Preparation method of porous carbon-doped high-dispersion cobalt-phosphide-loaded material and application of porous carbon-doped high-dispersion cobalt-phosphide-loaded material in electro-catalysis hydrogen evolution

A cobalt phosphide and chemical doping technology, applied in chemical instruments and methods, physical/chemical process catalysts, electrodes, etc., can solve the problems of poor conductivity of metal phosphides, difficult to conduct electrons effectively, and need to be optimized and simplified. Conducive to environmental protection, ensuring long-term durability, high thermal and chemical stability

Inactive Publication Date: 2016-01-06
NANKAI UNIV
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Problems solved by technology

For example, the paper Angew.Chem.Int.Ed.2014, 53, 12855 synthesizes FeOOH by hydrothermal method, and then protects it with nitrogen and uses NaH 2 PO 2 It comes from the high temperature treatment of phosphating agent, and the final obtained FeP shows good catalytic activity, but there is still a big gap compared with the noble metal Pt
This is mainly attributed to the poor conductivity of metal phosphides, which makes it difficult to effectively conduct electrons
At the same time, the traditional synthesis process still needs to be optimized and simplified.

Method used

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  • Preparation method of porous carbon-doped high-dispersion cobalt-phosphide-loaded material and application of porous carbon-doped high-dispersion cobalt-phosphide-loaded material in electro-catalysis hydrogen evolution
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  • Preparation method of porous carbon-doped high-dispersion cobalt-phosphide-loaded material and application of porous carbon-doped high-dispersion cobalt-phosphide-loaded material in electro-catalysis hydrogen evolution

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Experimental program
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Effect test

Embodiment 1

[0025] Under stirring at room temperature, 1.236 g of phosphonic acid HEDP was added into 100 ml of deionized water until clear, and then 1.01 g of melamine was slowly added. The temperature was raised to 105° C. to evaporate the solvent to dryness, and the resulting white solid product was continued to be treated at 80° C. under vacuum for 6 h. The product was under nitrogen protection, the nitrogen flow rate was 5ml / min, the temperature was programmed to 900°C for 3h, and the heating rate was 10°C / min, and it was naturally cooled to room temperature. The product was washed, further dried, and a sample was collected, which was recorded as NPC. The samples were characterized by XRD, nitrogen adsorption / desorption, SEM, TEM, XPS and Raman, etc., which confirmed that they were nitrogen-phosphorus co-doped carbon materials with mesoporous-macroporous structure. Among them, TEM and SEM show that the material has irregular macroporous channels. XRD and Raman spectra show that the ...

Embodiment 2

[0027] Under stirring at room temperature, 1.236 g of phosphonic acid HEDP was added into 100 ml of deionized water until clear, and then 1.01 g of melamine was slowly added. 0.012g of cobalt chloride hexahydrate was slowly added, the temperature was programmed to 105°C and the solvent was evaporated to dryness, and the obtained solid product was continued to be treated at 80°C under vacuum for 6h. The product was under the protection of nitrogen, the nitrogen flow rate was 50ml / min, the temperature was programmed to 900°C and kept for 3h, and the heating rate was 10°C / min, and it was naturally cooled to room temperature. The product was cross-washed with hydrochloric acid and water, further dried, and a sample was collected, which was designated as CoPNPC . The samples were characterized by XRD, nitrogen adsorption / desorption, SEM, TEM, XPS and Raman, etc., which confirmed that they were nitrogen-phosphorus co-doped carbon materials with mesoporous-macroporous structure and u...

Embodiment 3

[0029] In Example 1, 5 mg of the sample was taken as an electrocatalyst, ultrasonically dispersed in a mixed solution of 20 μl Nafion (Sigma-Aldrich), 0.2 ml isopropanol, and 0.8 ml deionized water, and ultrasonicated for 30 min. 10 μl of the dispersion solution was dropped onto a pre-polished glassy carbon (GC) electrode with a radius of 3 mm, and dried overnight at room temperature. Electrochemical tests were performed on a computer-controlled electrochemical workstation with a rotating rod. The scanning range of the disk electrode is 0 to -0.6V (vs reversible hydrogen electrode). Figure 5 The linear sweep polarization curves and Tafel curves of the synthesized catalysts are shown. The onset overpotential of electrochemical hydrogen evolution of NPC sample is 126mV, and the slope of Tafel curve is 148mV / dec.

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Abstract

The invention belongs to preparation of a porous nano catalytic material, and particularly relates to a preparation method and application of a porous carbon-doped high-dispersion cobalt-phosphide-loaded material. The material is a carbon-based composite material which is of a mesoporous-macropore hierarchical porous structure and in which nitrogen atoms and phosphorus atoms are chemically doped in carbon skeletons and cobalt phosphide nanoparticles are loaded in a high-dispersion mode, and the specific surface area reaches up to 867 m<2> / g. The material is synthesized through the method comprising the steps that prepolymerization is firstly performed on organic phosphonic acid and melamine, and then high-temperature carbonization is performed. The material is applied to electro-catalysis hydrolysis hydrogen production and has the good effect. Used equipment is simple, the synthesis conditions are mild, the raw materials are easy to obtain, and the material is suitable for industrialized mass production.

Description

technical field [0001] The invention relates to a preparation method of a carbon-doped highly dispersed and loaded cobalt phosphide nanoparticle catalytic material with a fine pore structure and a high specific surface area, which is used for electrocatalytic decomposition of water to produce hydrogen, and belongs to the field of inorganic nano-catalytic materials. Background technique [0002] The widespread use of fossil energy has not only promoted the rapid development of human society, but also caused adverse consequences such as environmental pollution and energy crisis. In order to achieve the goal of sustainable development, it is extremely urgent to find and develop renewable green energy. Among them, hydrogen energy, as the best clean energy for future economic and social development, is regarded as one of the most promising secondary energy sources in the 21st century. Therefore, the research on hydrogen production by electrolysis of water involved in the product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/20B01J27/185C25B11/06C25B1/04
CPCY02E60/36
Inventor 袁忠勇朱运培刘玉萍
Owner NANKAI UNIV
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