CN105478143A - Method for preparing narrow-bandgap In-rich type AgInS2 photocatalyst with visible-light response - Google Patents
Method for preparing narrow-bandgap In-rich type AgInS2 photocatalyst with visible-light response Download PDFInfo
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- CN105478143A CN105478143A CN201510981334.6A CN201510981334A CN105478143A CN 105478143 A CN105478143 A CN 105478143A CN 201510981334 A CN201510981334 A CN 201510981334A CN 105478143 A CN105478143 A CN 105478143A
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- photochemical catalyst
- band gap
- narrow band
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000004044 response Effects 0.000 title abstract description 4
- 229910003373 AgInS2 Inorganic materials 0.000 title abstract 4
- 239000011941 photocatalyst Substances 0.000 title abstract 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000010521 absorption reaction Methods 0.000 claims abstract description 17
- 230000003595 spectral effect Effects 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 150000002471 indium Chemical class 0.000 claims abstract description 8
- 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
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012265 solid product Substances 0.000 claims abstract description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 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
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- 239000003054 catalyst Substances 0.000 claims description 34
- 229910052738 indium Inorganic materials 0.000 claims description 30
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 7
- 239000005864 Sulphur Substances 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-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 2
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical group N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 229910000337 indium(III) sulfate 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
- 230000009466 transformation Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 28
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000033558 biomineral tissue development Effects 0.000 abstract description 3
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 2
- 239000002184 metal Substances 0.000 abstract 2
- 150000003839 salts Chemical class 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 229910052709 silver Inorganic materials 0.000 abstract 1
- 239000004332 silver Substances 0.000 abstract 1
- -1 silver ions Chemical class 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 230000032683 aging Effects 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
- 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
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000000975 co-precipitation Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 229910052976 metal sulfide Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000011734 sodium 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
- 239000000126 substance Substances 0.000 description 2
- 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
- 230000015572 biosynthetic process Effects 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
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000003292 diminished effect 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
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 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
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 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
-
- B01J35/39—
-
- B01J35/613—
-
- 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
Abstract
The invention relates to a method for preparing a narrow-bandgap In-rich type AgInS2 photocatalyst with a visible-light response. The method comprises the following steps of fully dissolving silver salt and indium salt in a certain proportion in an organic alcohol solution to form a metal salt precursor; carrying out reaction on the metal salt precursor and an excessive sulfide (a sulfur source) under certain temperature through continuous stirring; enabling the sulfide to react with silver ions at first to form taupe silver sulfide, enabling the silver sulfide to react with the indium salt to generate phase variation with the prolongation of reaction time, and finally obtaining a bronzing solid product; washing and drying the bronzing solid product to obtain the narrow-bandgap In-rich type AgInS2 photocatalyst with a controllable and adjustable spectral absorption range and the visible-light response. The method disclosed by the invention has the outstanding advantages that preparation conditions are gentle, the yield is high, and the spectral absorption range of narrow-bandgap In-rich type AgInS2 is controllable and adjustable; the product, namelyAgInS2, has very high visible light catalyzation and mineralization property and higher regeneration ability.
Description
Technical field
The present invention relates to the rich indium type AgInS of a kind of visible light-responded narrow band gap
2the preparation method of photochemical catalyst, particularly relates to a kind of low-temperature co-precipitation method and prepares the narrow band gap richness indium type AgInS that spectral absorption range-controllable regulated, had visible light-responded and high catalysis mineralization ability
2photochemical catalyst.
Background technology
Dyestuff has enriched our life, but the environmental problem that waste water from dyestuff brings should not be underestimated.Waste water from dyestuff has that the water yield is large, colourity is dark, organic pollution content is high, complicated component, Acidity of Aikalinity are strong, non-oxidizability is strong, difficult for biological degradation, bio-toxicity are large and contain the multiple organic matter causing " three cause " (carcinogenic, teratogenesis, mutagenesis) performance.These waste water from dyestuff are in line, not only can worsen water quality, soil property, also threaten the health and safety of aquatic organism and the mankind.Therefore, how efficiently to control waste water from dyestuff and pollute the significant task having become environmentalist and endeavoured to study.
