CN116876022A - Preparation method of self-supporting bifunctional electrolyzed water catalyst - Google Patents
Preparation method of self-supporting bifunctional electrolyzed water catalyst Download PDFInfo
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- CN116876022A CN116876022A CN202310735046.7A CN202310735046A CN116876022A CN 116876022 A CN116876022 A CN 116876022A CN 202310735046 A CN202310735046 A CN 202310735046A CN 116876022 A CN116876022 A CN 116876022A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000003054 catalyst Substances 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 57
- 230000001588 bifunctional effect Effects 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 159
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 102
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 51
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 37
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 37
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000006260 foam Substances 0.000 claims abstract description 36
- 239000012535 impurity Substances 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 24
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 24
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 22
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 18
- NKHCNALJONDGSY-UHFFFAOYSA-N nickel disulfide Chemical compound [Ni+2].[S-][S-] NKHCNALJONDGSY-UHFFFAOYSA-N 0.000 claims abstract description 17
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims description 43
- 239000012528 membrane Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- 238000000855 fermentation Methods 0.000 claims description 15
- 230000004151 fermentation Effects 0.000 claims description 15
- 239000002808 molecular sieve Substances 0.000 claims description 15
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000005373 pervaporation Methods 0.000 claims description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 12
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 10
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000006477 desulfuration reaction Methods 0.000 claims description 9
- 230000023556 desulfurization Effects 0.000 claims description 9
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 239000004317 sodium nitrate Substances 0.000 claims description 6
- 235000010344 sodium nitrate Nutrition 0.000 claims description 6
- 235000010288 sodium nitrite Nutrition 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 230000009977 dual effect Effects 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 claims description 3
- 229920001661 Chitosan Polymers 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910000003 Lead carbonate Inorganic materials 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000004697 Polyetherimide Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 230000029936 alkylation Effects 0.000 claims description 3
- 238000005804 alkylation reaction Methods 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005262 decarbonization Methods 0.000 claims description 3
- 238000005261 decarburization Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 229910000464 lead oxide Inorganic materials 0.000 claims description 3
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- 229920001601 polyetherimide Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 230000009466 transformation Effects 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000005342 ion exchange Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000008092 positive effect Effects 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- -1 sodium sulfate Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
Classifications
-
- 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
-
- 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
- C25B11/054—Electrodes comprising electrocatalysts supported on a carrier
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the technical field of preparation of electrolytic water catalysts, and discloses a preparation method of a self-supporting bifunctional electrolytic water catalyst, which adopts impurity removal treatment of nickel nitrate hexahydrate; mixing nickel nitrate hexahydrate, urea and thioacetamide with ionized water, and performing ultrasonic treatment for 15min; standing for 40min; adding foam nickel, and performing a hydrothermal reaction to obtain a nickel disulfide precursor growing on the foam nickel in situ; and mixing the nickel disulfide precursor which grows on the foam nickel in situ with a solution containing sodium molybdate and a nickel source, and performing a secondary hydrothermal reaction to obtain the electrolytic water catalyst. The sodium molybdate prepared by the sodium molybdate preparation method has high purity, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved; meanwhile, the absolute ethyl alcohol prepared by the absolute ethyl alcohol preparation method has high quality, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved.
Description
Technical Field
The invention belongs to the technical field of preparation of an electrolyzed water catalyst, and particularly relates to a preparation method of a self-supporting bifunctional electrolyzed water catalyst.
Background
Electrolyzed water generally refers to the process of producing a product from water containing salts (e.g., sodium sulfate, which may not produce chlorine) after electrolysis. The electrolyzed water is neutral per se, other ions can be added, or water with two properties can be generated through separation of a semi-permeable membrane. One of which is basic ionized water and the other of which is acidic ionized water. The electrolytic water using sodium chloride as electrolyte contained in water contains sodium hydroxide, hypochlorous acid and sodium hypochlorite after electrolysis (if pure water is electrolyzed, only hydroxide ions, hydrogen, oxygen and hydrogen ions are generated); however, sodium molybdate adopted in the existing preparation method of the electrolyzed water catalyst contains impurities, which affect the quality of the prepared electrolyzed water catalyst; meanwhile, the quality of the adopted absolute ethyl alcohol serving as a raw material is poor, so that the quality of the catalyst for manufacturing the electrolytic water is affected.
