Citation: SONG Hua, ZHANG Fu-yong, SONG Hua-lin, DAI Min, WAN Xia, XU Xiao-wei. Preparation of supported nickel phosphide catalyst by solvothermal method and its hydrodesulfurization performance[J]. Journal of Fuel Chemistry and Technology, ;2015, 43(6): 714-719. shu

Preparation of supported nickel phosphide catalyst by solvothermal method and its hydrodesulfurization performance

SONG Hua ^1,2,, ,
ZHANG Fu-yong ¹ ,
SONG Hua-lin ^2,, ,
DAI Min ^1,3 ,
WAN Xia ^1,3 ,
XU Xiao-wei ¹

1.
1. Provincial Key Laboratory of Oil & Gas Chemical Technology, Northeast Petroleum University, Daqing 163318, China;

Corresponding author: SONG Hua, SONG Hua-lin,
Received Date: 27 February 2015
Available Online: 13 April 2015
Fund Project: 国家自然科学基金(21276048) (21276048)黑龙江省自然科学基金(ZD201201) (ZD201201)黑龙江省教育厅项目(12541060)。 (12541060)

The supported Ni₂P/MCM-41 catalyst was prepared by a solvothermal method using triphenylphosphine (TPP) as a cheap phosphorus material and tri-n-octylamine (TOA) as the coordinating liquid reaction system. The catalysts were characterized by X-ray diffraction (XRD), N₂-adsorption, CO uptake, X-ray photoelectronspectroscopy (XPS) and transmission electron microscopy (TEM). The solvothermal synthesis was performed at atmospheric pressure and 330 ℃, at least 300 ℃ lower than the temperature for preparing the corresponding catalysts by temperature-programmed reduction (H₂-TPR) method. The structure and hydrodesulfurization (HDS) performance of the as-prepared Ni₂P/MCM-41 catalyst are compared with those prepared by H₂-TPR, with dibenzothiophene (DBT) as a model compound. The results showed that the solvothermal method can decrease the aggregation of P species on the catalyst surface so as to achieve a Ni₂P catalyst with high surface area (690 m²/g) and then promote the formation of small and highly dispersed Ni₂P active phase. The catalyst from solvothermal synthesis exhibits distinctly a superior HDS performance to that prepared by H₂-TPR method. Under the conditions of 340 ℃, 3.0 MPa, a H₂/oil volume ratio of 500(volume ratio), and a weight hourly space velocity (WHSV) of 2.0 h^-1, the conversion of DBT reaches 96.8% over the catalyst from solvothermal synthesis, which is 10.6% higher than that over the catalyst prepared via H₂-TPR.
- solvothermal method,
- nickel phosphide,
- dibenzothiophene (DBT),
- hydrodesulfurization (HDS)
1. [1]
  [1] SONG C S. An overview of new approaches to deep desulfurization for ultra-clean gasoline, diesel fuel and jet fuel[J]. Catal Today, 2003, 86(1/4): 211-263.
2. [2]
  [2] KORANYI T I. Phosphorus promotion of Ni(Co)-containing Mo-free catalysts in thiophene hydrodesulfurization[J]. Appl Catal A: Gen, 2003, 239(1/2): 253-267.
3. [3]
  [3] 宋华, 代敏, 宋华林. Ni₂P加氢脱硫催化剂[J]. 化学进展, 2012, 24(5): 43-47. (SONG Hua, DAI Min, SONG Hua-lin. Ni₂P catalyst for hydrodesulfurization[J]. Prog Chem, 2012, 24(5): 43-47.)
4. [4]
