CN116356363A - Porous carbon loaded branch-leaf-shaped Ni 2 P catalyst and application thereof in hydrogen evolution reaction - Google Patents

Porous carbon loaded branch-leaf-shaped Ni 2 P catalyst and application thereof in hydrogen evolution reaction Download PDF

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CN116356363A
CN116356363A CN202310225400.1A CN202310225400A CN116356363A CN 116356363 A CN116356363 A CN 116356363A CN 202310225400 A CN202310225400 A CN 202310225400A CN 116356363 A CN116356363 A CN 116356363A
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porous carbon
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朱孝吉
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water

Abstract

The invention relates to the technical field of novel electrocatalysts, and discloses an N-doped porous carbon-loaded dendritic Ni 2 P composite material, relative to Ni alone 2 P electrocatalyst, composite material with stronger activity in electrochemical hydrogen evolution reaction and Ni with special morphology 2 P has larger specific surface area, improves the catalytic efficiency of the composite material, and the porous structure has larger specific surface area, which provides a large number of hydrogen evolution reaction catalytic active sites, and the porous structure connected with each other also provides a timely diffusion channel for reactants and products, so that reactant molecules can contact with more active sites, improves the utilization efficiency of the active sites, and the conductivity of porous carbon loads Ni 2 After P, the conductivity of the composite material is obviously increased, and the nitrogen doped porous carbon can provide more energy storage sites for the composite material, and increase the conductivity of the porous carbon, thereby further improvingElectrocatalytic efficiency of the composite material in hydrogen evolution reactions.

