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CN118932409A - A strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide by modifying it with organic thiol ligands - Google Patents

A strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide by modifying it with organic thiol ligands Download PDF

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CN118932409A
CN118932409A CN202411303788.3A CN202411303788A CN118932409A CN 118932409 A CN118932409 A CN 118932409A CN 202411303788 A CN202411303788 A CN 202411303788A CN 118932409 A CN118932409 A CN 118932409A
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molybdenum disulfide
hydrogen evolution
thiol
carbon paper
improving
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黄毅超
刘宇航
裴宗慧
刘旭
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China University of Petroleum East China
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China University of Petroleum East China
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    • 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
    • C25B11/095—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 at least one of the compounds being organic
    • 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
    • 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
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

本发明涉及新能源催化材料技术领域，具体为一种用于提高二硫化钼电催化析氢性能的硫醇有机配体修饰策略。包括:选取3‑巯基丙酸(C3H6O2S)作为硫醇修饰配体，以碳纸为自支撑载体，采取两步水热法将3‑巯基丙酸修饰到二硫化钼表面，所获得的硫醇修饰二硫化钼表现出优秀的中性电解水析氢反应性能。本发明中3‑巯基丙酸的修饰一方面改善了二硫化钼的亲水性，另一方面在二硫化钼表面引入了羧基官能团(‑COOH)，在电催化析氢过程中起到了“质子泵”的作用，极大提升了其在中性条件下的电催化析氢反应动力学。

The present invention relates to the technical field of new energy catalytic materials, specifically a mercaptan organic ligand modification strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide. Including: selecting 3-mercaptopropionic acid (C 3 H 6 O 2 S) as a thiol-modified ligand, using carbon paper as a self-supporting carrier, adopting a two-step hydrothermal method to modify 3-mercaptopropionic acid to the surface of molybdenum disulfide, and the obtained thiol-modified molybdenum disulfide shows excellent neutral electrolytic water hydrogen evolution reaction performance. The modification of 3-mercaptopropionic acid in the present invention improves the hydrophilicity of molybdenum disulfide on the one hand, and introduces a carboxyl functional group (-COOH) on the surface of molybdenum disulfide on the other hand, plays the role of a "proton pump" in the electrocatalytic hydrogen evolution process, and greatly improves its electrocatalytic hydrogen evolution reaction kinetics under neutral conditions.

