CN113249753B - Molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material and in-situ synthesis method and application - Google Patents

Molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material and in-situ synthesis method and application Download PDF

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CN113249753B
CN113249753B CN202110371557.6A CN202110371557A CN113249753B CN 113249753 B CN113249753 B CN 113249753B CN 202110371557 A CN202110371557 A CN 202110371557A CN 113249753 B CN113249753 B CN 113249753B
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蒋继波
孙冉
黄星
丛海山
王云云
唐佳斌
陈宇凯
韩生
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Shanghai Institute of Technology
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    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention relates to a molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material, an in-situ synthesis method and application, wherein the method comprises the following steps: preparing a mixed aqueous solution A of 2-methylimidazole and cobalt nitrate hexahydrate; placing the foam liquid into the mixed aqueous solution A prepared in S1, standing and soaking to obtain Co-MOF/NF; mixing ammonium molybdate hydrate, sodium sulfide nonahydrate and deionized water to obtain a mixed solution B; transferring Co-MOF/NF into the mixed solution B, and obtaining MoS after constant potential electrodeposition reaction2@ Co-MOF/NF. Compared with the prior art, the method increases the specific surface area of the material, improves the contact area of the material and water, facilitates the preparation of hydrogen, improves the nanostructure of the material, and improves the hydrogen evolution performance and stability of the material by self-loading the flaky Co-MOF on the NF.

Description

Molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material and in-situ synthesis method and application
Technical Field
The invention relates to the technical field of hydrogen energy, in particular to a molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material, an in-situ synthesis method and application.
Background
With the increasing exhaustion of fossil fuels, various new energy sources are continuously developed and utilized. The hydrogen energy is used as a renewable secondary energy source, has wide source, high heat value, cleanness and good combustion stability, and is a new generation of energy carrier widely adopted after non-renewable energy sources such as fossil fuel and the like.
Electrocatalytic water decomposition consists of Oxygen Evolution Reactions (OERs) and Hydrogen Evolution Reactions (HERs), which are considered to produce high purity hydrogen (H) due to their sustainability and carbon emission-free2) An effective technique of (1).Much work has been devoted to elucidating the cost-effective HER performance of electrolysis in acidic electrolytes with emphasis on preparing high performance electrocatalysts to reduce dynamic overpotentials. However, in strongly acidic electrolytes (e.g. 0.5M H)2SO4) Of these, few electrocatalysts remain stable to HER performance. At the same time, in alkaline solutions, there are fewer materials used for high energy radiation, which requires the ability to overcome higher energy barriers compared to acidic electrolytes.
In general, high activity HER electrocatalysts require several characteristics (1) inherently high specific surface area, (2) high conductivity and fast electron transfer pathways, and (3) large number of active sites and fast mass transport pathways (including transport of reaction substrates and diffusion of gaseous products). Although Pt and Ru/Ir based composites are considered the most advanced electrocatalysts for HER and OER, their high cost and scarcity severely hamper large scale applications. Therefore, much research effort has been devoted to developing earth-abundant alternatives with high efficiency and stability.
Disclosure of Invention
The invention aims to solve the problems and provide a molybdenum sulfide @ cobalt-MOF/NF hydrogen evolution material, an in-situ synthesis method and application thereof.
The purpose of the invention is realized by the following technical scheme:
the first purpose of the invention is to protect an in-situ synthesis MoS2A method of @ Co-MOF/NF hydrogen evolution material comprising the steps of:
s1: preparing a mixed aqueous solution A of 2-methylimidazole and cobalt nitrate hexahydrate;
s2: placing the foam liquid into the mixed aqueous solution A prepared in S1, standing and soaking to obtain Co-MOF/NF;
s3: mixing ammonium molybdate hydrate, sodium sulfide nonahydrate and deionized water, and adjusting the pH value of the solution to a target value to obtain a mixed solution B;
s4: transferring Co-MOF/NF into the mixed solution B, and performing constant potential electrodeposition reaction to obtain the final productMoS2@Co-MOF/NF。
Further, the preparation process of the mixed aqueous solution a in S1 is as follows: mixing 2-methylimidazole, cobalt nitrate hexahydrate and deionized water, and performing magnetic stirring to obtain a mixed solution A;
the molar ratio of the 2-methylimidazole to the cobalt nitrate hexahydrate is 1:1, the ratio of the molar amount of the 2-methylimidazole to the volume of the water is 1mmol:30mL, and the ratio of the molar amount of the cobalt nitrate hexahydrate to the volume of the water is 1mmol:50 mL. After standing, 2-methylimidazole with different contents and cobalt nitrate hexahydrate generate MOFs materials with different structures, and the optimal proportion is selected.
