CN112981429A - Metal organic framework and hydroxide heterojunction electrocatalyst and in-situ preparation method and application thereof - Google Patents
Metal organic framework and hydroxide heterojunction electrocatalyst and in-situ preparation method and application thereof Download PDFInfo
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- CN112981429A CN112981429A CN202110208375.7A CN202110208375A CN112981429A CN 112981429 A CN112981429 A CN 112981429A CN 202110208375 A CN202110208375 A CN 202110208375A CN 112981429 A CN112981429 A CN 112981429A
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Abstract
The invention provides a metal organic framework and hydroxide heterojunction electrocatalyst, an in-situ preparation method and application thereof, and belongs to the technical field of catalysts. The invention firstly constructs a metal organic framework taking terephthalic acid as a ligand, then constructs the metal organic framework taking potassium tris-oxalate ferrate as the ligand by adopting an epitaxial growth method, and obtains the heterostructure of the metal organic framework and hydroxide through in-situ conversion in an alkaline environment. The preparation method is simple and efficient, and the heterojunction electrocatalyst constructed by the method has rich phase interfaces and more defects, has excellent electrocatalytic oxygen evolution performance, and can be directly used for various electrocatalytic applications.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a metal organic framework and hydroxide heterojunction electrocatalyst, an in-situ preparation method and application thereof.
Background
Metal-Organic Frameworks (MOFs) are of interest to researchers because of their unique pore structure, large specific surface area and abundant structural types. However, the direct use of metal-organic frameworks for electrocatalysts often has the disadvantages of poor conductivity and few active sites. Therefore, there are many studies trying to compound a metal organic framework with another material to further improve the catalytic performance of the material. For example, in order to further improve the conductivity of the catalyst, the scholars compound MOF with graphene, and utilize the high conductivity of graphene to further improve the catalytic activity of the whole material. In addition, the activity of the catalyst is also improved by introducing defects through the recombination of a metal organic framework and an inorganic hydroxide. However, it is generally difficult to directly build heterogeneous materials on the surface of the metal organic framework because of the large difference between the materials.
In recent years, a method of epitaxial growth of a metal organic frame material has been proposed, in which a metal organic frame material is re-grown on the outer surface of a metal organic frame material. According to previous researches, the inventor finds that certain metal organic framework materials can be converted into hydroxide in an alkaline solution. Thus, the inventors have suggested that: namely, two metal organic framework materials are grown by an epitaxial method, and then can be converted into a heterostructure of a metal organic framework and hydroxide through proper conversion conditions. By utilizing the special in-situ conversion method, the metal organic framework and hydroxide heterojunction electrocatalyst can be effectively constructed, and the efficiency of constructing the heterostructure can be greatly improved.
Based on the metal organic framework and hydroxide heterojunction electrocatalyst, an in-situ preparation method and application thereof are provided.
Disclosure of Invention
The first purpose of the invention is to provide an in-situ preparation method of the metal organic framework and hydroxide heterojunction electrocatalyst.
It is a second object of the present invention to provide a metal organic framework and hydroxide heterojunction electrocatalyst as described above.
The third purpose of the invention is to provide the application of the metal organic framework and hydroxide heterojunction electrocatalyst in electrocatalytic reaction.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the first aspect of the invention provides an in-situ preparation method of a metal organic framework and hydroxide heterojunction electrocatalyst, which comprises the following steps:
step 1: preparation of metal organic framework MOF-1 with terephthalic acid as ligand
Cleaning foamed nickel, placing the cleaned foamed nickel in a container, adding N, N-dimethylformamide, water, ethanol, terephthalic acid and chloride, heating to react until the reaction is finished, taking out a product, cleaning and airing to obtain the metal organic framework MOF-1;
step 2: preparation of metal organic framework MOF-1@ MOF-2 with potassium tris (oxalato) ferrite as ligand
Putting the metal organic framework MOF-1 prepared in the step 1 into water, adding chloride and potassium triallate ferrate to perform a dissolving reaction, taking out a product when the solution is turbid, and cleaning and airing the product to obtain the metal organic framework MOF-1@ MOF-2;
and step 3: preparation of metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH
And (3) injecting potassium hydroxide alkali liquor into the metal organic framework MOF-1@ MOF-2 prepared in the step (2) for conversion reaction, taking out a product after the reaction is finished, cleaning and airing the product, and thus obtaining the metal organic framework and the hydroxide heterojunction electrocatalyst MOF-1@ LDH.