Description

Thiol organic ligand modification strategy for improving electrocatalytic hydrogen evolution performance of molybdenum disulfide
The invention relates to the technical field of new materials, in particular to a mercaptan organic ligand modification strategy for improving electrocatalytic hydrogen evolution performance of molybdenum disulfide.
Background
Today, the world is facing serious energy problems, and searching for clean green energy is an urgent need for social development. The hydrogen energy is considered to be the renewable clean energy with the most development potential because of the characteristics of rich sources, high heat value, wide application range, environmental protection, no pollution and the like. The problem of sustainable clean production of hydrogen energy becomes a difficult problem which hinders the large-scale application of the hydrogen energy, and in a plurality of hydrogen production modes, water is used as a reaction raw material for hydrogen production by water electrolysis, and the hydrogen production process is green and pollution-free, has simple device and high efficiency, and is considered as a clean hydrogen production mode with great development prospect. Noble metal platinum (Pt) based catalysts are considered to be the best electrolytic water hydrogen evolution reaction catalysts at present, but the noble metal platinum (Pt) based catalysts are expensive and have low reserves, so that the noble metal platinum (Pt) based catalysts are greatly restricted to be applied to a large scale, and therefore, the development of the cheap and efficient hydrogen evolution reaction electrocatalysts has very important research significance and economic value.
Molybdenum disulfide (MoS 2) is a typical non-noble metal catalyst, which has low cost, good HER reactivity at the edge, unique nanosheet structure, controllable electronic structure, and excellent chemical stability, and in recent years, moS 2 electrocatalyst has been attracting attention in the field of hydrogen production by water electrolysis. However, moS 2 still has the defects of poor conductivity, large inert base surface, easy agglomeration, poor hydrophilicity and the like, which greatly hinders the application process of the MoS 2 catalyst in the field of hydrogen production by water electrolysis. Therefore, how to improve the electrocatalytic hydrogen evolution reaction performance of MoS 2 becomes a research hot spot in the field of hydrogen production by water electrolysis.
Disclosure of Invention
The invention aims to provide a mercaptan organic ligand modification strategy for improving the electrocatalytic hydrogen evolution reaction performance of molybdenum disulfide, so as to solve the problem of poor performance of MoS 2 in the background technology.
In order to achieve the above object, the present invention provides a thiol organic ligand modification strategy for improving electrocatalytic hydrogen evolution performance of molybdenum disulfide, comprising:
3-mercaptopropionic acid (C 3H6O2 S) is selected as a mercaptan modification ligand, and the mercaptan ligand is modified on the surface of molybdenum disulfide by adopting a two-step hydrothermal method, so that the hydrogen evolution reaction performance of the molybdenum disulfide is improved.
And the carbon paper is used as a self-supporting carrier, and molybdenum disulfide grows on the carbon paper through a hydrothermal method, so that the conductivity of the molybdenum disulfide is improved.
The preparation method comprises the following steps:
Step 1: 82.6mg of ammonium molybdate tetrahydrate ((NH 4)6Mo7O24·4H2 O) was dissolved in 30mL of distilled water, then 650mg of thiourea (CH 4N2 S) and 30mL of DMF were added, the pH of the mixed solution was adjusted to 1-2 with 1M of HCl, after ultrasonic stirring uniformly, the obtained solution was transferred to a 100mL polytetrafluoroethylene-lined autoclave, carbon paper was immersed in the solution in the autoclave, reacted at 180℃for 24 hours, after the reaction was completed, the carbon paper grown molybdenum disulfide was taken out and washed with deionized water, and dried at room temperature.
Step 2: 87uL of thiol ligand was dissolved in a mixed solution of 30mL DMF and 30mL distilled water, and then transferred to a 100mL polytetrafluoroethylene-lined autoclave. Immersing the carbon paper obtained in the step 1 into the solution in the autoclave, reacting for 4 hours at 180 ℃, taking out the carbon paper after the reaction is finished, immersing and washing the carbon paper with deionized water, and drying the carbon paper at room temperature overnight after the washing is clean, thus obtaining the 3-mercaptopropionic acid modified molybdenum disulfide sample growing on the carbon paper.
