Preparation method for alpha-alumina supported nickel phosphide catalyst

An alumina-loaded, nickel-phosphide technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of difficult to treat phosphorus-containing wastewater, complicated implementation process, etc., and achieve no three-waste formation. , Simple steps, good feasibility effect

Inactive Publication Date: 2013-07-31
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] However, the preparation process of the hypophosphite decomposition method has significantly more unit steps than the temperature-programmed reduction method, and the implementation process is more complicated. At the same time, the phosphorus-containing wastewater generated during the reaction process is difficult to treat, forming an environmental protection problem that cannot be ignored.

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  • Preparation method for alpha-alumina supported nickel phosphide catalyst
  • Preparation method for alpha-alumina supported nickel phosphide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Such as figure 1 As shown, the α-alumina supported nickel phosphide catalyst (Ni 2 P) a preparation method comprising the steps of:

[0031] The first step, preparation of impregnation solution: PdCl 2 Mixed Ni(NO 3 ) 2 ·6H 2 O, NH 4 h 2 PO 4 , dissolved in ultrapure water, so that the prepared solution [Ni 2+ ] is 3.0mol / L, [Pd 2+ ] is 0.05 mol / L, P / Ni molar ratio in the precursor=0.8;

[0032] The second step, equal volume impregnation: under vacuum or normal pressure, α-Al 2 o 3 The equal volume of 50g of carrier is immersed in 25ml of impregnating solution;

[0033] The third step, drying: drying at 60°C for 6 hours;

[0034] The fourth step, roasting: roasting at 500°C for 3 hours;

[0035] The fifth step, the second procedure: immerse the prepared precursor in 25ml of immersion solution again in equal volume, and then repeat steps 3 to 4;

[0036] The sixth step, reduction: reduction in hydrogen at atmospheric pressure, the temperature condition is ...

Embodiment 2

[0039] Such as figure 1 As shown, the α-alumina supported nickel phosphide catalyst (Ni 12 P 5 Type) preparation method, the same steps as in Example 1 will not be repeated, the difference is:

[0040] The first step, preparation of impregnation solution: PdCl 2 Mixed Ni(NO 3 ) 2 ·6H 2 O, NH 4 h 2 PO 4 , dissolved in ultrapure water, so that the prepared solution [Ni 2+ ] is 3.0mol / L, [Pd 2+ ] is 0.05 mol / L, and the P / Ni molar ratio in the precursor is 0.5.

[0041] The XRD figure of nickel phosphide made in the present embodiment is as follows figure 2 As shown by the b line in the middle, the crystal phase of nickel phosphide is Ni 12 P 5 , calculated by the Scherrer formula, the particle size is <15nm, and the Pd content of the catalyst is 0.05 wt.%.

Embodiment 3

[0043] Such as figure 1 As shown, the α-alumina supported nickel phosphide catalyst (Ni 3 P type) preparation method, the same steps as in Example 1 will not be repeated, the difference is:

[0044] The first step, preparation of impregnation solution: PdCl 2 Mixed Ni(NO 3 ) 2 ·6H 2 O, NH 4 h 2 PO 4 , dissolved in ultrapure water, so that the prepared solution [Ni 2+ ] is 3.0mol / L, [Pd 2+ ] is 0.05 mol / L, and the P / Ni molar ratio in the precursor is 0.4.

[0045] The XRD pattern of nickel phosphide made in this embodiment is shown in figure 2 As shown by the line c in the middle, the crystal phase of nickel phosphide is Ni 3 P, the particle size calculated by the Scherrer formula is <15nm, and the Pd content of the catalyst is 0.05 wt.%.

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Abstract

The invention provides a preparation method for an alpha-alumina supported nickel phosphide catalyst. The preparation method comprises the following steps of preparing an impregnation liquid, equivalent-volume impregnating, drying, calcining, carrying out the procedures again and reducing. The preparation method is improved based on a temperature-programmed reduction method. Nickel and phosphor precursors are transferred into nickel phosphide under the catalytic reduction action of a trace amount of Pd or Ru (less than or equal to 0.1 wt.%) by using the alpha-Al2O3 as a carrier. A core of the preparation method lies in that a reduction temperature is reduced to below a 500 DEG C by using catalytic action of Pd or Ru in the temperature-programmed reduction process, thereby effectively preventing the disadvantages brought by high temperature reduction. The preparation method has good practicability and usage effects without forming three wastes (waste gas, waste water and waste residues), and is safe and environment-friendly.

Description

technical field [0001] The invention relates to the preparation of a catalytic material, in particular to a preparation method of a nickel phosphide catalyst. Background technique [0002] In recent years, researchers have found that nickel phosphide has excellent performance and can be applied in the fields of deep hydrodesulfurization, denitrogenation, dehalogenation and dearomatization. It is a new type of highly active hydrogenation catalytic material. The key to the industrial application of new catalytic materials lies in the feasible industrial preparation process. This includes engineering feasibility, engineering economy, and environmental protection. [0003] At present, the common preparation methods of nickel phosphide catalysts include solvothermal method, temperature-programmed reduction method and hypophosphite decomposition method: [0004] 1. Solvothermal method [0005] The solvothermal method is a common method for preparing Ni2P grains in the laborator...

Claims

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Application Information

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IPC IPC(8): B01J27/185
Inventor 刘旭光张宝泉张萍萍
Owner QINGDAO UNIV OF SCI & TECH
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