Universal preparation method of nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide

A transition metal, co-doping technology, applied in the preparation/purification of carbon, phosphide, chemical instruments and methods, etc., can solve the problems of low flash point, easy volatility, and high toxicity of organic phosphine compounds and organic phosphine compounds, Achieve the effect of important application value, low price and simple synthesis process

Pending Publication Date: 2021-12-28
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, organic solvents and phosphines have low flash points and are volatile, and organic phosphines are highly toxic, so professional skills training is required fo

Method used

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  • Universal preparation method of nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide
  • Universal preparation method of nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide
  • Universal preparation method of nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide

Examples

Experimental program
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Effect test

Embodiment 1

[0031] This example is a universal preparation method for nitrogen-phosphorus co-doped carbon-supported transition metal phosphides. The specific process is:

[0032] 1) Disperse 14g of melamine polyphosphate powder in 800mL of deionized water, and ultrasonically treat it to obtain a uniformly dispersed white emulsion;

[0033] 2) Add 0.523g of ruthenium chloride to the white emulsion prepared in step 1), and stir for 2 hours;

[0034] 3) The emulsion in step 2) is separated, washed, dried for 12 hours, and ground into a fine powder;

[0035] 4) Put the powder obtained in step 3) into a porcelain boat, raise the temperature to 800° C. at a rate of 5° C. / min under argon protection, and calcinate for 2.5 hours. After cooling to room temperature, nitrogen and phosphorus co-doped carbon-supported ruthenium phosphide (RuP 2 @NPC).

[0036] The product obtained in this embodiment is a coral-like structure, such as figure 1 shown in a and 1b. Through XRD analysis, it can be seen...

Embodiment 2

[0038] This embodiment includes the following steps:

[0039] 1) Evenly mix 5g of melamine polyphosphate with 0.25g of tungsten oxide powder;

[0040] 2) Put the powder obtained in step 1) into a porcelain boat, raise it to 900°C at a rate of 5°C / min under the protection of argon and calcinate for 2 hours, and cool to room temperature to obtain nitrogen-phosphorus co-doped carbon-supported tungsten phosphide Materials (WC / WP@NPC).

[0041] The product obtained in this example is a composite of nanoparticles and porous carbon, such as image 3 shown. XRD analysis shows that the tungsten oxide raw material is converted into tungsten phosphide after being calcined with melamine polyphosphate, accompanied by the generation of tungsten carbide ( Figure 4 ). According to this example, a nitrogen-phosphorus co-doped carbon-supported tungsten phosphide material was successfully prepared based on the one-step reaction of melamine polyphosphate.

Embodiment 3

[0043] This embodiment includes the following steps:

[0044] 1) Disperse 7g of melamine polyphosphate powder in 400mL of deionized water, and ultrasonically disperse to obtain a uniform white emulsion;

[0045] 2) Add 0.133g of chromium chloride to the emulsion prepared in step 1), and stir for 2h;

[0046] 3) The emulsion in step 2) is separated and washed, then dried at a constant temperature for 12 hours, and then ground into a fine powder;

[0047] 4) Put the powder obtained in step 3) into a porcelain boat, raise it to 1500°C at a rate of 10°C / min under the protection of argon and calcined for 1h, and after cooling to room temperature, a nitrogen-phosphorus co-doped carbon-supported phosphating Chromium material (CrP@NPC).

[0048] The microscopic morphology of the product obtained in this example is a sheet structure, and a large number of nanoparticles are loaded at the same time, such as Figure 5 shown. Through XRD analysis, it can be known that the product phase...

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Abstract

The invention relates to a universal preparation method of a nitrogen and phosphorus co-doped carbon-loaded transition metal phosphide. The method comprises the following steps: taking melamine polyphosphate as a carbon source, a nitrogen source and a phosphorus source, compounding the melamine polyphosphate with a transition metal raw material, and calcining at high temperature to obtain the nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide. In the preparation method provided by the invention, melamine polyphosphate is pyrolyzed to obtain a nitrogen-phosphorus co-doped carbon material while a transition metal raw material is converted into a corresponding phosphide, so that one-step synthesis of the carbon-loaded transition metal phosphide is realized. Compared with the prior art, the preparation method has the advantages that complicated precursor preparation and phosphating treatment processes are not needed, and the preparation process of the carbon material loaded transition metal phosphide is remarkably simplified. The method provided by the invention is low in raw material cost, high in universality and simple to operate, can realize large-scale preparation of the carbon-loaded transition metal phosphide, and has important application value.

Description

technical field [0001] The invention belongs to the field of composite material preparation and relates to a universal preparation method for nitrogen-phosphorus co-doped carbon-loaded transition metal phosphides. Background technique [0002] Transition metal phosphides can be regarded as binary alloys formed by phosphorus atoms occupying the metal lattice in a doped manner. The introduction of phosphorus atoms can weaken the interaction force between metal atoms, causing the center of the d-band to shift, and at the same time close to the Fermi The density of states of the energy levels also increases. This unique electronic structure endows transition metal phosphides with excellent physical and chemical properties, showing important application prospects in energy storage, catalysis, electronics and other fields. Efficient synthesis is the basis for the large-scale application of materials. However, transition metal phosphides are easily agglomerated during the preparat...

Claims

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Application Information

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IPC IPC(8): C01B25/08C01B32/05B01J27/24
CPCC01B25/08C01B32/05B01J27/24C01P2004/03C01P2004/04C01P2002/72C01P2004/61C01P2004/62
Inventor 艾伟杜祝祝杜洪方黄维杨凯
Owner NORTHWESTERN POLYTECHNICAL UNIV
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