Through the above analysis, the problems and defects existing in the prior art are as follows:
1. sodium molybdate impurity problem: sodium molybdate adopted in the existing preparation method of the electrolyzed water catalyst contains impurities, and the impurities can be embedded into the structure of the catalyst to influence the structure and the performance of the catalyst. Further, these impurities may hinder electron transport during electrolysis, resulting in a decrease in electrolysis efficiency.
2. Absolute ethanol quality problem: the absolute ethanol used in the existing preparation method has poor quality and may contain moisture or other impurities. These impurities may affect the catalyst preparation process, resulting in uneven catalyst surface or unstable structure.
3. The preparation process of the catalyst is complex: in the prior art, the preparation process of the catalyst involves multiple steps such as hydrothermal reaction, washing, drying, etc. These steps can result in cumbersome and time consuming preparation procedures, increasing the cost of the preparation.
4. Catalyst stability and activity problems: existing electrolyzed water catalysts may have stability and activity problems. During electrolysis, the catalyst may gradually lose activity, resulting in a decrease in electrolysis efficiency. In addition, since the existing catalyst may have a problem of unstable structure, the catalyst may be damaged in structure to affect its performance after long-term use.
5. Problems of byproducts in electrolyzed water: in the prior art, byproducts generated by electrolysis of water, such as chlorine, hypochlorous acid, sodium hypochlorite, etc., may have negative effects on the environment and human health. Thus, there is a need to find more environmentally friendly electrolytic processes and catalysts to reduce the production of these by-products.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method of a self-supporting bifunctional water electrolysis catalyst.
The invention is realized in such a way that a preparation method of a self-supporting bifunctional electrolytic water catalyst is characterized by comprising the following steps:
step one, preparing a nickel sulfate precursor: removing impurities in nickel nitrate hexahydrate, mixing nickel sulfate, urea and thioacetamide with ionized water, and carrying out ultrasonic treatment for 30 minutes to uniformly disperse the mixture; adding foam nickel into the mixture, and performing a hydrothermal reaction at 180 ℃ for 24 hours to form a nickel sulfate precursor on the surface of the foam nickel;
step two, preparing an electrolyzed water catalyst by a real-time monitoring system: preparing a solution containing sodium molybdate and a nickel source, wherein the sodium molybdate is an oxidant, provides oxygen atoms for the oxidation process of the electrolytic water reaction, and the nickel source is used for the catalytic reduction reaction; mixing a nickel sulfate precursor and a solution containing sodium molybdate and a nickel source, and performing a secondary hydrothermal reaction at 200 ℃ for 36 hours to convert the nickel sulfate precursor into an electrolyzed water catalyst; the real-time monitoring system is used for monitoring the temperature, the pressure and the concentration of substances in the reaction process;
step three, treating an electrolyzed water catalyst: repeatedly washing the prepared electrolyzed water catalyst with distilled water and absolute ethyl alcohol for a plurality of times to remove residual ions and impurities; the washed electrode was dried in an oven to obtain a highly efficient electrolyzed water catalyst.
Further, the preparation method of the self-supporting bifunctional electrolyzed water catalyst comprises the following steps:
step one, removing impurities from nickel nitrate hexahydrate; mixing nickel nitrate hexahydrate, urea and thioacetamide with ionized water, and performing ultrasonic treatment for 15min; standing for 40min; adding foam nickel, and performing a hydrothermal reaction to obtain a nickel disulfide precursor growing on the foam nickel in situ;
the urea preparation method comprises the following steps:
the raw material coal uses steam and air as gasifying agents to generate semi-water gas in a gas producer, and the gas is purified by the processes of primary desulfurization, transformation, secondary desulfurization, decarburization, fine desulfurization, methanol, alkylation and the like to remove various impurities;
compressing the pure nitrogen-hydrogen mixture to high pressure, and synthesizing ammonia at high temperature in the presence of a catalyst; purifying and compressing carbon dioxide desorbed by decarbonization, sending the carbon dioxide and ammonia into a urea synthesizing tower, and synthesizing urea at proper temperature and pressure;
mixing a nickel disulfide precursor growing in situ on foam nickel with a solution containing sodium molybdate and a nickel source, and performing a secondary hydrothermal reaction to obtain an electrolyzed water catalyst;
and thirdly, repeatedly washing the electrolyzed water catalyst with distilled water and absolute ethyl alcohol for a plurality of times, and drying the washed electrode in an oven to obtain the high-efficiency electrolyzed water catalyst.
Further, the mass ratio of the nickel nitrate hexahydrate, urea, thioacetamide and ionized water is 0.1:0.2:0.3:11.