Description

Porous carbon loaded branch-leaf-shaped Ni 2 P catalyst and application thereof in hydrogen evolution reaction
Technical Field
The invention relates to the technical field of novel electrocatalysts, in particular to a porous carbon supported dendritic Ni 2 P catalyst and its application in hydrogen evolution reaction.
Background
Hydrogen is considered as an ideal substitute for fossil fuels, has zero carbon emission and high combustion value, and at present, hydrogen production technologies such as biological hydrogen production, solar hydrogen production, electrocatalytic water diversion and the like emerge like spring bamboo shoots after rain, wherein electrocatalytic water decomposition is taken as a high-efficiency, safe and sustainable large-scale hydrogen production method, and is increasingly valued by people, a Hydrogen Evolution Reaction (HER) is a cathode half reaction in electrolyzed water, noble metals (Pt and Pd) are used as main catalysts of the hydrogen evolution reaction due to high activity, but the commercial application of the noble metals is limited by the scarcity and high cost of resources, so that the search for cheap and efficient catalyst materials to replace noble metal catalyst materials has become urgent.
In recent years, research on non-noble metal electrocatalysts has been increasingly focused, among many non-noble metal electrocatalysts, nickel and nickel alloys with high activity and stability are considered as ideal materials for replacing noble metal (Pt, pd) electrocatalysts, nickel phosphide is a transition metal phosphide and has various phases, and due to the unique physicochemical properties, the nickel phosphide has great application value in the fields of magnetism, electrochemical devices and the like, and has excellent electrochemical properties, and is often used in the fields of hydrogen evolution reaction catalysts and the like, but nickel phosphide has various defects such as poor conductivity, easy agglomeration and the like, and porous carbon has the advantages of large specific surface area, strong conductivity, stable chemical properties and the like, and is often used as a carrier of the electrocatalyst and added into hydrogen evolution reaction.
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a porous carbon supported dendritic Ni 2 P catalyst and application thereof in hydrogen evolution reaction, and solves the problem of Ni 2 The electrocatalytic hydrogen evolution activity of the P-based catalyst is poor.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: n-doped porous carbon-loaded dendritic Ni 2 P composite material, N-doped porous carbon loaded dendritic Ni 2 The preparation method of the P composite material comprises the following steps:
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, adding N, N-dimethylformamide, and carrying out modification reaction under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, uniformly stirring in deionized water, placing in a carbonization furnace, performing carbonization reaction under argon atmosphere, and washing and drying after the reaction is finished to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in the de-solventAdding urea and nitrogen doped porous carbon into ionized water, stirring uniformly, transferring into a reaction kettle, sealing, performing hydrothermal sealing reaction, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon loaded branch-leaf-shaped Ni 2 P composite material.
Preferably, the mass ratio of cellulose to carbonyl diimidazole in the step (1) is 100:80-120.
Preferably, the temperature of the modification reaction in the step (1) is 40-70 ℃, and the reaction time is 10-16h.
Preferably, the mass ratio of the imidazole modified cellulose to the potassium hydroxide in the step (2) is 100:60-100.
Preferably, the temperature of the carbonization reaction in the step (2) is 750-850 ℃, and the reaction time is 0.5-1.5h.
Preferably, in the step (3), the mass ratio of nickel sulfate, sodium dodecyl benzene sulfonate, urea and nitrogen doped porous carbon is 60-80:40-50:40-60:100.
Preferably, the temperature of the hydrothermal sealing reaction in the step (3) is 160-190 ℃, and the reaction time is 10-16h.
(III) beneficial technical effects
Compared with the prior art, the invention has the following experimental principles and beneficial technical effects:
the N-doped porous carbon loaded branch-leaf-shaped Ni 2 The preparation method comprises the steps of (1) preparing a P composite material, wherein carbonyl diimidazole has high reactivity, can perform modification reaction with hydroxyl on the surface of cellulose to form imidazole modified cellulose, introducing nitrogen element into the cellulose, then performing activation modification on the imidazole modified cellulose by taking the imidazole modified cellulose as a carbon source and a nitrogen source through a potassium hydroxide template, performing carbonization reaction under an argon atmosphere to obtain N-doped porous carbon, taking the N-doped porous carbon as a carrier, taking nickel sulfate as a nickel source, taking white phosphorus as a phosphorus source, taking urea as a pH regulator, and preparing N-doped porous carbon-loaded dendritic Ni by a hydrothermal method through the assistance of a surfactant 2 P composite material, ni in hydrothermal synthesis reaction 2 P is uniformly distributed in the porous carbon structure, so that the agglomeration behavior is avoided, and meanwhile, due to multiple componentsPorous carbon multistage pore structure, ni 2 The growth of P crystal is limited to form smaller crystal structure, and the porous carbon has large specific surface area and strong conductivity and can be matched with Ni 2 P forms a synergistic effect, and the activity of the composite material in the electrochemical hydrogen evolution reaction is improved.
The N-doped porous carbon loaded branch-leaf-shaped Ni 2 P composite material, relative to Ni alone 2 P electrocatalyst, composite material with stronger activity in electrochemical hydrogen evolution reaction and Ni 2 The special morphology of P imparts Ni 2 P has larger specific surface area, which improves the contact probability with reactants, and simultaneously, the higher specific surface area also provides more active sites, which improves the catalytic efficiency of the composite material, and the porous carbon is used as a carrier to load dendritic Ni 2 P, the porous structure has larger specific surface area, which provides a large number of hydrogen evolution reaction catalytic active sites, and Ni 2 The P electrocatalyst is uniformly dispersed in the porous carbon structure, thus preventing agglomeration and improving Ni 2 The activity of P in electrochemical hydrogen evolution reaction, and simultaneously, the pore-shaped structures connected with each other provide timely diffusion channels for reactants and products, so that reactant molecules can be contacted with more active sites, the utilization efficiency of the active sites is obviously improved, the subsequent electrocatalytic hydrogen evolution reaction is facilitated, in addition, the conductivity of porous carbon is improved, and Ni is loaded on the porous carbon 2 After P, the conductivity of the composite material is obviously increased, which is favorable for improving the kinetics of hydrogen evolution reaction, and the nitrogen doped porous carbon can provide more energy storage sites for the composite material, increase the conductivity of the porous carbon and further improve the electrocatalytic efficiency of the composite material in the hydrogen evolution reaction.
