CN111013591B - CoFe catalytic material with hydrogen evolution function and preparation method thereof - Google Patents
CoFe catalytic material with hydrogen evolution function and preparation method thereof Download PDFInfo
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- CN111013591B CN111013591B CN201911328266.8A CN201911328266A CN111013591B CN 111013591 B CN111013591 B CN 111013591B CN 201911328266 A CN201911328266 A CN 201911328266A CN 111013591 B CN111013591 B CN 111013591B
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 43
- 229910003321 CoFe Inorganic materials 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000001257 hydrogen Substances 0.000 title claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 229940011182 cobalt acetate Drugs 0.000 claims description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000001530 fumaric acid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 7
- 238000001556 precipitation Methods 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 229910000510 noble metal Inorganic materials 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000002238 attenuated effect Effects 0.000 abstract description 2
- 239000010411 electrocatalyst Substances 0.000 abstract description 2
- 239000012621 metal-organic framework Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013246 bimetallic metal–organic framework Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B01J35/33—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- 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
- C25B11/073—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
-
- 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 CoFe catalytic material with a hydrogen evolution function and a preparation method thereof 2 O 4 Then CoFe is added 2 O 4 Annealing treatment is carried out in a tube furnace, and the CoFe catalytic material is synthesized by adopting a reduction method. The catalyst has excellent HER catalytic performance, and the HER precipitation potential is only 95mV vs RHE. And the catalyst has better catalytic stability, and the precipitation potential and the current density are not attenuated after 1000 cycles of CV circulation. The invention adopts cheap non-noble metal raw materials, the preparation process is simple, the synthesized CoFe catalytic material has excellent HER catalytic performance and stable catalytic performance, is a high-efficiency and durable electrocatalyst, can simplify equipment and reduce cost, can improve efficiency, and has good electrolytic water catalysis application prospect.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a CoFe catalytic material with a hydrogen evolution function and a preparation method thereof.
Background
Metal-organic framework (MOF) has a highly ordered pore structure, extremely high porosity and an ultra-high specific surface area, and typically the pore volume of MOF accounts for more than 50% of its total volume. The excellent pore structure of the MOF material provides more active sites for electrochemical redox reactions. Currently, most MOF derived materials are monometallic compounds, and the synthesis of bimetallic compounds derived from MOFs remains difficult: the high complexity of the MOF formation process will result in segregation of nucleation and growth of coordination polymers when the second metal ion is added.
In the prior art, however, the noble metal materials have high price, such as platinum, palladium, ruthenium and the like, and have the problems of low storage amount in the earth and poor stability in the catalytic process; the non-noble metal material has poor catalytic performance, the catalyst for electrolyzing water to produce hydrogen has slow catalytic process, and the bimetallic MOF material with good and stable catalytic performance is not available, so that the research on hydrogen separation is less.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a CoFe catalytic material with a hydrogen evolution function and a preparation method thereof, the CoFe catalytic material is synthesized by adopting a template method and a reduction method, and the catalyst can be used for producing hydrogen by electrolyzing water and has excellent HER catalytic performance and catalytic stability.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
a CoFe catalytic material with hydrogen evolution function and a preparation method thereof comprise the following steps:
1) Dissolving fumaric acid in a DMF solution, adding cobalt acetate and ferric nitrate during stirring, stirring to dissolve, transferring into a polytetrafluoroethylene hydrothermal kettle, heating to 80-120 ℃, keeping for 12h, cooling to room temperature, and drying to obtain a precursor;
2) Putting the precursor into a tube furnace, and annealing in a nitrogen atmosphere to obtain CoFe 2 O 4 ；
3) CoFe is added 2 O 4 And putting the mixture into a tubular furnace to carry out annealing treatment in the nitrogen/hydrogen atmosphere to obtain the CoFe catalytic material.
As a further improvement of the above scheme, the molar ratio of the cobalt acetate to the iron nitrate is (1-3): 1, preferably 2:1.
as a further improvement of the above scheme, the rate in the step 1) temperature raising procedure is 10 ℃/min. Preferably 100 deg.c.
As a further improvement of the above scheme, step 1) further comprises the following steps before drying: several centrifugations and washes were performed with absolute ethanol and DMF.
As a further improvement of the scheme, the drying temperature in the step 1) is 50-80 ℃.
As a further improvement of the above scheme, the annealing treatment process in step 2) is as follows: heating to 450 deg.C at a speed of 2 deg.C/min, maintaining for 2h, cooling to 400 deg.C at a speed of 3 deg.C/min, and naturally cooling.
As a further improvement of the above scheme, the annealing treatment process of step 3) is as follows: heating to 500 deg.C at 2 deg.C/min, maintaining for 2h, cooling to 400 deg.C at 3 deg.C/min, and naturally cooling.
A CoFe catalytic material with hydrogen evolution function is prepared according to the preparation method.
The invention has the beneficial effects that: the invention provides a CoFe catalytic material with a hydrogen evolution function and a preparation method thereof 2 O 4 Then adding CoFe 2 O 4 Annealing treatment is carried out in a tubular furnace, and the CoFe catalytic material is synthesized by adopting a reduction method. The catalyst has excellent HER catalytic performance, and the HER precipitation potential is only 95mV vsRhHE. And the catalyst has better catalytic stability, and the precipitation potential and the current density are not attenuated after 1000 cycles of CV circulation. The invention adopts cheap non-noble metal raw materials, the preparation process is simple, the synthesized CoFe catalytic material has excellent HER catalytic performance and stable catalytic performance, is a high-efficiency and durable electrocatalyst, can simplify equipment and reduce cost, can improve efficiency, and has good electrolytic water catalysis application prospect.
