CN110368995A - A kind of preparation method based on two sulphur indium silver electro-catalysis complete solution water materials - Google Patents
A kind of preparation method based on two sulphur indium silver electro-catalysis complete solution water materials Download PDFInfo
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- CN110368995A CN110368995A CN201910806916.9A CN201910806916A CN110368995A CN 110368995 A CN110368995 A CN 110368995A CN 201910806916 A CN201910806916 A CN 201910806916A CN 110368995 A CN110368995 A CN 110368995A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- YNXRTZDUPOFFKZ-UHFFFAOYSA-N [In].[Ag]=S Chemical compound [In].[Ag]=S YNXRTZDUPOFFKZ-UHFFFAOYSA-N 0.000 title claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 33
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910003373 AgInS2 Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 8
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 13
- 239000012467 final product Substances 0.000 claims description 2
- WQKHTJFZNMYFQC-UHFFFAOYSA-L dichloroiron;hydrate Chemical compound O.Cl[Fe]Cl WQKHTJFZNMYFQC-UHFFFAOYSA-L 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/095—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 at least one of the compounds being organic
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
A kind of preparation method based on two sulphur indium silver electro-catalysis complete solution water materials of the present invention, preparation method are: with it is conventional it has been reported that method prepare AgInS2.Ferric chloride hexahydrate and 2- amino terephthalic acid (TPA) are dissolved in n,N-Dimethylformamide, stir the mixture for reacting, then by AgInS2It is added in above-mentioned mixed solution, continues stirring until being uniformly dispersed；Then above-mentioned mixed solution is transferred in reaction kettle and is reacted.After being cooled to room temperature, product is collected, up to product after washed, drying.The present invention has the advantages that material prepared by 1. for electro-catalysis decomposes water entirely high-efficient, current density 10mA/cm2When, the cell voltage of splitting water is 1.59V；It is good that 3. material prepared by for electro-catalysis decomposes water stability entirely, at least can continuous work still keep very high activity for 24 hours；4. material preparation is simple, at low cost, it is applicable in and is widely applied.
Description
Technical field
The present invention relates to a kind of preparation methods based on two sulphur indium silver electro-catalysis complete solution water materials, belong to environmentally friendly new energy
Field.
Background technique
Utilization of the mankind to fossil energy has pushed the high speed development of society and civilization.But it is needed along with global energy
The problem of environmental pollution that the exhaustion and burning of the growth and fossil energy asked generate, countries in the world are increasingly heavier to energy problem
Depending on.Therefore, it is extremely urgent that high efficiency, the sustainable new green energy of cleaning of low cost and environmental protection are developed.
New green energy includes wind energy, solar energy, tide energy, Hydrogen Energy etc..Wherein the development and utilization of hydrogen is concerned,
Main cause is that it has the characteristics that rich reserves, renewable, pollution-free.A large amount of existing water, are exactly the one of Hydrogen Energy on the earth
A huge source.Water electrolysis hydrogen production can be avoided generation polluted gas, the H of generation2Purity is high is the core side of the following hydrogen industry
To.The key of water electrolysis hydrogen production technology is cheap and efficient stable the catalyst of design to realize the decomposition of low energy consumption catalytic water.
Water decomposition is divided into evolving hydrogen reaction (HER) and oxygen evolution reaction (OER), the two half-reactions are most important for water decomposition.Wherein,
HER has relatively simple reaction mechanism, it is only necessary to which lower overpotential can drive, and be easier to realize.However, OER
Reaction mechanism it is complicated, and oxygen evolution kinetic is very slow, it is therefore desirable to which higher overpotential could drive, this can reduce whole
Body catalytic efficiency and significantly increase energy consumption.Therefore, make HER and OER while the full decomposition water reaction effectively carried out is often restricted
In the reaction efficiency of OER, whole efficiency is lower.New and effective electrocatalysis material is researched and developed, the efficiency of complete solution water is effectively improved, is
The research hotspot of common concern at present.Based on the above technical background, this technology has invented a kind of new and effective complete solution water hydrogen manufacturing electricity
The preparation method of catalysis material, and in particular to a kind of preparation method based on two sulphur indium silver electro-catalysis complete solution water materials is related
Technology has not been reported.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods based on two sulphur indium silver electro-catalysis complete solution water materials.