Detailed Description
In order to achieve the above object, the present invention provides the following specific embodiments and examples: n-doped porous carbon-loaded dendritic Ni 2 The preparation method of the P composite material comprises the following steps:
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:80-120, and carrying out modification reaction at 40-70 ℃ for 10-16 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:60-100, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction in an argon atmosphere, wherein the temperature of the carbonization reaction is 750-850 ℃, the reaction time is 0.5-1.5h, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, adding urea and nitrogen doped porous carbon, wherein the mass ratio of the nickel sulfate to the sodium dodecyl benzene sulfonate to the urea to the nitrogen doped porous carbon is 60-80:40-50:40-60:100, uniformly stirring, transferring to a reaction kettle, sealing, performing a hydrothermal sealing reaction at 160-190 ℃ for 10-16h, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon supported dendritic Ni 2 P composite material.
Example 1
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:80, and carrying out modification reaction at 40 ℃ for 10 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:60, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction under argon atmosphere, wherein the temperature of the carbonization reaction is 750 ℃, the reaction time is 0.5, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, and adding urea and nitrogen doped porous carbon, wherein the nickel sulfate, the sodium dodecyl benzene sulfonate, the urea and the nitrogenThe mass ratio of the doped porous carbon to the doped porous carbon is 60:40:40:100, after being uniformly stirred, the mixture is transferred into a reaction kettle, sealed and subjected to a hydrothermal sealing reaction, the reaction temperature is 160 ℃, the reaction time is 10 hours, and after the reaction is finished, the N-doped porous carbon loaded branch-leaf-shaped Ni is obtained after filtering, washing and drying 2 P composite material.
Example 2
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:90, and carrying out modification reaction at 50 ℃ for 12 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:70, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction under argon atmosphere, wherein the temperature of the carbonization reaction is 780 ℃, the reaction time is 0.8h, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, adding urea and nitrogen doped porous carbon, wherein the mass ratio of the nickel sulfate to the sodium dodecyl benzene sulfonate to the urea and the nitrogen doped porous carbon is 65:42:45:100, uniformly stirring, transferring into a reaction kettle, sealing, performing a hydrothermal sealing reaction at 170 ℃ for 12 hours, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon loaded branch-leaf Ni 2 P composite material.
Example 3
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:110, and carrying out modification reaction at 60 ℃ for 14 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:80, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction under argon atmosphere, wherein the temperature of the carbonization reaction is 820 ℃, the reaction time is 1.2h, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, adding urea and nitrogen doped porous carbon, wherein the mass ratio of the nickel sulfate to the sodium dodecyl benzene sulfonate to the urea to the nitrogen doped porous carbon is 70:48:55:100, uniformly stirring, transferring to a reaction kettle, sealing, performing a hydrothermal sealing reaction at 180 ℃ for 14 hours, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon supported branch-leaf Ni 2 P composite material.
Example 4
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:120, and carrying out modification reaction at 70 ℃ for 16 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:100, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction under argon atmosphere, wherein the temperature of the carbonization reaction is 850 ℃, the reaction time is 1.5h, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, adding urea and nitrogen doped porous carbon, wherein the mass ratio of the nickel sulfate to the sodium dodecyl benzene sulfonate to the urea to the nitrogen doped porous carbon is 80:50:60:100, uniformly stirring, transferring into a reaction kettle, sealing, performing a hydrothermal sealing reaction at 190 ℃ for 16 hours, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon supported branch-leaf Ni 2 P composite material.
Comparative example 1
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:60, and carrying out modification reaction at 30 ℃ for 8 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:48, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction under argon atmosphere, wherein the temperature of the carbonization reaction is 600 ℃, the reaction time is 0.4h, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, adding urea and nitrogen doped porous carbon, wherein the mass ratio of the nickel sulfate to the sodium dodecyl benzene sulfonate to the urea and the nitrogen doped porous carbon is 48:30:30:100, uniformly stirring, transferring into a reaction kettle, sealing, performing a hydrothermal sealing reaction at 120 ℃ for 8 hours, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon supported branch-leaf Ni 2 P composite material.
Comparative example 2
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, and adding N, N-dimethylformamide, wherein the mass ratio of the cellulose to the carbonyl diimidazole is 100:160, and carrying out modification reaction at 90 ℃ for 20 hours under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, wherein the mass ratio of the imidazole modified cellulose to the potassium hydroxide is 100:120, uniformly stirring in deionized water, then placing in a carbonization furnace, carrying out carbonization reaction under argon atmosphere at 1100 ℃ for 2 hours, and washing and drying after the reaction is completed to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, adding urea and nitrogen doped porous carbon, wherein the mass ratio of the nickel sulfate to the sodium dodecyl benzene sulfonate to the urea to the nitrogen doped porous carbon is 100:65:80:100, uniformly stirring, transferring to a reaction kettle, sealing, performing a hydrothermal sealing reaction at 240 ℃ for 20 hours, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon loaded branch-leaf Ni 2 P composite material.
Polishing a glassy carbon electrode into a smooth surface by using an alumina suspension, cleaning, airing, dispersing 5mg of composite material in Nafion (5%) solution and isopropanol aqueous solution, uniformly ultrasonic-homogenizing, depositing a formed pasty catalyst on a glassy carbon electrode substrate, airing, taking the pasty catalyst as a negative electrode, taking a Pt sheet as a counter electrode and Ag/AgCl as a reference electrode, testing electrochemical performance in a standard three-electrode system, taking an argon saturated dilute sulfuric acid solution as an electrolyte, and carrying out linear scanning voltammetry test at a scanning speed of 2 mV.s -1 。
Figure BDA0004118241660000081

