CN111097451A - Preparation method of porous cobalt disulfide catalyst with titanium mesh as substrate, porous cobalt disulfide crystal nanosheet and application - Google Patents
Preparation method of porous cobalt disulfide catalyst with titanium mesh as substrate, porous cobalt disulfide crystal nanosheet and application Download PDFInfo
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 94
- XUKVMZJGMBEQDE-UHFFFAOYSA-N [Co](=S)=S Chemical compound [Co](=S)=S XUKVMZJGMBEQDE-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000000758 substrate Substances 0.000 title claims abstract description 61
- 239000013078 crystal Substances 0.000 title claims abstract description 46
- 239000002135 nanosheet Substances 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 39
- -1 cobalt-aluminum compound Chemical class 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000002243 precursor Substances 0.000 claims abstract description 37
- 230000008569 process Effects 0.000 claims abstract description 24
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims abstract description 14
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 239000011593 sulfur Substances 0.000 claims abstract description 13
- 238000005530 etching Methods 0.000 claims abstract description 11
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 8
- 239000010941 cobalt Substances 0.000 claims abstract description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 32
- 239000004202 carbamide Substances 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 10
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- 239000002064 nanoplatelet Substances 0.000 claims 2
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 23
- 239000000523 sample Substances 0.000 description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 15
- 239000001257 hydrogen Substances 0.000 description 15
- 229910052739 hydrogen Inorganic materials 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- 238000005406 washing Methods 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- XGBOQPVRRBPDDF-UHFFFAOYSA-M sodium;urea;hydroxide Chemical compound [OH-].[Na+].NC(N)=O XGBOQPVRRBPDDF-UHFFFAOYSA-M 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- SWCIQHXIXUMHKA-UHFFFAOYSA-N aluminum;trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SWCIQHXIXUMHKA-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000012476 oxidizable substance Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B01J35/33—
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- B01J35/61—
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/30—Sulfides
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
The invention relates to the technical field of nano materials, in particular to a preparation method of a porous cobalt disulfide catalyst taking a titanium mesh as a substrate, a porous cobalt disulfide crystal nanosheet and application thereof; synthesizing a cobalt-aluminum compound precursor with a titanium mesh as a substrate by adopting a hydrothermal synthesis process; etching the cobalt-aluminum compound precursor with the titanium mesh as the substrate to remove aluminum elements in the cobalt-aluminum compound precursor to obtain a porous cobalt hydroxide crystal with the titanium mesh as the substrate; mixing the porous cobalt hydroxide crystal taking the titanium mesh as the substrate with a sulfur-containing compound, regulating the proportion of sulfur element and cobalt element, and synthesizing the porous cobalt disulfide crystal nanosheet taking the titanium mesh as the substrate through a hydrothermal synthesis process.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a porous cobalt disulfide catalyst taking a titanium mesh as a substrate, a porous cobalt disulfide crystal nanosheet and application.
Background
The development of human civilization and science and technology greatly increases the demand of people on energy, the massive use of traditional fossil energy enables people to consider searching for novel environment-friendly sustainable energy, the sustainable energy obtained by electrolyzing water is a convenient and environment-friendly method, the anodic oxygen evolution reaction is the main bottleneck in the water electrolysis process, the theoretical electrode potential of the oxygen evolution of the electrolyzed water is 1.23VvsRHE, and the high overpotential limits the large-scale practical application of the hydrogen production of the electrolyzed water.
Urea is an inexpensive and reproducible electro-oxidizable substance, and the theoretical electrode potential for electrolytic urea oxidation is 0.37 VvsSHE. Thus, electricityThe urea electrolysis can obtain higher energy conversion efficiency, the urea electrolysis can be applied to the treatment of water body pollution caused by urea, urea is easily converted into ammonia nitrogen, the water body eutrophication can be caused by the excessive ammonia nitrogen, and nitrate harmful to the environment is generated by the ammonia nitrogen through the digestion effect, so the urea which is easier to electrolyze and oxidize replaces water is a more energy-saving and environment-friendly hydrogen production method, the urea electrolysis comprises the hydrogen evolution reaction of a cathode and the oxidation reaction of an anode, the hydrogen is separated out from the cathode in the urea electrolysis process, and the N is separated out from the anode2And Co2。
The noble metal electrochemical catalyst is a good electrochemical catalyst at present, but the noble metal is expensive, and the large-scale practical application of the noble metal electrochemical catalyst is limited due to the scarcity of the earth reserves. Transition metals are abundant in mineral products on earth, transition metal sulfides have high HER activity and low cost, and attract people to pay attention to the transition metals, and cobalt-based sulfides can effectively work for a long time in the whole PH range. In practical applications, in order to further improve the catalytic performance of the electrochemical catalyst, several methods are generally used: other elements are doped, the morphology of the electrochemical catalyst is changed, the specific surface area of the catalyst is improved, the active sites of the catalyst are increased, the material is subjected to sulfur phosphorization, and the active sites of the electrochemical catalyst can also be increased.
