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Method for preparing transition metal phosphide

A transition metal and phosphide technology, applied in the field of solvothermal synthesis preparation, can solve problems such as high cost, pollution, and irregular product particles, and achieve the effects of increasing yield, avoiding pollution, and simplifying the production process

Inactive Publication Date: 2011-02-16
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the existing production process, such as expensive raw materials and equipment costs, or irregular product particles, etc., to provide a preparation method for transition metal phosphides, which not only has a simple production process, but also has a high yield and no toxic by-product pollution

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  • Method for preparing transition metal phosphide
  • Method for preparing transition metal phosphide
  • Method for preparing transition metal phosphide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of the transition metal phosphide of the present embodiment is carried out according to the following steps:

[0026] 1) Add ethylene glycol and water with a volume ratio of 1:1 into the autoclave, mix and stir the solution evenly, add 0.01g of nickel salt per milliliter of the solution, and stir until the solid is completely dissolved to form a transparent solution; the nickel salt Select nickel sulfate;

[0027] 2) transfer the transparent solution into the polytetrafluoroethylene lining of 50mL, the filling degree of this polytetrafluoroethylene lining is 80%, add the yellow phosphorus of 0.005g in every milliliter of transparent solution, then put the polytetrafluoroethylene The lining is sealed into a stainless steel mold, heated from room temperature under airtight conditions and reacted at 140°C for 12 hours;

[0028] 3) After the reaction is completed, cool to room temperature with the furnace, and then filter with rapid quantitative filt...

Embodiment 2

[0032] The preparation method of the transition metal phosphide of the present embodiment is carried out according to the following steps:

[0033] 1) Add ethylene glycol and water with a volume ratio of 1:3 into the autoclave, mix and stir the solution evenly, add 0.03g of nickel salt per milliliter of the solution, and stir until the solid is completely dissolved to form a transparent solution; the nickel salt Select nickel chloride;

[0034] 2) transfer the transparent solution into the polytetrafluoroethylene liner of 50mL, the filling degree of this polytetrafluoroethylene liner is 80%, add the yellow phosphorus of 0.02g in every milliliter of transparent solution, then put the polytetrafluoroethylene The lining is sealed into a stainless steel mold, heated from room temperature under airtight conditions and reacted at 180°C for 12 hours;

[0035] 3) After the reaction is completed, cool to room temperature with the furnace, and then filter with rapid quantitative filter...

Embodiment 3

[0039] The preparation method of the transition metal phosphide of the present embodiment is carried out according to the following steps:

[0040] 1) Add ethylene glycol and water with a volume ratio of 1:2 into the autoclave, mix and stir the solution evenly, add 0.02g of nickel salt per milliliter of the solution, and stir until the solid is completely dissolved to form a transparent solution; the nickel salt Select nickel nitrate;

[0041] 2) transfer the transparent solution into the polytetrafluoroethylene lining of 50mL, the filling degree of this polytetrafluoroethylene lining is 80%, add the yellow phosphorus of 0.01g in every milliliter of transparent solution, then put the polytetrafluoroethylene The lining is sealed into a stainless steel mold, heated from room temperature under airtight conditions and reacted at 160°C for 12 hours;

[0042] 3) After the reaction is completed, cool to room temperature with the furnace, and then filter with rapid quantitative filte...

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Abstract

The invention discloses a method for preparing transition metal phosphide, which comprises the following steps: adding ethylene glycol and water in a preset volume ratio, and then mixing the ethylene glycol and the water evenly; adding nickel salt into the obtained mixture, then stirring the obtained solution until the solution is transparent; adding yellow phosphorus into the transparent solution, then heating the obtained mixture from room temperature under an airtight condition so as to carry out reaction on the obtained mixture for 12h at a temperature of 140 to 180 DEG C; after the reaction is completed, cooling the obtained product to room temperature with a reacting furnace, then filtering the obtained product so as to obtain coarse products; washing the obtained coarse products sequentially by benzene, ethanol and distilled water; putting the washed products in a vacuum drying oven to carry out vacuum drying at a temperature of 50 DEG C, then obtaining the transition metal phosphide. In the invention, because of adopting a method for carrying out liquid solid chemical reaction in a solvent thermal system, the preparation of the transition metal phosphide can be realized by conventional equipment at a low temperature; and the water and the ethylene glycol are used as solvent, which reduces the production cost, simplifies the production process, avoids the pollution caused by toxic by-products, and raises the yield; and meanwhile, the application of toxic and difficultly-synthesized metal organic compounds and expensive raw materials is also avoided.

Description

technical field [0001] The invention belongs to the field of solvothermal synthesis preparation methods, in particular to a preparation technology involving transition metal phosphides with two compositions. Background technique [0002] Transition metal phosphides are another new type of catalytic material after transition metal carbides and nitrides. Due to their similar physical properties to carbides and nitrides and excellent hydrodesulfurization and denitrification activities and selectivity, It has thus become a hotspot in the field of new catalytic materials research and has been successfully applied in chemical fields such as petroleum processing. Nickel phosphide is a very good anti-oxidation, anti-corrosion and wear-resistant material. It is a new type of catalytic material, light-emitting device and electronic component material with high activity, high stability and anti-sulfur poisoning performance, so its application prospect is very broad. [0003] At presen...

Claims

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Application Information

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IPC IPC(8): C01B25/08
Inventor 刘淑玲仝建波程芳玲
Owner SHAANXI UNIV OF SCI & TECH
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