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Preparation method of nickel phosphide

A technology of nickel phosphide and nickel hypophosphite, applied in phosphide and other directions, can solve the problem that the preparation method of transition metal phosphide is rarely studied.

Inactive Publication Date: 2010-06-16
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Although transition metal phosphides have important application prospects as catalysts, the preparation methods of transition metal phosphides are rarely studied (Chem. Eur. J. 2004 Vol. 10, pp. 3364-3371)

Method used

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  • Preparation method of nickel phosphide
  • Preparation method of nickel phosphide
  • Preparation method of nickel phosphide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Press H 2 PO 2 - : Ni 2+ Dissolve nickel hypophosphite and ammonium hypophosphite in deionized water with a ratio of 3, stir, and evaporate to dryness in a 333K water bath. Take 5.0 g of the above precursor, put it in a tube furnace, pass N 2 , heated up to the reaction temperature at a rate of 2K / min, stabilized for 3h, and cooled to room temperature with O 2 Take out after 1% nitrogen passivation for 3 hours. Among them, N 2 The flow rate is 100ml / min, and the final temperature is 473K. The roasted samples were first washed with ammonia until colorless, then washed with deionized water until neutral, and dried. The specific surface area of ​​the prepared sample (named NP3) is 14m 2 / g, XRD spectrum see figure 1 .

Embodiment 2

[0026]Dissolve 1.78g of nickel hypophosphite and 0.50g of ammonium hypophosphite in 6.6g of deionized water, add 6.0g of activated carbon (AC, see Table 1 for structural properties, equivalent dipping point 1.1ml / g), stir, and dry in the shade. Get impregnated sample 5.0g and roast, wash and dry in 473K nitrogen, method is the same as embodiment 1. The prepared catalyst was named NPAC. The structural properties of the supports and supported catalysts are listed in Table 1.

[0027] Table 1 Structural properties of catalysts and supports.

[0028]

Embodiment 3

[0030] Dissolve 5.94g of nickel hypophosphite and 1.66g of ammonium hypophosphite in 14.0g of deionized water, add 5.0g of mesoporous carbon (see Table 1 for the structural properties, and the equivalent immersion point is 2.8ml / g), stir, and dry in the shade. Get impregnated sample 5.0g and roast, wash and dry in 473K nitrogen, method is the same as embodiment 1. The prepared catalyst was named NPMC. The structural properties of the carrier and the loaded catalyst are shown in Table 1, and the XRD spectrum is shown in figure 1 .

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Abstract

On the premise of deep hydrodesulfurization, the main problem in diesel fuel's hydrotreatment is to rid the refractory sulfide and hydrogenate polycyclic aromatic hydrocarbon. Loaded nickel phosphide catalyst demonstrates higher hydrodesulfurization activity and better activity stability. However, the traditional nickel phosphide catalyst is prepared by temperature programming of nickel phosphide, so that dispersion degree of active components is low. In the invention, through solid-phase reaction between phosphorous acid ions and nickel ions, bulk phase and loaded nickel phosphide catalyst with higher active component dispersion degree and fine catalytic activity are obtained at low temperature. The invention is applicable to diesel oil hydroprocessing.

Description

technical field [0001] The invention relates to a preparation method of a nickel phosphide catalyst used for diesel hydrotreating. Background technique [0002] Transportation fuel oil mainly includes gasoline, diesel and aviation kerosene, which account for the majority of petroleum products. Over the past decade, countries around the world have put forward higher and higher requirements on the exhaust emissions of vehicles, mainly to reduce the emissions of harmful gases and greenhouse gases in the exhaust. The current European IV fuel oil standard (EU 2005) requires that the sulfur content in gasoline and diesel oil be less than 50ppmw, and the European V fuel oil standard (EU 2009), which will take effect on January 1, 2009, requires the sulfur content to be less than 10ppmw ( Journal of Process Engineering, Vol. 7, 2007, pp. 176-185). my country's current automotive gasoline standards (GB 19730-1999) and diesel standards (GB / T 19147-2003) both require the sulfur conte...

Claims

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Application Information

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IPC IPC(8): C01B25/08
Inventor 沈俭一石国军王和志傅玉川
Owner NANJING UNIV
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