A method for controlling the synthesis of nano-nickel phosphide in different phases

A technology of nickel phosphide and nickel chloride hexahydrate, which is applied in the direction of phosphide, nanotechnology, nanotechnology, etc., can solve the problems of easy agglomeration, harsh synthesis conditions, and difficulties, and achieve easy industrial production, low cost, and mild conditions Effect

Active Publication Date: 2022-03-11
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a series of problems such as high preparation cost of nano-nickel phosphide, harsh synthesis conditions, large surface energy of nanoparticles, easy agglomeration, and difficulty in controlling the synthesis of nano-nickel phosphide in different phases. A Relatively Inexpensive, Mild and Simple Controlled Synthesis of Nano-NiP in Different Phases

Method used

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  • A method for controlling the synthesis of nano-nickel phosphide in different phases
  • A method for controlling the synthesis of nano-nickel phosphide in different phases

Examples

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Effect test

Embodiment 1

[0016] Weigh 0.2377g of nickel chloride hexahydrate and 0.264g of sodium dihydrogen hypophosphite and dissolve in 20mL of ethylene glycol, pour the resulting solution into a round bottom flask with a reflux device, and treat it in an oil bath at 170°C for 5h , to obtain nickel phosphide intermediate A.

Embodiment 2

[0018] Weigh 0.2377g of nickel chloride hexahydrate and 0.264g of sodium dihydrogen hypophosphite and dissolve in 20mL of ethylene glycol, pour the resulting solution into a round bottom flask with a reflux device, and treat it in an oil bath at 170°C for 5h , to obtain nickel phosphide intermediate. The resulting nickel phosphide intermediate was placed in a tube furnace under N 2 The heat treatment is carried out under the atmosphere. Heat treatment conditions are: N 2 The flow rate is 20mL / min; the heating rate is 2.5°C / min; the temperature is 300°C; the final temperature holding time is 2h. Nano nickel phosphide B was obtained under the above synthesis conditions.

Embodiment 3

[0020] Weigh 0.2377g of nickel chloride hexahydrate and 0.264g of sodium dihydrogen hypophosphite and dissolve in 20mL of ethylene glycol, pour the resulting solution into a round bottom flask with a reflux device, and treat it in an oil bath at 170°C for 5h , to obtain nickel phosphide intermediate. The resulting nickel phosphide intermediate was placed in a tube furnace under N 2 The heat treatment is carried out under the atmosphere. Heat treatment conditions are: N 2 The flow rate is 20mL / min; the heating rate is 2.5°C / min; the temperature is 400°C; the final temperature holding time is 2h. The above synthesis conditions obtain nano-nickel phosphide C.

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Abstract

The invention relates to a method for controlling and synthesizing nano-nickel phosphide in different phases. In the method, cheap nickel salt and hypophosphite are used as raw materials, and an intermediate of nano-nickel phosphide is firstly synthesized in an ordinary flask. Then the nickel phosphide intermediate is placed in a tube furnace for heat treatment, and nano-nickel phosphide particles in different phases can be obtained by controlling the synthesis conditions. The synthesis method has the advantages of mild conditions, low cost, simple process and easy realization of industrial production.

Description

technical field [0001] The invention relates to the technical field of transition metal phosphides and their preparation, in particular to a method for controlling and synthesizing nano-nickel phosphide in different phases. Background technique [0002] Transition metal phosphides are another new type of catalytic material after nitrides and carbides. This type of material has good thermal stability, high hardness, strong oxidation resistance and corrosion resistance, and exhibits a higher surface active site density. Studies have found that transition metal phosphides have excellent hydrotreating activity and hydrodesulfurization / denitrogenation selectivity, and consume less hydrogen. To a certain extent, they can replace noble metal Pt, which has attracted great attention in the field of new catalytic materials. Among the currently studied transition metal phosphides, nickel phosphide exhibits superior hydrogenation activity and is expected to become a new generation of h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08B82Y30/00
CPCB82Y30/00C01B25/08C01P2002/72C01P2004/03
Inventor 刘平张志翔朱雅露李永昕
Owner CHANGZHOU UNIV
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