Therefore, in order to solve the above problems, the present invention urgently needs to provide a preparation method, a nanomaterial, and a use of a porous cobalt disulfide catalyst based on a titanium mesh.
Disclosure of Invention
The invention aims to provide a preparation method of a porous cobalt disulfide catalyst taking a titanium mesh as a substrate, a porous cobalt disulfide crystal nanosheet and application thereof.
The invention provides a preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate, which comprises the following preparation steps:
synthesizing a cobalt-aluminum compound precursor with a titanium mesh as a substrate by adopting a hydrothermal synthesis process;
etching the cobalt-aluminum compound precursor with the titanium mesh as the substrate to remove aluminum elements in the cobalt-aluminum compound precursor to obtain a porous cobalt hydroxide crystal with the titanium mesh as the substrate;
mixing the porous cobalt hydroxide crystal taking the titanium mesh as the substrate with a sulfur-containing compound, regulating the proportion of sulfur element and cobalt element, and synthesizing the porous cobalt disulfide crystal nanosheet taking the titanium mesh as the substrate through a hydrothermal synthesis process.
Preferably, the etching process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate is as follows: and (3) putting the cobalt-aluminum compound precursor with the titanium mesh as the substrate into sodium hydroxide, and stirring for 10-24h to obtain the porous cobalt hydroxide crystal with the titanium mesh as the substrate.
Preferably, the concentration of sodium hydroxide is 1.0-5.0 mol/L.
Preferably, the elemental sulfur to cobalt ratio is 1-3: 1.
Preferably, the synthesis process of the cobalt-aluminum compound precursor with the titanium mesh as the base comprises the following steps: mixing cobalt nitrate hexahydrate, aluminum nitrate nonahydrate, urea, ammonium fluoride, a titanium mesh and deionized water, and obtaining a cobalt-aluminum compound precursor through a hydrothermal synthesis process.
Preferably, the amounts of the substances of cobalt nitrate hexahydrate, aluminum nitrate nonahydrate, urea and ammonium fluoride are respectively 6-10mmol, 0.6-1.0mmol, 20.0-30.0mmol and 4.0-7.0 mmol; 40.0-60.0mL of deionized water; the area of the titanium mesh is 6-20cm2。
Preferably, in the synthesis process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate, the hydrothermal temperature is 110-160 ℃, and the hydrothermal time is 8-24 h; mixing the porous cobalt hydroxide crystal with the titanium mesh as the substrate with a sulfur-containing compound to synthesize the porous cobalt disulfide crystal nanosheet with the titanium mesh as the substrate, wherein the hydrothermal temperature is 160-200 ℃, and the hydrothermal time is 10-24 h.
The invention also provides a porous cobalt disulfide crystal nanosheet prepared by the preparation method of the porous cobalt disulfide catalyst with the titanium mesh as the substrate.
Preferably, the pore diameter of the porous cobalt disulfide crystal nanosheet is 10-90 nm.
The invention also comprises the application of the porous cobalt disulfide crystal nanosheet.
The invention provides a preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate, a porous cobalt disulfide crystal nanosheet and application. Compared with the prior art, the method has the following advantages:
1. the invention provides a preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate, which synthesizes mesoporous cobalt disulfide nanosheets with the titanium mesh as the substrate by etching aluminum in a cobalt-aluminum compound precursor, has higher catalytic activity in an electrochemical catalytic decomposition reaction system for hydrogen evolution, oxygen evolution and total hydrolysis of electrolytic urea, provides a new catalyst for hydrogen production of the electrolytic urea, improves the energy-saving efficiency of hydrogen production of the electrolytic urea, and provides a new method for treating sewage.
2. The invention provides a preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate, and the process for preparing the porous cobalt disulfide crystal nanosheet is simple, easy to repeat and high in yield.