Further, in the step 1, the volume ratio of the N, N-dimethylformamide to the water to the ethanol is 5:1: 1.
Further, in the step 1, the concentration of the terephthalic acid is 0.02-0.2 mmol; the concentration of the chloride is 0.05-0.5 mmol.
Further, in step 1 or 2, the chloride salt is selected from one of nickel chloride, cobalt chloride, ferrous chloride, manganese chloride, copper chloride and zinc chloride.
Further, in step 1, the heating reaction conditions are as follows: reacting for 4-12 h at 90-120 ℃.
Further, in the step 2, the concentration of the potassium tris (oxalato) ferrite is 0.05-0.5 mmol; the concentration of the chloride is 0.1-1 mmol.
Further, in the step 3, the time of the conversion reaction is 1-3 h.
In a second aspect the present invention provides a metal organic framework and hydroxide heterojunction electrocatalyst made by the above method.
In another aspect of the invention there is provided the use of a metal organic framework and hydroxide heterojunction electrocatalyst as described above in an electrocatalytic reaction.
Further, the electrocatalytic reaction comprises an electrocatalytic oxygen evolution reaction and an electrocatalytic hydrogen evolution reaction.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the preparation method is simple and efficient, and the heterojunction electrocatalyst MOF-1@ LDH of the metal organic framework and hydroxide is obtained by in-situ conversion in an alkaline environment, has rich phase interfaces and more defects, has excellent electrocatalytic oxygen evolution performance, and can be directly used for various electrocatalytic applications.
Drawings
FIG. 1 is a scanning electron micrograph of a metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH prepared in example 1 of the present invention;
FIG. 2 is an electrocatalytic oxygen evolution diagram of the metal organic framework and hydroxide heterojunction electrocatalyst, MOF-1@ LDH, prepared in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following figures and preferred examples, which are carried out on the premise of the technical scheme of the present invention, and detailed embodiments and processes are given, but the scope of the present invention is not limited to the following examples, and the experimental methods without specific conditions noted in the following examples are generally performed according to conventional conditions or according to conditions suggested by manufacturers.
The reagents used in the examples of the present invention are shown in table 1 below, but not limited thereto:
TABLE 1
Example 1
Step 1: preparation of metal organic framework MOF-1 with terephthalic acid as ligand
Cleaning foamed nickel, cutting into 1cm x 3cm, placing into a polytetrafluoroethylene bottle, adding 5mLN, N-dimethylformamide, 1mL of water, 1mL of ethanol, 0.02mmol of terephthalic acid and 0.05mmol of nickel chloride hexahydrate; and (3) placing the polytetrafluoroethylene bottle in a reaction kettle, reacting for 4 hours at 120 ℃, taking out after the reaction is finished, cleaning and airing to obtain the metal organic framework MOF-1.
Step 2: preparation of metal organic framework MOF-1@ MOF-2 with potassium tris (oxalato) ferrite as ligand
And (2) placing the metal organic framework MOF-1 prepared in the step (1) into a 10mL glass bottle, adding 6mL of water, adding 0.05mmol of potassium triallate ferrate and 0.1mmol of nickel chloride hexahydrate for dissolution, taking out a product when the solution is turbid, cleaning and drying to obtain the metal organic framework MOF-1@ MOF-2.
And step 3: preparation of metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH
And (3) putting the metal organic framework MOF-1@ MOF-2 prepared in the step (2) into a glass bottle, injecting 1M potassium hydroxide solution into the glass bottle, reacting for 1 hour, taking out a product, cleaning and airing the product, and thus obtaining the metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH.
