CN113106482A - Wood-based hydrogen evolution electrode and preparation method thereof - Google Patents

Wood-based hydrogen evolution electrode and preparation method thereof Download PDF

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CN113106482A
CN113106482A CN202110375005.2A CN202110375005A CN113106482A CN 113106482 A CN113106482 A CN 113106482A CN 202110375005 A CN202110375005 A CN 202110375005A CN 113106482 A CN113106482 A CN 113106482A
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hydrogen evolution
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nickel
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CN113106482B (en
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李彩彩
杨彩霞
柳宗琳
孙庆丰
姜林伟
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Zhejiang A&F University ZAFU
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Abstract

The invention discloses a wood-based hydrogen evolution electrode and a preparation method thereof, wherein the preparation method comprises the following steps: s1: carbonizing wood to obtain carbonized wood; s2: dissolving nickel salt and thiourea in ethylene glycol to obtain a precursor solution; s3: carbonizing wood obtained in the step S1Putting the precursor solution prepared in the step S2 into the solvent thermal reaction, and collecting a product; s4: dissolving palladium chloride, sodium chloride and sodium citrate in deionized water to obtain an electrodeposition solution; s5: and carrying out electrodeposition reaction on the product obtained in the step S3 in the electrodeposition solution obtained in the step S4 to obtain an electrode. The invention takes carbonized wood as a carrier, synthesizes a nickel sulfide/palladium layered composite structure by adopting a solvent thermal bonding electrodeposition mode, shows excellent hydrogen evolution catalytic activity, and can reach 10mA/cm only by 55mV overpotential2Current density and can last for 100 hours.

Description

Wood-based hydrogen evolution electrode and preparation method thereof
Technical Field
The invention relates to the field of hydrogen evolution by electrolyzing water, in particular to a wood-based hydrogen evolution electrode and a preparation method thereof.
Background
Future clean and renewable energy based supplies will greatly reduce the dependence on fossil fuels, solving the problem of increasingly severe energy crisis and environmental pollution. Hydrogen energy is considered as an ideal green new energy source due to the advantages of cleanness, high calorific value, reproducibility, various utilization forms and the like. Electrolysis of water is an effective way to produce hydrogen energy. However, in the water electrolysis reaction process, a relatively large overpotential is required for the Hydrogen Evolution Reaction (HER), and overcoming the overpotential in the water electrolysis hydrogen production process can cause excessive energy waste, so that a catalyst is required to be used for reducing the overpotential to avoid excessive energy consumption.
At present, noble metal-based (e.g., platinum, iridium) catalysts exhibit the best electrochemical performance among electrocatalysts for hydrogen evolution reaction, but the high cost and scarcity of noble metal-based electrocatalysts greatly hamper their commercial application. The preparation of the electrolyzed water catalyst by using transition metals (such as nickel, iron, cobalt, molybdenum, tungsten and the like) with rich earth crust reserves is a feasible means for solving the cost problem and realizing scale production, for example, the Chinese patent application with the application publication number of CN105551810A discloses a solvothermal preparation method of an in-situ electrode, which comprises the steps of dissolving nickel salt in ethylene glycol solution, adding thiourea and ethylenediamine, uniformly mixing, and adding conductive glass for solvothermal reaction to obtain the nickel sulfide in-situ electrode. However, the catalytic efficiency of the current transition metal catalyst is low, and is generally only about 50%.
In addition, in the electrolytic water, the electrodes are generally assembled using a binder, which may hinder the transfer of the electrolyte, and a large amount of hydrogen gas generated at a high current density has no time to diffuse, thereby blocking active sites, and finally decreasing hydrogen evolution activity.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a wood-based hydrogen evolution electrode, which synthesizes a layered composite structure of nickel sulfide/palladium by taking carbonized wood as a substrate and adopting a solvent thermal bonding electrodeposition mode, and has high catalytic activity and good stability.
The invention provides a wood-based hydrogen evolution electrode on the other hand, and the hydrogen evolution electrode has high catalytic activity and good stability.
In order to achieve the above object, an aspect of the present invention provides a method for preparing a woody-based hydrogen evolution electrode, the method comprising the steps of:
s1: carbonizing wood to obtain carbonized wood;
s2: dissolving nickel salt and thiourea in ethylene glycol to obtain a precursor solution;
s3: putting the carbonized wood prepared in the step S1 into the precursor solution prepared in the step S2 for solvothermal reaction, and collecting a product;
s4: dissolving palladium chloride, sodium chloride and sodium citrate in deionized water to obtain an electrodeposition solution;
s5: and carrying out electrodeposition reaction on the product obtained in the step S3 in the electrodeposition solution obtained in the step S4 to obtain an electrode.