Further, the stirring time described in S1 was 30min, and a purple mixed solution a was obtained after the stirring.
Further, in S2, deionized water and absolute ethyl alcohol are sequentially used to wash the nickel foam, which is repeated three times, and the dried nickel foam is soaked in the solution a at room temperature for 10 hours, and the nickel foam after soaking is washed with absolute ethyl alcohol and deionized water for 2 times, and then dried in a vacuum oven overnight at 60 ℃. The loading capacity of the methylimidazole and the cobalt nitrate hexahydrate in the foamed nickel is 10-20 wt%.
Furthermore, the molar ratio of Mo to S in the mixed solution B in S3 is 1:4, and the ratio of the molar amount of the sodium sulfide nonahydrate to the volume of the deionized water is 2mmol:50 mL.
Further, the PH was adjusted to the target value by adding nitric acid in S3.
Further, in S3, the PH is adjusted to the target value by the color change of the solution, which is marked by the change of the solution from yellow to red brown.
Further, the constant potential range of the constant potential electrodeposition in S4 is-0.8V to-1.0V, and the time range of the constant potential electrodeposition is 1200S to 7200S.
A second object of the invention is to protect a MoS obtained by the above-mentioned preparation process2@ Co-MOF/NF hydrogen evolution materials.
A third object of the present invention is to protect a MoS2@ Co-MOF/NF hydrogen evolution material in electrocatalytic hydrogen evolution reactionThe use of (1).
Further, the MoS is used2The @ Co-MOF/NF hydrogen evolution material is used as a working electrode in the electrocatalytic hydrogen evolution reaction.
Compared with the prior art, the invention has the technical advantages that:
1) the Tafel slope and the overpotential of the hydrogen evolution material prepared in the technical scheme are low, so that the breakthrough energy barrier required by hydrogen evolution is low, the hydrogen conversion rate is high, the hydrogen rate is high, the raw material cost is low, the preparation method is environment-friendly, the preparation mode is simple, the hydrogen evolution effect of the material in an alkaline solution is good, and the material is expected to be developed towards industrialization.
2) In the invention of the hydrogen evolution material, the adopted foam nickel is a sound absorption porous metal with excellent performance of a three-dimensional full-through mesh structure, the porosity of the foam nickel is about 95 percent, water or gas can pass through the foam nickel smoothly without obstruction, the nickel frameworks are hollow and are mutually connected in a metallurgical state, and the foam nickel has the advantages of good stability, high porosity, thermal shock resistance, small bulk density, large specific surface area and the like.
3) In the technical scheme, the flaky Co-MOF is self-loaded on NF, so that the specific surface area of the material is increased, the contact area of the material and water is increased, hydrogen is easier to prepare, the nano structure of the material is improved, and the hydrogen evolution performance and stability of the material are improved.
Detailed Description
As a part of the concept of the technical scheme, the foamed nickel used in the technical scheme is a commercial metal functional material with three-dimensional open pores and communicated pores with a metal framework, has a large electrochemical reaction interface, and has a wide application prospect in the aspect of electrochemical electrode materials.
As part of the present solution concept, in order to solve the above problems and further improve the electrochemical activity, several strategies have been proposed to address the above critical issues, such as using Transition Metal Disulfides (TMDs) as catalytic cathode HER, since it has Pt-like catalytic properties with near zero free energy hydrogen adsorption
Figure BDA0003009511040000031
And excellent thermodynamic stability. However, individual MoS2Due to less active site exposure and poorer electrical conductivity, the technical scheme further improves the catalytic performance of the TMDs-based catalysts to meet the practical application.
The present invention is described in detail below with reference to specific examples, but the present invention is not limited thereto in any way.
