CN111871463B - Preparation method of electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs - Google Patents
Preparation method of electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs Download PDFInfo
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- CN111871463B CN111871463B CN202010672120.1A CN202010672120A CN111871463B CN 111871463 B CN111871463 B CN 111871463B CN 202010672120 A CN202010672120 A CN 202010672120A CN 111871463 B CN111871463 B CN 111871463B
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- 239000000463 material Substances 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000013207 UiO-66 Substances 0.000 title claims abstract description 21
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 18
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 15
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1815—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
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- B01J35/33—
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- B01J35/50—
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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
Abstract
The invention discloses a preparation method of an electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs, which comprises the following steps: to Co (NO)3)2·6H2And adding UiO-66 into the methanol solution of O, then adding the methanol solution of dimethyl imidazole, and stirring for reaction at room temperature to finally obtain the product. The invention has the following advantages: 1. the prepared material has regular appearance and is a regular three-dimensional blocky structure; 2. the prepared material has high efficiency of electrocatalysis full water decomposition; 3. the prepared material has good stability when being used for electrocatalysis full decomposition of water; 4. the material is simple to prepare, low in cost and suitable for large-area popularization and application.
Description
Technical Field
The invention belongs to the technical field of energy environmental protection, and particularly relates to a preparation method of an electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs.
Background
With the over consumption of global fossil energy and the consequent environmental pollution problem, the search for green and renewable clean energy becomes a research hotspot in the field of energy environmental protection. The water resource on earth is rich, and water is decomposed into H by electrocatalysis2And O2The electric energy can be converted into chemical energy to be stored. If it is to be H2And O2The stored chemical energy can be released and used after burning, and the product is cleanH2And O, realizing the circulation of the substances. Meanwhile, solar energy can be converted into electric energy through the photoelectric conversion equipment, so that solar energy can be indirectly stored by utilizing electric decomposition water, and the storage and use efficiency of almost inexhaustible solar energy is improved. Therefore, the development of the electrocatalytic full water decomposition technology has important significance for solving the problems of energy shortage and environmental pollution at present.
The water electrolysis process consists of two parts, namely Hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER). In view of the slow kinetic process of the OER reaction, the OER reaction often becomes the rate-limiting step of fully decomposing water, and often needs a large overpotential to realize fully decomposing water, which increases energy consumption and increases cost, and is not favorable for popularization and application of the fully decomposing water technology. Therefore, the development of a cheap and efficient catalytic material for water electrolysis and the improvement of the efficiency of water electrolysis by electrocatalysis become important research contents in the field.
Disclosure of Invention
The invention aims to solve the technical problems and provides a preparation method of an electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs, so that an electrocatalytic full-decomposition water nanometer material with high efficiency and low cost can be prepared.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs is characterized by comprising the following preparation steps:
(1) preparing MOF material UiO-66 by adopting a method in the prior art;
(2) mixing Co (NO)3)2·6H2Dissolving O in 70mL of methanol, and fully stirring to form a uniform solution; co (NO) used3)2·6H2The amount of O is 0.8-8 mmol;
(3) adding UiO-66 into the solution obtained in the step (2), wherein the addition amount is 20-150 mg, and stirring for 1-2 hours at 20-25 ℃;
(4) and (3) dissolving 20mmol of dimethyl imidazole in 70mL of methanol, slowly pouring into the solution obtained in the step (3), stirring for 15-25 h at the temperature of 20-25 ℃, and centrifugally drying to obtain the final product.
The obtained final product is a composite nano material based on two MOFs, namely ZIF-67 and UiO-66, and has excellent electrocatalytic full water decomposition performance.
The invention has the advantages that: 1. the prepared material has regular appearance and is a regular three-dimensional blocky structure; 2. the prepared material has high efficiency of electrocatalysis full water decomposition; 3, the prepared material has good stability when being used for electrocatalysis full decomposition of water; 4. the material is simple to prepare, low in cost and suitable for large-area popularization and application.
