CN105478143B - It is a kind of to prepare with the rich indium type AgInS of visible light-responded narrow band gap2The method of photochemical catalyst - Google Patents
It is a kind of to prepare with the rich indium type AgInS of visible light-responded narrow band gap2The method of photochemical catalyst Download PDFInfo
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- CN105478143B CN105478143B CN201510981334.6A CN201510981334A CN105478143B CN 105478143 B CN105478143 B CN 105478143B CN 201510981334 A CN201510981334 A CN 201510981334A CN 105478143 B CN105478143 B CN 105478143B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 32
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 150000003839 salts Chemical class 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 238000010521 absorption reaction Methods 0.000 claims abstract description 17
- 150000002471 indium Chemical class 0.000 claims abstract description 8
- 230000003595 spectral effect Effects 0.000 claims abstract description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052946 acanthite Inorganic materials 0.000 claims abstract description 7
- 229940056910 silver sulfide Drugs 0.000 claims abstract description 7
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 claims abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000005864 Sulphur Substances 0.000 claims abstract description 5
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012265 solid product Substances 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 3
- 230000009466 transformation Effects 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 18
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 3
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 20
- 238000002360 preparation method Methods 0.000 abstract description 10
- 229910003373 AgInS2 Inorganic materials 0.000 abstract description 7
- 230000002045 lasting effect Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 13
- 229910002651 NO3 Inorganic materials 0.000 description 9
- 239000003153 chemical reaction reagent Substances 0.000 description 9
- 238000009833 condensation Methods 0.000 description 9
- 230000005494 condensation Effects 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 9
- 239000000975 dye Substances 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 230000001376 precipitating effect Effects 0.000 description 9
- 238000010992 reflux Methods 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 8
- 238000002242 deionisation method Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000000975 co-precipitation Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 229910052976 metal sulfide Inorganic materials 0.000 description 3
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000372132 Hydrometridae Species 0.000 description 1
- 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 description 1
- 206010034960 Photophobia Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 208000013469 light sensitivity Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- 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
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
Prepared the present invention relates to a kind of with the rich indium type AgInS of visible light-responded narrow band gap2The method of photochemical catalyst.A certain proportion of silver salt and indium salts are fully dissolved in organic alcoholic solution, metal salt precursor is formed；Metal salt precursor and excessive sulfide（Sulphur source）Lasting stirring is reacted at a certain temperature；Sulfide reacts with silver ion first, forms the silver sulfide of taupe, with the extension in reaction time, and silver sulfide reacts and phase transformation with indium salts, final to obtain red brown solid product；Red brown solid product is washed, dried, the regulation of spectral absorption range-controllable is produced, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.The outstanding advantages of this method are that preparation condition is gentle, yield is high, the rich indium type AgInS of controllable adjustment narrow band gap2Spectral absorption scope, product AgInS2With very high visible light catalytic mineralising performance and higher power of regeneration.
Description
Technical field
The present invention relates to a kind of rich indium type AgInS of visible light-responded narrow band gap2The preparation method of photochemical catalyst, is especially related to
And a kind of low-temperature co-precipitation method prepares the regulation of spectral absorption range-controllable, with the narrow of visible light-responded and high catalysis mineralization ability
Band gap richness indium type AgInS2Photochemical catalyst.
Background technology
Dyestuff enriches our life, but the environmental problem that waste water from dyestuff is brought should not be underestimated.Waste water from dyestuff has water
Measure big, colourity depth, organic pollution content height, complicated component, acid-base property is strong, inoxidizability is strong, difficult for biological degradation, bio-toxicity
Cause " three cause " greatly and containing a variety of（Carcinogenic, teratogenesis, mutagenesis）The organic matter of performance.These waste water from dyestuff are in line, not only can
Deteriorate water quality, soil property, also threaten aquatic organism and the health and safety of the mankind.Therefore, how efficiently waste water from dyestuff is controlled to pollute
The significant task that environmentalist endeavours research is turned into.
Conductor photocatalysis is as a kind of very promising high-level oxidation technology, with reaction condition is gentle, preparation technology
It is easy, the advantages of energy consumption is low, reaction speed is fast, both can efficient-decomposition Some Organic Pollutants, also effectively organic dyestuff can be entered
Row decolourizes to remove, or even can be translated into CO2、SO4 2-、NO3 -, the inorganic molecules material such as halogen.Therefore, photocatalysis is utilized
Technical finesse waste water from dyestuff to mitigating circumstances problem, maintaining ecological balance, realize that sustainable development is significant.
