CN110354903A - A kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material - Google Patents
A kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material Download PDFInfo
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- CN110354903A CN110354903A CN201910806932.8A CN201910806932A CN110354903A CN 110354903 A CN110354903 A CN 110354903A CN 201910806932 A CN201910806932 A CN 201910806932A CN 110354903 A CN110354903 A CN 110354903A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 14
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 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
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 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
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 9
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 9
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 7
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 6
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- KYCHGXYBBUEKJK-UHFFFAOYSA-K indium(3+);trichloride;hydrate Chemical compound O.Cl[In](Cl)Cl KYCHGXYBBUEKJK-UHFFFAOYSA-K 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- -1 and high-efficient Substances 0.000 abstract description 2
- 150000002431 hydrogen Chemical class 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000011160 research 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
- 238000003912 environmental pollution Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001681 protective effect 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/2243—At least one oxygen and one nitrogen atom present as complexing atoms in an at least bidentate or bridging ligand
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/226—Sulfur, e.g. thiocarbamates
-
- 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
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/10—Complexes comprising metals of Group I (IA or IB) as the central metal
- B01J2531/17—Silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/30—Complexes comprising metals of Group III (IIIA or IIIB) as the central metal
- B01J2531/33—Indium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/40—Complexes comprising metals of Group IV (IVA or IVB) as the central metal
- B01J2531/48—Zirconium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- 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)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses a kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material, preparation method is: in the DMF that zirconium chloride and 2- amino terephthalic acid (TPA) are dissolved in, mixture is transferred in autoclave and carries out solvent thermal reaction, after reaction, naturally cool to room temperature, product is obtained by centrifugation, obtains intermediate A after washed, drying.Silver nitrate and four chloride hydrate indiums are dissolved in ethylene glycol respectively, after forming homogeneous solution, the two is mixed.Then A is added thereto, the thioacetamide added is stirred to react, aging, then collects product, washed, be drying to obtain final products.The present invention has the advantages that 1. is green and pollution-free, the visible photocatalysis aquatic products hydrogen in sunlight can use；2. material catalysis water decomposition prepared by produces hydrogen, and high-efficient, hydrogen-producing speed is up to 2647 μm of ol/g/h；3. 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 of photocatalysis Decomposition aquatic products hydrogen material, belong to environmentally friendly new energy field.
Background technique
The use of the fossil energies such as petroleum, natural gas, coal has pushed the high speed development of society and civilization significantly.But
These fossil energies are non-renewable energy resources, some day can be exhausted.In addition, the problem of environmental pollution that fossil energy burning generates
Also the development of human society is increasingly influenced.How to cope with lack of energy and corresponding problem of environmental pollution increasingly obtains the world
The attention of various countries.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.Inherently a kind of environmentally protective technology of photocatalysis technology.Photocatalysis Decomposition aquatic products hydrogen will utilize solar energy
Exploitation with Hydrogen Energy associates, and does not generate polluted gas, the H of preparation2Purity is high, low energy consumption, and pollution is small, has wide answer
Use prospect.The key of photocatalytic hydrogen production by water decomposition technology is cheap and efficient stable the catalyst of design to realize that low energy consumption is catalyzed
The decomposition of water.Water decomposition is divided into evolving hydrogen reaction (HER) and oxygen evolution reaction (OER), the two half-reactions are for water decomposition to Guan Chong
It wants.Wherein, HER has relatively simple reaction mechanism, it is only necessary to which lower overpotential can drive, and be easier to realize.
However, the reaction mechanism of OER is complicated, and oxygen evolution kinetic is very slow, it is therefore desirable to higher overpotential could drive, this
Whole catalytic efficiency can be reduced and significantly increase energy consumption.Therefore, photochemical catalyzing is concentrated mainly on research relatively at present
The HER easily realized, and the generation of OER is avoided in the form of sacrifice agent is added.But generally speaking photocatalytic water splitting at present
The efficiency of HER is still lower, researches and develops new and effective catalysis material, effectively improves the efficiency for decomposing water, is generally to close at present
The research hotspot of note.Based on the above technical background, this technology has invented a kind of new and effective photocatalysis Decomposition aquatic products hydrogen material
Preparation method, the relevant technologies have not been reported.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of photocatalysis Decomposition aquatic products hydrogen material.