Drawings
FIG. 1 is a scanning electron micrograph of a product according to example 2 of the present invention;
FIG. 2 is a LSV diagram of electrocatalytic full-hydrolysis of the product of example 2 of the present invention;
FIG. 3 is a graph showing the change of current with time in electrocatalytic full-hydrolysis of the product of example 2 of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail with reference to the specific embodiments of the present application. However, the scope of the present invention is not limited to the following specific examples.
Example 1
The MOF material UiO-66 is synthesized by adopting one of the prior methods such as a microwave synthesis method, a microfluidic method, a continuous flow method, a solvent-free method and the like.
0.8 mmol of Co (NO)3)2·6H2Dissolving O in 70mL of methanol to form a uniform solution, adding 20mg of prepared UiO-66 into the uniform solution, stirring the mixture at room temperature for 1.5 h, dissolving 20mmol of dimethylimidazole in 70mL of methanol, slowly pouring the mixture into the solution, stirring the mixture at the temperature of 20 ℃ for 15 h, and centrifugally drying the mixture to obtain the double MOF material ZIF-67@ UiO-66.
Example 2
The MOF material UiO-66 is synthesized by adopting the prior art method.
2 mmol of Co (NO)3)2·6H2O is dissolved in 70mL of methanol to form a homogeneous solution, andadding 40 mg of prepared UiO-66, stirring at room temperature for 1 h, dissolving 20mmol of dimethyl imidazole in 70mL of methanol, slowly pouring into the solution, stirring at 25 ℃ for 20 h, and centrifugally drying to obtain the double MOF material ZIF-67@ UiO-66.
Example 3
The MOF material UiO-66 is synthesized by adopting the prior art method.
3 mmol of Co (NO)3)2·6H2Dissolving O in 70mL of methanol to form a uniform solution, adding 60 mg of prepared UiO-66 into the uniform solution, stirring the mixture at room temperature for 1.5 h, dissolving 20mmol of dimethylimidazole in 70mL of methanol, slowly pouring the mixture into the solution, stirring the mixture at the temperature of 25 ℃ for 20 h, and centrifugally drying the mixture to obtain the double MOF material ZIF-67@ UiO-66.
Example 4
The MOF material UiO-66 is synthesized by adopting the prior art method.
Adding 8mmol of Co (NO)3)2·6H2Dissolving O in 70mL of methanol to form a uniform solution, adding 150mg of prepared UiO-66 into the uniform solution, stirring the solution at room temperature for 2 h, dissolving 20mmol of dimethylimidazole in 70mL of methanol, slowly pouring the solution into the solution, stirring the solution at the temperature of 25 ℃ for 25h, and centrifugally drying the solution to obtain the double MOF material ZIF-67@ UiO-66.
As shown in FIG. 1, as can be seen from the scanning electron microscope image of the product of example 2, the morphology of the material is a uniform and regular three-dimensional block structure. FIG. 2 is a diagram of LSV of the product of example 2 in electrocatalytic full-hydrolysis; FIG. 3 is a graph of the change of current with time when the product of example 2 is subjected to electrocatalytic full-hydrolysis.
The foregoing is a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations are also regarded as the protection scope of the present invention.
Claims (1)
1. A preparation method of an electrocatalytic full-decomposition water material based on ZIF-67 and UiO-66 double MOFs is characterized by comprising the following preparation steps:
(1) preparing MOF material UiO-66 by adopting a method in the prior art;
(2) mixing Co (NO)3)2·6H2Dissolving O in 70mL of methanol, and fully stirring to form a uniform solution; co (NO) used3)2·6H2The amount of O is 0.8-8 mmol;
(3) adding UiO-66 into the solution obtained in the step (2), wherein the addition amount is 20-150 mg, and stirring for 1-2 hours at 20-25 ℃;
(4) and (3) dissolving 20mmol of dimethyl imidazole in 70mL of methanol, slowly pouring into the solution obtained in the step (3), stirring for 15-25 h at the temperature of 20-25 ℃, and centrifugally drying to obtain the final product.
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| CN112432979B (en) * | 2020-12-08 | 2022-02-15 | 重庆医科大学 | Nanocomposite, ESAT-6 electrochemical aptamer sensor and preparation and detection methods thereof |
| 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 |
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