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Method for preparing transition metal phosphide

A transition metal, phosphide technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve the problems of small specific surface area of ​​binary or ternary phosphide, research and practical application limitations, etc. , to achieve the effect of easy large-scale preparation, low cost and high specific surface area

Inactive Publication Date: 2005-09-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the specific surface area of ​​binary or ternary phosphides prepared by existing technologies is generally small, which limits their further research and practical application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Molybdenum phosphide (MoP) was prepared by using citric acid as the hydroxy acid.

[0016] Weigh 8.85 g of ammonium molybdate with target phosphide (MoP) stoichiometric ratio (molybdenum: phosphorus = 1: 1), mix with 6.65 g of diammonium hydrogen phosphate and dissolve in 60 ml of water until the solution is clear to obtain phosphorus-molybdenum aqueous solution. Add citric acid and metal to the above solution at a ratio of 0.4:1 (molar ratio), and dissolve citric acid completely until the solution is clear to obtain a sol, then obtain a gel at 90°C, solidify and foam at 120°C, and finally dissolve in flowing air Under atmosphere, calcined at 500°C for 6h to obtain the precursor. The precursor is ground, pressed into tablets, and sieved to obtain 24-32 mesh particles. Under a hydrogen atmosphere, the precursor was raised from room temperature to 300 °C in 0.5 h, then raised to 650 °C at a rate of 1 °C / min, kept at this temperature for 2 h, and then cooled to ...

Embodiment 2

[0017] Example 2 Molybdenum phosphide (MoP) and tungsten phosphide (WP) prepared with citric acid, malic acid, lactic acid, and tartaric acid as hydroxy acids.

[0018] The preparation method is the same as in Example 1. The preparation conditions and the specific surface area of ​​the obtained target phosphide (MoP, WP) are listed in Table 1, wherein the tungsten salt adopts metatungstic acid:

[0019] Phosphide

Embodiment 3

[0023] Embodiment 3 is the nickel phosphide (Ni phosphide) prepared by hydroxyacid with citric acid 2 P).

[0024] Weigh the target phosphide (Ni 2 P) Nickel nitrate 14.6g of stoichiometric ratio (nickel: phosphorus = 2: 1) is mixed with diammonium hydrogen phosphate 3.3g and dissolved in 60ml of water, and citric acid is added to the metal according to the ratio (molar ratio, 2: 1) For the above solution, citric acid was completely dissolved until the solution was clear to obtain a sol, then a gel was obtained at 90°C, solidified and foamed at 120°C, and finally calcined at 480°C for 6 hours under a flowing air atmosphere to obtain a precursor. The precursor is ground, pressed into tablets, and sieved to obtain 40-60 mesh particles. Under a hydrogen atmosphere, the precursor was raised from room temperature to 300 °C within 0.5 h, then raised to 550 °C at a rate of 2 °C / min, kept at this temperature for 2 h, and then cooled to room temperature. In order to prevent the viol...

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PUM

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Abstract

The invention relates to the preparation method of a transition metal phosphide. The main operation processes are: dissolve the target phosphor-origin matters and the dissolvable metal salt in water, add hydroxyl acid, the mole ratio of the hydroxyl acid to metal is 0.2-4.5, get the gel in 70-90 Deg. C, froth and solidify in 100-160 Deg. C, burn it in 500 Deg. C for more than four hours to get the front body of target phosphide, revert the front body using program calefactive reverting technology, passivate it in house temperature to get big-area phosphide. The surface area of the invention is as 10 times as the original one.

Description

field of invention [0001] The invention relates to the preparation of metal phosphorus compounds, in particular to a method for preparing transition metal phosphides with a large specific surface area. Background technique [0002] Phosphide has noble metal catalytic properties, and is a new type of catalytic material after transition metal carbides and nitrides. It has been successfully applied to deep hydrodesulfurization and hydrodenitrogenation reactions of gasoline, and it can greatly replace the existing Co( Ni)MoS / Al 2 o 3 Potential for commercial use of the catalyst. According to reports, this new type of substance has broad application prospects in many hydrogen-related reactions, such as hydrogenation reaction, ammonia synthesis, NO reduction and electrochemical reduction reaction. Among them MoP, WP, Ni 2 P is a better catalyst. [0003] The method of preparing phosphide developed in the 1930s and 1940s is a method similar to metallurgy. For example, metal m...

Claims

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Application Information

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IPC IPC(8): B01J27/14B01J27/185B01J27/188B01J37/28
Inventor 程瑞华张涛郑明远李宁丛昱刘茜李林王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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