The present invention uses following means:
(1) with it is conventional it has been reported that method prepare AgInS2；
(2) ferric chloride hexahydrate and 2- amino terephthalic acid (TPA) are dissolved in 54mL N,N-dimethylformamide (DMF)
In, the range of ferric chloride hexahydrate amount is 0.1g-1g, and the range of 2- amino terephthalic acid (TPA) amount is 0.2g-0.8g, and solution is stirred
Mixing 30 minutes makes to be completely dissolved；
(3) by AgInS2It is added to by (2) acquired solution, AgInS2The range of amount is 10mg-500mg, and it is straight to continue stirring
To being uniformly dispersed.Then above-mentioned mixed solution is transferred in reaction kettle and is reacted, range of reaction temperature is 100 DEG C -180
DEG C, reaction time range is 10-20 hours.After being cooled to room temperature, product is collected, up to final product after washed, drying.
The present invention has the advantages that material prepared by 1. decomposes entirely for electro-catalysis, water is high-efficient, and current density is
10mA/cm2When, the cell voltage of splitting water is 1.59V；It is good that 3. material prepared by for electro-catalysis decomposes water stability entirely,
At least can continuous work still keep very high activity for 24 hours；4. material preparation is simple, at low cost, it is applicable in and is widely applied.
Detailed description of the invention
LSV figure when Fig. 1 is 3 product electro-catalysis complete solution water of the embodiment of the present invention；
Electric current changes over time figure when Fig. 2 is 3 product electro-catalysis complete solution water of the embodiment of the present invention.
Specific embodiment
Embodiment 1
With it is conventional it has been reported that method prepare AgInS2。
0.1g ferric chloride hexahydrate and 0.2g 2- amino terephthalic acid (TPA) are dissolved in 54mL N,N-dimethylformamide
(DMF) it in, stirs the mixture for 30 minutes, later by 10mg AgInS2Be added in above-mentioned mixed solution, continue stirring until
It is uniformly dispersed；Then above-mentioned mixed solution is transferred in reaction kettle, and is heated 10 hours at 100 DEG C.After being cooled to room temperature,
Product is collected, up to product after washed, drying.
Embodiment 2
With it is conventional it has been reported that method prepare AgInS2。
0.4g ferric chloride hexahydrate and 0.4g 2- amino terephthalic acid (TPA) are dissolved in 54mL N,N-dimethylformamide
(DMF) it in, stirs the mixture for 30 minutes, later by 100mg AgInS2It is added in above-mentioned mixed solution, it is straight to continue stirring
To being uniformly dispersed；Then above-mentioned mixed solution is transferred in reaction kettle, and is heated 16 hours at 140 DEG C.It is cooled to room temperature
Afterwards, product is collected, up to product after washed, drying.
Embodiment 3
With it is conventional it has been reported that method prepare AgInS2。
0.8g ferric chloride hexahydrate and 0.6g 2- amino terephthalic acid (TPA) are dissolved in 54mL N,N-dimethylformamide
(DMF) it in, stirs the mixture for 30 minutes, later by 300mg AgInS2It is added in above-mentioned mixed solution, it is straight to continue stirring
To being uniformly dispersed；Then above-mentioned mixed solution is transferred in reaction kettle, and is heated 18 hours at 160 DEG C.It is cooled to room temperature
Afterwards, product is collected, up to product after washed, drying.
Embodiment 4
With it is conventional it has been reported that method prepare AgInS2。
1g ferric chloride hexahydrate and 0.8g 2- amino terephthalic acid (TPA) are dissolved in 54mL N,N-dimethylformamide
(DMF) it in, stirs the mixture for 30 minutes, later by 500mg AgInS2It is added in above-mentioned mixed solution, it is straight to continue stirring
To being uniformly dispersed；Then above-mentioned mixed solution is transferred in reaction kettle, and is heated 20 hours at 180 DEG C.It is cooled to room temperature
Afterwards, product is collected, up to product after washed, drying.
