CN108993539A - A kind of light-catalysed method of raising indium sulfide - Google Patents
A kind of light-catalysed method of raising indium sulfide Download PDFInfo
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- CN108993539A CN108993539A CN201810886192.9A CN201810886192A CN108993539A CN 108993539 A CN108993539 A CN 108993539A CN 201810886192 A CN201810886192 A CN 201810886192A CN 108993539 A CN108993539 A CN 108993539A
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- 238000000034 method Methods 0.000 title claims abstract description 46
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 36
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 claims abstract description 9
- 238000007146 photocatalysis Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- ZOMNDSJRWSNDFL-UHFFFAOYSA-N sulfanylidene(sulfanylideneindiganylsulfanyl)indigane Chemical compound S=[In]S[In]=S ZOMNDSJRWSNDFL-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 238000013019 agitation Methods 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 12
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 12
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000004570 mortar (masonry) Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- LGZXYFMMLRYXLK-UHFFFAOYSA-N mercury(2+);sulfide Chemical compound [S-2].[Hg+2] LGZXYFMMLRYXLK-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000004073 vulcanization Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 description 26
- 238000006731 degradation reaction Methods 0.000 description 26
- 239000000243 solution Substances 0.000 description 22
- 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 21
- 229940012189 methyl orange Drugs 0.000 description 21
- 239000000047 product Substances 0.000 description 8
- 244000248349 Citrus limon Species 0.000 description 4
- 235000005979 Citrus limon Nutrition 0.000 description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 4
- 239000011260 aqueous acid Substances 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003165 hydrotropic effect Effects 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of methods for improving indium sulfide photocatalysis efficiency, and the method includes carrying out hydro-thermal process to it after synthesis indium sulfide, wherein the time of hydro-thermal process is 4-24 hours.The indium sulfide photocatalysis efficiency of hydrothermal treatment is obviously improved.
Description
Technical field
The present invention relates to photocatalysis fields, and in particular to a kind of light-catalysed method of raising indium sulfide.
Background technique
With advances in technology with the raising of human living standard, energy shortage, problem of environmental pollution are also more and more prominent
Out.Semiconductor light-catalyst can carry out catalytic degradation to waste water using solar energy, thus obtain the concern of various circles of society.β-
In2S3It is n-type semiconductor, has the characteristics that high carrier mobility, hypotoxicity and high stability.In2S3Forbidden bandwidth about
It is excellent visible-light photocatalyst for 1.9-2.2eV. In2S3Nano particle is under solar fuel cell, visible light conditions
There is important application value in terms of photocatalytically degradating organic dye and photocatalysis dissociation water hydrogen manufacturing.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for improving indium sulfide photocatalysis efficiency, and the method includes synthesis
Hydro-thermal process is carried out to it after indium sulfide, wherein the time of the hydro-thermal process is 4~24 hours.
Further, after 4~24 hours obtain hydro-thermal process, indium sulfide is as photochemical catalyst in 350W xenon lamp visible light
Carry out the degradation rate of photocatalytic degradation 84% or more according to the lower 10mg/L methyl orange solution to 50ml, further 90% with
On, further 93% or more
Further, the time of the hydro-thermal process is 4 hours or 16~24 hours;
Further, the time of the hydro-thermal process is that 4 hours, 8 hours, 12 hours, 16 hours, 20 hours or 24 are small
When.
Further, the method for the synthesis indium sulfide is the following steps are included: be added dropwise to lemon for indiumchloride solution
In aqueous acid, solvent is deionized water, needs to stir in the process of dropwise addition, after dropwise addition under constant magnetic agitation;Then
Sodium sulfide solution is added dropwise in the solution system of inidum chloride and citric acid, magnetic agitation, obtains the suspension of yellow;
Then, product is centrifuged, dehydrated alcohol and deionized water are washed repeatedly, and vacuum drying obtains the indium sulfide of Chinese red after grinding
Powder particle.
