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Preparation method of flaky tungsten sulfide/tungsten phosphide/carbon catalytic material

A sheet-like structure, tungsten sulfide technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor conductivity, high energy consumption for preparation, low catalytic activity, etc., to reduce costs. , the synthesis process is simple, the effect of high electrochemical hydrogen evolution activity

Pending Publication Date: 2020-09-01
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide an easy-to-prepare, high catalytic activity, good electrical conductivity and stable catalyst for the problems of high energy consumption, low catalytic activity and poor electrical conductivity in the existing tungsten sulfide catalytic materials used in the electrochemical hydrogen evolution process. Preparation method of strong flake tungsten sulfide / tungsten phosphide / carbon catalytic material

Method used

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  • Preparation method of flaky tungsten sulfide/tungsten phosphide/carbon catalytic material
  • Preparation method of flaky tungsten sulfide/tungsten phosphide/carbon catalytic material
  • Preparation method of flaky tungsten sulfide/tungsten phosphide/carbon catalytic material

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Effect test

Embodiment 1

[0028] (1) Weigh 4.8g bismuth nitrate dissolved in 10ml 20% nitric acid solution (as solution B), weigh 1.6g sodium tungstate dissolved in 40ml distilled water (as solution A), mix A solution and B solution evenly, use NaOH The pH value of the solution was adjusted to 7, washed and dried, and the product was placed in a muffle furnace for 5 o C / min heating up to 400 o C calcined for 4h. Weigh 4 g of the obtained product, acidify with 150 mL of 6M hydrochloric acid for 100 h, and dry in vacuo. Take 3g of the prepared material and 10.5g of dodecylamine, add 150ml of cyclohexane, react at room temperature for 72h, wash with absolute ethanol 3 times, and obtain the intercalation precursor material.

[0029] (2) Weigh 0.2g intercalation precursor material and 3.2g thiourea, mix the two materials evenly and put them into the corundum boat, put the corundum boat into the vacuum tube furnace, 2 Under the atmosphere, the temperature was raised to 750°C at 2°C / min and kept at a const...

Embodiment 2

[0032] (1) Weigh 5g bismuth oxide and dissolve in 7ml 30% nitric acid solution (as solution B), weigh 2g sodium tungstate and dissolve in 50ml distilled water (as solution A), mix A solution and B solution evenly and adjust the pH value to 7.5, after washing and drying, place in the muffle furnace for 3 o C / min heating up to 450 o C constant temperature 3h. Weigh 4g of the obtained product and acidify it with 180mL 5M hydrochloric acid solution for 100h. 3.5 g of the prepared material and 40 ml of ethylenediamine were dissolved in 150 ml of cyclohexane, reacted at room temperature for 72 h, washed 3 times with cyclohexane, and dried in vacuum to obtain an intercalation precursor material.

[0033] (2) Weigh 0.3g of the intercalation precursor material and 4.8g of thiourea, mix the two materials evenly and grind them into a corundum boat, put the corundum boat into a vacuum tube furnace, 2 Under the atmosphere, the temperature was raised to 700°C at 2°C / min and kept at a con...

Embodiment 3

[0036] (1) Weigh 4.85g bismuth nitrate and dissolve it in 10ml 20% nitric acid solution (as solution B), weigh 1.65g sodium tungstate and dissolve it in 40ml distilled water (as solution A), mix solution A and solution B and adjust the pH value to 8. The product was placed in a muffle furnace for 5 o C / min heating up to 500 o C, cooled to room temperature. Weigh 4g of the prepared material, acidify it with 100mL 10M hydrochloric acid for 72h, and dry it by suction filtration. 3 g of the prepared material and 150 ml of n-butylamine were dissolved in 100 ml of heptane, reacted at room temperature for 60 h, washed 3 times with heptane, and dried in vacuum to obtain an intercalation precursor material.

[0037] (2) Weigh 0.3g intercalation precursor material and 2.5g sulfur element, grind and mix the two materials evenly and place them in a corundum boat, put the corundum boat into a vacuum tube furnace, and 2 Under the atmosphere, the temperature was raised to 800°C at 3°C / mi...

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Abstract

The invention belongs to the field of electrochemical hydrogen evolution, and particularly relates to a preparation method of a flaky tungsten sulfide / tungsten phosphide / carbon catalytic material, which comprises the following steps: (1) mixing tungsten oxide and bismuth oxide, carrying out programmed heating, carrying out constant-temperature calcination for several hours, naturally cooling to room temperature, and acidifying with an inorganic acid to obtain a layered tungsten-based oxide; (2) carrying out stirring reaction on the layered tungsten-based oxide and organic amine, and carrying out washing, suction filtration and drying to obtain an intercalation precursor material; (3) uniformly mixing the intercalation precursor material with a sulfur source, carrying out programmed heating, keeping the temperature constant for several hours, and naturally cooling to obtain a tungsten sulfide / carbon material; and (4) separately placing tungsten sulfide / carbon and a phosphorus source, carrying out programmed heating, carrying out constant-temperature calcination for several hours, and naturally cooling to obtain the tungsten sulfide / tungsten phosphide / carbon catalytic material. The method is low in cost and easy to operate, and the synthesized material has excellent electrochemical hydrogen evolution catalytic activity, conductivity and stability.

Description

technical field [0001] The invention belongs to the field of preparation of electrochemical hydrogen evolution catalysts, in particular to a preparation method of a tungsten sulfide / tungsten phosphide / carbon catalytic material with a sheet structure. Background technique [0002] As a clean energy with abundant reserves, renewable, high energy density and no pollution, hydrogen is considered to be one of the new energy sources most likely to replace fossil energy in the future. The production of hydrogen by electrolysis of water is an important method to alleviate the fossil energy crisis and reduce environmental pollution. So far, using electrolysis of water to produce hydrogen is one of the most mature methods for producing hydrogen. At present, the most stable and efficient catalysts for electrolyzing water to produce hydrogen are mainly precious metal platinum and other precious metal catalysts. However, precious metal catalysts are very scarce and expensive, so they ca...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J37/08C25B1/04C25B11/06
CPCB01J27/188B01J37/08C25B1/04B01J35/33Y02E60/36
Inventor 杨占旭杨金洲
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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