Further, the preparation method of the sodium molybdate comprises the following steps:
1) The sodium nitrate is reduced by lead, the sodium nitrate is heated and melted, a small amount of metallic lead is added, and stirring and continuous heating are carried out until the lead is totally oxidized. The resulting cake was divided into small pieces while cooling, and the resulting lead oxide was extracted several times with hot water. Introducing carbon dioxide gas to generate lead carbonate precipitate, filtering, accurately neutralizing the filtrate with dilute nitric acid, evaporating, concentrating, and separating out sodium nitrite;
2) At normal temperature, dropwise adding a sodium nitrite solution into an ammonium molybdate solution, and controlling the atomic mole ratio of sodium to molybdenum to be 3:1, continuously stirring to generate white precipitate, aging for 13h, respectively washing with distilled water and absolute ethyl alcohol for 4 times, filtering, and drying to obtain white flaky sodium molybdate finished products.
Further, the preparation method of the absolute ethyl alcohol comprises the following steps:
1) Removing impurities from the ethanol fermentation liquid; the ethanol fermentation liquid is divided into at least two parts, one part enters a rectifying tower I, an ethanol material flow I with the concentration of 65wt% is obtained at the top of the rectifying tower I, and the other part enters a rectifying tower II, and an ethanol material flow II with the concentration of 65wt% is obtained at the top of the rectifying tower II;
2) The ethanol material flow I and the ethanol material flow II are respectively mixed and sent into a pervaporation separator after passing through a heating device and a second reboiler of a tower kettle of a rectifying tower I, and are dehydrated by the pervaporation separator to obtain an ethanol material flow III with the concentration of 96 wt%;
3) The ethanol material flow III is overheated by saturated steam and enters a molecular sieve pressure swing adsorber, and the top material flow of the molecular sieve pressure swing adsorber enters a first reboiler of a tower kettle of a rectifying tower I to be condensed to obtain an absolute ethanol product with the concentration of more than 98 weight percent;
the number of tower plates of the rectifying tower I is 33, the temperature of the tower top is 85 ℃, the temperature of the tower bottom is 102 ℃, the operating pressure is 75kPa, and the position of a feeding plate is positioned at the 7 th tower plate from top to bottom; the column plate number of the rectifying column II is 30, the temperature of the column top is 120 ℃, the temperature of the column bottom is 130 ℃, the operating pressure is 1800kPa, and the position of the feeding plate is positioned at the 7 th column plate from top to bottom.
Further, the concentration of the ethanol in the ethanol fermentation liquid is 11% by weight, and the ratio of the ethanol fermentation liquid to the ethanol entering the rectifying tower I and the rectifying tower II is 2:1 by weight.
Further, the ethanol concentration in the ethanol fermentation broth was 9% by weight.
Further, the number of tower plates of the rectifying tower I is 33, the temperature of the tower top is 79 ℃, and the temperature of the tower bottom is 99 ℃; the number of tower plates of the rectifying tower II is 30, the temperature of the tower top is 110 ℃, and the temperature of the tower bottom is 110 ℃.
Further, the pervaporation separator was operated at a temperature of 85℃and at a pressure of 86kPa.
Further, the membrane material used in the pervaporation separator is a selective permeable membrane selected from an organic membrane, an inorganic membrane or an organic-inorganic hybrid membrane, and the membrane material can selectively permeate ethanol and water.
Further, the membrane material is selected from a silicon-aluminum molecular sieve membrane, a chitosan membrane, a polyvinyl alcohol membrane, a polyetherimide membrane or a polyvinyl alcohol-Na molecular sieve membrane;
the molecular sieve pressure swing adsorber operates at 130℃and 290kPa.
In combination with the technical scheme and the technical problems to be solved, the technical scheme to be protected has the following advantages and positive effects:
firstly, the sodium molybdate prepared by the sodium molybdate preparation method has high purity, so that the quality of the catalyst for preparing electrolyzed water is greatly improved; meanwhile, the absolute ethyl alcohol prepared by the absolute ethyl alcohol preparation method has high quality, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved.
1) High-efficiency catalyst: the prepared electrolyzed water catalyst has high-efficiency catalysis, can promote the electrolysis reaction of water, improve the reaction rate and efficiency, can catalyze the oxidation-reduction reaction of water, and can convert harmful substances into harmless substances, thereby having dual functions.
2) Is simple and easy to implement: the preparation method adopts simple reaction steps and treatment methods, is easy to realize and operate, does not need complex equipment and technical conditions, and can be widely applied to laboratory or industrial production.