Drawings
FIG. 1 is H at 0.5M 2 SO 4 In electrolyte, the HER catalytic performance curve of the CoFe catalytic material prepared in example 1;
FIG. 2 is a graph of the HER catalytic stability of the CoFe catalytic material prepared in example 1.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It is to be expressly understood that the examples are for illustrative purposes only and are not to be construed as limiting the scope of the present invention, as those skilled in the art will appreciate that many insubstantial modifications and variations of the present invention are possible in light of the above teachings. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercially available products; the process steps or extraction methods not mentioned in detail are all process steps or extraction methods known to the person skilled in the art.
Example 1
A preparation method of a CoFe catalytic material with a hydrogen evolution function comprises the following steps:
1) Weighing 16mmol of fumaric acid, dissolving in 20ml of DMF solution, fully dissolving and stirring for 4h, then adding 0.5mmol of cobalt acetate and 1mmol of ferric nitrate while continuously stirring, fully dissolving and stirring for 4h, finally transferring the solution into a 50ml of polytetrafluoroethylene hydrothermal kettle, heating to 100 ℃ at the speed of 10 ℃/min and keeping for 12h. After the temperature is reduced to room temperature, absolute ethyl alcohol and DMF are used for carrying out centrifugal washing for a plurality of times, and the precursor is obtained after drying at 60 ℃.
2) Putting the precursor into a tube furnace, annealing in nitrogen atmosphere, heating to 450 ℃ at the speed of 2 ℃/min, keeping for 2h, cooling to 400 ℃ at the speed of 3 ℃/min, and naturally cooling to obtain CoFe 2 O 4 A material.
3) The synthesized CoFe 2 O 4 And (3) putting the mixture into a tubular furnace to carry out annealing treatment in the nitrogen/hydrogen atmosphere, raising the temperature to 500 ℃ at the speed of 2 ℃/min, keeping the temperature for 2h, reducing the temperature to 400 ℃ at the speed of 3 ℃/min, and then naturally cooling to obtain the CoFe catalytic material.
Example 2
The CoFe catalytic material prepared in example 1 was subjected to a performance test for hydrogen evolution by electrolysis. The performance of hydrogen evolution and oxygen evolution of the material is carried out in a three-electrode system, and the electrolyte is 0.5M H 2 SO 4 Under the condition of (3), testing the catalytic performance by using cyclic voltammetry. CoFe electrode material is used as an active substance, and Nafion (perfluorosulfonic acid) is used as a binder. 4mg of the active substance and 80. Mu.L of 5wt% Nafion binder were measured and dispersed in 1mL of a mixture of water and ethanol. And (5) carrying out ultrasonic treatment for 1h until the solution is black. Then 5 mul of dispersion liquid is measured and dropped on a glassy carbon electrode with the diameter of 5mm, and the hydrogen evolution catalysis performance is tested.
As can be seen from FIG. 1, the synthesized CoFe has excellent hydrogen evolution catalytic performance, and the precipitation potential is only 95mV vs RHE.
Example 3
The CoFe catalytic material prepared in example 1 is subjected to a catalytic stability performance test, and a precipitation potential and a current density are tested.
As can be seen from FIG. 2, the synthesized CoFe has good catalytic stability, and the precipitation potential and the current density do not decay after 1000 CV cycles.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art based on the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the protection scope of the present invention.
Claims (7)
1. A preparation method of a CoFe catalytic material with a hydrogen evolution function is characterized by comprising the following steps:
1) Dissolving fumaric acid in a DMF solution, adding cobalt acetate and ferric nitrate during stirring, stirring for dissolving, transferring into a polytetrafluoroethylene hydrothermal kettle, heating to 80-120 ℃, keeping for 12h, cooling to room temperature, and drying to obtain a precursor;
2) Putting the precursor into a tube furnace, and annealing in a nitrogen atmosphere to obtain CoFe 2 O 4 ；
3) Mixing CoFe 2 O 4 Putting the mixture into a tube furnace to carry out annealing treatment in the nitrogen/hydrogen atmosphere to obtain a CoFe catalytic material;
the annealing treatment process of the step 2) comprises the following steps: heating to 450 deg.C at 2 deg.C/min, maintaining for 2h, cooling to 400 deg.C at 3 deg.C/min, and naturally cooling.
2. The method according to claim 1, wherein the molar ratio of the cobalt acetate to the iron nitrate is 0.5:1.
3. the method according to claim 1, wherein the rate in the temperature raising process of step 1) is 10 ℃/min.
4. The method according to claim 1, wherein the step 1) further comprises the following steps before drying: several centrifugations and washes were performed with absolute ethanol and DMF.
5. The method according to claim 1, wherein the drying temperature in the step 1) is 50 to 80 ℃.
6. The preparation method according to claim 1, wherein the annealing treatment process of the step 3) is as follows: heating to 500 deg.C at 2 deg.C/min, maintaining for 2h, cooling to 400 deg.C at 3 deg.C/min, and naturally cooling.
7. A CoFe catalytic material having a hydrogen evolution function, characterized by being produced by the production method according to any one of claims 1 to 6.
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| CN103046163A (en) * | 2012-09-03 | 2013-04-17 | 江苏科技大学 | One-dimensional magnetic Fe-Co alloy/cobalt ferrite composite nano-fibers and preparation method thereof |
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2019
- 2019-12-20 CN CN201911328266.8A patent/CN111013591B/en active Active
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