Further, the method for the synthesis indium sulfide is the following steps are included: be added dropwise to lemon for indiumchloride solution
In aqueous acid, solvent is deionized water, needs to stir in the process of dropwise addition, stirs 2 under constant magnetic agitation after dropwise addition
A hour;Then sodium sulfide solution is added dropwise in the solution system of inidum chloride and citric acid, magnetic agitation 1 hour, is obtained
To the suspension of yellow;Then, product is centrifuged, dehydrated alcohol and deionized water are washed 4-5 times repeatedly, in 60 DEG C of vacuum
Drying box is dry, and the indium sulfide powder particle of Chinese red is finally obtained after mortar grinder.
Further, the volume ratio of the indiumchloride solution, aqueous citric acid solution and sodium sulfide solution is 1:2:1.
Further, the concentration ratio of the indiumchloride solution, aqueous citric acid solution and sodium sulfide solution be 1:(0.1~
0.15): 2, it is further 14:1.9:28.
Further, the hydrothermal treatment process is distributed to the following steps are included: weighing indium sulfide powder in deionized water
In, ultrasound is carried out, uniform suspension liquid is transferred in autoclave, is placed in electric drying oven with forced convection, constant temperature is protected
Temperature;To which after reaction, cooled to room temperature is washed with dehydrated alcohol and deionization respectively again by centrifuge separation product
It washs, is finally dried in vacuo, the indium sulfide powder after grinding obtains hydro-thermal process.
In the synthetic method of the application indium sulfide, sodium sulfide solution is added dropwise to the molten of inidum chloride and citric acid
It in liquid system and stirs, being added dropwise and stirring makes to react more abundant and uniform, and such dropwise addition sequence is more advantageous to sulphur
The sulphion changed in sodium sufficiently forms indium sulfide in conjunction with indium ion.
Further, the hydrothermal treatment process is distributed to the following steps are included: weighing 500 milligrams of indium sulfide powder
In 40ml deionized water, then ultrasound 1 hour, uniform suspension liquid is transferred in the autoclave of 100 ml, is placed on
In electric drying oven with forced convection, 4~24 hours are kept the temperature under constant temperature at 140 DEG C, further heat preservation 4 hours or 16~24 hours;
To which after reaction, cooled to room temperature respectively washs three with dehydrated alcohol and deionized water again by being centrifugated product
It is secondary, 8 hours, the indium sulfide after hydro-thermal process is obtained after mortar grinder are finally dried in 60 DEG C of vacuum oven
Powder.
Further, the described method comprises the following steps: by 25ml concentration be 0.112mol/L indiumchloride solution dropwise
It is added in the aqueous citric acid solution that 50ml concentration is 15.2mmol/L, solvent is deionized water, is stirred in the process needs of dropwise addition
It mixes, stirs two hours after dropwise addition under constant magnetic agitation;Then 25ml concentration is molten for the vulcanized sodium of 0.224mol/L
Liquid is added dropwise in the solution system of inidum chloride and citric acid, one hour of magnetic agitation, obtains the suspension of yellow;So
Afterwards, product being centrifuged, dehydrated alcohol and deionized water are washed 4-5 times repeatedly, and it is dry in 60 DEG C of vacuum ovens, most pass through afterwards
The indium sulfide powder particle of Chinese red is obtained after crossing mortar grinder;It weighs 500 milligrams of indium sulfide powder and is distributed to and gone in 40ml
In ionized water, then ultrasound 1 hour, uniform suspension liquid is transferred in the autoclave of 100ml, electric heating air blast is placed on
In drying box, 4~24 hours are kept the temperature under constant temperature at 140 DEG C, further heat preservation 4 hours or 16~24 hours;Wait react knot
Shu Hou, cooled to room temperature are respectively washed three times again with dehydrated alcohol and deionized water by being centrifugated product, are finally existed
Dry 8 hours, the indium sulfide powder after hydro-thermal process is obtained after mortar grinder in 60 DEG C of vacuum oven.
Compared to the prior art, the synthetic method of indium sulfide of the present invention is simple, is more advantageous to manual operation, repeatability is very
It is good, and synthesis process is without using strong acid such as nitric acid, it is safer in experimentation;By the indium sulfide of invention preparation by of the invention
Method can be obviously improved the photocatalysis efficiency of indium sulfide after carrying out hydro-thermal process, and have repeatability well.