Example 2
The only difference compared to example 1 is: in the step 1, 0.05mmol of cobalt chloride hexahydrate is adopted to replace 0.05mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Example 3
The only difference compared to example 1 is: in the step 2, 0.1mmol of cobalt chloride hexahydrate is adopted to replace 0.1mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Example 4
The only difference compared to example 1 is: in the step 1, 0.05mmol of copper chloride dihydrate is adopted to replace 0.05mmol of nickel chloride hexahydrate; in the step 2, 0.1mmol of cobalt chloride hexahydrate is adopted to replace 0.1mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Example 5
The only difference compared to example 1 is: in the step 1, 0.05mmol of ferrous chloride hexahydrate is adopted to replace 0.05mmol of nickel chloride hexahydrate; in the step 2, 0.1mmol of cobalt chloride hexahydrate is adopted to replace 0.1mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Example 6
The only difference compared to example 1 is: in the step 1, 0.05mmol of ferrous chloride tetrahydrate is adopted to replace 0.05mmol of nickel chloride hexahydrate; in the step 2, 0.1mmol of zinc chloride is adopted to replace 0.1mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Example 7
The only difference compared to example 1 is: in the step 1, 0.05mmol of ferrous chloride tetrahydrate is adopted to replace 0.05mmol of nickel chloride hexahydrate; in the step 2, 0.1mmol of ferrous chloride tetrahydrate is adopted to replace 0.1mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Example 8
The only difference compared to example 1 is: in the step 1, 0.05mmol of ferrous chloride tetrahydrate is adopted to replace 0.05mmol of nickel chloride hexahydrate; in the step 2, 0.1mmol of manganese chloride tetrahydrate is adopted to replace 0.1mmol of nickel chloride hexahydrate; the rest is the same as in example 1.
Performance characterization
1. Topography determination
Morphology was determined using the metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH prepared in example 1 as an example. The results of measurement under vacuum conditions and 3kV acceleration voltage conditions using a field emission scanning electron microscope (S-4800, Nikkiso K.K.) are shown in FIG. 1. From fig. 1, it can be seen that there exist nanoplatelets and polyhedra, and a large number of nanoplatelets exist on the surface of the nanoplatelets. In addition, the nano-sheets and the polyhedrons are embedded mutually, which shows that the metal organic framework and the hydroxide heterojunction electrocatalyst MOF-1@ LDH prepared by the invention have better stability.
2. Analysis of electrocatalytic oxygen evolution capacity
The electrocatalytic oxygen evolution capacity analysis was performed using the metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH prepared in example 1 as an example. The specific method comprises the following steps: a traditional three-electrode device is adopted to evaluate the oxygen evolution capacity of the catalyst, a platinum electrode is used as a counter electrode, Hg/HgO is used as a reference electrode, and the prepared MOF-1@ LDH is directly used as a working electrode. The three electrodes were connected by Chenghua electrochemical workstation (CHI 760E) and tested by current sweep voltammetry, the results of which are shown in FIG. 2. As can be seen from FIG. 2, the metal-organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH prepared by the invention only needs 220mV overpotential to reach 10mAcm-2And thus has excellent catalytic activity.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. An in-situ preparation method of a metal organic framework and hydroxide heterojunction electrocatalyst is characterized by comprising the following steps of:
step 1: preparation of metal organic framework MOF-1 with terephthalic acid as ligand
Cleaning foamed nickel, placing the cleaned foamed nickel in a container, adding N, N-dimethylformamide, water, ethanol, terephthalic acid and chloride, heating to react until the reaction is finished, taking out a product, cleaning and airing to obtain the metal organic framework MOF-1;
step 2: preparation of metal organic framework MOF-1@ MOF-2 with potassium tris (oxalato) ferrite as ligand
Putting the metal organic framework MOF-1 prepared in the step 1 into water, adding chloride and potassium triallate ferrate to perform a dissolving reaction, taking out a product when the solution is turbid, and cleaning and airing the product to obtain the metal organic framework MOF-1@ MOF-2;
and step 3: preparation of metal organic framework and hydroxide heterojunction electrocatalyst MOF-1@ LDH
And (3) injecting potassium hydroxide alkali liquor into the metal organic framework MOF-1@ MOF-2 prepared in the step (2) for conversion reaction, taking out a product after the reaction is finished, cleaning and airing the product, and thus obtaining the metal organic framework and the hydroxide heterojunction electrocatalyst MOF-1@ LDH.
