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Hydro-thermal synthesis process of phosphide

A technology of hydrothermal synthesis and phosphide, applied in the direction of phosphide, phosphorus compound, inorganic chemistry, etc., can solve the problems of danger, personal and environmental damage in the heat treatment process of white phosphorus, and achieve the goal of increasing yield, avoiding pollution and reducing production cost Effect

Inactive Publication Date: 2010-03-03
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many disadvantages in using unstable white phosphorus as phosphorus source, organic solvent or ammonia water as reaction solvent
On the one hand, the pressure in the reaction vessel is high, and the solvothermal treatment process of white phosphorus is very dangerous; on the other hand, ethylenediamine and ammonia have a strong pungent odor, which will cause damage to people and the environment
[0004] At present, the method of preparing metal phosphides by hydrothermal method using non-toxic and stable red phosphorus as phosphorus source and water as solvent is rarely reported at home and abroad.

Method used

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Examples

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Effect test

Embodiment 1

[0020] (1) Weigh 4.863g NiCl 2 ·6H 2 O. 6.335g of red phosphorus is fully ground by adding 5mL of deionized water; then place it in a 75mL lined stainless steel hydrothermal kettle, add deionized water until the filling volume is 80% of the liner volume, and tighten.

[0021] (2) Heat the hydrothermal kettle to 200°C and keep it warm for 24 hours; then cool it down to room temperature naturally.

[0022] (3) Open the hydrothermal kettle, filter the obtained solution with suction, and then wash several times with deionized water and absolute ethanol respectively.

[0023] (4) Put the obtained powder in a drying oven, and dry at 40° C. to obtain Ni2P powder.

[0024] Ni prepared by this embodiment 2 The phase of P powder is as figure 1 As shown, it can be seen from the figure that the obtained Ni 2 P powder is pure in phase.

Embodiment 2

[0026] (1) Weigh 4.863g NiCl 2 ·6H 2 O. 6.335g of red phosphorus is fully ground by adding 5mL of deionized water; then place it in a 75mL lined stainless steel hydrothermal kettle, add deionized water until the filling volume is 80% of the liner volume, and tighten.

[0027] (2) Heat the hydrothermal kettle to 200° C. and keep it warm for 48 hours; then cool down naturally to room temperature.

[0028] (3) Open the hydrothermal kettle, filter the obtained solution with suction, and then wash several times with deionized water and absolute ethanol respectively.

[0029] (4) Place the obtained powder in a drying oven and dry at 40°C to obtain Ni 12 P 5 Powder.

[0030] Ni prepared by this embodiment 12 P 5 The phase of the powder is like figure 2 As shown, it can be seen from the figure that the obtained Ni 12 P 5 The powder is pure in phase.

Embodiment 3

[0032] (1) Weigh 1.439g ultra-fine copper powder, 6.925g red phosphorus and add 5mL deionized water to fully grind; then place it in an 80mL lined stainless steel hydrothermal kettle, add deionized water until the filling volume is the liner volume 80% tightened.

[0033] (2) Heat the hydrothermal kettle to 200°C and keep it warm for 24 hours; then cool it down to room temperature naturally.

[0034] (3) Open the hydrothermal kettle, filter the obtained solution with suction, and then wash several times with deionized water and absolute ethanol respectively.

[0035] (4) Place the obtained powder in a drying oven and dry at 40°C to obtain Cu 3 P powder.

[0036] Cu prepared by this embodiment 3 The phase of P powder is as image 3 As shown, it can be seen from the figure that the obtained Cu 3 P powder is pure in phase.

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Abstract

The invention discloses a hydro-thermal synthesis process of phosphide, which is characterized by comprising the following steps: firstly, crushing red phosphorus, metal element or metal salt into powder, and then mixing crused powder and water or water solution to obtain suspension; placing the suspension in a closed vessel for heating for 2-72 hours at a temperature between 100 and 300 DEG C; then, naturally cooling reaction products and the reaction vessel to room temperature; and finally taking out the reaction products, and filtering, washing and drying sequentially to obtain the needed phosphide. The invention uses no-toxic and stable red phosphorus to replace common white phosphorus and other phosphorus sources and water to replace common ethene diamine and other organic reagents, reduces the production cost, simplifies the production process, avoids the pollution of toxic by-products and improves the yield.

Description

technical field [0001] The invention relates to a hydrothermal synthesis process of phosphide, belonging to the technical field of hydrothermal synthesis. Background technique [0002] Metal phosphides as catalysts have attracted people's attention since 1998. Oyama et al. prepared molybdenum phosphide by a temperature-programmed reduction method and found that it had good hydrodenitrogenation performance. Since then, people have conducted in-depth research on phosphides, a new type of catalytic material, from composition to structure, and then to the changes of their surface active sites during the catalytic reaction process, and have continued to understand and understand. [0003] The more commonly used methods for the preparation of metal phosphides reported in the literature at present mainly include: simple substance direct chemical method, solid-state replacement reaction, reaction of metal halide and phosphine, decomposition of organometallic compounds, electrolysis ...

Claims

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Application Information

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IPC IPC(8): C01B25/08C01B25/45
Inventor 黄翔刘宗义戴金辉朱志斌
Owner OCEAN UNIV OF CHINA
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