Detailed description of the invention
4~24 hour hour after cure indium of hydro-thermal process is bent to the light degradation of methyl orange in Fig. 1-6 respectively embodiment 2
Line chart, wherein C indicates the concentration of the methyl orange at some time point, C0Indicate to reach the dense of the methyl orange before absorption-desorption balance
Degree, Blank indicate blank group, In2S3The indium sulfide group for indicating non-hydrothermal treatment, 4h, 8h, 12h, 16h, 20h, distinguishes for 24 hours
Indicate the indium sulfide group through these time hydro-thermal process, in which:
Fig. 1 is 4 hours after cure indiums of hydro-thermal process in embodiment 2 to the degradation rate of methyl orange;Wherein, three curves by
The indium sulfide of blank group, the indium sulfide of non-hydro-thermal process and hydrothermal treatment 4 hours ground is followed successively by under to methyl orange
Degradation rate.
Fig. 2 is 8 hours after cure indiums of hydro-thermal process in embodiment 2 to the degradation rate of methyl orange;Wherein, three curves by
The indium sulfide of blank group, the indium sulfide of non-hydro-thermal process and hydrothermal treatment 8 hours ground is followed successively by under to methyl orange
Degradation rate.
Fig. 3 is 12 hours after cure indiums of hydro-thermal process in embodiment 2 to the degradation rate of methyl orange;Wherein, three curves by
The indium sulfide of blank group, the indium sulfide of non-hydro-thermal process and hydrothermal treatment 12 hours ground is followed successively by under to methyl orange
Degradation rate.
Fig. 4 is 16 hours after cure indiums of hydro-thermal process in embodiment 2 to the degradation rate of methyl orange;Wherein, three curves by
The indium sulfide of blank group, the indium sulfide of non-hydro-thermal process and hydrothermal treatment 16 hours ground is followed successively by under to methyl orange
Degradation rate.
Fig. 5 is 20 hours after cure indiums of hydro-thermal process in embodiment 2 to the degradation rate of methyl orange;Wherein, three curves by
The indium sulfide of blank group, the indium sulfide of non-hydro-thermal process and hydrothermal treatment 20 hours ground is followed successively by under to methyl orange
Degradation rate.
Fig. 6 is 24 hours after cure indiums of hydro-thermal process in embodiment 2 to the degradation rate of methyl orange;Wherein, three curves by
The indium sulfide of blank group, the indium sulfide of non-hydro-thermal process and hydrothermal treatment 24 hours ground is followed successively by under to methyl orange
Degradation rate.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below.It should be appreciated that the embodiment that the present invention provides
It is merely to illustrate the present invention, the range being not intended to restrict the invention.
Test method without specific conditions in following embodiments, usually according to normal condition or according to manufacturer
Proposed condition.Unless otherwise defined, all professional and scientific terms as used herein and one skilled in the art institute are ripe
The meaning known is identical.
In addition, any method similar to or equal to what is recorded and material can be applied to the method for the present invention.Text
Described in preferred implement methods and materials be for illustrative purposes only.
The preparation of 1 indium sulfide powder particle of embodiment
The indiumchloride solution that 25ml concentration is 0.112mol/L is added dropwise to the lemon that 50ml concentration is 15.2 mmol/L
In lemon aqueous acid, solvent is deionized water, needs to stir in the process of dropwise addition, stir under constant magnetic agitation after dropwise addition
Mix two hours;Then the sodium sulfide solution that 25ml concentration is 0.224mol/L is added dropwise to inidum chloride and citric acid
In solution system, one hour of magnetic agitation, the suspension of yellow is obtained.Then, product is centrifuged, dehydrated alcohol and go from
Sub- water washs 4-5 times repeatedly, dry in 60 DEG C of vacuum ovens, and the vulcanization of Chinese red is finally obtained after mortar grinder
Indium powder particle.