3. The porous cobalt disulfide crystal nanosheet provided by the invention has mesopores, is uniform in pore size distribution, can be used as a catalyst for catalyzing urea, and is high in catalytic activity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a block diagram of the steps of the preparation method of the porous cobalt disulfide catalyst based on titanium mesh according to the invention;
FIG. 2 is an XRD pattern of a titanium mesh-based porous cobalt disulfide catalyst as described in example one;
FIG. 3 is a scanning electron microscope image of the porous cobalt disulfide catalyst based on titanium mesh in the first embodiment;
FIG. 4 is a transmission electron microscope image of the porous cobalt disulfide catalyst based on titanium mesh in the first example;
FIG. 5 is a graph of oxygen evolution performance of porous cobalt disulfide nanosheets and cobalt disulfide nanosheets based on a titanium mesh in a mixed solution of 1.0mol/L KOH and 0.3mol/L urea in the first example;
FIG. 6 is a graph of hydrogen evolution performance of porous cobalt disulfide nanosheets and cobalt disulfide nanosheets based on a titanium mesh in a mixed solution of 1.0mol/L KOH and 0.3mol/L urea in the first example;
FIG. 7 is a graph of the total hydrolysis performance of the porous cobalt disulfide nanosheets and cobalt disulfide nanosheets based on titanium mesh in a mixed solution of 1.0mol/L KOH and 0.3mol/L urea in the first example.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate, which comprises the following preparation steps:
s1) adopting a hydrothermal synthesis process to synthesize a cobalt-aluminum compound precursor with a titanium mesh as a substrate, namely Co10Al(OH)x/Ti；
S2) etching the precursor of the cobalt-aluminum compound with the titanium mesh as the substrate to remove the aluminum element in the precursor of the cobalt-aluminum compound and obtain the porous cobalt hydroxide crystal with the titanium mesh as the substrate, namely P-Co (OH)x/Ti；
S3) mixing the porous cobalt hydroxide crystal with the titanium mesh as the substrate with a sulfur-containing compound, regulating the ratio of sulfur element to cobalt element, and synthesizing the porous cobalt disulfide crystal nanosheet with the titanium mesh as the substrate, namely P-CoS, by a hydrothermal synthesis process2/Ti。
Specifically, the etching process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate is as follows: and (3) putting the cobalt-aluminum compound precursor with the titanium mesh as the substrate into sodium hydroxide, and stirring for 10-24h to obtain the porous cobalt hydroxide crystal with the titanium mesh as the substrate.
Specifically, the concentration of sodium hydroxide is 1.0 to 5.0 mol/L.
Specifically, the ratio of elemental sulfur to elemental cobalt is 1-3: 1.
Specifically, the synthesis process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate comprises the following steps: mixing cobalt nitrate hexahydrate, aluminum nitrate nonahydrate, urea, ammonium fluoride, a titanium mesh and deionized water, and obtaining a cobalt-aluminum compound precursor through a hydrothermal synthesis process.
Specifically, the amounts of cobalt nitrate hexahydrate, aluminum nitrate nonahydrate, urea and ammonium fluoride are respectively 6-10mmol, 0.6-1.0mmol, 20.0-30.0mmol and 4.0-7.0 mmol; 40.0-60.0mL of deionized water; the area of the titanium mesh is 6-20cm2。
Specifically, in the synthesis process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate, the hydrothermal temperature is 110-; mixing the porous cobalt hydroxide crystal with the titanium mesh as the substrate with a sulfur-containing compound to synthesize the porous cobalt disulfide crystal nanosheet with the titanium mesh as the substrate, wherein the hydrothermal temperature is 160-200 ℃, and the hydrothermal time is 10-24 h.
The invention also provides a porous cobalt disulfide crystal nanosheet prepared by the preparation method of the porous cobalt disulfide catalyst with the titanium mesh as the substrate.
Specifically, the pore diameter of the porous cobalt disulfide crystal nanosheet is 10-90 nm.
The invention also provides application of the porous cobalt disulfide crystal nanosheet.
The invention provides a preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate, which synthesizes mesoporous cobalt disulfide nanosheets with the titanium mesh as the substrate by etching aluminum in a cobalt-aluminum compound precursor, has higher catalytic activity in an electrochemical catalytic decomposition reaction system for hydrogen evolution, oxygen evolution and total hydrolysis of electrolytic urea, provides a new catalyst for hydrogen production of the electrolytic urea, improves the energy-saving hydrogen production efficiency of the electrolytic urea, and provides a new method for treating sewage.