3) Environmental protection sustainable: the raw materials and the solvent used in the preparation process are all environment-friendly substances, and cannot pollute and harm the environment. The prepared electrolyzed water catalyst can be used in the fields of environmental protection, water treatment and the like, and has good application prospect.
4) Economical and practical: the preparation method has the advantages that the cost of raw materials and equipment required is low, meanwhile, the prepared electrolyzed water catalyst has longer service life and higher catalytic efficiency, the production and treatment cost can be reduced, and the method has economical practicability.
Secondly, the sodium molybdate prepared by the sodium molybdate preparation method has high purity, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved; meanwhile, the absolute ethyl alcohol prepared by the absolute ethyl alcohol preparation method has high quality, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved.
Drawings
FIG. 1 is a flow chart of a preparation method of a self-supporting bifunctional electrolyzed water catalyst provided by an embodiment of the invention.
Fig. 2 is a flow chart of a method for preparing sodium molybdate according to an embodiment of the present invention.
Fig. 3 is a flowchart of a method for preparing absolute ethanol according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The preparation method provided by the embodiment of the invention specifically comprises the following three steps.
First, preparing a nickel disulfide precursor
1.1 impurity removal treatment: impurities in the nickel nitrate hexahydrate are removed so as not to influence the subsequent preparation process.
1.2 preparation of mixture: nickel nitrate hexahydrate, urea and thioacetamide were mixed with ionized water and the mixture was uniformly dispersed by ultrasonic treatment for 15 minutes.
1.3 foam Nickel addition: nickel foam is added to the mixture and a nickel disulfide precursor is formed on the surface of the nickel foam by a single hydrothermal reaction.
Second step, preparing electrolytic water catalyst
2.1 preparation of solution: a solution containing sodium molybdate and a nickel source was prepared. Sodium molybdate is an oxidizing agent in this solution that provides oxygen atoms for the oxidation process of the electrolytic water reaction, while the nickel source is for the catalytic reduction reaction.
2.2 mixing reaction: and mixing the nickel disulfide precursor with a solution containing sodium molybdate and a nickel source, and converting the nickel disulfide precursor into an electrolyzed water catalyst through a secondary hydrothermal reaction.
Third step, electrolyzed water catalyst treatment
3.1 washing: the prepared electrolyzed water catalyst is repeatedly washed with distilled water and absolute ethyl alcohol for a plurality of times to remove any residual ions and impurities.
3.2 drying: the washed electrode was dried in an oven to obtain a highly efficient electrolyzed water catalyst.
In general, this preparation method prepares an electrolyzed water catalyst having a dual function through a series of reaction and treatment steps. The catalyst can promote the electrolysis reaction of water to produce hydrogen and oxygen, and can catalyze the oxidation-reduction reaction of water to convert harmful substances into harmless substances.
The following are six specific embodiments of the present invention:
example 1:
1.1 impurity removal treatment: impurities in the nickel nitrate hexahydrate are removed so as not to influence the subsequent preparation process.
1.2 preparation of mixture: 0.1 mol of nickel nitrate hexahydrate, 0.2 mol of urea and 0.1 mol of thioacetamide were mixed with 50 ml of ionized water, and the mixture was uniformly dispersed by ultrasonic treatment for 15 minutes.
1.3 foam Nickel addition: 1 gram of nickel foam is added to the mixture and a nickel disulfide precursor is formed on the surface of the nickel foam by a single hydrothermal reaction.
Example 2:
2.1 preparation of solution: a solution containing sodium molybdate and a nickel source was prepared by mixing 0.01 mole of sodium molybdate and 0.01 mole of nickel nitrate hexahydrate.
2.2 mixing reaction: the nickel disulfide precursor prepared in example 1 and the solution containing sodium molybdate and nickel source prepared in example 2 were mixed and converted into an electrolyzed water catalyst by a secondary hydrothermal reaction.
Example 3:
3.1 washing: the electrolyzed water catalyst prepared in example 2 was repeatedly washed with distilled water and absolute ethanol 5 times to remove any remaining ions and impurities.
3.2 drying: the washed electrode was dried in an oven at 80 c for 12 hours to obtain a highly efficient electrolyzed water catalyst.
Example 4:
the molar amount of urea was increased to 0.5 mole based on example 1 to increase the nitrogen content of the catalyst, thereby increasing its catalytic activity.
Example 5:
the molar amount of sodium molybdate was increased to 0.02 mole based on example 2 to increase the oxidation capacity of the catalyst, thereby increasing the efficiency of oxygen generation in electrolyzed water.