2. The method for preparing a metal organic framework and hydroxide heterojunction electrocatalyst according to claim 1, wherein in step 1, the volume ratio of N, N-dimethylformamide, water and ethanol is 5:1: 1.
3. The in-situ preparation method of the metal organic framework and hydroxide heterojunction electrocatalyst according to claim 1, wherein in step 1, the concentration of the terephthalic acid is 0.02 to 0.2 mmol; the concentration of the chloride is 0.05-0.5 mmol.
4. The in-situ preparation method of the metal organic framework and hydroxide heterojunction electrocatalyst according to claim 1, wherein in the step 2, the concentration of the potassium tris oxalate ferrate is 0.05 to 0.5 mmol; the concentration of the chloride is 0.1-1 mmol.
5. The method for preparing a metal organic framework and hydroxide heterojunction electrocatalyst according to claim 1 or 3 or 4, wherein in step 1 or 2, the chloride salt is selected from one of nickel chloride, cobalt chloride, ferrous chloride, manganese chloride, copper chloride, zinc chloride.
6. The method of claim 1, wherein in step 1, the heating reaction is performed under the following conditions: reacting for 4-12 h at 90-120 ℃.
7. The in-situ preparation method of the metal organic framework and hydroxide heterojunction electrocatalyst according to claim 1, wherein in step 3, the time of the conversion reaction is 1-3 h.
8. The metal organic framework and hydroxide heterojunction electrocatalyst prepared by the in-situ preparation method of the metal organic framework and hydroxide heterojunction electrocatalyst according to any one of claims 1 to 7.
9. Use of a metal organic framework and hydroxide heterojunction electrocatalyst according to claim 8 in electrocatalytic reactions.
10. Use of a metal organic framework and hydroxide heterojunction electrocatalyst according to claim 9 in electrocatalytic reactions, characterized in that the electrocatalytic reactions comprise electrocatalytic oxygen evolution reactions, electrocatalytic hydrogen evolution reactions.
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| CN115425237A (en) * | 2022-08-15 | 2022-12-02 | 南开大学 | Lithium-oxygen battery bimetal organic frame anode catalyst and preparation method thereof |
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| CN114411167A (en) * | 2022-01-18 | 2022-04-29 | 陕西科技大学 | Total hydrolysis amorphous hydroxide material and preparation method and application thereof |
| CN114411167B (en) * | 2022-01-18 | 2023-03-14 | 陕西科技大学 | Total hydrolysis amorphous hydroxide material and preparation method and application thereof |
| CN114990630A (en) * | 2022-05-25 | 2022-09-02 | 安徽师范大学 | Preparation method and application of ZIF-67-derived hollow bimetal MOF/nitrogen-doped carbon composite material electrocatalyst |
| CN114990630B (en) * | 2022-05-25 | 2023-06-13 | 安徽师范大学 | Preparation method and application of hollow bimetallic MOF/nitrogen-doped carbon composite material electrocatalyst based on ZIF-67 derivative |
| CN114892184A (en) * | 2022-06-11 | 2022-08-12 | 蚌埠学院 | Preparation method of MOFs derivative electrocatalyst |
| CN115029713A (en) * | 2022-06-27 | 2022-09-09 | 海南大学 | Preparation method of nickel-based MOF self-reconfigurable heterojunction for electrolytic water oxygen evolution reaction, obtained product and application |
| CN115029713B (en) * | 2022-06-27 | 2023-04-18 | 海南大学 | Preparation method of nickel-based MOF self-reconfigurable heterojunction for electrolytic water-oxygen evolution reaction, obtained product and application |
| CN115425237A (en) * | 2022-08-15 | 2022-12-02 | 南开大学 | Lithium-oxygen battery bimetal organic frame anode catalyst and preparation method thereof |
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Application publication date: 20210618 |