Specifically, in step S1, the wood carbonization method includes: the method comprises the steps of pre-carbonizing dry natural wood at 200-300 ℃ for 5-6 hours, and then carbonizing the dry natural wood at 900-1200 ℃ for 5-7 hours.
Preferably, in step S2, the molar ratio of the nickel salt to the thiourea is 1: (2-5).
Preferably, in step S2, the nickel salt is nickel nitrate hexahydrate, nickel sulfate, nickel chloride or nickel acetate.
Specifically, in step S3, the conditions of the solvothermal reaction are as follows: reacting for 8-16 h at 100-200 ℃.
Preferably, in step S3, the collected product is subjected to washing and drying treatment, the washing includes washing with deionized water and/or absolute ethyl alcohol, and the drying manner is vacuum drying.
Preferably, in step S4, the molar ratio of the palladium chloride, the sodium chloride and the sodium citrate is 1: (2-3): (0.1-0.5).
Specifically, in step S5, the conditions of the electrodeposition reaction are: the current density is 5-20 mA/cm2And the reaction time is 2-20 min.
Further, in step S5, after the electrodeposition reaction, the electrode is cleaned and dried, where the cleaning includes cleaning with deionized water and/or absolute ethyl alcohol; the drying mode is vacuum drying.
In another aspect, the invention provides a wood-based hydrogen evolution electrode, which is prepared by the preparation method.
Through the technical scheme, the invention has the following beneficial effects:
1. the invention takes carbonized wood as a carrier, synthesizes a layered composite structure of nickel sulfide/palladium by adopting a solvent thermal bonding electrodeposition mode, and compared with single nickel sulfide and palladium, the electrode of the invention shows excellent hydrogen evolution catalytic activity due to a special layered structure and electronic interaction between the nickel sulfide and the palladium, and can reach 10mA/cm only by 55mV overpotential2The current density can last for 100 hours, the catalytic activity is high, the stability is good, and the possibility is provided for realizing a large-scale water electrolysis process.
2. Compared with other substrates in the prior art, the porous carbonized wood substrate has high mechanical strength and good electrical conductivity after twice high-temperature calcination, and meanwhile, the multi-scale ordered pore channel structure is favorable for the infiltration of electrolyte and the rapid transmission of gas, so that the catalytic reaction kinetics can be accelerated, the catalytic activity is improved, and the wood source is rich, so that the carbonized wood is used as a catalyst carrier, and the cost of catalytic hydrogen evolution is favorably reduced.
Drawings
FIG. 1 is a scanning electron micrograph of an electrode prepared according to example 3 of the present invention;
FIG. 2 is a hydrogen evolution polarization curve of the electrodes prepared in example 3, comparative example 1 and comparative example 2 of the present invention;
FIG. 3 is a hydrogen evolution polarization curve of electrodes prepared in examples 1 to 3 of the present invention;
fig. 4 is a stability graph of an electrode prepared in example 3 of the present invention.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of a wood-based hydrogen evolution electrode, which comprises the following steps:
s1: carbonizing wood to obtain carbonized wood;
specifically, in step S1, the wood carbonization method includes: the method comprises the steps of pre-carbonizing dry natural wood at 200-300 ℃ for 5-6 hours, and then carbonizing the dry natural wood at 900-1200 ℃ for 5-7 hours. The wood is natural wood, such as basswood, pine, beech, etc.
The electrode takes the porous carbonized wood as the substrate, and is subjected to high-temperature calcination twice, compared with other conventional substrates, the electrode has high mechanical strength and good conductivity, and meanwhile, the multi-scale ordered pore structure is favorable for the infiltration of electrolyte and the rapid transmission of gas, so that the catalytic reaction kinetics can be accelerated, and the catalytic activity can be improved. In addition, the wood source is rich, and carbonized wood is used as a catalyst carrier, so that the cost of catalytic hydrogen evolution is reduced.
S2: dissolving nickel salt and thiourea in ethylene glycol to obtain a precursor solution;
preferably, in step S2, the molar ratio of the nickel salt to the thiourea is 1: (2-5).
Preferably, in step S2, the nickel salt is nickel nitrate hexahydrate, nickel sulfate, nickel chloride or nickel acetate.
