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Preparation method of nickel phosphide hollow nano microspheres

A technology of nano-microspheres and nickel phosphide, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of high price, high specific surface area, and difficulty in putting into production, and achieve easy operation, simple process flow, and low cost Effect

Inactive Publication Date: 2016-12-07
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the thermal decomposition synthesis method of trioctylphosphine, trioctylphosphine is used as the phosphorus source and metal organic compounds or metal nano-elements are dissolved in an organic solvent, and then heated to about 300°C in a vacuum-tight container to generate transition metal phosphorus Compounds, this method obtains small particles, uniform particle dispersion, and high specific surface area, but trioctylphosphine has high chemical activity, unstable air, expensive prices, and is difficult to put into production

Method used

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  • Preparation method of nickel phosphide hollow nano microspheres
  • Preparation method of nickel phosphide hollow nano microspheres
  • Preparation method of nickel phosphide hollow nano microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Raw material NiCl 2 ·6H 2 O, NH 4 h 2 PO 4 and CH 3 The masses of COONa are 5g, 24.4g and 2.9g respectively, NiCl 2 ·6H 2 O, NH 4 h 2 PO 4 and CH 3 Dissolve COONa in 100ml deionized water, adjust the pH of the mixed solution to 8 with 1M KOH solution, put it in an oil bath at 90°C for 60min, filter and wash, freeze at -40°C for 24h and dry the obtained solid, and store in N 2 (Flow rate 100sccm) at 10°C / min to 300°C, keep warm for 60min, cool naturally, then soak in 20% HCl for 12h and freeze-dry.

[0027] X-ray diffraction (XRD) showed that the obtained product was an amorphous phase.

Embodiment 2

[0029] The difference from Example 1 is:

[0030] Raw material NiCl 2 ·6H 2 O, NH 4 h 2 PO 4 and CH 3 The masses of COONa are 5g, 24.4g and 2.9g respectively, NiCl 2 ·6H 2 O, NH 4 h 2 PO 4 and CH 3 Dissolve COONa in 100ml deionized water, adjust the pH of the mixed solution to 8 with 1M KOH solution, put it in an oil bath at 90°C for 60min, filter and wash, freeze at -40°C for 24h and dry the obtained solid, and store in N 2 (Flow rate 100sccm) at 10°C / min to 400°C, keep warm for 60min, cool naturally, then soak in 20% HCl for 12h and freeze-dry.

[0031] X-ray diffraction (XRD) showed that the obtained product was pure Ni 3 P crystal phase.

Embodiment 3

[0033] The difference from Example 1 is:

[0034] Raw material NiCl 2 ·6H 2 O, NH 4 h 2 PO 4 and CH 3 The masses of COONa are 5g, 24.4g and 2.9g respectively, NiCl 2 ·6H 2 O, NH 4 h 2 PO 4 and CH 3 Dissolve COONa in 100ml deionized water, adjust the pH of the mixed solution to 8 with 1M KOH solution, put it in an oil bath at 90°C for 60min, filter and wash, freeze at -40°C for 24h and dry the obtained solid, and store in N 2 (flow rate 100sccm) at 10°C / min to 500°C, keep warm for 60min, cool naturally, then soak in 20% HCl for 12h and freeze-dry.

[0035] X-ray diffraction (XRD) showed that the obtained product was pure Ni 3 P crystal phase.

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Abstract

The invention provides a preparation method of nickel phosphide hollow nano microspheres. The preparation method comprises the following steps: dissolving nickel chloride hexahydrate, sodium hypophosphite and anhydrous sodium acetate in deionized water to obtain a precursor solution; adjusting the pH value of the precursor solution by using a potassium hydroxide solution to obtain a mixed solution; transferring the mixed solution into an oil bath to react; after the reaction is finished, filtering and washing the product, and freeze-drying the product; sintering the freeze-dried product under inert gas to obtain a mixture of elemental nickel and nickel phosphide; and immersing the mixture in hydrochloric acid to be treated to obtain pure-phase nickel phosphide, freeze-drying the pure-phase nickel phosphide to obtain uniform hollow nickel phosphide nano microspheres. A phase separation reaction is adopted, the crystallization degree of the nickel phosphide is controlled by changing the sintering temperature, so as to obtain the nickel phosphide nano microspheres with good crystallinity.

Description

technical field [0001] The invention relates to a method for preparing nickel phosphide hollow nanometer microspheres, which belongs to the field of energy and catalytic materials. Background technique [0002] Transition metal phosphides have similar physical and chemical properties to carbides, borides, and nitrides, such as: stable structure, ceramic and metal characteristics, good thermal and electrical conductivity, and thermodynamic stability. Transition metal phosphides are widely used in hydrorefining, hydrodesulfurization, hydrodenitrogenation, hydrodechlorination, electronic materials, biomedical environmental protection, and lithium-ion batteries. [0003] There are many methods for the synthesis of transition metal phosphides. Because phosphorus has various valence compounds and simple substances such as phosphate, phosphite, hypophosphite, red phosphorus and white phosphorus, it can just provide a phosphorus source for its preparation. So far, the synthesis me...

Claims

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Application Information

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IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 黄智鹏金立煌
Owner JIANGSU UNIV
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