The raw materials used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
Figure BDA0003009511040000041
The hydrogen evolution material is prepared by the preparation method comprising the following steps:
respectively dissolving 1mmol of 2-methylimidazole and 1mmol of cobalt nitrate hexahydrate in 30mL of deionized water and 50mL of deionized water, mixing, and stirring in a magnetic stirrer for 30min until no solid particles exist in the solution and the color is purple. Soaking foamed nickel with the thickness of 1mm multiplied by 4mm multiplied by 1mm at room temperature for 10h, washing the soaked Co-MOF/NF with absolute ethyl alcohol and deionized water for 2 times respectively, vacuumizing at 60 ℃ and drying overnight; dissolving 0.07mmol of ammonium molybdate tetrahydrate and 2mmol of sodium sulfide nonahydrate in 50mL of deionized water, and dripping 0.1mL of nitric acid to adjust the pH value, wherein the solution is changed from yellow to reddish brown; taking the dried Co-MOF/NF as a working electrode, and carrying out constant potential electrodeposition at a chi760e electrochemical workstation, wherein the voltage is as follows: -0.8V; electrodeposition time: 1200 s. Finally obtaining MoS2@ Co-MOF/NF hydrogen evolution materials.
Application example 1
The MoS of example 1 was added2The @ Co-MOF/NF hydrogen evolution material can be directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(1)MoS2The @ Co-MOF/NF hydrogen evolution material is washed twice by deionized water and isopropanol respectively and directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(2) 1.0M potassium hydroxide solution is prepared to be used as electrocatalytic electrolyteIntroducing nitrogen to drive off air, and then adding MoS2The @ Co-MOF/NF, Ag/AgCl and platinum electrodes are respectively used as a working electrode, a reference electrode and a counter electrode, and are connected with an electrochemical workstation, and the electrocatalytic hydrogen evolution performance of the electrode material is measured in electrolyte. The Tafel slope of the material is 126.24mV dec-1At a current density of 10mA cm-2The overpotential of (2) is 255 mV.
Example 2
Figure BDA0003009511040000051
The hydrogen evolution material is prepared by the preparation method comprising the following steps:
respectively dissolving 1mmol of 2-methylimidazole and 1mmol of cobalt nitrate hexahydrate in 30mL of deionized water and 50mL of deionized water, mixing, and stirring in a magnetic stirrer for 30min until no solid particles exist in the solution and the color is purple. Soaking foamed nickel with the thickness of 1mm multiplied by 4mm multiplied by 1mm at room temperature for 10h, washing the soaked Co-MOF/NF with absolute ethyl alcohol and deionized water for 2 times respectively, vacuumizing at 60 ℃ and drying overnight; dissolving 0.07mmol of ammonium molybdate tetrahydrate and 2mmol of sodium sulfide nonahydrate in 50mL of deionized water, and dripping 0.1mL of nitric acid to adjust the pH value, wherein the solution is changed from yellow to reddish brown; taking the dried Co-MOF/NF as a working electrode, and carrying out constant potential electrodeposition at a chi760e electrochemical workstation, wherein the voltage is as follows: -0.8V; electrodeposition time: 2400 s. Finally obtaining MoS2@ Co-MOF/NF hydrogen evolution materials.
Application example 2
The MoS of example 2 was added2The @ Co-MOF/NF hydrogen evolution material can be directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(1)MoS2The @ Co-MOF/NF hydrogen evolution material is washed twice by deionized water and isopropanol respectively and directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalytic electrolyte, introducing nitrogen to drive off air, and then adding MoS2The @ Co-MOF/NF, Ag/AgCl and platinum electrodes are respectively used as a working electrode, a reference electrode and a counter electrode to be connected with electrochemical workAnd measuring the electrocatalytic hydrogen evolution performance of the electrode material in the electrolyte. The Tafel slope of the material is 38.33mV dec-1At a current density of 10mA cm-2The overpotential of (3) is 165 mV. And the deviation between the LSV curve after 1000 CV tests and the LSV curve before the CV tests is not large, which indicates that the material has good stability.