Example one
Sample one P-CoS2The synthesis process of Ti:
1) cutting 2X 3cm2The titanium mesh is soaked in concentrated hydrochloric acid for 10min, the temperature of the concentrated hydrochloric acid is 60 ℃, after soaking, the titanium mesh is washed by deionized water and ethanol respectively, dried and placed into a hydrothermal reaction kettle; weighing 8mmol of cobalt nitrate hexahydrate, 0.8mmol of aluminum nitrate nonahydrate, 25mmol of urea and 6.0mmol of ammonium fluoride, mixing, dissolving by 50mL of deionized water, pouring into a hydrothermal reaction kettle provided with a titanium mesh for hydrothermal synthesis, wherein the hydrothermal temperature is 140 ℃, and the hydrothermal time is 12 hours; after hydrothermal synthesis, taking out a synthesized sample, washing with deionized water and absolute ethyl alcohol, and drying to obtain a cobalt-aluminum compound precursor, namely Co10Al(OH)x/Ti；
2) Preparing 3.0mol/L, 60ml sodium hydroxide solution, and drying cobalt aluminum compound precursor (Co)10Al(OH)xSoaking Ti in sodium hydroxide solution, stirring for 18h, washing with deionized water and absolute ethyl alcohol, and drying to obtain porous crystal, namely P-Co (OH) x/Ti;
3) putting the porous crystal into a new hydrothermal reaction kettle, pouring 2.0g of sodium sulfide and 50mL of water, and carrying out hydrothermal reaction at 200 ℃ for 12 h; after the hydrothermal synthesis is finished, taking out a sample, washing the sample with deionized water and absolute ethyl alcohol, and drying to obtain the porous cobalt disulfide crystal nanosheet, namely P-CoS2and/Ti, wherein P represents porous.
Control sample CoS2Preparation of Ti:
1) cutting 2X 3cm2The titanium mesh is soaked in concentrated hydrochloric acid for 10min, the temperature of the concentrated hydrochloric acid is 60 ℃, the titanium mesh is washed by deionized water and ethanol respectively after soaking, and the titanium mesh is dried and then is placed into a hydrothermal reaction kettle; weighing 8mmol of cobalt nitrate hexahydrate, 0.8mmol of aluminum nitrate nonahydrate, 25mmol of urea and 6.0mmol ofMixing ammonium fluoride, dissolving with 50mL of deionized water, pouring into a hydrothermal reaction kettle provided with a titanium mesh after dissolving, and carrying out hydrothermal synthesis at the hydrothermal temperature of 140 ℃ for 12 h; after hydrothermal synthesis, taking out a synthesized sample, washing with deionized water and absolute ethyl alcohol, and drying to obtain a cobalt-aluminum compound precursor, namely Co10Al(OH)x/Ti；
2) Putting the obtained cobalt-aluminum compound precursor into a new hydrothermal reaction kettle, pouring 2.0g of sodium sulfide and 50mL of water, and carrying out hydrothermal reaction at the hydrothermal temperature of 200 ℃ for 12 h; after the hydrothermal synthesis is finished, taking out a sample, washing the sample by using deionized water and absolute ethyl alcohol, and drying to obtain CoS2/Ti。
P-CoS2Analysis of the results of the/Ti test:
FIG. 2 is P-CoS2XRD pattern of/Ti, and data analysis result shows that the prepared multi-P-CoS2CoS with higher Ti purity2And (4) forming.
FIG. 3 is P-CoS2SEM image of/Ti, in which P-CoS2the/Ti is uniformly distributed on the titanium net.
FIG. 4 shows P-CoS2Transmission Electron microscopy of/Ti, P-CoS2A mean pore diameter of 10-70nm for Ti, P-CoS2The distribution of the/Ti is uniform, and the structure is convenient for exposing active sites and is beneficial to improving the electrochemical performance.
The prepared P-CoS2Cutting Ti nano sheet into multiple pieces of 0.5 multiplied by 0.5cm2P-CoS of2A Ti nanosheet, a P-CoS to be tailored2A/Ti nanosheet is used as a working electrode to form a three-electrode system in a urea sodium hydroxide system for testing electrochemical hydrogen precipitation/oxygen precipitation/total hydrolysis performance, and a saturated calomel electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, 1.0mol/L KOH and 0.3mol/L urea solution is used as electrolyte to form the three-electrode system.