Example 6:
on the basis of example 3, the number of washings was increased to 7 and the drying temperature was increased to 100 ℃ to ensure better removal of residual materials and moisture, thereby improving the stability and activity of the catalyst.
As shown in fig. 1, the invention provides a preparation method of a self-supporting bifunctional electrolyzed water catalyst, which comprises the following steps:
s101, removing impurities from nickel nitrate hexahydrate; mixing nickel nitrate hexahydrate, urea and thioacetamide with ionized water, and performing ultrasonic treatment for 15min; standing for 40min; adding foam nickel, and performing a hydrothermal reaction to obtain a nickel disulfide precursor growing on the foam nickel in situ;
the urea preparation method comprises the following steps:
the raw material coal uses steam and air as gasifying agents to generate semi-water gas in a gas producer, and the gas is purified by the processes of primary desulfurization, transformation, secondary desulfurization, decarburization, fine desulfurization, methanol, alkylation and the like to remove various impurities;
compressing the pure nitrogen-hydrogen mixture to high pressure, and synthesizing ammonia at high temperature in the presence of a catalyst; carbon dioxide desorbed from decarbonization is purified and compressed, and then sent into a urea synthesizing tower together with ammonia, and urea is synthesized under proper temperature and pressure.
As an optimization scheme of the embodiment of the invention, the refinement of the first step is as follows:
1.1 impurity removal treatment: first, nickel nitrate hexahydrate is treated to remove impurities therein. The method can be realized by a recrystallization method or an ion exchange method, and the like, so that the purity of the nickel nitrate hexahydrate is ensured to be higher, and the influence on the subsequent preparation process is avoided.
1.2 formulation of the mixture: a molar amount of nickel nitrate hexahydrate, urea and thioacetamide are mixed with a volume of ionized water to form a mixed solution. The composition and performance of the electrolyzed water catalyst can be controlled by adjusting the molar ratio of each component.
1.3 ultrasonic treatment: the mixed solution was placed in an ultrasonic treatment apparatus and subjected to ultrasonic treatment for 15 minutes. The ultrasonic treatment helps to uniformly disperse the components in the mixture and improves the uniformity of subsequent reactions.
1.4 standing: and standing the mixed solution after ultrasonic treatment for 40 minutes to enable components in the mixed solution to fully react, so that the subsequent addition of foam nickel is facilitated.
1.5 foam Nickel addition: and adding a certain mass of foam nickel into the mixed solution, and fully stirring to fully contact the foam nickel with the mixed solution.
1.6 one hydrothermal reaction: and placing the mixed solution added with the foam nickel into a high-pressure reaction kettle for one-time hydrothermal reaction. By controlling the temperature and time of the hydrothermal reaction, a nickel disulfide precursor can be grown in situ on the surface of the foam nickel.
The first step after refining comprises impurity removal treatment of nickel nitrate hexahydrate, mixture preparation, ultrasonic treatment, standing, foam nickel addition and one-time hydrothermal reaction, and finally the nickel disulfide precursor growing on the foam nickel in situ is obtained.
S102, mixing a nickel disulfide precursor growing on foam nickel in situ with a solution containing sodium molybdate and a nickel source, and performing a secondary hydrothermal reaction to obtain an electrolyzed water catalyst;
s103, repeatedly washing the electrolyzed water catalyst with distilled water and absolute ethyl alcohol for a plurality of times, and drying the washed electrode in an oven to obtain the high-efficiency electrolyzed water catalyst.
The mass ratio of the nickel nitrate hexahydrate, the urea, the thioacetamide and the ionized water is 0.1:0.2:0.3:11.
As shown in FIG. 2, the preparation method of sodium molybdate provided by the invention comprises the following steps:
s201, reducing sodium nitrate by lead, heating and melting sodium nitrate, adding a small amount of metallic lead, stirring and continuously heating until the lead is totally oxidized. The resulting cake was divided into small pieces while cooling, and the resulting lead oxide was extracted several times with hot water. Introducing carbon dioxide gas to generate lead carbonate precipitate, filtering, accurately neutralizing the filtrate with dilute nitric acid, evaporating, concentrating, and separating out sodium nitrite;
s202, dropwise adding a sodium nitrite solution into an ammonium molybdate solution at normal temperature, controlling the atomic molar ratio of sodium to molybdenum to be 3:1, continuously stirring, generating white precipitate immediately, aging for 13h, respectively washing with distilled water and absolute ethyl alcohol for 4 times, filtering, and drying to obtain a white flaky sodium molybdate finished product.
