Preparation method and application of molybdenum carbide microspheres

A micro-sphere, molybdenum carbide technology, applied in chemical instruments and methods, carbides, tungsten/molybdenum carbides, etc., can solve the problems of uncontrollable size and morphology, reduced electrocatalyst activity, and easy catalyst detachment. High stability, high current density, and low requirements for preparation conditions

Active Publication Date: 2016-07-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem with this mode is that the supported catalyst is easy to fall off, and the binder will also reduce the activity of the electrocatalyst, especially in the case of high loading
The traditional method of synthesizing molybdenum carbide requires a complex process, the size and shape of which are uncontrollable, and irregular molybdenum carbide powders are obtained, which need to be loaded on various carriers or pressed into shape before they can be used in catalytic reactions

Method used

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  • Preparation method and application of molybdenum carbide microspheres
  • Preparation method and application of molybdenum carbide microspheres
  • Preparation method and application of molybdenum carbide microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 5 grams of D201 type anion exchange resin and add to 20 milliliters, 0.5 mole per liter of sodium molybdate solution, add a stirring bar and stir for 24 hours at room temperature. Slowly add the solution into a suction filter bottle for suction filtration, and dry the obtained solid at 100° C. for 24 hours to obtain an ion exchange resin adsorbing molybdenum ions. Put the obtained powder into a ceramic crucible, place it in an atmosphere tube furnace, and under the protection of nitrogen gas, heat up to 900 °C at a heating rate of 5 °C per minute in the tube type furnace for 2 hours, and cool naturally to room temperature to obtain molybdenum carbide Microspheres. The microspheres were characterized by X-ray electron diffraction as a molybdenum carbide component, as figure 1 ; Observing micron spherical shape by scanning electron microscope, diameter is 200-500 micron (as figure 2 ), the surface of the microspheres has a granular composition and a porous struct...

Embodiment 2

[0048] Weigh 2g of 201×4 type anion exchange resin and add it into 40 ml of sodium molybdate solution with 2 moles per liter, add a stirring bar and stir for 12 hours at normal temperature. The obtained solution was filtered with suction, and the obtained solid was dried at 100° C. for 48 hours. Under the protection of argon gas, the obtained solid was heated up to 1000°C for 2 hours at a heating rate of 5°C / min, and then naturally cooled to room temperature to obtain molybdenum carbide microspheres. The X-ray diffraction results were as follows: Figure 8 ; The morphology of molybdenum carbide is obtained by grinding and pulverizing, such as Figure 9 .

[0049] With the molybdenum carbide prepared in this example as electrocatalyst, the result of its polarization curve Figure 10 , the hydrogen overpotential is 0.22 volts.

Embodiment 3

[0051] The preparation steps are the same as in Example 1, except that the anion exchange resin is D202 type, and the temperature is raised to 800° C. for 2 hours in a tube furnace at a heating rate of 5° C. per minute. The morphology of the obtained molybdenum carbide microspheres is as follows: Figure 11 , the X-ray powder diffraction results are as follows Figure 12 . Its specific surface area obtained by nitrogen absorption and desorption test is 42.8 square meters per gram ( Figure 13 ), indicating that the molybdenum carbide microspheres are porous.

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Abstract

The invention discloses a preparation method of molybdenum carbide microspheres. The method comprises the following steps of: (1) adding strongly alkaline anion exchange resin to a molybdate solution, carrying out stirring reaction at a room temperature, obtaining a molybdenum ion-resin compound through washing and suction filtration, and drying the molybdenum ion-resin compound to obtain ion exchange resin microspheres containing a molybdenum element; and (2) putting the ion exchange resin microspheres containing the molybdenum element obtained in the step (2) into a ceramic crucible, roasting the microspheres at 700-1,000 DEG C in the presence of an inert gas for 1-4 hours, and naturally cooling the product to a room temperature to obtain the molybdenum carbide microspheres. The invention further discloses application of the molybdenum carbide microspheres in hydrogen production through electrolysis of water. The preparation conditions are low in demands; the raw materials are cheap and available; the prepared molybdenum carbide microspheres have electrochemical activity of catalytic low overpotential and good stability.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a preparation method and application of molybdenum carbide microspheres. Background technique [0002] Due to the abundance of hydrogen energy resources, wide sources, high combustion calorific value of hydrogen, clean and pollution-free, it has attracted more and more attention from scientists from all over the world. Hydrogen production by electrolysis of water is currently the most mature, easy-to-industrialize, and environmentally friendly method. The traditional hydrogen production by electrolyzing water is to load the electrolytic water catalyst powder on the conductive electrode through the binder to electrolyze water to produce hydrogen. The problem with this mode is that the supported catalyst is easy to fall off, and the binder will also reduce the activity of the electrocatalyst, especially in the case of high loading. Molybdenum carbide is a highly efficient catalyst widely...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/34B01J27/22C25B1/10C01B32/949
CPCB01J27/22C01P2004/03C01P2002/72C01P2002/80C01P2002/82C01P2004/60C01P2006/40C25B1/04C25B9/73Y02E60/36
Inventor 周伟家陈洁佟庆笑唐正华
Owner SOUTH CHINA UNIV OF TECH
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