The prepared control sample CoS2Cutting Ti into multiple pieces of 0.5 × 0.5cm2CoS2A Ti nanosheet, a tailored CoS2the/Ti nano-sheet is used as a working electrode to form a three-electrode system in a urea sodium hydroxide system for electrochemical hydrogen precipitation/oxygen precipitationAnd (3) testing the hydrolysis performance, namely forming a three-electrode system by using a saturated calomel electrode as a reference electrode, a platinum sheet electrode as a counter electrode, 1.0mol/L KOH and 0.3mol/L urea solution as electrolyte.
FIG. 5, FIG. 6 and FIG. 7 are P-CoS, respectively2Ti nanosheet and CoS2The oxygen evolution, hydrogen evolution and total hydrolysis performance graphs of the/Ti nanosheet in the mixed solution of 1.0mol/L KOH and 0.3mol/L urea can be seen as follows: P-CoS2Oxygen evolution, Hydrogen evolution and Per-hydrolytic Activity ratio of Ti CoS2More excellent is/Ti.
Example two
Sample II P-CoS2The synthesis process of Ti:
1) cutting 2X 3cm2The titanium mesh is soaked in concentrated hydrochloric acid for 10min, the temperature of the concentrated hydrochloric acid is 60 ℃, the titanium mesh is washed by deionized water and ethanol respectively after soaking, and the titanium mesh is dried and then is placed into a hydrothermal reaction kettle; weighing 8mmol of cobalt nitrate hexahydrate, 0.8mmol of aluminum nitrate nonahydrate, 25mmol of urea and 6.0mmol of ammonium fluoride, mixing, dissolving by 50mL of deionized water, pouring into a hydrothermal reaction kettle provided with a titanium mesh for hydrothermal synthesis, wherein the hydrothermal temperature is 140 ℃, and the hydrothermal time is 12 hours; after hydrothermal synthesis, taking out a synthesized sample, washing with deionized water and absolute ethyl alcohol, and drying to obtain a cobalt-aluminum compound precursor, namely Co10Al(OH)x/Ti；
2) Preparing 5.0mol/L, 60ml sodium hydroxide solution, and drying the cobalt aluminum compound precursor (Co)10Al(OH)xSoaking Ti in sodium hydroxide solution, stirring for 18h, washing with deionized water and absolute ethyl alcohol, and drying to obtain porous crystal, namely P-Co (OH) x/Ti;
3) putting the porous crystal into a new hydrothermal reaction kettle, pouring 2.0g of sodium sulfide and 50mL of water, and carrying out hydrothermal reaction at 200 ℃ for 12 h; after the hydrothermal synthesis is finished, taking out a sample, washing the sample with deionized water and absolute ethyl alcohol, and drying to obtain the porous cobalt disulfide crystal nanosheet, namely P-CoS2and/Ti, P stands for porous.
Sample prepared is di P-CoS2Average pore diameter of TiAbout 20-80nm, and is uniformly distributed on the cobalt disulfide nano-chip.
The difference between the embodiment and the first embodiment is only that the sodium hydroxide concentration is different, the sodium hydroxide is used for removing the Al, the sodium hydroxide concentration is different, different effects can be generated on the Al etching, and the sodium hydroxide concentration is regulated and controlled, so that the Al etching is realized, the aperture size can be adjusted, and the effect of controlling the morphology is achieved.
EXAMPLE III
Sample three P-CoS2The synthesis process of Ti:
1) cutting 2X 3cm2The titanium mesh is soaked in concentrated hydrochloric acid for 10min, the temperature of the concentrated hydrochloric acid is 60 ℃, the titanium mesh is washed by deionized water and ethanol respectively after soaking, and the titanium mesh is dried and then is placed into a hydrothermal reaction kettle; weighing 8mmol of cobalt nitrate hexahydrate, 2.4mmol of aluminum nitrate nonahydrate, 25mmol of urea and 6.0mmol of ammonium fluoride, mixing, dissolving with 50mL of deionized water, pouring into a hydrothermal reaction kettle with a titanium mesh for hydrothermal synthesis at the hydrothermal temperature of 140 ℃ for 12 hours; after hydrothermal synthesis, taking out a synthesized sample, washing with deionized water and absolute ethyl alcohol, and drying to obtain a cobalt-aluminum compound precursor, namely Co10Al(OH)x/Ti；
2) Preparing 3.0mol/L, 60ml sodium hydroxide solution, and drying cobalt aluminum compound precursor (Co)10Al(OH)xSoaking Ti in sodium hydroxide solution, stirring for 18h, washing with deionized water and absolute ethyl alcohol, and drying to obtain porous crystal, namely P-Co (OH) x/Ti;
3) putting the porous crystal into a new hydrothermal reaction kettle, pouring 2.0g of sodium sulfide and 50mL of water, and carrying out hydrothermal reaction at 200 ℃ for 12 h; after the hydrothermal synthesis is finished, taking out a sample, washing the sample with deionized water and absolute ethyl alcohol, and drying to obtain the porous cobalt disulfide crystal nanosheet, namely P-CoS2The symbol,/Ti, P indicates porous.