As shown in FIG. 3, the preparation method of the absolute ethyl alcohol provided by the invention comprises the following steps:
s301, carrying out impurity removal treatment on the ethanol fermentation liquor; the ethanol fermentation liquid is divided into at least two parts, one part enters a rectifying tower I, an ethanol material flow I with the concentration of 65wt% is obtained at the top of the rectifying tower I, and the other part enters a rectifying tower II, and an ethanol material flow II with the concentration of 65wt% is obtained at the top of the rectifying tower II;
s302, respectively passing the ethanol material flow I and the ethanol material flow II through a heating device and a second reboiler of a tower kettle of the rectifying tower I, mixing, sending the mixture into a pervaporation separator, and dehydrating the mixture through the pervaporation separator to obtain an ethanol material flow III with the concentration of 96 wt%;
s303, the ethanol material flow III is overheated by saturated steam and enters a molecular sieve pressure swing adsorber, and the material flow at the top of the molecular sieve pressure swing adsorber enters a first reboiler of a tower kettle I of a rectifying tower to be condensed to obtain an absolute ethanol product with the concentration of more than 98 weight percent;
the number of tower plates of the rectifying tower I is 33, the temperature of the tower top is 85 ℃, the temperature of the tower bottom is 102 ℃, the operating pressure is 75kPa, and the position of a feeding plate is positioned at the 7 th tower plate from top to bottom; the column plate number of the rectifying column II is 30, the temperature of the column top is 120 ℃, the temperature of the column bottom is 130 ℃, the operating pressure is 1800kPa, and the position of the feeding plate is positioned at the 7 th column plate from top to bottom.
The ethanol concentration in the ethanol fermentation liquid provided by the invention is 11% by weight, and the proportion of the ethanol fermentation liquid entering the rectifying tower I and the rectifying tower II is 2:1.
the concentration of ethanol in the ethanol fermentation liquid provided by the invention is 9% by weight.
The number of tower plates of the rectifying tower I is 33, the temperature of the tower top is 79 ℃, and the temperature of the tower bottom is 99 ℃; the number of tower plates of the rectifying tower II is 30, the temperature of the tower top is 110 ℃, and the temperature of the tower bottom is 110 ℃.
The operation temperature of the pervaporation separator provided by the invention is 85 ℃, and the operation pressure is 86kPa.
The membrane material used in the pervaporation separator provided by the invention is a selective permeable membrane selected from an organic membrane, an inorganic membrane or an organic-inorganic hybrid membrane, and can selectively permeate ethanol and water.
The membrane material provided by the invention is selected from a silicon-aluminum molecular sieve membrane, a chitosan membrane, a polyvinyl alcohol membrane, a polyether imide membrane or a polyvinyl alcohol-Na molecular sieve membrane;
the molecular sieve pressure swing adsorber operates at 130℃and 290kPa.
The sodium molybdate prepared by the sodium molybdate preparation method has high purity, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved; meanwhile, the absolute ethyl alcohol prepared by the absolute ethyl alcohol preparation method has high quality, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved.
The preparation method provided by the embodiment of the invention has the following advantages and positive effects:
1) High-efficiency catalyst: the prepared electrolyzed water catalyst has high-efficiency catalysis, can promote the electrolysis reaction of water, improve the reaction rate and efficiency, can catalyze the oxidation-reduction reaction of water, and can convert harmful substances into harmless substances, thereby having dual functions.
2) Is simple and easy to implement: the preparation method adopts simple reaction steps and treatment methods, is easy to realize and operate, does not need complex equipment and technical conditions, and can be widely applied to laboratory or industrial production.
3) Environmental protection sustainable: the raw materials and the solvent used in the preparation process are all environment-friendly substances, and cannot pollute and harm the environment. The prepared electrolyzed water catalyst can be used in the fields of environmental protection, water treatment and the like, and has good application prospect.
4) Economical and practical: the preparation method has the advantages that the cost of raw materials and equipment required is low, meanwhile, the prepared electrolyzed water catalyst has longer service life and higher catalytic efficiency, the production and treatment cost can be reduced, and the method has economical practicability.
In conclusion, the preparation method has the advantages and positive effects of high efficiency, simplicity, environmental protection, economy and the like, and can provide a new catalyst preparation scheme for the fields of electrolytic water reaction, water treatment and the like.
