00)资助~~
摘    要:采用溶胶-凝胶法制备了TiO2-Al2O3复合载体,以柠檬酸(CA)为络合剂采用浸渍法制备了Ni2P负载的TiO2-Al2O3复合载体催化剂,并用X射线衍射(XRD)、N2吸附比表面积测定、H2程序升温氢还原(H2-TPR)、程序升温氧化(TPO)、X射线光电子能谱(XPS)技术对催化剂的结构和性质进行了表征,考察了CA/Ni摩尔比对在Ni2P/TiO2-Al2O3催化剂上进行的二苯并噻吩(DBT)加氢脱硫(HDS)性能的影响.结果表明:适量的CA可以丰富催化剂的孔道,提高催化剂的比表面积.当n(CA)/n(Ni)=2:1时,催化剂的比表面积达到126.75m2·g-1,与不加CA时相比,提高了57.05m2·g-1.调节n(CA)/n(Ni)能够改善活性相的分布,改变活性相的种类;引入CA使Ni和P前驱体的还原温度明显降低,促进活性相Ni2P的生成,一定程度上能够抑制催化剂表面炭的形成和沉积,提高其稳定性.n(CA)/n(Ni)=2:1时,催化剂具有最好的加氢脱硫活性,在360°C,3.0MPa,氢油比为500(V/V),液时体积空速为2.0h-1的条件下,二苯并噻吩转化率为99.5%,可将模拟油中硫含量由2%(w)降低到0.01%(w).

关 键 词:加氢脱硫  磷化二镍  二氧化钛  三氧化二铝  柠檬酸  络合剂  
收稿时间:2011-08-05
修稿时间:2011-12-29

Effect of Citric Acid on the Hydrodesulfurization Performance of Ni2 P/TiO2 -Al2O3 Catalyst
SONG Hua,ZHANG Yong-Jiang,SONG Hua-Lin,DAI Min.Effect of Citric Acid on the Hydrodesulfurization Performance of Ni2 P/TiO2 -Al2O3 Catalyst[J].Acta Physico-Chimica Sinica,2012,28(3):661-666.
Authors:SONG Hua  ZHANG Yong-Jiang  SONG Hua-Lin  DAI Min
Institution:1. College of Chemistry & Chemical Engineering, Northeast Petroleum University, Daqing 163318, Heilongjiang Province, P. R. China; 2. Provincial Key Laboratory of Oil & Gas Chemical Technology, Northeast Petroleum University, Daqing 163318, Heilongjiang Province, P. R. China; 3. Department of Image School, Mudanjiang Medical University, Mudanjiang 157011, Heilongjiang Province, P. R. China
Abstract:A TiO 2 -Al 2 O 3 complex support was prepared by the sol-gel method.Nickel phosphide catalyst, Ni 2 P/TiO 2 -Al 2 O 3 ,with citric acid(CA)as a chelating agent,was prepared by impregnation.The catalyst was characterized by X-ray diffraction(XRD),BET specific surface area measurements,H 2 -temperature programmed reduction(TPR)and temperature programmed oxidation(TPO),and X-ray photoelectron spectroscopy(XPS).The effects of the molar ratio of CA to Ni on catalyst activity for hydrodesulfurization (HDS)of dibenzothiophene(DBT)were studied.Addition of an appropriate amount of CA into the catalyst can change the pores of the Ni 2 P/TiO 2 -Al 2 O 3 catalyst,increasing the surface area.The specific surface area reached 126.75 m 2 ·g -1 for n(CA)/n(Ni)of 2/1,an improvement of 57.05 m 2 ·g -1 compared with the catalyst without CA.Regulating n(CA)/n(Ni)can improve the distribution of the active phase and change the active phase species.Addition of CA decreased the temperature required for reduction of nickel and the phosphorus precursor,as well as promoting the formation of the active phase.CA can limit the deposition of carbon on the catalyst surface to some extent,improving its stability.A molar ratio of n(CA)/n(Ni)of 2/1 was found to be optimal for the catalytic activity of the Ni 2 P/TiO 2 -Al 2 O 3 catalyst prepared with CA as a chelating agent.At a reaction temperature of 360°C,pressure of 3.0 MPa,hydrogen/oil ratio of 500(V/V), and liquid hourly space velocity of 2.0 h -1 ,the HDS conversion of DBT was 99.5%,which can reduce the sulfur content of a model oil from 2%(w)to 0.01%(w).
Keywords:Hydrodesulfurization  Nickel phosphide  Titanium dioxide  Al 2 O 3  Citric acid  Chelating agent
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