Embodiment 2 carries out hydrothermal treatment process to indium sulfide
It weighs 500 milligrams of indium sulfide powder (preparation of embodiment 1) to be distributed in 40ml deionized water, then ultrasound 1 is small
When, uniform suspension liquid is transferred in the autoclave of 100ml, is placed in electric drying oven with forced convection, at 140 DEG C
4~24 hours (4,8,12,16,20,24 hours) are kept the temperature under constant temperature respectively.To after reaction, cooled to room temperature,
It is respectively washed three times with dehydrated alcohol and deionized water by being centrifugated product, is finally done in 60 DEG C of vacuum oven again
Dry 8 hours, the indium sulfide powder after hydro-thermal process is obtained after mortar grinder.
Photocatalysis experimental result: using it is untreated and respectively 4~24 hours indium sulfides of hydro-thermal process as photocatalysis
Agent carries out photocatalytic degradation to the 10mg/L methyl orange solution of 50ml under 350W xenon lamp visible light photograph and is measured, passes through
Result after 50min degradation is as shown in Fig. 1-6 and table 1.
Degradation rate of the 1 hydro-thermal process after cure indium of table to methyl orange
The result shows that the indium sulfide of non-hydrothermal treatment only has the degradation rate of methyl orange by the degradation of 50min
10%, and by 4~24 hours indium sulfides of hydro-thermal process to the degradation rate of methyl orange 84% or more, and work as hydro-thermal process
When time is 4 hours, indium sulfide is to the degradation rate of methyl orange up to 93.3%;In addition, extending degradation time to 2 hours, vulcanize
Indium (respectively through 4,8,12,16,20,24 hours hydro-thermal process) can reach 97% to the degradation rate of methyl orange.
In addition, the application attempt to use other methods (for example, method as follows) prepare indium sulfide with reality
It applies under 2 the same terms of example, tests its degradation effect to methyl orange, as a result, it has been found that the indium sulfide that other methods are prepared can not
It realizes the excellent catalytic efficiency of the application, even if extending degradation time to 3 hours, can not also obtain the degradation effect of the application
Fruit.
Other methods
By 0.69 part of In (NO3)3·4.5H2O and 1.0 part of Na2S·9H2O is separately added into 40 parts of deionized waters, is made into
Vulcanized sodium hydrotropic solution is added in indium nitrate aqueous solution under stiring, and controls by indium nitrate aqueous solution and sodium sulfide solution
Speed is added to ensure to be formed uniform colloidal sol;Later, it is added 0.25 part of 1mol/L nitric acid solution, sol pH adjusting is arrived
1-3 or so;Finally, acidic sol is fitted into reaction kettle, make the compactedness 80% of reaction kettle, and anti-respectively at 180 DEG C
It answers 16,20,24 hours;After reaction kettle cooled to room temperature, by product filtering, with deionized water and ethanol wash, and
It is dried in vacuo at 55 DEG C, obtains 0.3 part of indium sulfide photocatalyst.
It should be understood that invention described herein is not limited to specific methodology, experimental program or reagent, because these
It can change.Discussion provided in this article and example present merely to describing specific embodiment and are not intended to limit
The scope of the present invention processed, the scope of the present invention are only limited by claim.
Claims (9)
1. a kind of method for improving indium sulfide photocatalysis efficiency, the method includes carrying out at hydro-thermal after synthesis indium sulfide to it
Reason, wherein the time of hydro-thermal process is 4-24 hours.
2. the method according to claim 1, wherein the time of the hydro-thermal process is 4 hours or 16-24 small
When.
3. method according to claim 1 or 2, which is characterized in that it is described synthesis indium sulfide method the following steps are included:
Indiumchloride solution is added dropwise in aqueous citric acid solution, solvent is deionized water, needs to stir in the process of dropwise addition, is added dropwise
Afterwards under constant magnetic agitation;Then sodium sulfide solution is added dropwise in the solution system of inidum chloride and citric acid, magnetic
Power stirring, obtains the suspension of yellow;Then, product being centrifuged, dehydrated alcohol and deionized water are washed repeatedly, vacuum drying,
The indium sulfide powder particle of Chinese red is obtained after grinding.