S3: putting the carbonized wood prepared in the step S1 into the precursor solution prepared in the step S2 for solvothermal reaction, and collecting a product;
nickel salt and thiourea are used as precursors, ethylene glycol is used as a solvent, and a solvothermal method is adopted to prepare the nickel sulfide nano-layered structure. The glycol acid has moderate alkalinity, and the carbonized wood can not be pulverized under the high-temperature and high-pressure conditions of the solvothermal reaction, thereby being beneficial to keeping the stability of the electrode structure.
Specifically, in step S3, the conditions of the solvothermal reaction are as follows: reacting for 8-16 h at 100-200 ℃.
Preferably, in step S3, the collected product is subjected to washing and drying treatment, the washing includes washing with deionized water and/or absolute ethyl alcohol, and the drying manner is vacuum drying.
S4: dissolving palladium chloride, sodium chloride and sodium citrate in deionized water to obtain an electrodeposition solution;
preferably, in step S4, the molar ratio of the palladium chloride, the sodium chloride and the sodium citrate is 1: (2-3): (0.1-0.5).
S5: and carrying out electrodeposition reaction on the product obtained in the step S3 in the electrodeposition solution obtained in the step S4 to obtain an electrode.
Specifically, in step S5, the conditions of the electrodeposition reaction are: the current density is 5-20 mA/cm2And the reaction time is 2-20 min.
Further, in step S5, after the electrodeposition reaction, the electrode is cleaned and dried, where the cleaning includes cleaning with deionized water and/or absolute ethyl alcohol; the drying mode is vacuum drying.
Preparing an electrodeposition solution by adopting palladium chloride, sodium chloride and sodium citrate, depositing a very small amount of metal palladium on the surface of the nickel sulfide by a constant current deposition method, and finally forming a layered structure of nickel sulfide/palladium.
Due to the nature of different materials such as nickel sulfide and metallic palladiumThe quality difference is large, a layered structure of nickel sulfide/palladium cannot be obtained by adopting single solvothermal method, when an electrodeposition method is adopted, although the layered structure of nickel sulfide/palladium can be formed, when a compound synthesized by the method is subjected to an electrocatalytic hydrogen evolution test, as long-time solvothermal treatment is not carried out, the capacitive current generated by the carbonized wood carrier can greatly influence the hydrogen evolution activity, the hydrogen evolution current in the test is larger, and the analysis of the catalytic activity is not facilitated. Therefore, aiming at the special carbonized wood carrier, the invention synthesizes a layered composite structure of nickel sulfide/palladium by adopting a solvent thermal bonding electrodeposition mode. Compared with single nickel sulfide and palladium, due to the special layered structure and the electronic interaction between the nickel sulfide and the palladium, the electrode provided by the invention shows excellent hydrogen evolution catalytic activity, and can reach 10mA/cm only by 55mV of overpotential2The current density can last for 100 hours, and the method provides possibility for realizing a large-scale water electrolysis process.
In another aspect, the invention provides a wood-based hydrogen evolution electrode, which is prepared by the preparation method.
The present invention is further illustrated by the following examples.
Example 1
The preparation method of the wood-based hydrogen evolution electrode comprises the following steps:
s1: cutting a basswood block into a sheet shape with the length of 3cm and the width of 2cm, then sequentially ultrasonically cleaning the basswood block by deionized water and absolute ethyl alcohol for 10min, then placing the basswood block into a vacuum drying oven with the temperature of 60 ℃ for drying for 8h, pre-carbonizing the basswood block in a muffle furnace at the temperature of 200 ℃ for 6h, and then transferring the basswood block into a quartz tube furnace for carbonizing the basswood block at the temperature of 900 ℃ for 7 h;
s2: mixing nickel chloride and thiourea according to a molar ratio of 1: 2, dissolving in 60mL of ethylene glycol, and stirring until the solution is dissolved to obtain a precursor solution;
s3: transferring the precursor solution into a 100mL reaction kettle containing a carrier carbonized wood, carrying out solvothermal reaction for 16h at 100 ℃, naturally cooling and collecting a product, cleaning the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product;
s4: mixing palladium chloride, sodium chloride and sodium citrate according to a molar ratio of 1: 2: dissolving 0.1 in 100mL of deionized water to obtain an electrodeposition solution;
s5: at a current density of 5mA/cm2And carrying out electrodeposition in the electrodeposition solution for 20min, naturally cooling and collecting a product, washing the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product to obtain the electrode.