Conductor photocatalysis is as the very promising high-level oxidation technology of one, there is the advantages such as reaction condition gentleness, preparation technology is easy, energy consumption is low, reaction speed is fast, both can efficient-decomposition Some Organic Pollutants, also effectively can carry out decolouring to organic dyestuff and remove, even can be translated into CO
2, SO
4 2-, NO
3 -, the inorganic molecules material such as halogen.Therefore, utilize photocatalysis technology dye wastewater treatment to mitigating circumstances problem, maintaining ecological balance, realize sustainable development and be significant.
Binary metal sulfide is for common CdS photochemical catalyst, and its energy gap is 2.3eV, has very high photocatalytic activity.CdS is unstable in aqueous, the process of an anodic solution can be experienced, its photocatalytic activity is reduced rapidly, usually need to add the reducing agent such as sodium sulfite and vulcanized sodium and carry out trapped hole, light-catalyzed reaction is carried out, and most of sulfide have toxicity and unstability.
Based on the ternary metal sulfide I-III-VI that binary metal sulfide develops gradually, both inherited the characteristic of binary sulfide, there is again the characteristic that other are new.Silver sulfide indium is a kind of typical ternary low bandgap material, has AgInS
2and AgIn
5s
8two kinds of forms.The two all has good light sensitivity, stability and non-oxidizability, and forbidden band is narrower, visible light-responded by force, recycling rate of waterused is high, in photocatalytically degradating organic dye, photocatalytic water, opto-electronic conversion etc., have very important application.
At present, AgInS is prepared
2common methods has spray pyrolysis technologies, pyrolysismethod and hydro-thermal method, and these preparation methods have the shortcomings such as reaction temperature is high, energy consumption is high, preparation process is complicated, the reaction time is long.The invention provides a kind of low-temperature co-precipitation method controlled synthesis and there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, the method is simple, energy consumption is low, mild condition, consuming time short, the rich indium type AgInS of narrow band gap
2the spectral absorption range-controllable of photochemical catalyst regulates, and has good photocatalysis performance under visible light.
Summary of the invention
The object of the invention is to for AgInS
2the shortcomings such as existing preparation condition is harsh, operating procedure is complicated, propose the preparation of a kind of low-temperature co-precipitation method and have the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, AgInS prepared by this method
2stable chemical nature, the energy gap of photochemical catalyst be narrow, have stronger light absorption, spectral absorption range-controllable regulates, preferably photocatalytically degradating organic dye pollutant ability and there is higher power of regeneration.
The object of the invention is to be achieved through the following technical solutions, its preparation methods steps is as follows: a certain proportion of silver salt and indium salt are fully dissolved in Organic Alcohol solution, forms slaine precursor; Slaine precursor and excess of sulfur compound (sulphur source) Keep agitation react at a certain temperature; First sulfide react with silver ion, and form the silver sulfide of taupe, along with the prolongation in reaction time, silver sulfide and indium salt react and phase transformation, final acquisition red brown solid product; Red brown solid product deionized water and absolute ethyl alcohol are washed three times, respectively then at 60-100
odry under C, obtain spectral absorption range-controllable and regulate, there is the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Described silver salt is silver nitrate or silver acetate.
Described indium salt is indium nitrate or indium sulfate.
Described sulphur source is Na
2s, thioacetamide, Cys or thiocarbamide.
Described Organic Alcohol is ethanol, propyl alcohol, ethylene glycol or isopropyl alcohol.
Described Ag/In mol ratio is 1:5 ~ 1:11.
Described Ag/S mol ratio is 0.6:5 ~ 0.6:15.
Described reaction temperature is 55 ~ 95
oc.