The sodium molybdate prepared by the sodium molybdate preparation method has high purity, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved; meanwhile, the absolute ethyl alcohol prepared by the absolute ethyl alcohol preparation method has high quality, so that the quality of the catalyst for preparing the electrolyzed water is greatly improved.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (10)
1. A method for preparing a self-supporting bifunctional electrolyzed water catalyst, which is characterized by comprising the following steps:
step one, preparing a nickel sulfate precursor: removing impurities in nickel nitrate hexahydrate, mixing nickel sulfate, urea and thioacetamide with ionized water, and carrying out ultrasonic treatment for 30 minutes to uniformly disperse the mixture; adding foam nickel into the mixture, and performing a hydrothermal reaction at 180 ℃ for 24 hours to form a nickel sulfate precursor on the surface of the foam nickel;
step two, preparing an electrolyzed water catalyst by a real-time monitoring system: preparing a solution containing sodium molybdate and a nickel source, wherein the sodium molybdate is an oxidant, provides oxygen atoms for the oxidation process of the electrolytic water reaction, and the nickel source is used for the catalytic reduction reaction; mixing a nickel sulfate precursor and a solution containing sodium molybdate and a nickel source, and performing a secondary hydrothermal reaction at 200 ℃ for 36 hours to convert the nickel sulfate precursor into an electrolyzed water catalyst; the real-time monitoring system is used for monitoring the temperature, the pressure and the concentration of substances in the reaction process;
step three, treating an electrolyzed water catalyst: repeatedly washing the prepared electrolyzed water catalyst with distilled water and absolute ethyl alcohol for a plurality of times to remove residual ions and impurities; the washed electrode was dried in an oven to obtain a highly efficient electrolyzed water catalyst.
2. The method for preparing a self-supporting dual-function electrolyzed water catalyst according to claim 1, further comprising the steps of:
step one, removing impurities from nickel nitrate hexahydrate; mixing nickel nitrate hexahydrate, urea and thioacetamide with ionized water, and performing ultrasonic treatment for 15min; standing for 40min; adding foam nickel, and performing a hydrothermal reaction to obtain a nickel disulfide precursor growing on the foam nickel in situ;
the urea preparation method comprises the following steps:
the raw material coal uses steam and air as gasifying agents to generate semi-water gas in a gas producer, and the gas is purified by the processes of primary desulfurization, transformation, secondary desulfurization, decarburization, fine desulfurization, methanol, alkylation and the like to remove various impurities;
compressing the pure nitrogen-hydrogen mixture to high pressure, and synthesizing ammonia at high temperature in the presence of a catalyst; purifying and compressing carbon dioxide desorbed by decarbonization, sending the carbon dioxide and ammonia into a urea synthesizing tower, and synthesizing urea at proper temperature and pressure;
mixing a nickel disulfide precursor growing in situ on foam nickel with a solution containing sodium molybdate and a nickel source, and performing a secondary hydrothermal reaction to obtain an electrolyzed water catalyst;
and thirdly, repeatedly washing the electrolyzed water catalyst with distilled water and absolute ethyl alcohol for a plurality of times, and drying the washed electrode in an oven to obtain the high-efficiency electrolyzed water catalyst.
3. The method for preparing the self-supporting bifunctional electrolyzed water catalyst of claim 1, wherein the refinement of the first step is as follows:
impurity removal treatment: first, nickel nitrate hexahydrate is treated to remove impurities therein. The method can be realized by a recrystallization method or an ion exchange method, so that the purity of the nickel nitrate hexahydrate is ensured to be higher, and the influence on the subsequent preparation process is avoided;
preparing a mixture: mixing a certain molar amount of nickel nitrate hexahydrate, urea and thioacetamide with a certain volume of ionized water to form a mixed solution; the composition and the performance of the electrolyzed water catalyst can be controlled by adjusting the molar ratio of each component;
and (3) ultrasonic treatment: placing the mixed solution in an ultrasonic treatment instrument, and carrying out ultrasonic treatment for 15 minutes; the ultrasonic treatment is helpful for uniformly dispersing each component in the mixture and improving the uniformity of subsequent reactions;
standing: standing the mixed solution after ultrasonic treatment for 40 minutes to fully react the components in the mixed solution, so that the subsequent addition of foam nickel is facilitated;
foam nickel addition: adding foam nickel with certain mass into the mixed solution, and fully stirring to fully contact the foam nickel with the mixed solution;
primary hydrothermal reaction: placing the mixed solution added with the foam nickel into a high-pressure reaction kettle for primary hydrothermal reaction; by controlling the temperature and time of the hydrothermal reaction, a nickel disulfide precursor can be grown in situ on the surface of the foam nickel.