Example 3
Figure BDA0003009511040000061
The hydrogen evolution material is prepared by the preparation method comprising the following steps:
respectively dissolving 1mmol of 2-methylimidazole and 1mmol of cobalt nitrate hexahydrate in 30mL of deionized water and 50mL of deionized water, mixing, and stirring in a magnetic stirrer for 30min until no solid particles exist in the solution and the color is purple. Soaking foamed nickel with the thickness of 1mm multiplied by 4mm multiplied by 1mm at room temperature for 10h, washing the soaked Co-MOF/NF with absolute ethyl alcohol and deionized water for 2 times respectively, vacuumizing at 60 ℃ and drying overnight; dissolving 0.07mmol of ammonium molybdate tetrahydrate and 2mmol of sodium sulfide nonahydrate in 50mL of deionized water, and dripping 0.1mL of nitric acid to adjust the pH value, wherein the solution is changed from yellow to reddish brown; taking the dried Co-MOF/NF as a working electrode, and carrying out constant potential electrodeposition at a chi760e electrochemical workstation, wherein the voltage is as follows: -0.8V; electrodeposition time: 7200 s. Finally obtaining MoS2@ Co-MOF/NF hydrogen evolution materials.
Application example 3
The MoS of example 3 was added2The @ Co-MOF/NF hydrogen evolution material can be directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(1)MoS2The @ Co-MOF/NF hydrogen evolution material is washed twice by deionized water and isopropanol respectively and directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalytic electrolyte, introducing nitrogen to drive off air, and then adding MoS2The @ Co-MOF/NF, Ag/AgCl and platinum electrodes are respectively used as working electrodes, reference electrodes and counter electrodes, and are connected with an electrochemical workstation, and the electrodes are measured in electrolyteThe material electrocatalytic hydrogen evolution performance. The Tafel slope of the material is 96.12mV dec-1At a current density of 10mA cm-2The overpotential of (2) is 249 mV.
Comparative example 1
2-methylimidazole 1.0mmol
Cobalt nitrate hexahydrate 1.0mmol
80.0ml of deionized water
The hydrogen evolution material is prepared by the preparation method comprising the following steps:
respectively dissolving 10mmol of 2-methylimidazole and 1mmol of cobalt nitrate hexahydrate in 30mL of deionized water and 50mL of deionized water, mixing, and stirring in a magnetic stirrer for 30min until no solid particles exist in the solution and the color is purple. Soaking foamed nickel with the thickness of 1mm multiplied by 4mm multiplied by 1mm at room temperature for 10h, washing the soaked Co-MOF/NF with absolute ethyl alcohol and deionized water for 2 times respectively, vacuumizing at 60 ℃ and drying overnight; obtaining the Co-MOF/NF hydrogen evolution material.
Application comparative example 1
The Co-MOF/NF hydrogen evolution material of the comparative example 1 is dried and directly used as a working electrode in the electrocatalytic hydrogen evolution reaction.
(1) Preparing 1.0M potassium hydroxide solution as electrocatalysis electrolyte, introducing nitrogen to drive away air, taking Co-MOF/NF, Ag/AgCl electrode and platinum electrode as working electrode, reference electrode and counter electrode respectively, connecting with electrochemical workstation, and measuring the electrocatalysis hydrogen evolution performance of the electrode material in the electrolyte. The Tafel slope of the material is 90.19mV dec-1At a current density of 10mA cm-2The overpotential of (3) was 275 mV. Individual Co-MOFs have higher specific surface area, porosity but electrodeposition loaded MoS2The electrochemical performance of the sample can be further improved, and thus the electrochemical performance of the comparative example is reduced relative to the embodiment.
Comparative example 2
Figure BDA0003009511040000071
The hydrogen evolution material is prepared by the preparation method comprising the following steps:
dissolving 0.07mmol of ammonium molybdate tetrahydrate and 2mmol of sodium sulfide nonahydrate in 50mL of deionized water, and dripping 0.1mL of nitric acid to adjust the pH value, wherein the solution is changed from yellow to reddish brown; the dried NF was used as a working electrode, and constant potential electrodeposition was performed at a chi760e electrochemical workstation, voltage: -0.8V; electrodeposition time: 2400 s. Finally obtaining MoS2/NF hydrogen evolution material.
Comparative application example 2
MoS of comparative example 22the/NF hydrogen evolution material can be directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without drying.
(1)MoS2The NF hydrogen evolution material is directly used as a working electrode in the electrocatalytic hydrogen evolution reaction without being dried after being washed twice by deionized water and isopropanol respectively.