Binary metal sulfide is by taking common CdS photochemical catalysts as an example, and its energy gap is 2.3eV, with very high
Photocatalytic activity.CdS is unstable in aqueous, can undergo the process of an anodic solution, its photocatalytic activity is dropped rapidly
It is low, it usually needs to add the reducing agent such as sodium sulfite and vulcanized sodium and carry out trapped hole, light-catalyzed reaction is carried out, and big portion
Divide sulfide that there is toxicity and unstability.
The ternary metal sulfide I-III-VI gradually developed based on binary metal sulfide, both inherits binary sulfide
Characteristic, has other new characteristics again.Silver sulfide indium is a kind of typical ternary low bandgap material, there is AgInS2And AgIn5S8Two
The form of kind.The two is respectively provided with good light sensitivity, stability and inoxidizability, and forbidden band is narrower, visible light-responded strong, repetition profit
It is high with rate, there is very important application in terms of photocatalytically degradating organic dye, photocatalytic water, opto-electronic conversion.
At present, AgInS is prepared2Common methods have spray pyrolysis technologies, pyrolysismethod and hydro-thermal method, and these preparation methods have
The shortcomings of reaction temperature height, high energy consumption, preparation process are complicated, the reaction time is long.The invention provides a kind of low-temperature co-precipitation method
Controllable preparation has the rich indium type AgInS of visible light-responded narrow band gap2The method of photochemical catalyst, this method is simple and easy to apply, energy consumption
Low, mild condition, time-consuming short, narrow band gap richness indium type AgInS2The spectral absorption range-controllable regulation of photochemical catalyst, in visible ray
There is down preferable photocatalysis performance.
The content of the invention
It is an object of the invention to for AgInS2The shortcomings of existing preparation condition is harsh, operating procedure is complicated, proposes one
Low-temperature co-precipitation method is planted to prepare with the rich indium type AgInS of visible light-responded narrow band gap2The method of photochemical catalyst, this method system
Standby AgInS2The chemical property of photochemical catalyst is stable, energy gap is narrow, with stronger light absorbs, spectral absorption range-controllable
Regulation, the ability of preferable photocatalytically degradating organic dye pollutant simultaneously have higher power of regeneration.
The purpose of the present invention is achieved through the following technical solutions, and its preparation methods steps are as follows：Will be a certain proportion of
Silver salt and indium salts fully dissolve in organic alcoholic solution, form metal salt precursor；Metal salt precursor and excessive sulfide（Sulphur
Source）Lasting stirring is reacted at a certain temperature；Sulfide reacts with silver ion first, forms the silver sulfide of taupe, with
The extension in reaction time, silver sulfide reacts and phase transformation with indium salts, final to obtain red brown solid product；Bronzing is consolidated
Body product is washed three times respectively with deionized water and absolute ethyl alcohol, then in 60-100oDried under C, produce spectral absorption scope
Controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
The silver salt is silver nitrate or silver acetate.
The indium salts are indium nitrate or indium sulfate.
The sulphur source is Na2S, thioacetamide, Cys or thiocarbamide.
The Organic Alcohol is ethanol, propyl alcohol, ethylene glycol or isopropanol.
The Ag/In mol ratios are 1:5~1:11.
The Ag/S mol ratios are 0.6:5~0.6:15.
The reaction temperature is 55~95oC。
Rich indium type AgInS prepared by the present invention2The advantage of photochemical catalyst：
（1）The rich indium type AgInS that the present invention is provided2Preparation method be low-temperature co-precipitation method, operation is simple, preparation time
Short, energy consumption is low, and applicability is wide；
（2）The present invention can be by regulating and controlling Ag/In mol ratios, the rich indium type AgInS of regulation and control2Spectral absorption scope；
（3）Rich indium type AgInS prepared by the present invention2The chemical property of photochemical catalyst is stable, and energy gap is narrow, can effectively divide
From photo-generated carrier, there is stronger light absorbs and photocatalysis mineralization ability under visible light, and have higher stability and
Regenerability.
Brief description of the drawings
Fig. 1 is the AgInS of prepared difference [Ag]/[In] ratio in embodiments of the invention 2 and example 82Photochemical catalyst：
a: [Ag]/[In]=0.6:3, b: [Ag]/[In]=0.6:5.The XRD spectrum of comparative sample, as seen from the figure, suitably increases In
Amount, the X ray diffracting data of sample does not change, the AgInS with standard2Phase（PDF#25-1328）It is consistent, is presented oblique
Prismatic crystal phase.
