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Nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst and preparing method and application thereof

A tungsten carbide catalyst and co-doping technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of active center trouble synthesis, complicated manufacturing process, low yield, etc., and achieve structural Controllable, clear structure, good dispersion effect

Active Publication Date: 2018-05-08
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the production process of most materials is complicated, the cost is high, and the yield is low. During the synthesis process, problems such as agglomeration of nanoparticles and low-density active centers still plague the synthesis of such materials.

Method used

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  • Nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst and preparing method and application thereof
  • Nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst and preparing method and application thereof
  • Nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of nitrogen-phosphorus co-doped carbon-supported molybdenum carbide catalyst, comprising the following steps:

[0034] (1) Heteropolyacid (NH 4 ) 4 [NiMo 6 o 24 h 6 ] (NiMo 6 ) synthesis: 5.00g (4.2mmol) (NH 4 ) 6 Mo 7 o 24 Dissolve in 80ml of deionized water, stir the solution and heat to boiling, then add 20mL containing 0.76g (3.0mmol) NiSO 4 ·7H 2 The aqueous solution of O is slowly added dropwise to the above boiling aqueous solution of ammonium molybdate, and recrystallized twice in water to obtain colorless crystals (NH 4 ) 4 [NiMo 6 o 24 h 6 ] (NiMo 6 ).

[0035] (2) Preparation of SEP (Surfactant encapsulate polyoxometalate, surfactant-encapsulated heteropolyacid) composite material: 1.08g (1.0mmol) (NH 4 ) 3 [NiMo 6 o 24 h 6 ] was dissolved in 80mL deionized water (A solution), 2.20g (10.0mmol) cetyltrimethylammonium bromide (surfactant) was dissolved in 20mL ethanol (B solution); at a temperature of 85 ° C, violently ...

Embodiment 2

[0042] A preparation method of nitrogen-phosphorus co-doped carbon-supported molybdenum carbide catalyst, comprising the following steps:

[0043] (1) Heteropolyacid (NH 4 ) 4 [(HPO 3 ) 2 Mo 5 o 15 ]·4H 2 Synthesis of O: Dissolve 4.1g of phosphorous acid (50mmol) in 70mL of water, then add 7mL of 15mol / L ammonia water (105mmol), heat the solution to boiling, and add 14.4g of MoO to the solution in small amounts for several times 3 (100mol), after 40-45min the powder was dissolved, the solution was filtered, the filtrate was boiled and evaporated to reduce the volume to 20-25mL, then cooled to room temperature, the crystalline powder was collected by filtration, washed with 7mL of ice water, dried in the air to obtain colorless The crystal is (NH 4 ) 4 [(HPO 3 ) 2 Mo 5 o 15 ]·4H 2 O.

[0044] (2) Preparation of SEP (Surfactant encapsulate polyoxometalate, surfactant-encapsulated heteropolyacid) composite material: 0.54g (0.5mmol) (NH 4 ) 4 [(HPO 3 ) 2 Mo 5 o ...

Embodiment 3

[0049] A preparation method of nitrogen-phosphorus co-doped carbon-supported molybdenum carbide catalyst, comprising the following steps:

[0050] (1) Heteropolyacid (NH 4 ) 6 [NiMo 9 o 32 ]·6H 2 Synthesis of O: 10 mL of Ni(NO 3 ) 2 and 0.1mol / L (NH 4 ) 2 Mo 7 o 24 The mixed solution was heated to 70°C, then 10 mL of ammonium persulfate solution with a concentration of 0.01 mol / L was added, and 0.1 mol / L of H 2 SO 4 The pH of the reaction system was adjusted to 4.4, and then the solution was boiled for half an hour. The solution was finally cooled slowly overnight to obtain black-red crystals. The crude product was obtained by suction filtration, and then the crude product was recrystallized 3-5 times, dried at 60°C, and the obtained colorless crystal was (NH 4 ) 6 [NiMo 9 o 32 ]·6H 2 O.

[0051] (2) Preparation of SEP (Surfactant encapsulate polyoxometalate, surfactant-encapsulated heteropolyacid) composite material: 1.08g (1.0mmol) (NH 4 ) 3 [NiMo 6 o 2...

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Abstract

The invention provides a nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst and a preparing method and application thereof. The preparing method includes the following steps that a coprecipitation method is used for preparing a SEP compound material from a surfactant and heteropolyacid or polyoxometalate, the surfactant is a cationic surfactant or ionic liquid surfactant, and the heteropolyacid or polyoxometalate contains molybdenum or tungsten; the SEP compound material, melamine and phytic acid are used as raw materials for synthesizing a SEP-MA-PA compound material through a mixing and dissolving method; under protection of inert gas, the SEP-MA-PA compound material is subjected to heat treatment and cooled to obtain the nitrogen-phosphorus codopedcarbon loaded molybdenum carbide or tungsten carbide catalyst. Nanoparticles of the nitrogen-phosphorus codoped carbon loaded molybdenum carbide or tungsten carbide catalyst are small in size and areof a porous structure, by means of nitrogen-phosphorus heteroatom doping, the conductivity of the catalyst is enhanced, and the catalyst has efficient performance of electrolyzing water for preparinghydrogen.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a molybdenum carbide or tungsten carbide catalyst supported by nitrogen and phosphorus co-doped carbon, a preparation method and application thereof. Background technique [0002] Hydrogen is rich in resources and comes from a wide range of sources. It is the most common element in nature and constitutes 75% of the mass of the universe. In addition to the hydrogen contained in the air, it is mainly stored in water in the form of compounds, and water is the most widespread substance on the earth. In addition, hydrogen has a high combustion calorific value, good combustion performance, good thermal conductivity, and will not produce any pollution after combustion; hydrogen is the lightest element, and has the advantages of storability and transportability, making it the best choice for traditional fossil energy. good substitute. Hydrogen production by ele...

Claims

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Application Information

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IPC IPC(8): B01J27/22C25B1/04C25B11/06B01J37/03B01J37/04B01J37/08
CPCB01J27/22B01J37/038B01J37/04B01J37/082C25B1/04C25B11/04Y02E60/36
Inventor 卢玉坤郭新新孙道峰柳云骐刘晨光
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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