磷镍物质的量比对溶剂热法制备的磷化镍催化剂加氢脱硫性能的影响

发布时间：2018-03-19 09:29

本文选题：溶剂热法　切入点：NiP　出处：《燃料化学学报》2016年05期 　论文类型：期刊论文

【摘要】：以三苯基膦(PPh3)为磷源,以三正辛胺(TOA)为液相反应体系,采用溶剂热法制备了负载型Ni-P(x)/MCM-41催化剂(x为初始P/Ni物质的量比),并用X射线衍射(XRD)、N2吸附比表面积测定(BET)、CO吸附、X射线光电子能谱(XPS)和TEM对催化剂进行了结构表征。以含质量分数1%二苯并噻吩(DBT)的十氢萘溶液为原料,在连续固定床反应装置上,研究了初始P/Ni物质的量比对加氢脱硫(HDS)性能的影响。结果表明,在初始P/Ni物质的量比为0.5时,生成的磷化镍物相为以Ni12P5为主,含有少量Ni2P的混合相;初始P/Ni物质的量比大于0.5时,可得到纯Ni_2P相,且随着P/Ni物质的量比的提高,Ni2P晶粒粒径减小,分散度提高。在反应温度613 K,压力3.0 MPa,H_2/oil体积比500,质量空速2.0 h-1时,Ni-P(6)/MCM-41和Ni-P(10)/MCM-41催化剂的DBT转化率接近100%。
[Abstract]:Using triphenylphosphine (PPh3) as phosphorus source and trioctylamine (TOA) as liquid phase reaction system, The supported Ni-P(x)/MCM-41 catalyst (x) was prepared by solvothermal method. The catalyst was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (TEM) and X-ray photoelectron spectroscopy (TEM). Decalin solution containing 1% dibenzothiophene (DBT) was used as raw material. In a continuous fixed-bed reactor, the effect of the ratio of initial P / Ni on the properties of HDS was studied. The results show that when the initial ratio of P- / Ni is 0.5, the phase of nickel phosphide is composed of Ni12P5 and a small amount of Ni2P. The pure Ni_2P phase can be obtained when the initial ratio of P / Ni is greater than 0.5, and the grain size of Ni _ 2P decreases with the increase of the ratio of P / Ni. When the reaction temperature is 613K, the pressure is 3.0 MPA / H, the oil volume ratio is 500, and the mass space velocity is 2.0 h ~ (-1), the DBT conversion of Ni-Pu / MCM-41 and Ni-P(10)/MCM-41 catalyst is close to 100g.
【作者单位】：东北石油大学化学化工学院;东北石油大学石油与天然气化工省重点实验室;CPE新疆石油勘察设计研究院(有限公司);
【基金】：国家自然科学基金(21276048) 黑龙江省教育厅面上项目(12541060) 东北石油大学研究生创新科研项目(YJSCX2014-022NEPU)资助~~
【分类号】：TE624.9

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