The present invention uses following means:
(1) zirconium chloride and 2- amino terephthalic acid (TPA) are dissolved in the DMF of 50mL and form solution, the range of zirconium chloride amount exists
The range of 0.1 to 0.5g, 2- amino terephthalic acid (TPA) amount is 0.1 to 0.6g.By above-mentioned solution be transferred in autoclave into
Row solvent thermal reaction.For range of reaction temperature at 80-180 DEG C, reaction time range can be at 12-60 hours.After reaction, natural
It is cooled to room temperature, product is obtained by centrifugation, washed, drying obtains intermediate A；
(2) silver nitrate and four chloride hydrate indiums are dissolved in respectively in the ethylene glycol of 25mL, form homogeneous solution.Nitric acid silver content
Range be 0.0.5-0.5g, the ranges of four chloride hydrate indium amounts is 0.5-5g.By the second two of silver nitrate and four chloride hydrate indiums
Alcoholic solution mixing.
(3) intermediate A is added in by (2) acquired solution, the range of A amount is 20-100mg.It is stirred at room temperature after A is added
30min is mixed, thioacetamide is then added thereto, the range of thioacetamide amount is 0.5-5g.Mixed liquor is mixed into reaction, instead
Answering temperature is 50-120 DEG C, reaction time 2-6h.Then aging 20h after reaction collects product, washed, dry, i.e.,
Obtain final products.
The present invention has the advantages that 1. is green and pollution-free, the visible photocatalysis aquatic products hydrogen in sunlight can use；
2. material catalysis water decomposition prepared by produces hydrogen, and high-efficient, hydrogen-producing speed is up to 2647 μm of ol/g/h；3. material preparation is simple,
It is at low cost, it is applicable in and is widely applied.
Detailed description of the invention
Fig. 1 is the XRD diagram of the intermediate A of the embodiment of the present invention 2；
Fig. 2 is the scanning electron microscope (SEM) photograph of 2 product of the embodiment of the present invention, it is seen that material is nanoparticle structure；
Fig. 3 is that hydrogen output when 2 product visible light catalytic of the embodiment of the present invention decomposes water changes over time figure.
Specific embodiment
Embodiment 1
The 2- amino terephthalic acid (TPA) of the zirconium chloride of 0.1g and 0.1g are dissolved in the DMF of 50mL, mixture is transferred to
Solvent thermal reaction is carried out in autoclave, is reacted 12 hours under conditions of 80 DEG C, after reaction, is naturally cooled to room temperature,
Product is obtained by centrifugation, obtains intermediate A after washed, drying.
The four chloride hydrate indiums of the silver nitrate of 0.05g and 0.5g are dissolved in respectively in the ethylene glycol of 25mL, are formed uniformly molten
After liquid, the two is mixed.Then 20mg A is added thereto, adds the thioacetamide of 0.5g, 50 DEG C of stirring 2h, aging
20h.Then product is collected, it is washed, be drying to obtain final products.
Embodiment 2
The 2- amino terephthalic acid (TPA) of the zirconium chloride of 0.2g and 0.2g are dissolved in the DMF of 50mL, mixture is transferred to
Solvent thermal reaction is carried out in autoclave, is reacted 24 hours under conditions of 120 DEG C, after reaction, is naturally cooled to room temperature,
Product is obtained by centrifugation, obtains intermediate A after washed, drying.
The four chloride hydrate indiums of the silver nitrate of 0.2g and 2g are dissolved in respectively in the ethylene glycol of 25mL, homogeneous solution is formed
Afterwards, the two is mixed.Then 40mg A is added thereto, adds the thioacetamide of 2g, 80 DEG C of stirrings 3h, aging 20h.So
After collect product, it is washed, be drying to obtain final products.