Fig. 2 is AgInS prepared in embodiments of the invention 2 and example 82The diffusing reflection figure and band-gap energy figure of photochemical catalyst
Spectrum.As seen from the figure, AgInS has been widened in the increase of In amounts2Response to visible ray, makes its energy gap diminish.
Fig. 3 is AgInS prepared in embodiments of the invention 2 and example 82Nitrogen adsorption-desorption of photochemical catalyst and hole
Footpath distribution curve, as seen from the figure, [Ag]/[In] are 0.6:When 3, the specific surface area of photochemical catalyst is 68.59 m2/ g, [Ag]/
[In] is 0.6:When 5, specific surface area is 74.15 m2/ g, with increasing for the In amounts in precursor salting liquid, its specific surface area value
Slightly increase, but its thermoisopleth all belongs to the IV types in IUPAC classification, H3 hysteresis loops.
Fig. 4 is AgInS prepared in embodiments of the invention 2 and example 82The visible ray of photochemical catalyst declines solution methyl orange
Curve, as seen from the figure, appropriate increase In amounts, hence it is evident that be conducive to raising AgInS2Photocatalytic activity.
Embodiment
Following examples are intended to illustrate invention rather than limitation of the invention further.
Embodiment 1
（1）By 0.6 mmol AgNO3With 3 mmol In (NO3)3It is dissolved in 170 mL ethanol, ultrasonic dissolution formation metal
The clear solution of salt precursor.
（2）10 mmol thioacetamides are dissolved in 10 mL ethanol, strong stirring forms precipitating reagent.Under continuous stirring
Precipitant solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 55oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 2
（1）By 0.6 mmol AgNO3With 3 mmol In (NO3)3It is dissolved in 170 mL ethylene glycol, ultrasonic dissolution forms gold
Belong to the clear solution of salt precursor.
（2）10 mmol thioacetamides are dissolved in 10 mL ethylene glycol, strong stirring forms precipitating reagent.In lasting stirring
It is lower precipitant solution to be added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 70oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 3
（1）By 0.6 mmol CH3COOAg and 3 mmol In2(SO4)3170 mL propyl alcohol are dissolved in, ultrasonic dissolution forms gold
Belong to the clear solution of salt precursor.
（2）5 mmol thioacetamides are dissolved in 10 mL propyl alcohol, strong stirring forms precipitating reagent.Under continuous stirring will
Precipitant solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 95oC, water bath time is 3 hours.
（4）Reaction terminate after, be aged a few hours, discard the supernatant of yellow, sediment russet centrifuged, spend from
Sub- water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding is produced
Spectral absorption range-controllable is adjusted, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 4
（1）By 0.6 mmol AgNO3With 3 mmol In (NO3)3It is dissolved in 170 mL isopropanols, ultrasonic dissolution formation metal
The clear solution of salt precursor.
（2）15 mmol thiocarbamides are dissolved in 10 mL isopropanols, strong stirring forms precipitating reagent.Under continuous stirring will be heavy
Shallow lake agent solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 70oC, water bath time is 3 hours.
（4）Reaction terminate after, be aged a few hours, discard the supernatant of yellow, sediment russet centrifuged, spend from
Sub- water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding is produced
Spectral absorption range-controllable is adjusted, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 5
（1）By 0.6 mmol AgNO3With 3 mmol In (NO3)3It is dissolved in 170 mL ethylene glycol, ultrasonic dissolution formation metal
The clear solution of salt precursor.
（2）10 mmol Cys are dissolved in 10 mL ethylene glycol strong stirrings, precipitating reagent is formed.In lasting stirring
It is lower precipitant solution to be added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 55oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 6
（1）By 0.6 mmol AgNO3With 3 mmol In (NO3)3It is dissolved in 170mL ethylene glycol, ultrasonic dissolution formation metal salt
The clear solution of precursor.
（2）10 mmol thiocarbamides are dissolved in 10 mL ethylene glycol strong stirrings, precipitating reagent is formed.Under continuous stirring will precipitation
Agent solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 70oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 7
（1）By 0.6 mmol AgNO3With 6.6 mmol In (NO3)3170 mL ethylene glycol are dissolved in, ultrasonic dissolution forms gold
Belong to the clear solution of salt precursor.