Example 2
The preparation method of the wood-based hydrogen evolution electrode comprises the following steps:
s1: cutting a basswood block into a sheet shape with the length of 3cm and the width of 2cm, then sequentially ultrasonically cleaning the basswood block by deionized water and absolute ethyl alcohol for 10min, then placing the basswood block into a vacuum drying oven with the temperature of 60 ℃ for drying for 8h, pre-carbonizing the basswood block in a muffle furnace at the temperature of 300 ℃ for 5h, and then transferring the basswood block into a quartz tube furnace for carbonizing the basswood block at the temperature of 1200 ℃ for 5 h;
s2: mixing nickel sulfate and thiourea according to a molar ratio of 1: 5, dissolving in 60mL of ethylene glycol, and stirring until the ethylene glycol is dissolved to obtain a precursor solution;
s3: transferring the precursor solution into a 100mL reaction kettle containing a carrier carbonized wood, carrying out solvothermal reaction for 8h at the temperature of 200 ℃, naturally cooling and collecting a product, cleaning the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product;
s4: mixing palladium chloride, sodium chloride and sodium citrate according to a molar ratio of 1: 3: dissolving 0.5 in 100mL of deionized water to obtain an electrodeposition solution;
s5: at a current density of 20mA/cm2And carrying out electrodeposition in the electrodeposition solution for 2min, naturally cooling and collecting a product, washing the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product to obtain the electrode.
Example 3
The preparation method of the wood-based hydrogen evolution electrode comprises the following steps:
s1: cutting a basswood block into a sheet shape with the length of 3cm and the width of 2cm, then sequentially ultrasonically cleaning the basswood block by deionized water and absolute ethyl alcohol for 10min, then placing the basswood block into a vacuum drying oven with the temperature of 60 ℃ for drying for 8h, pre-carbonizing the basswood block in a muffle furnace at the temperature of 260 ℃ for 6h, and then transferring the basswood block into a quartz tube furnace for carbonizing the basswood block at the temperature of 1000 ℃ for 6 h;
s2: nickel nitrate hexahydrate and thiourea are mixed according to a molar ratio of 1: 3, dissolving in 60mL of ethylene glycol, and stirring until the mixture is dissolved to obtain a precursor solution;
s3: transferring the precursor solution into a 100mL reaction kettle containing a carrier carbonized wood, carrying out solvothermal reaction for 12h at 180 ℃, naturally cooling and collecting a product, cleaning the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product;
s4: mixing palladium chloride, sodium chloride and sodium citrate according to a molar ratio of 1: 2.5: dissolving 0.2 in 100mL of deionized water to obtain an electrodeposition solution;
s5: at a current density of 10mA/cm2And carrying out electrodeposition in the electrodeposition solution for 5min, naturally cooling and collecting a product, washing the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product to obtain the electrode.
Comparative example 1
S1: cutting a basswood block into a sheet shape with the length of 3cm and the width of 2cm, then sequentially ultrasonically cleaning the basswood block by deionized water and absolute ethyl alcohol for 10min, then placing the basswood block into a vacuum drying oven with the temperature of 60 ℃ for drying for 8h, pre-carbonizing the basswood block in a muffle furnace at the temperature of 260 ℃ for 6h, and then transferring the basswood block into a quartz tube furnace for carbonizing the basswood block at the temperature of 1000 ℃ for 6 h;
s2: mixing nickel nitrate hexahydrate and thiourea in a ratio of 1: 3, dissolving the mixture in 60mL of ethylene glycol, and magnetically stirring the mixture until the mixture is dissolved to obtain a precursor solution;
s3: solvent thermal reaction: and transferring the precursor solution into a 100mL reaction kettle containing a carrier carbonized wood, carrying out solvothermal reaction at 180 ℃, naturally cooling and collecting a product after 12h of reaction, washing the product by deionized water and absolute ethyl alcohol, and drying the product in vacuum to obtain the electrode.
Comparative example 2
S1: cutting a basswood block into a sheet shape with the length of 3cm and the width of 2cm, then sequentially ultrasonically cleaning the basswood block by deionized water and absolute ethyl alcohol for 10min, then placing the basswood block into a vacuum drying oven with the temperature of 60 ℃ for drying for 8h, pre-carbonizing the basswood block in a muffle furnace at the temperature of 260 ℃ for 6h, and then transferring the basswood block into a quartz tube furnace for carbonizing the basswood block at the temperature of 1000 ℃ for 6 h;
s2: mixing palladium chloride, sodium chloride and sodium citrate in a ratio of 1: 2.5: dissolving the mixture in deionized water of which the molar ratio is 0.2 in 100mL, and stirring the mixture until the mixture is dissolved to obtain an electrodeposition solution;
s3: and (3) electrodeposition reaction: at a current density of 10mA/cm2And carrying out electrodeposition in the solution for 5min, naturally cooling and collecting a product, washing the product by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying on the product to obtain the electrode.
