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Preparation method of MoP, FeP and redox graphene three-phase composite material

A composite material and graphene technology, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc., can solve problems such as long time, reduced catalytic activity, high phosphating temperature, etc., to achieve good stability, high Catalytic activity, effect of preventing particle aggregation

Active Publication Date: 2018-05-01
青岛旭晟东阳新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional preparation method of molybdenum phosphide is cumbersome, the required phosphating temperature is high (≥850°C), and the time is long (≥5h), the obtained molybdenum phosphide is basically sintered, and the catalytic activity is reduced.

Method used

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  • Preparation method of MoP, FeP and redox graphene three-phase composite material
  • Preparation method of MoP, FeP and redox graphene three-phase composite material

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preparation example Construction

[0021] What the present invention proposes is the preparation method of MoP, FeP, redox graphene three-phase composite material, comprises the following steps:

[0022] 1. Dissolve a certain amount of molybdenum acetylacetonate and iron acetylacetonate in a certain amount of ethanol, and then disperse a certain amount of graphene oxide in the above solution. Preferably, the best preparation method is: the addition ratio of molybdenum acetylacetonate and iron acetylacetonate is 1:1 (mass ratio).

[0023] 2. Take part of the sample obtained in step 1 and place it in an oven at 80°C to dry the graphene oxide-loaded iron acetylacetonate and molybdenum acetylacetonate composite material as a precursor.

[0024] 3. Put the sample obtained in step 2 and a certain amount of sodium hypophosphite in a tube furnace for phosphating. Preferably, the best preparation method is: phosphating temperature 800° C., phosphating time 1 h.

[0025] 4. Take the phosphating sample and rinse it sever...

Embodiment 1

[0028] Example 1: 150 mg iron acetylacetonate and 150 mg molybdenum acetylacetonate were dissolved in 30 ml ethanol, ultrasonicated for 30 minutes, then 100 mg graphene oxide was dispersed into the above solution, ultrasonicated for 30 minutes, and the solution was transferred to an oven at 80 ° C after ultrasonic treatment Dry for 24 hours to obtain the composite precursor. It was then cooled to room temperature and the product was collected.

[0029] Sodium hypophosphite (1.0g) was placed on the upstream side of the tube furnace, the above composite precursor (100mg) was placed downstream in another ceramic boat, and the sample was heated and kept at 750°C for 0.5h at a heating rate of 3 °C / min. Then it was naturally cooled to room temperature under the protection of Ar2.

Embodiment 2

[0030] Example 2: During precursor synthesis: 100 mg of iron acetylacetonate and 200 mg of molybdenum acetylacetonate were dissolved in 30 ml of ethanol, ultrasonicated for 30 minutes, then 100 mg of graphene oxide was dispersed into the above solution, ultrasonicated for 30 minutes, and the solution was dissolved after ultrasonic treatment Transfer to an oven at 80°C and dry for 24 hours to obtain a composite precursor. Other processing is the same as the implementation example 1.

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Abstract

The invention provides a preparation method of an MoP, FeP and redox graphene oxide three-phase composite material. The method is characterized in that ferric acetylacetonate and molybdenyl acetylacetonate are loaded onto graphene oxide; the material is used as a precursor and is then subjected to high-temperature short-time phosphorization to obtain the MoP, FeP and redox graphene three-phase composite material.

Description

technical field [0001] The invention relates to the technical field of preparation of nanomaterials, in particular to a method for preparing a three-phase composite material of MoP, FeP and redox graphene, and its application in electrocatalytic hydrolysis for hydrogen production. Background technique [0002] The urgent need for clean and renewable energy drives the exploration of catalysts for hydrogen production from water electrolysis. Recently, transition metal phosphides (TMPs) have been shown to be highly active, highly stable HER catalysts, and have nearly 100% efficiency not only in strongly acidic solutions but also in strongly alkaline and neutral media. Faraday efficiency. A large number of studies have shown that nano-hybrids as catalysts can combine the advantages of each component, and produce synergistic effects at the heterogeneous interface, greatly improving the performance of catalytic hydrogen production. Therefore, the preparation of nanocomposites ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J37/28C25B11/06C25B1/04
CPCB01J27/19B01J37/28C25B1/04C25B11/04Y02E60/36
Inventor 王晓东
Owner 青岛旭晟东阳新材料有限公司