（2）5 mmol thioacetamides are dissolved in 10 mL ethylene glycol strong stirrings, precipitating reagent is formed.Under continuous stirring
Precipitant solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 70oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 8
（1）By 0.6 mmol AgNO3With 5 mmol In (NO3)3It is dissolved in 170 mL ethylene glycol, ultrasonic dissolution formation metal
The clear solution of salt precursor.
（2）10 mmol thioacetamides are dissolved in 10 mL ethylene glycol strong stirrings, precipitating reagent is formed.Under continuous stirring
Precipitant solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 70oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Embodiment 9
（1）By 0.6 mmol CH3COOAg and 6 mmol In (NO3)3170 mL ethylene glycol are dissolved in, ultrasonic dissolution forms gold
Belong to the clear solution of salt precursor.
（2）By 10 mmol Na2S is dissolved in 10 mL ethylene glycol strong stirrings, forms precipitating reagent.Under continuous stirring will be heavy
Shallow lake agent solution is added dropwise in above-mentioned metal salt precursor solution.
（3）In the three-necked flask that solution after mixing is transferred to 250 mL, condensation reflux unit is added, and with appropriate
Speed is stirred, and bath temperature is 70oC, water bath time is 3 hours.
（4）After reaction terminates, a few hours are aged, the supernatant of yellow is discarded, reddish-brown precipitation thing is centrifuged, deionization is used
Water and absolute ethyl alcohol are washed three times respectively, then 60~100oCertain time is dried under C, natural cooling, grinding produces light
Compose absorption region controllable adjustment, with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst.
Claims (6)
1. a kind of prepare with the rich indium type AgInS of visible light-responded narrow band gap2The method of photochemical catalyst, it is characterised in that prepare
Step is as follows：It is 1 by Ag/In mol ratios:5~1:11 silver salt and indium salts fully dissolves in organic alcoholic solution, forms metal
Salt precursor；Metal salt precursor is persistently stirred with sulphur source, 55~95oC is reacted；Sulfide is anti-with silver ion first
Should, the silver sulfide of taupe is formed, with the extension in reaction time, silver sulfide reacts and phase transformation with indium salts, final to obtain
Red brown solid product；Red brown solid product is washed three times respectively with deionized water and absolute ethyl alcohol, then in 60-
100oDried under C, produce the regulation of spectral absorption range-controllable, with the rich indium type AgInS of visible light-responded narrow band gap2Photocatalysis
Agent.
A kind of prepared 2. according to claim 1 with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst
Method, it is characterised in that：The silver salt is silver nitrate or silver acetate.
A kind of prepared 3. according to claim 1 with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst
Method, it is characterised in that：The indium salts are indium nitrate or indium sulfate.
A kind of prepared 4. according to claim 1 with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst
Method, it is characterised in that：The sulphur source is Na2S, thioacetamide, Cys or thiocarbamide.
A kind of prepared 5. according to claim 1 with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst
Method, it is characterised in that：The Organic Alcohol is ethanol, propyl alcohol, ethylene glycol or isopropanol.
A kind of prepared 6. according to claim 1 with the rich indium type AgInS of visible light-responded narrow band gap2Photochemical catalyst
Method, it is characterised in that：Ag/S mol ratios are 0.6:5~0.6:15.
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| CN108845006B (en) * | 2018-03-01 | 2022-05-13 | 南昌航空大学 | Method for using silver indium sulfide modified glassy carbon electrode for 4-NP detection |
| CN108993604B (en) * | 2018-08-10 | 2021-07-20 | 淮阴师范学院 | High visible light activity AgIn5S8/UIO-66-NH2Composite material and preparation method and application thereof |
| CN110038605B (en) * | 2019-05-17 | 2021-10-22 | 贵州大学 | AgInS applied to photocatalytic nitrogen reduction synthesis of ammonia2/Ti3C2Application method of nano catalyst |
| CN110408386B (en) * | 2019-07-31 | 2022-08-23 | 上海电力大学 | Indium sulfide silver quantum dot changing from green light to red light and one-step synthesis method and application thereof |
| CN112058280A (en) * | 2020-09-17 | 2020-12-11 | 南昌航空大学 | Preparation method and application of indium silver sulfide |
| CN114011435A (en) * | 2021-12-07 | 2022-02-08 | 合肥工业大学 | Water-soluble silver-indium-sulfur quantum dot photocatalyst and room-temperature preparation method |
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