Claims (7)

1. N-doped porous carbon-loaded dendritic Ni 2 The P composite material is characterized in that: the N-doped porous carbon-loaded dendritic Ni 2 The preparation method of the P composite material comprises the following steps:
(1) Ultrasonically dispersing cellulose and carbonyl diimidazole in deionized water, adding N, N-dimethylformamide, and carrying out modification reaction under the condition of stirring to obtain imidazole modified cellulose;
(2) Fully grinding imidazole modified cellulose and potassium hydroxide, uniformly stirring in deionized water, placing in a carbonization furnace, performing carbonization reaction under argon atmosphere, and washing and drying after the reaction is finished to obtain N-doped porous carbon;
(3) Completely dissolving nickel sulfate and sodium dodecyl benzene sulfonate in deionized water, howeverAdding urea and nitrogen doped porous carbon, stirring uniformly, transferring into a reaction kettle, sealing, performing hydrothermal sealing reaction, filtering, washing and drying after the reaction is finished to obtain N doped porous carbon supported branch-leaf-shaped Ni 2 P composite material.
2. An N-doped porous carbon supported dendritic Ni according to claim 1 2 The P composite material is characterized in that: the mass ratio of cellulose to carbonyl diimidazole in the step (1) is 100:80-120.
3. An N-doped porous carbon supported dendritic Ni according to claim 1 2 The P composite material is characterized in that: the temperature of the modification reaction in the step (1) is 40-70 ℃, and the reaction time is 10-16h.
4. An N-doped porous carbon supported dendritic Ni according to claim 1 2 The P composite material is characterized in that: the mass ratio of the imidazole modified cellulose to the potassium hydroxide in the step (2) is 100:60-100.
5. An N-doped porous carbon supported dendritic Ni according to claim 1 2 The P composite material is characterized in that: the carbonization reaction temperature in the step (2) is 750-850 ℃, and the reaction time is 0.5-1.5h.
6. An N-doped porous carbon supported dendritic Ni according to claim 1 2 The P composite material is characterized in that: in the step (3), the mass ratio of nickel sulfate, sodium dodecyl benzene sulfonate, urea and nitrogen doped porous carbon is 60-80:40-50:40-60:100.
7. An N-doped porous carbon supported dendritic Ni according to claim 1 2 The P composite material is characterized in that: the temperature of the hydrothermal sealing reaction in the step (3) is 160-190 ℃, and the reaction time is 10-16h.
CN202310225400.1A 2023-03-10 2023-03-10 Porous carbon loaded branch-leaf-shaped Ni 2 P catalyst and application thereof in hydrogen evolution reaction Withdrawn CN116356363A (en)

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