Performance testing
The morphological characteristics of the electrode obtained in example 3 are represented by a scanning electron microscope, and fig. 1 (a) and (b) clearly show that the efficient catalytic hydrogen evolution electrode based on porous carbonized wood prepared in example 3 is uniformly loaded on a porous carbonized wood framework by an ultrathin nano layered structure, and the micro-nano structure and the porous structure of the substrate make an electrolyte more favorable for entering the inside of the electrode and can be contacted with more catalytic active sites, so that the catalytic activity of the electrode is improved.
Polarity tests were performed on the electrodes prepared in examples 1, 2, 3, 1, 2 and 2 (pure carbonized wood electrode, i.e., electrode obtained by carbonizing raw wood at high temperature and directly performing electrochemical tests as a self-supporting electrode) using the Shanghai Chenghua CHI electrochemical workstation, respectively, and the procedure was set to obtain hydrogen evolution polarization curves as shown in FIGS. 2 and 3 using the linear sweep voltammetry, and it can be seen from FIG. 2 that the electrode prepared in example 3 was 1mol L compared to the electrodes prepared in comparative examples 1, 2 and 2-1In the KOH electrolyte, only 55mV is needed to reach 10mA/cm2Shows excellent catalytic performance.
The electrode obtained in example 3 was subjected to an i-t test (i.e., the change of current with time at a specific voltage) to obtain a current of 10mA/cm2The stability curve at current density, as shown in fig. 4, the current density of the electrode prepared in example 3 was substantially kept constant, indicating that it has excellent stability and can be used for practical production.
The preferred embodiments of the present invention have been described in detail with reference to the examples, but the present invention is not limited to the details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. A preparation method of a wood-based hydrogen evolution electrode is characterized by comprising the following steps:
s1: carbonizing wood to obtain carbonized wood;
s2: dissolving nickel salt and thiourea in ethylene glycol to obtain a precursor solution;
s3: putting the carbonized wood prepared in the step S1 into the precursor solution prepared in the step S2 for solvothermal reaction, and collecting a product;
s4: dissolving palladium chloride, sodium chloride and sodium citrate in deionized water to obtain an electrodeposition solution;
s5: and carrying out electrodeposition reaction on the product obtained in the step S3 in the electrodeposition solution obtained in the step S4 to obtain an electrode.
2. The method for preparing a woody hydrogen-evolving electrode according to claim 1, wherein in step S1, the method for carbonizing wood comprises: the method comprises the steps of pre-carbonizing dry natural wood at 200-300 ℃ for 5-6 hours, and then carbonizing the dry natural wood at 900-1200 ℃ for 5-7 hours.
3. The method for preparing a wood-based hydrogen evolution electrode according to claim 1, wherein in step S2, the molar ratio of the nickel salt to the thiourea is 1: (2-5).
4. The method for producing a woody hydrogen evolution electrode according to claim 1, wherein in the step S2, the nickel salt is nickel nitrate hexahydrate, nickel sulfate, nickel chloride or nickel acetate.
5. The method for producing a woody hydrogen evolution electrode according to claim 1, wherein in step S3, the conditions of the solvothermal reaction are: reacting for 8-16 h at 100-200 ℃.
6. The method of claim 1, wherein the collected product is washed and dried in step S3, the washing includes washing with deionized water and/or absolute ethanol, and the drying is vacuum drying.
7. The method for producing a woody hydrogen evolution electrode according to claim 1, wherein in step S4, the molar ratio of the palladium chloride, the sodium chloride and the sodium citrate is 1: (2-3): (0.1-0.5).
8. The method for producing a woody hydrogen evolution electrode according to any one of claims 1 to 7, wherein in the step S5, the conditions of the electrodeposition reaction are: the current density is 5-20 mA/cm2And the reaction time is 2-20 min.
9. The method for preparing the wood-based hydrogen evolution electrode according to claim 1, wherein in step S5, the electrode is cleaned and dried after the electrodeposition reaction, and the cleaning comprises cleaning with deionized water and/or absolute ethanol; the drying mode is vacuum drying.
10. A woody-based hydrogen evolution electrode produced by the production method according to any one of claims 1 to 9.
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