4. The method for preparing the self-supporting bifunctional electrolyzed water catalyst of claim 1, wherein the sodium molybdate preparation method comprises the following steps:
1) The sodium nitrate is reduced by lead, the sodium nitrate is heated and melted, a small amount of metallic lead is added, and stirring and continuous heating are carried out until the lead is totally oxidized. The resulting cake was divided into small pieces while cooling, and the resulting lead oxide was extracted several times with hot water. Introducing carbon dioxide gas to generate lead carbonate precipitate, filtering, accurately neutralizing the filtrate with dilute nitric acid, evaporating, concentrating, and separating out sodium nitrite;
2) At normal temperature, dropwise adding sodium nitrite solution into ammonium molybdate solution, controlling the atomic mole ratio of sodium to molybdenum to be 3:1, continuously stirring, immediately generating white precipitate, aging for 13h, respectively washing with distilled water and absolute ethyl alcohol for 4 times, filtering, and drying to obtain white flaky sodium molybdate finished product.
5. The method for preparing the self-supporting bifunctional electrolyzed water catalyst of claim 1, wherein the method for preparing the absolute ethanol comprises the following steps:
1) Removing impurities from the ethanol fermentation liquid; the ethanol fermentation liquid is divided into at least two parts, one part enters a rectifying tower I, an ethanol material flow I with the concentration of 65wt% is obtained at the top of the rectifying tower I, and the other part enters a rectifying tower II, and an ethanol material flow II with the concentration of 65wt% is obtained at the top of the rectifying tower II;
2) The ethanol material flow I and the ethanol material flow II are respectively mixed and sent into a pervaporation separator after passing through a heating device and a second reboiler of a tower kettle of a rectifying tower I, and are dehydrated by the pervaporation separator to obtain an ethanol material flow III with the concentration of 96 wt%;
3) The ethanol material flow III is overheated by saturated steam and enters a molecular sieve pressure swing adsorber, and the top material flow of the molecular sieve pressure swing adsorber enters a first reboiler of a tower kettle of a rectifying tower I to be condensed to obtain an absolute ethanol product with the concentration of more than 98 weight percent;
the number of tower plates of the rectifying tower I is 33, the temperature of the tower top is 85 ℃, the temperature of the tower bottom is 102 ℃, the operating pressure is 75kPa, and the position of a feeding plate is positioned at the 7 th tower plate from top to bottom; the column plate number of the rectifying column II is 30, the temperature of the column top is 120 ℃, the temperature of the column bottom is 130 ℃, the operating pressure is 1800kPa, and the position of the feeding plate is positioned at the 7 th column plate from top to bottom.
6. The method for preparing the self-supporting bifunctional electrolyzed water catalyst as recited in claim 5, wherein the concentration of ethanol in the ethanol fermentation liquid is 11% by weight, and the ratio of the ethanol fermentation liquid to the rectification column I to the rectification column II is 2:1 by weight.
7. The method for preparing a self-supporting bifunctional electrolyzed water catalyst of claim 5, wherein the concentration of ethanol in the ethanol fermentation broth is 9% by weight; the number of tower plates of the rectifying tower I is 33, the temperature of the tower top is 79 ℃, and the temperature of the tower bottom is 99 ℃; the number of tower plates of the rectifying tower II is 30, the temperature of the tower top is 110 ℃, and the temperature of the tower bottom is 110 ℃.
8. The method for preparing a self-supporting dual function electrolyzed water catalyst according to claim 5, wherein said pervaporation separator is operated at a temperature of 85 ℃ and a pressure of 86kPa.
9. The method for preparing a self-supporting dual-function electrolytic water catalyst according to claim 5, wherein the membrane material used in the pervaporation separator is a selective permeable membrane selected from an organic membrane, an inorganic membrane or an organic-inorganic hybrid membrane, and the membrane material is selectively permeable to ethanol and water.
10. The method for preparing a self-supporting bifunctional electrolyzed water catalyst of claim 5, wherein the membrane material is selected from the group consisting of a silica alumina molecular sieve membrane, a chitosan membrane, a polyvinyl alcohol membrane, a polyetherimide membrane, and a polyvinyl alcohol-Na molecular sieve membrane;
the molecular sieve pressure swing adsorber operates at 130℃and 290kPa.
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| CN117661025B (en) * | 2024-02-02 | 2024-05-14 | 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 | Preparation method of urea electrolysis hydrogen production catalyst for clean energy |
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