And 3, performing electrochemical performance test on the electrocatalytic hydrogen evolution performance of the prepared electrode material by using a Shanghai Chen Hua electrochemical workstation CHI770E, and performing electrocatalytic hydrogen evolution test by using an Ag/AgC1 electrode as a reference electrode, a carbon rod as a counter electrode, and the prepared molybdenum disulfide-loaded carbon paper as a working electrode and a 1.0M PBs solution as an electrolyte solution.
Preferably, the organic mercaptan ligand is 3-mercaptopropionic acid, and the carboxyl is modified on the surface of molybdenum disulfide, so that the hydrophilicity of the molybdenum disulfide can be improved, and the hydrogen evolution performance of the molybdenum disulfide can be improved.
Preferably, the carbon paper is used as a self-supporting carrier for molybdenum disulfide growth, so that the conductivity of the molybdenum disulfide can be improved.
Preferably, the hydrothermal temperatures of the two-stage hydrothermal process are 180 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. The 3-mercaptopropionic acid is selected as a mercaptan organic ligand, and carboxyl in the structure of the 3-mercaptopropionic acid can be modified on the surface of molybdenum disulfide, so that the hydrophilicity of the molybdenum disulfide can be improved, and the electrocatalytic hydrogen evolution performance of the molybdenum disulfide can be greatly improved.
2. The carbon paper is selected as a self-supporting carrier for the growth of molybdenum disulfide, so that the conductivity of the molybdenum disulfide can be improved, and the catalytic hydrogen evolution performance of the molybdenum disulfide can be improved.
Drawings
FIG. 1 is a scanning electron microscope image of a catalyst of the present invention;
FIG. 2 is a scanning electron microscope image of a catalyst of the present invention;
FIG. 3 is an X-ray diffraction pattern of the catalyst of the present invention;
FIG. 4 is a linear sweep voltammogram of a catalyst of the present invention;
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-4, an embodiment of the present invention is provided:
a thiol organic ligand modification strategy for improving electrocatalytic hydrogen evolution performance of molybdenum disulfide, comprising the steps of:
Step 1: 82.6mg of ammonium molybdate tetrahydrate ((NH 4)6Mo7O24·4H2 O) was dissolved in 30mL of distilled water, then 650mg of thiourea (CH 4N2 S) and 30mL of DMF were added, the pH of the mixed solution was adjusted to 1-2 with 1M of HCl, after ultrasonic stirring uniformly, the obtained solution was transferred to a 100mL polytetrafluoroethylene-lined autoclave, carbon paper was immersed in the solution in the autoclave, reacted at 180℃for 24 hours, after the reaction was completed, the carbon paper grown molybdenum disulfide was taken out and washed with deionized water, and dried at room temperature.
Step 2: 87uL of mercaptopropionic acid ligand was dissolved in a mixed solution of 30mL DMF and 30mL distilled water and transferred to a 100mL polytetrafluoroethylene-lined autoclave. Immersing the carbon paper obtained in the step 1 into the solution in the autoclave, reacting for 4 hours at 180 ℃, taking out the carbon paper after the reaction is finished, immersing and washing the carbon paper with deionized water, and drying the carbon paper at room temperature overnight after the washing is clean, thus obtaining the 3-mercaptopropionic acid modified molybdenum disulfide sample growing on the carbon paper.
And 3, performing electrochemical performance test on the electrocatalytic hydrogen evolution performance of the prepared electrode material by using a Shanghai Chen Hua electrochemical workstation CHI770E, and performing electrocatalytic hydrogen evolution test by using an Ag/AgC1 electrode as a reference electrode, a carbon rod as a counter electrode, and the prepared molybdenum disulfide-loaded carbon paper as a working electrode and a 1.0M PBs solution as an electrolyte solution.
And using the obtained Scanning Electron Microscope (SEM) picture to show that the molybdenum disulfide modified by the thiol-propionic acid ligand is successfully synthesized into the nano-sheet.
Further, after the two-step hydrothermal method treatment, the structure of the thiol-modified molybdenum disulfide is determined by using an X-ray diffraction (XRD) technology. In the test results, the thiol-modified molybdenum disulfide is consistent with the common molybdenum disulfide peak.
Further, a Linear Sweep Voltammetry (LSV) curve of electrolyzed water hydrogen evolution obtained by utilizing the molybdenum disulfide modified by the mercaptan and common molybdenum disulfide can be seen that the molybdenum disulfide modified by the mercaptan has more excellent electrocatalytic hydrogen evolution reaction performance compared with unmodified molybdenum disulfide under the small current density of 10mA cm -2.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (5)