Not limited to this, any change or replacement expected without creative work should all be covered in guarantor of the invention
Within the scope of shield.Therefore, protection scope of the present invention should be determined by the scope of protection defined in the claims.
Claims (2)
1. a kind of preparation method based on two sulphur indium silver electro-catalysis complete solution water materials, it is characterised in that:
(1) with it is conventional it has been reported that method prepare AgInS2；
(2) ferric chloride hexahydrate and 2- amino terephthalic acid (TPA) are dissolved in 54mL n,N-Dimethylformamide (DMF), six
The range of chloride hydrate iron is 0.1g-1g, and the range of 2- amino terephthalic acid (TPA) amount is 0.2g-0.8g, and solution is stirred 30
Minute makes to be completely dissolved；
(3) by AgInS2It is added to by (2) acquired solution, AgInS2The range of amount is 10mg-500mg, continues stirring until dividing
It dissipates uniformly, then above-mentioned mixed solution is transferred in reaction kettle and is reacted, range of reaction temperature is 100 DEG C -180 DEG C, instead
Answering time range is 10-20 hours, after being cooled to room temperature, and product is collected, up to final product after washed, drying.
2. a kind of preparation method based on two sulphur indium silver electro-catalysis complete solution water materials according to claim 1, it is characterised in that:
The performance that there is obtained product excellent electro-catalysis to decompose water entirely.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910806916.9A CN110368995B (en) | 2019-08-29 | 2019-08-29 | Preparation method of electrocatalytic full-hydrolytic material based on silver indium disulfide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910806916.9A CN110368995B (en) | 2019-08-29 | 2019-08-29 | Preparation method of electrocatalytic full-hydrolytic material based on silver indium disulfide |
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| CN110368995B CN110368995B (en) | 2022-02-01 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106256432A (en) * | 2016-08-03 | 2016-12-28 | 江苏大学 | A kind of water oxidation reaction catalyst based on metallic organic framework graphene oxide and preparation method thereof |
| CN108393097A (en) * | 2018-05-15 | 2018-08-14 | 济南大学 | A kind of ferrous metals containing redox mediators-organic framework material type Fenton catalyst preparation method |
| CN110047657A (en) * | 2019-04-02 | 2019-07-23 | 常州大学 | A kind of compound preparation method for mixing molybdenum pucherite light anode of MIL series MOF |
-
2019
- 2019-08-29 CN CN201910806916.9A patent/CN110368995B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106256432A (en) * | 2016-08-03 | 2016-12-28 | 江苏大学 | A kind of water oxidation reaction catalyst based on metallic organic framework graphene oxide and preparation method thereof |
| CN108393097A (en) * | 2018-05-15 | 2018-08-14 | 济南大学 | A kind of ferrous metals containing redox mediators-organic framework material type Fenton catalyst preparation method |
| CN110047657A (en) * | 2019-04-02 | 2019-07-23 | 常州大学 | A kind of compound preparation method for mixing molybdenum pucherite light anode of MIL series MOF |
Non-Patent Citations (3)
| Title |
|---|
| ANDRÉ D.S. BARBOSA等: "Catalytic performance and electrochemical behaviour of Metal–organic frameworks: MIL-101(Fe) versus NH2-MIL-101(Fe)", 《POLYHEDRON》 * |
| TING-TING ZHU等: "Encapsulation of tungstophosphoric acid into harmless MIL-101(Fe) for effectively removing cationic dye from aqueous solution", 《RSC ADV.》 * |
| XUEQIN LI等: "Multifunctional electrochemical application of a novel 3D AgInS2/rGO nanohybrid for electrochemical detection and HER", 《J CHEM TECHNOL BIOTECHNOL》 * |
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