Rich indium type AgInS prepared by the present invention
2the advantage of photochemical catalyst:
(1) rich indium type AgInS provided by the invention
2preparation method be low-temperature co-precipitation method, operate simple and easy, preparation time is short, and energy consumption is low, and applicability is wide;
(2) the present invention by regulation and control Ag/In mol ratio, can regulate and control rich indium type AgInS
2spectral absorption scope;
(3) the rich indium type AgInS for preparing of the present invention
2the stable chemical nature of photochemical catalyst, energy gap is narrow, effectively can be separated photo-generated carrier, has stronger light absorption and photocatalysis mineralization ability under visible light, and has higher stability and regenerability.
Accompanying drawing explanation
Fig. 1 is the AgInS of difference [Ag]/[In] ratio prepared in embodiments of the invention 2 and example 8
2photochemical catalyst: a:[Ag]/[In]=0.6:3, b:[Ag]/[In]=0.6:5.The XRD collection of illustrative plates of comparative sample, as seen from the figure, suitably increase In amount, the X ray diffracting data of sample does not change, with the AgInS of standard
2phase (PDF#25-1328) is consistent, and presents iris phase.
Fig. 2 is AgInS prepared in embodiments of the invention 2 and example 8
2the diffuse reflection figure of photochemical catalyst and band-gap energy collection of illustrative plates.As seen from the figure, In measures increase and has widened AgInS
2to the response of visible ray, its energy gap is diminished.
Fig. 3 is AgInS prepared in embodiments of the invention 2 and example 8
2nitrogen adsorption-the desorption of photochemical catalyst and pore size distribution curve, as seen from the figure, when [Ag]/[In] is for 0.6:3, the specific area of photochemical catalyst is 68.59m
2/ g, when [Ag]/[In] is for 0.6:5, specific area is 74.15m
2/ g, with increasing of the In amount in precursor salting liquid, its specific surface area value slightly increases, but its thermoisopleth all belongs to the IV type in IUPAC classification, H3 hysteresis loop.
Fig. 4 is AgInS prepared in embodiments of the invention 2 and example 8
2the visible ray of photochemical catalyst declines and separates the curve of methyl orange, as seen from the figure, suitably increases In amount, is obviously conducive to improving AgInS
2photocatalytic activity.
Detailed description of the invention
Following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
(1) by 0.6mmolAgNO
3with 3mmolIn (NO
3)
3be dissolved in 170mL ethanol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 10mmol thioacetamide is dissolved in 10mL ethanol, strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 55
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 2
(1) by 0.6mmolAgNO
3with 3mmolIn (NO
3)
3be dissolved in 170mL ethylene glycol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 10mmol thioacetamide is dissolved in 10mL ethylene glycol, strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 70
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 3
(1) by 0.6mmolCH
3cOOAg and 3mmolIn
2(SO
4)
3be dissolved in 170mL propyl alcohol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 5mmol thioacetamide is dissolved in 10mL propyl alcohol, strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 95
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for sediment russet, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 4
(1) by 0.6mmolAgNO
3with 3mmolIn (NO
3)
3be dissolved in 170mL isopropyl alcohol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 15mmol thiocarbamide is dissolved in 10mL isopropyl alcohol, strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 70
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for sediment russet, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 5
(1) by 0.6mmolAgNO
3with 3mmolIn (NO
3)
3be dissolved in 170mL ethylene glycol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 10mmolL-cysteine is dissolved in 10mL ethylene glycol strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 55
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 6
(1) by 0.6mmolAgNO
3with 3mmolIn (NO
3)
3be dissolved in 170mL ethylene glycol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 10mmol thiocarbamide is dissolved in 10mL ethylene glycol strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 70
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 7
(1) by 0.6mmolAgNO
3with 6.6mmolIn (NO
3)
3be dissolved in 170mL ethylene glycol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 5mmol thioacetamide is dissolved in 10mL ethylene glycol strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 70
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 8
(1) by 0.6mmolAgNO
3with 5mmolIn (NO
3)
3be dissolved in 170mL ethylene glycol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) 10mmol thioacetamide is dissolved in 10mL ethylene glycol strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 70
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Embodiment 9
(1) by 0.6mmolCH
3cOOAg and 6mmolIn (NO
3)
3be dissolved in 170mL ethylene glycol, ultrasonic dissolution forms the clear solution of slaine precursor.