1.一种用于提高二硫化钼电催化析氢性能的硫醇有机配体修饰策略，其特征在于：1. A thiol organic ligand modification strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide, characterized in that: 采取两步水热法将有机硫醇配体修饰到二硫化钼表面，提高二硫化钼的析氢反应性能。步骤如下:A two-step hydrothermal method is used to modify the organic thiol ligand onto the surface of molybdenum disulfide to improve the hydrogen evolution reaction performance of molybdenum disulfide. The steps are as follows: 步骤1：将四水合钼酸铵((NH4)6Mo7O24·4H2O)溶解在蒸馏水中，然后加入硫脲(CH4N2S)和N,N-二甲基甲酰胺(DMF)，用1M HCl将混合溶液PH调至1-2，超声搅拌均匀后，将获得的溶液转移到聚四氟乙烯衬里的高压釜中，将碳纸浸入高压釜中的溶液内，在180℃下反应24小时，反应结束后，将生长二硫化钼的碳纸取出并用去离子水浸洗后室温干燥。Step 1: dissolve ammonium molybdate tetrahydrate ((NH 4 ) 6 Mo 7 O 24 ·4H 2 O) in distilled water, then add thiourea (CH 4 N 2 S) and N,N-dimethylformamide (DMF), adjust the pH of the mixed solution to 1-2 with 1M HCl, and after ultrasonic stirring, transfer the obtained solution to a polytetrafluoroethylene-lined autoclave, immerse carbon paper in the solution in the autoclave, and react at 180°C for 24 hours. After the reaction is completed, take out the carbon paper with molybdenum disulfide grown on it, rinse it with deionized water, and then dry it at room temperature. 步骤2：将硫醇配体溶于DMF和蒸馏水混合溶液中，然后转移到聚四氟乙烯衬里的高压釜中。将步骤1所得的碳纸浸入高压釜中的溶液内，在180℃下反应4小时，反应结束后，将碳纸取出，用去离子水浸洗，洗涤干净后室温干燥过夜，即可获得碳纸上生长的3-巯基丙酸修饰二硫化钼样品。Step 2: Dissolve the thiol ligand in a mixed solution of DMF and distilled water, and then transfer it to a polytetrafluoroethylene-lined autoclave. Immerse the carbon paper obtained in step 1 in the solution in the autoclave and react at 180°C for 4 hours. After the reaction is completed, take out the carbon paper, rinse it with deionized water, and dry it at room temperature overnight to obtain a 3-mercaptopropionic acid-modified molybdenum disulfide sample grown on the carbon paper. 2.根据权利要求1所述的一种用于提高二硫化钼电催化析氢性能的硫醇有机配体修饰策略，其特征在于：有机硫醇配体包括但不限于3-巯基丙酸等含有巯基的有机硫醇配体。2. A thiol organic ligand modification strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide according to claim 1, characterized in that the organic thiol ligand includes but is not limited to organic thiol ligands containing thiol groups such as 3-mercaptopropionic acid. 3.根据权利要求1所述的一种用于提高二硫化钼电催化析氢性能的硫醇有机配体修饰策略，其特征在于：使用包括但不限于四水合钼酸铵((NH4)6Mo7O24·4H2O)等含有钼的化合物作为钼源。3. A thiol organic ligand modification strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide according to claim 1, characterized in that: a compound containing molybdenum, including but not limited to ammonium molybdate tetrahydrate (( NH4 ) 6Mo7O24 · 4H2O ), is used as a molybdenum source. 4.根据权利要求1所述的一种用于提高二硫化钼电催化析氢性能的硫醇有机配体修饰策略，其特征在于：使用包括但不限于使用硫脲(CH4N2S)等含硫化合物作为硫源。4. A mercaptan organic ligand modification strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide according to claim 1, characterized in that: sulfur-containing compounds including but not limited to thiourea (CH4N2S ) are used as sulfur sources. 5.根据权利要求1所述的一种用于提高二硫化钼电催化析氢性能的硫醇有机配体修饰策略，其特征在于：使用包括但不限于使用碳纸作为自支撑导电载体用于生长二硫化钼，以提高催化剂的导电性。5. A thiol organic ligand modification strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide according to claim 1, characterized in that: using, including but not limited to using carbon paper as a self-supporting conductive carrier for growing molybdenum disulfide to improve the conductivity of the catalyst.
CN202411303788.3A 2024-09-19 2024-09-19 A strategy for improving the electrocatalytic hydrogen evolution performance of molybdenum disulfide by modifying it with organic thiol ligands Pending CN118932409A (en)

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