Novel method for preparing nickel phosphide by low-temperature reduction

A new method, the technology of low-temperature solvothermal method, is applied in the direction of phosphide, which can solve the problems of easy ignition of phosphine, environmental pollution, hidden dangers of production safety, etc., and achieves mild and fast reaction conditions, simple and mild reaction conditions, and large specific surface area Effect

Active Publication Date: 2010-12-01
NANKAI UNIV
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  • Application Information

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Problems solved by technology

These methods all require strict experimental conditions and equipment, and the selected phosphorus source is highly toxic, causing serious pollution to the environment.
Although the thermal decomposition method of hypophosphite can solve the above problems very well, the phosphine produced by its decomposition is easy to catch fire when it contacts with oxygen at high temperature, which brings hidden dangers to safe production

Method used

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  • Novel method for preparing nickel phosphide by low-temperature reduction
  • Novel method for preparing nickel phosphide by low-temperature reduction
  • Novel method for preparing nickel phosphide by low-temperature reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 0.3g NiCl respectively 2.6 h 2 O with 1.54g NaH 2 PO 2 .H 2 O was dried at 120°C, then dissolved in 25ml of ethylene glycol, and stirred magnetically at room temperature until the solution was clear and transparent. The solution was poured into a stainless steel autoclave lined with polytetrafluoroethylene, and placed in an electric thermostat blast drying oven heated to 140°C to react for 24 hours. After the reaction, the autoclave was taken out and cooled to room temperature naturally. Open the autoclave, and wash the black product obtained by the reaction with deionized water. Finally, the product was put into a vacuum oven and dried under vacuum at 60°C. That is, the Ni described in the present invention is obtained 12 P 5 catalyst, which has figure 1 Characteristics.

Embodiment 2

[0017] Weigh 0.2g NiCl respectively 2.6 h 2 O with 0.8g NaH 2 PO 2 .H 2 O was dried at 120°C, then dissolved in 25ml of glycerol, and stirred magnetically at room temperature until the solution was clear and transparent. The solution was poured into a stainless steel autoclave, and placed in an electric thermostat blast drying oven heated to 240° C. to react for 2 h. After the reaction, the autoclave was taken out and cooled to room temperature naturally. Open the autoclave, and wash the black product obtained by the reaction with deionized water. Finally, the product was put into a vacuum oven and dried under vacuum at 60°C. That is, the Ni described in the present invention is obtained 12 P 5 nanoparticles, which have figure 2 And attached image 3 Characteristics.

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Abstract

The invention provides a novel method for preparing nickel phosphide (Ni12P5) by the low-temperature solvothermal method. The method of the invention is characterized by dissolving anhydrous nickel chloride as a nickel source and sodium hypophosphite as a phosphorus source in a high-boiling-point organic solvent at the room temperature, stirring the materials until the organic solvent is transparent, sealing the organic solvent in a high-pressure kettle and heating up to 140-240 DEG C and reacting for certain time to obtain Ni12P5. The method of the invention is characterized by using a high-boiling point organic substance as the solvent, the reaction conditions are simple and mild and the generated Ni12P5 is the nano-particle with the size being 50nm to 200nm and the specific surface area being larger. The method is favorable for hydrodesulfurization, selective hydrogenation and other catalytic hydrogenation reactions, thus having wider application range.

Description

technical field [0001] The present invention proposes a kind of low-temperature solvothermal method to prepare nickel phosphide (Ni 12 P 5 ) of the new method. The method uses anhydrous nickel chloride as the nickel source, anhydrous hypophosphite as the phosphorus source, dissolves it in a high-boiling organic solvent at room temperature, stirs it to a transparent solution, seals it in an autoclave and raises the temperature to 140-240°C. After reacting for a certain period of time, Ni is obtained 12 P 5 . The present invention is characterized by using high-boiling-point organic substances as solvents, and the reaction conditions are simple and mild, and the generated Ni 12 P 5 It is a nano-scale particle with a particle size of 50-200nm and a large specific surface area, which is beneficial to hydrodesulfurization, selective hydrogenation and other catalytic hydrogenation reactions, and has a wide range of uses. Background technique [0002] Transition metal phosph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08
Inventor 李伟张濛关庆鑫
Owner NANKAI UNIV
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