  [4] LEE Y K, SHU Y Y, OYAMA S T. Active phase of a nickel phosphide (Ni₂P) catalyst supported on KUSY zeolite for the hydrodesulfurization of 4,6-DMDBT[J]. Appl Catal A: Gen, 2007, 322: 191-204.
5. [5]
  [5] GUAN J, WANG Y, QIN M, YANG Y, LI X, WANG A J. Synthesis of transition-metal phosphides from oxidic precursors by reduction in hydrogen plasma[J]. J Solid State Chem, 2009, 182(6): 1550-1555.
6. [6]
  [6] SONG H, DAI M, SONG H L, WAN X, XU X W. A novel synthesis of Ni₂P/MCM-41 catalysts by reducing a precursor of ammonium hypophosphite and nickel chloride at low temperature[J]. Appl Catal A: Gen, 2013, 462-463: 247-255.
7. [7]
  [7] WU P Y, LI Q Y, LAN L, LIU H F, JU Y N, PIAO J R, JI S F. Preparation, structure characterization and hydrodesulfurization performance B-Ni₂P/SBA-15/cordierite monolithic catalysts[J]. Chin J Chem Eng, 2014, 22: 903-908.
8. [8]
  [8] CHEN Y Z, SHE H D, LUO X H, YUE G H, PENG D L. Solution-phase synthesis of nickel phosphide single-crystalline nanowires[J]. J Crystal Growth, 2009, 311(4): 1229-1233.
9. [9]
  [9] 宋华, 王紫东, 代敏, 宋华林, 万霞, 李锋. Ni₂P催化剂的低温还原法合成及其HDS性能[J]. 燃料化学学报, 2014, 42(6): 733-737. (SONG Hua, WANG Zi-dong, DAI Min, SONG Hua-lin, WAN Xia, LI Feng. Preparation of Ni₂P catalysts at low reduction temperature and its HDS performance[J]. J Fuel Chem Technol, 2014, 42(6): 733-737.)
10. [10]
  [10] MELÉNDEZ-ORTIZ H I, CARCÍA-CERDA L A, OLIVARES-MALDONADO Y, CASTRUITA G, MERCADO-SILVA J A, PERERA-MERCADO Y A. Preparation of spherical MCM-41 molecular sieve at room temperature: Influence of the synthesis conditions in the structural properties[J]. Ceram Int, 2012, 38(8): 6353-6358.
11. [11]
  [11] SONG H, DAI M, SONG H L, WAN X, XU X W, JIN Z S. A solution-phase synthesis of supported Ni₂P catalysts with high activity for hydrodesulfurization of dibenzothiophene[J]. J Mol Catal A: Chem, 2014, 385: 149-159.
12. [12]
  [12] SONG H, DAI M, GUO Y T, ZHANG Y J. Preparation of composite TiO₂-Al₂O₃ supported nickel phosphide hydrotreating catalysts and catalytic activity for hydrodesulfurization of dibenzothiophene[J]. Fuel Process Technol, 2012, 96(48): 228-236.
13. [13]
  [13] OYAMA S T, WANG X, LEE Y, BANDO K, REQUEJO F G. Effect of phosphorus content in nickel phosphide catalysts studied by XAFS and other techniques[J]. J Catal, 2002, 210(1): 207-217.
14. [14]
  [14] LAYMAN K A, BUSSELL M E. Infrared spectroscopic investigation of CO adsorption on silica-supported nickel phosphide catalysts[J]. J Phys Chem B, 2004, 108(30): 10930-10941.
15. [15]
  [15] OYAMA S T. Novel catalysts for advanced hydroprocessing: Transition metal phosphides[J]. J Catal, 2003, 216(1/2): 343-352.
16. [16]
  [16] LEE Y K, SHU Y Y, OYAMA S T. Active phase of a nickel phosphide (Ni₂P) catalyst supported on KUSY zeolite for the hydrodesulfurization of 4,6-DMDBT[J]. Appl Catal A: Gen, 2007, 322: 191-204.
17. [17]
  [17] OYAMA S T, LEE Y K. The active site of nickel phosphide catalysts for the hydrodesulfurization of 4,6-DMDBT[J]. J Catal, 2008, 258(2): 393-400.
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