Sample prepared TriP-CoS2The average pore diameter of the/Ti is about 25-90nm, and the Ti is uniformly distributed on the cobalt disulfide nano-chip.
The present embodiment is different from the first embodimentThe invention prepares porous P-CoS only by changing the quality of aluminum nitrate nonahydrate2The quality of aluminum nitrate nonahydrate/Ti has large influence on the system, and the comparison with the sample I shows that the sample III P-CoS2The average pore diameter of Ti is about 25-90nm, the pore diameter of the sample I has certain change, and the quality of aluminum nitrate nonahydrate is opposite to that of P-CoS2the/Ti has certain influence on the aperture and can regulate and control the appearance.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a porous cobalt disulfide catalyst with a titanium mesh as a substrate is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
synthesizing a cobalt-aluminum compound precursor with a titanium mesh as a substrate by adopting a hydrothermal synthesis process;
etching the cobalt-aluminum compound precursor with the titanium mesh as the substrate to remove aluminum elements in the cobalt-aluminum compound precursor to obtain a porous cobalt hydroxide crystal with the titanium mesh as the substrate;
mixing the porous cobalt hydroxide crystal taking the titanium mesh as the substrate with a sulfur-containing compound, regulating the proportion of sulfur element and cobalt element, and synthesizing the porous cobalt disulfide crystal nanosheet taking the titanium mesh as the substrate through a hydrothermal synthesis process.
2. The method for preparing the porous cobalt disulfide catalyst based on the titanium mesh as the substrate according to claim 1, which is characterized in that: the etching process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate comprises the following steps: and (3) putting the cobalt-aluminum compound precursor with the titanium mesh as the substrate into sodium hydroxide, and stirring for 10-24h to obtain the porous cobalt hydroxide crystal with the titanium mesh as the substrate.
3. The method for preparing the porous cobalt disulfide catalyst based on the titanium mesh as the substrate as the claim 2, which is characterized in that: the concentration of the sodium hydroxide is 1.0-5.0 mol/L.
4. The method for preparing the porous cobalt disulfide catalyst based on the titanium mesh as the substrate according to claim 1, which is characterized in that: the ratio of the sulfur element to the cobalt element is 1-3: 1.
5. The method for preparing the porous cobalt disulfide catalyst based on the titanium mesh as the substrate according to claim 1, which is characterized in that: the synthesis process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate comprises the following steps: mixing cobalt nitrate hexahydrate, aluminum nitrate nonahydrate, urea, ammonium fluoride, a titanium mesh and deionized water, and obtaining a cobalt-aluminum compound precursor through a hydrothermal synthesis process.
6. The method for preparing the porous cobalt disulfide catalyst based on titanium mesh as claimed in claim 5, wherein: the amounts of cobalt nitrate hexahydrate, aluminum nitrate nonahydrate, urea and ammonium fluoride are respectively 6-10mmol, 0.6-1.0mmol, 20.0-30.0mmol and 4.0-7.0 mmol; 40.0-60.0mL of deionized water; the area of the titanium mesh is 6-20cm2。
7. The method for preparing the porous cobalt disulfide catalyst based on the titanium mesh as the substrate according to claim 1, which is characterized in that: in the synthesis process of the cobalt-aluminum compound precursor with the titanium mesh as the substrate, the hydrothermal temperature is 110-160 ℃, and the hydrothermal time is 8-24 h; mixing the porous cobalt hydroxide crystal with the titanium mesh as the substrate with a sulfur-containing compound to synthesize the porous cobalt disulfide crystal nanosheet with the titanium mesh as the substrate, wherein the hydrothermal temperature is 160-200 ℃, and the hydrothermal time is 10-24 h.
8. A porous cobalt disulfide crystal nanosheet prepared by the method for preparing a titanium mesh-based porous cobalt disulfide catalyst as defined in any one of claims 1 to 7.
9. Porous cobalt disulphide crystalline nanoplatelets according to claim 8, characterized in that: the pore diameter of the porous cobalt disulfide crystal nanosheet is 10-90 nm.
10. Use of porous cobalt disulphide crystalline nanoplatelets according to claim 8 or 9.
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