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Preparation method and application of nano nickel phosphide

A nickel phosphide, nanotechnology, applied in chemical instruments and methods, phosphine, nanotechnology and other directions, can solve the problems of harsh conditions, complex processes, high reaction temperature, good reusability, large specific surface area, catalytic The effect of more active points

Active Publication Date: 2013-01-09
NANTONG ZHONGXING MAGNETIC IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has high reaction temperature, complicated process and harsh conditions.

Method used

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  • Preparation method and application of nano nickel phosphide
  • Preparation method and application of nano nickel phosphide
  • Preparation method and application of nano nickel phosphide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 0.1 g of sodium dodecylbenzenesulfonate (SDBS), 3 mmol of nickel chloride and 10 mmol of sodium hypophosphite in 30 ml of water, stir vigorously, and add 0.2 g of white phosphorus. After mixing evenly, the resulting mixed solution was poured into a stainless steel autoclave lined with polytetrafluoroethylene, and heated to 170° C. for 15 hours to react. After the reaction, cool the autoclave to room temperature, wash the obtained black product several times with deionized water, and dry it in a vacuum oven at 50°C. The obtained product is porous nickel phosphide nanospheres with catalytic hydrogenation activity of nitrobenzene

[0022] The product (Cu Kα ray, λ=0.154060nm, scanning speed 0.02° / s) of implementation experiment 1 is carried out phase identification with Japan Shimao Feng XRD-6000 type X-ray powder diffractometer, as figure 1 shown in . Compared with the JCPDS standard card (74-1381), all diffraction peaks are related to Ni 12 P 5 It fits perfec...

Embodiment 2

[0024] Dissolve 0.08 g of sodium dodecylbenzenesulfonate (SDS), 3 mmol of nickel acetate and 10 mmol of sodium potassium hypophosphite in 25 ml of water, stir vigorously, and add 0.25 g of white phosphorus. After mixing evenly, the resulting mixed solution was poured into a stainless steel autoclave lined with polytetrafluoroethylene, and heated to 160° C. for 15 hours. After the reaction, cool the autoclave to room temperature, wash the obtained black product several times with deionized water, and dry it in a vacuum oven at 50°C. The obtained product is porous nickel phosphide nanospheres with catalytic hydrogenation activity of nitrobenzene

Embodiment 3

[0026] Dissolve 0.15 g of sodium dodecylbenzenesulfonate (SDBS), 3 mmol of nickel nitrate and 12 mmol of sodium hypophosphite in 35 ml of water, stir vigorously, and add 0.3 g of white phosphorus. After mixing evenly, the resulting mixed solution was poured into a stainless steel autoclave lined with polytetrafluoroethylene, and heated to 160° C. for 12 hours. After the reaction, cool the autoclave to room temperature, wash the obtained black product several times with deionized water, and dry it in a vacuum oven at 50°C. The obtained product is porous nickel phosphide nanospheres with catalytic hydrogenation activity of nitrobenzene

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Abstract

The invention discloses a preparation method and application of nano nickel phosphide. The preparation method comprises the following steps: dissolving an anion type surfactant, soluble nickel salt and a reducing agent into distilled water, and evenly stirring; adding simple substance phosphorus; heating to 130-170 DEG C; reacting for 6-15 hours; cooling to the room temperature, and washing for multiple times with absolute ethyl alcohol and deionized water; and drying the product to the constant weight in a vacuum drying oven at 50-60 DEG C to prepare the nano nickel phosphide. Compared with the prior art, the invention has the advantages that a simple water heating method is utilized, a phosphorus source is the simple substance phosphorus, and the temperature and time of the reaction arequite short, which is beneficial to industrial mass production. When the nano particles of the prepared nickel phosphide are used in the catalytic hydrogenation production of nitrobenzene, the hydrogenation of the nitrobenzene can be catalyzed at lower temperature and under lower pressure, the reusability is good and the industrial use value is high because of porous surface structure, large specific surface area and multiple catalytic activity points.

Description

technical field [0001] The invention relates to a preparation method and application of nanomaterials, in particular to a preparation method and application of transition metal phosphide nanomaterials. Background technique [0002] The traditional method of preparing transition metal phosphides is through highly toxic phosphine or PCl 5 Produced by direct reaction with metals or metal salts. Transition metal phosphide nanocrystals mostly use solution-phase method and microemulsion method, using organic reagents containing phosphorus such as P(SiMe 3 ) 3 And TOP, etc. as a phosphorus source in the system. In the above methods, special solvents, highly toxic reagents or high temperature are usually required, the operation is cumbersome, and the cost is high, so it is difficult to realize large-scale production. It is reported in literature that triphenylphosphine is used as phosphorus source, and organic reagents such as n-hexane and ethanol are used to prepare nickel phos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/185C01B25/06B82Y40/00
Inventor 倪永红夏军
Owner NANTONG ZHONGXING MAGNETIC IND
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