(2) Preparing 1.0M potassium hydroxide solution as electrocatalytic electrolyte, introducing nitrogen to drive off air, and then adding MoS2the/NF, Ag/AgCl and platinum electrodes are respectively used as a working electrode, a reference electrode and a counter electrode to be connected with an electrochemical workstation, and the electrocatalytic hydrogen evolution performance of the electrode material is measured in electrolyte. The Tafel slope of the material is 148.15mV dec-1At a current density of 10mA cm-2The overpotential of (2) is 225 mV.
Comparative example 3
Mo-S/NF hydrogen evolution material in CN111359636A, and a preparation method and application thereof, wherein the preparation method comprises the following steps: 1) mixing ammonium tetrathiomolybdate and thiourea with water, and performing ultrasonic dispersion to obtain a mixed solution; 2) adding the mixed solution into a reaction kettle, adding foamed nickel serving as a carrier into the reaction kettle, and performing hydrothermal reaction to obtain Mo-S/NF; 3) and calcining the Mo-S/NF under the anaerobic condition to obtain the Mo-S/NF hydrogen evolution material. The Tafel slope of the material is 98mV dec-1At a current density of 10mA cm-2The overpotential of (2) is 225 mV.
Compared with the comparative example 3, the technical scheme can obtain better electrochemical performance only by self-loading and electrodeposition, and the sample wrapping the polyhedron can be formed by self-loading and electrodeposition, so that the active specific surface area of the sample is greatly increased, and the electrochemical performance of the sample is improved.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (5)

1. In-situ synthesis MoS2A method of @ Co-MOF/NF hydrogen evolution material, comprising the steps of:
s1: preparing a mixed aqueous solution A of 2-methylimidazole and cobalt nitrate hexahydrate;
s2: placing the foam liquid into the mixed aqueous solution A prepared in S1, standing and soaking to obtain Co-MOF/NF;
s3: mixing ammonium molybdate hydrate, sodium sulfide nonahydrate and deionized water, and adjusting the pH value of the solution to a target value to obtain a mixed solution B;
s4: transferring Co-MOF/NF into the mixed solution B, and obtaining MoS after constant potential electrodeposition reaction2@Co-MOF/NF；
The preparation process of the mixed aqueous solution A in the S1 comprises the following steps: mixing 2-methylimidazole, cobalt nitrate hexahydrate and deionized water, and performing magnetic stirring to obtain a mixed solution A;
the molar ratio of the 2-methylimidazole to the cobalt nitrate hexahydrate is 1:1, the ratio of the molar amount of the 2-methylimidazole to the volume of the water is 1mmol:30mL, and the ratio of the molar amount of the cobalt nitrate hexahydrate to the volume of the water is 1mmol:50 mL;
the molar ratio of Mo to S in the mixed solution B in S3 is 1:4, and the ratio of the molar weight of the sodium sulfide nonahydrate to the volume of the deionized water is 2mmol:50 mL;
adjusting the pH to a target value by adding nitric acid in S3;
in S3, the PH value is determined and adjusted to a target value through the color change of the solution, and the color change is marked in the way that the solution is changed from yellow to brownish red;
the time range of constant potential electrodeposition is 1200 s-7200, and the deposition voltage is-0.8V.
2. An in situ synthesized MoS according to claim 12A method for a @ Co-MOF/NF hydrogen evolution material is characterized in that deionized water and absolute ethyl alcohol are sequentially used for washing foamed nickel in S2 for three times respectively, dried foamed nickel is soaked in a solution A at room temperature for 10 hours, the soaked foamed nickel is washed with the absolute ethyl alcohol and the deionized water for 2 times respectively, a vacuum-pumping oven is used for drying overnight, and the temperature is 60 ℃.
3. MoS obtained by the preparation method according to any one of claims 1 to 22@ Co-MOF/NF hydrogen evolution materials.
4. A MoS as claimed in claim 32The application of the @ Co-MOF/NF hydrogen evolution material in electrocatalytic hydrogen evolution reaction.
5. MoS according to claim 42The application of the @ Co-MOF/NF hydrogen evolution material in electrocatalytic hydrogen evolution reaction is characterized in that the MoS is subjected to a reaction treatment2The @ Co-MOF/NF hydrogen evolution material is used as a working electrode in the electrocatalytic hydrogen evolution reaction.
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