4. according to the method described in claim 3, it is characterized in that, the method for the synthesis indium sulfide will be the following steps are included: will
Indiumchloride solution is added dropwise in aqueous citric acid solution, and solvent is deionized water, needs to stir in the process of dropwise addition, after dropwise addition
2 hours are stirred under constant magnetic agitation;Then sodium sulfide solution is added dropwise to the solution of inidum chloride and citric acid
In system, magnetic agitation 1 hour, the suspension of yellow is obtained;Then, product is centrifuged, dehydrated alcohol and deionized water are repeatedly
Washing 4-5 times, it is dry in 60 DEG C of vacuum ovens, the indium sulfide powder of Chinese red is finally obtained after mortar grinder
Grain.
5. the method according to claim 3 or 4, which is characterized in that the indiumchloride solution, aqueous citric acid solution and vulcanization
The volume ratio of sodium solution is 1:2:1.
6. method according to any one of claim 3 to 5, which is characterized in that the indiumchloride solution, citric acid are water-soluble
The concentration of liquid and sodium sulfide solution ratio is 1:(0.1~0.15): 2, it is further 14:1.9:28.
7. method according to any one of claim 1 to 6, which is characterized in that the hydrothermal treatment process includes following
Step: it weighs indium sulfide powder and is distributed in deionized water, carry out ultrasound, uniform suspension liquid is transferred to reaction under high pressure
It in kettle, is placed in electric drying oven with forced convection, constant temperature heat preservation;To which after reaction, cooled to room temperature is produced by centrifuge separation
Object is washed with dehydrated alcohol and deionized water respectively again, is finally dried in vacuo, the indium sulfide after grinding obtains hydro-thermal process
Powder.
8. according to the method described in claim 6, it is characterized in that, the hydrothermal treatment process is the following steps are included: weigh 500
The indium sulfide powder of milligram is distributed in 40ml deionized water, then ultrasound 1 hour, and uniform suspension liquid is transferred to
It in the autoclave of 100ml, is placed in electric drying oven with forced convection, 4~24 hours is kept the temperature under constant temperature at 140 DEG C, into one
Step heat preservation 4 hours or 16~24 hours;To which after reaction, cooled to room temperature is used anhydrous again by centrifuge separation product
Ethyl alcohol and deionized water are respectively washed three times, finally dry 8 hours in 60 DEG C of vacuum oven, after mortar grinder
Indium sulfide powder after to hydro-thermal process.
9. method according to any one of claim 1 to 8, which is characterized in that the described method comprises the following steps: will
The indiumchloride solution that 25ml concentration is 0.112mol/L is added dropwise to the aqueous citric acid solution that 50ml concentration is 15.2mmol/L
In, solvent is deionized water, needs to stir in the process of dropwise addition, stirs two hours after dropwise addition under constant magnetic agitation;
Then the sodium sulfide solution that 25ml concentration is 0.224mol/L is added dropwise in the solution system of inidum chloride and citric acid, magnetic
Power stirs a hour, obtains the suspension of yellow;Then, product is centrifuged, dehydrated alcohol and deionized water wash 4-5 repeatedly
It is secondary, it is dry in 60 DEG C of vacuum ovens, the indium sulfide powder particle of Chinese red is finally obtained after mortar grinder;It weighs
500 milligrams of indium sulfide powder is distributed in 40ml deionized water, then ultrasound 1 hour, and uniform suspension liquid is transferred to
It in the autoclave of 100ml, is placed in electric drying oven with forced convection, 4~24 hours is kept the temperature under constant temperature at 140 DEG C, into one
Step heat preservation 4 hours or 16~24 hours;To which after reaction, cooled to room temperature is used anhydrous again by centrifuge separation product
Ethyl alcohol and deionized water are respectively washed three times, finally dry 8 hours in 60 DEG C of vacuum oven, after mortar grinder
Indium sulfide powder after to hydro-thermal process.
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