Embodiment 3
The 2- amino terephthalic acid (TPA) of the zirconium chloride of 0.3g and 0.4g are dissolved in the DMF of 50mL, mixture is transferred to
Solvent thermal reaction is carried out in autoclave, is reacted 48 hours under conditions of 160 DEG C, after reaction, is naturally cooled to room temperature,
Product is obtained by centrifugation, obtains intermediate A after washed, drying.
The four chloride hydrate indiums of the silver nitrate of 0.3g and 3g are dissolved in respectively in the ethylene glycol of 25ml, homogeneous solution is formed
Afterwards, the two is mixed.Then 80mg A is added thereto, adds the thioacetamide of 3g, 100 DEG C of stirrings 5h, aging 20h.
Then product is collected, it is washed, be drying to obtain final products.
Embodiment 4
The 2- amino terephthalic acid (TPA) of the zirconium chloride of 0.5g and 0.6g are dissolved in the DMF of 50mL, mixture is transferred to
Solvent thermal reaction is carried out in autoclave, is reacted 60 hours under conditions of 180 DEG C, after reaction, is naturally cooled to room temperature,
Product is obtained by centrifugation, obtains intermediate A after washed, drying.
The four chloride hydrate indiums of the silver nitrate of 0.5g and 5g are dissolved in respectively in the ethylene glycol of 25mL, homogeneous solution is formed
Afterwards, the two is mixed.Then 100mg A is added thereto, adds the thioacetamide of 5g, 120 DEG C of stirrings 6h, aging 20h.
Then product is collected, it is washed, be drying to obtain final products.
Claims (2)
1. a kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material, it is characterised in that:
(1) zirconium chloride and 2- amino terephthalic acid (TPA) are dissolved in the DMF of 50mL and form solution, the range of zirconium chloride amount is 0.1
To 0.5g, the range of 2- amino terephthalic acid (TPA) amount 0.1 to 0.6g, above-mentioned solution is transferred in autoclave carry out it is molten
Agent thermal response, for range of reaction temperature at 80-180 DEG C, reaction time range can be 12-60 hours, after reaction, natural cooling
To room temperature, product is obtained by centrifugation, washed, drying obtains intermediate A；
(2) silver nitrate and four chloride hydrate indiums are dissolved in respectively in the ethylene glycol of 25mL, form homogeneous solution, the model of nitric acid silver content
It encloses for 0.0.5-0.5g, the range of four chloride hydrate indium amounts is 0.5-5g, and the ethylene glycol of silver nitrate and four chloride hydrate indiums is molten
Liquid mixing；
(3) intermediate A is added in by (2) acquired solution, the range of A amount is 20-100mg, is stirred at room temperature after A is added
Then thioacetamide is added in 30min thereto, the range of thioacetamide amount is 0.5-5g, and mixed liquor is mixed reaction, is reacted
Temperature is 50-120 DEG C, reaction time 2-6h, after reaction aging 20h, then collects product, it is washed, dry to get
To final products.
2. a kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material according to claim 1, it is characterised in that: products obtained therefrom can
Hydrogen is produced using the catalysis water decomposition of visible light efficient rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910806932.8A CN110354903A (en) | 2019-08-29 | 2019-08-29 | A kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material |
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| CN201910806932.8A CN110354903A (en) | 2019-08-29 | 2019-08-29 | A kind of preparation method of photocatalysis Decomposition aquatic products hydrogen material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117205944A (en) * | 2023-03-16 | 2023-12-12 | 盐城工学院 | Novel oxysulfide photocatalyst and preparation method and application thereof |
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2019
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| CN104755166A (en) * | 2012-09-21 | 2015-07-01 | Toto株式会社 | Composite photocatalyst, and photocatalyst material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117205944A (en) * | 2023-03-16 | 2023-12-12 | 盐城工学院 | Novel oxysulfide photocatalyst and preparation method and application thereof |
| CN117205944B (en) * | 2023-03-16 | 2024-04-30 | 盐城工学院 | Oxysulfide photocatalyst and preparation method and application thereof |
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Application publication date: 20191022 |