(2) by 10mmolNa
2s is dissolved in 10mL ethylene glycol strong stirring, forms precipitating reagent.Under continuous stirring precipitant solution is dropwise added in above-mentioned slaine precursor solution.
(3) transfer in the there-necked flask of 250mL by the solution after mixing, add condensation reflux unit, and stir with suitable speed, bath temperature is 70
oc, water bath time is 3 hours.
(4), after reaction terminates, ageing a few hours, discard yellow supernatant, by centrifugal for reddish-brown precipitation thing, wash three times respectively, then 60 ~ 100 with deionized water and absolute ethyl alcohol
odry certain hour under C, cools naturally, grinding, obtains spectral absorption range-controllable and regulates, has the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
Claims (8)
1. prepare there is the rich indium type AgInS of visible light-responded narrow band gap for one kind
2the method of photochemical catalyst, is characterized in that preparation process is as follows: a certain proportion of silver salt and indium salt are fully dissolved in Organic Alcohol solution, forms slaine precursor; Slaine precursor and sulphur source Keep agitation react at a certain temperature; First sulfide react with silver ion, and form the silver sulfide of taupe, along with the prolongation in reaction time, silver sulfide and indium salt react and phase transformation, final acquisition red brown solid product; Red brown solid product deionized water and absolute ethyl alcohol are washed three times, respectively then at 60-100
odry under C, obtain spectral absorption range-controllable and regulate, there is the rich indium type AgInS of visible light-responded narrow band gap
2photochemical catalyst.
2. a kind of preparation according to claim 1 there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, is characterized in that: described silver salt is silver nitrate or silver acetate.
3. a kind of preparation according to claim 1 there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, is characterized in that: described indium salt is indium nitrate or indium sulfate.
4. the rich indium type AgInS of a kind of narrow band gap of getting everything ready visible light-responded according to claim 1
2the method of photochemical catalyst, is characterized in that: described sulphur source is Na
2s, thioacetamide, Cys or thiocarbamide.
5. a kind of preparation according to claim 1 there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, is characterized in that: described Organic Alcohol is ethanol, propyl alcohol, ethylene glycol or isopropyl alcohol.
6. a kind of preparation according to claim 1 there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, is characterized in that: Ag/In mol ratio is 1:5 ~ 1:11.
7. a kind of preparation according to claim 1 there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, is characterized in that: Ag/S mol ratio is 0.6:5 ~ 0.6:15.
8. a kind of preparation according to claim 1 there is the rich indium type AgInS of visible light-responded narrow band gap
2the method of photochemical catalyst, is characterized in that: reaction temperature is for being 55 ~ 95
oc.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004255355A (en) * | 2003-02-28 | 2004-09-16 | Japan Science & Technology Agency | AgGaS2 PHOTOCATALYST INDICATING HIGH ACTIVITY UNDER VISIBLE LIGHT IRRADIATION IN HYDROGEN PRODUCTION FROM AQUEOUS SOLUTION CONTAINING SULFUR COMPOUND |
| CN103657686A (en) * | 2013-12-02 | 2014-03-26 | 南昌航空大学 | Method for preparing SnIn4S photocatalyst through low-temperature coprecipitation method |
-
2015
- 2015-12-24 CN CN201510981334.6A patent/CN105478143B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004255355A (en) * | 2003-02-28 | 2004-09-16 | Japan Science & Technology Agency | AgGaS2 PHOTOCATALYST INDICATING HIGH ACTIVITY UNDER VISIBLE LIGHT IRRADIATION IN HYDROGEN PRODUCTION FROM AQUEOUS SOLUTION CONTAINING SULFUR COMPOUND |
| CN103657686A (en) * | 2013-12-02 | 2014-03-26 | 南昌航空大学 | Method for preparing SnIn4S photocatalyst through low-temperature coprecipitation method |
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