CN105664973A - Three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and preparation method thereof - Google Patents
Three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and preparation method thereof Download PDFInfo
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title abstract description 9
- 230000001699 photocatalysis Effects 0.000 title abstract description 3
- 239000004005 microsphere Substances 0.000 title abstract 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006555 catalytic reaction Methods 0.000 claims description 45
- 150000001875 compounds Chemical class 0.000 claims description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 235000013877 carbamide Nutrition 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 7
- 230000004044 response Effects 0.000 claims description 7
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 229950000845 politef Drugs 0.000 claims description 6
- 238000005349 anion exchange Methods 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910009112 xH2O Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 2
- 239000002135 nanosheet Substances 0.000 abstract 2
- 229910052717 sulfur Inorganic materials 0.000 abstract 2
- 239000011593 sulfur Substances 0.000 abstract 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 239000000969 carrier Substances 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000005342 ion exchange Methods 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- -1 sulfur ions Chemical class 0.000 abstract 1
- 238000000034 method Methods 0.000 description 15
- 238000002474 experimental method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000005297 material degradation process Methods 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000004065 semiconductor Substances 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 150000002013 dioxins Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8659—Removing halogens or halogen compounds
- B01D53/8662—Organic halogen compounds
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/51—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
- B01D2258/0291—Flue gases from waste incineration plants
Abstract
The invention discloses a three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and a preparation method thereof, belonging to the field of pollution control and technology. The preparation method comprises the following steps of taking thioacetamide as a sulfur source, substituting lattice oxygen in the In2O3 with sulfur ions through an ion exchange reaction, performing in situ generation of an In2S3 nanosheet on the surface of flower-like In2O3, and forming a heterojunction structure, wherein the morphology of the three-dimensional flower-like In2O3 is uniform, and the particle size of the three-dimensional flower-like In2O3 is 3.0 to 6.5 microns; coating the surface of /In2O3 microflowers with the In2S3 nanosheet. The used raw materials are low in price and easily-obtained, reaction conditions are easily controlled and the requirement on equipment is low, so the preparation method disclosed by the invention is an environmental-friendly preparation method. By using In2S3/In2O3 composite microspheres, the utilization rate of the In2O3 to visible light can be improved, and the compounding of photon-generated carriers is inhibited; the In2S3/In2O3 composite microspheres have good application value and prospect in the field of volatile organic contaminants.
Description
Technical field
The invention belongs to field of environment pollution control, relate to a kind of novel three-dimensional flower-shaped In2S3/In2O3The preparation method of compound micron ball catalysis material, concretely relates to a kind of three-dimensional flower-shaped In for gas phase o-dichlorohenzene of degrading2S3/In2O3Compound micron ball catalysis material.
Background technology
City garbage burning problem has caused the common concern of people in recent years, in the process of city garbage burning, can produce chloride VOC (Cl VOCs). Wherein, two English (PCDDs) and polychlorinated dibenzo (PCDFs) are also belonged to dioxins by many chlorodiphenyls, it is listed in persistence organic pollutant (POPs), having higher toxicity, environmental persistence and carcinogenecity, therefore many countries have formulated strict discharge standard for PCDD/Fs. Improvement to this pollutant, traditional method is Production by Catalytic Combustion Process. But this process energy consumption is significantly high, equipment requirements is strict, particularly when processing the pollutant of low concentration (ppb), relatively costly problem is particularly evident. Photocatalysis technology has degradation efficiency height, reaction condition gentleness, non-secondary pollution, can utilize solar energy and to advantages such as the selectivity of pollutant are low, had become as in recent years a kind of there is applications well prospect remove the method for organic pollution in environment.
In2O3It it is a kind of important n-type III VI metal-oxide, indirect bandgap is 2.8eV, have certain visible light-responded, but the utilization rate that still suffers from visible ray is limited, and the problem such as photo-generated carrier recombination probability is bigger, in order to solve the two key issue, numerous bibliographical informations chooses the narrower quasiconductor of other energy gaps and In2O3Couple, build In2O3Base semiconductor hetero-junctions, reaches improve the utilization rate of visible ray and promote the purpose of photo-generated carrier high efficiency separation. Yu et al. (YuL.H., HuangY., XiaoG.C., etal.J.Mater.Chem.A, 2013,1,9637 9640) has synthesized the In that p-CuO quantum dot is modified2O3Hetero-junctions, with pure CuO and In2O3Compare, this CuO-QD In2O3Rhodamine B (RhB) is shown good visible light photocatalytic degradation effect by composite photo-catalyst.Li et al. (LiZ.M., ZhangP.Y., LiJ.E., etal.JPhotochPhotobioA, 2013,271,111 116) has synthesized In2O3/ graphene composite photocatalyst, this composite catalyst shows higher catalysis activity in degrading perfluorinated sad process. In2S3There are three kinds of crystal formation α-In2S3, β-In2S3With γ-In2S3. Wherein β-In2S3Physicochemical properties are the most stable, and energy gap narrower (2.0 2.3eV), as a kind of visible light catalyst, are widely used. Li et al. (LiH.H., ChenC., HuangX.Y., etal.J.PowerSources, 2014,247,915 919) reports a kind of In2O3In2S3Nucleocapsid electrode, shows good effect in the process of decomposition water.
At present, In2S3Nanometer sheet modifies three-dimensional flower-shaped In2O3There are no report, adopt hydro-thermal method to synthesize three-dimensional flower-shaped In in conjunction with original position anion exchange method simultaneously2S3/In2O3Compound micron ball catalysis material, and it is applied to visible light photocatalytic degradation o-dichlorohenzene (model compound of a kind of two English classes, its structure is similar with 2,4,7,8-tetrachloro dibenzo two English), also there is not been reported both at home and abroad. The present invention has synthesized three-dimensional flower-shaped In first2S3/In2O3Compound micron ball catalysis material, not only increases In2O3Utilization rate to visible ray, and inhibit the compound of photo-generated carrier.
Summary of the invention
The technical problem to be solved in the present invention is to provide one and prepares three-dimensional flower-shaped In2S3/In2O3The method of compound micron ball catalysis material. Adopt hydro-thermal method in conjunction with original position anion exchange method, prepare by In2S3Nanometer sheet wraps up flower-shaped In2O3Composite photocatalyst material. By improving, the utilization rate of visible ray and the separation efficiency of photo-generated carrier are improved three-dimensional flower-shaped In2O3Visible light catalysis activity. The three-dimensional flower-shaped In that this method prepares2S3/In2O3Compound micron ball catalysis material pattern is homogeneous, and cheaper starting materials used in preparation process is easy to get, and reaction condition is easily controllable, low for equipment requirements, is the preparation method of a kind of environmental protection. The VOCs that this composite catalyzing material is chloride to photocatalytic degradation, especially has good catalytic effect to o-dichlorohenzene.
Technical scheme:
A kind of three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material includes In2S3Nanometer sheet and three-dimensional flower-shaped In2O3; Three-dimensional flower-shaped In2O3Diameter be 3.0 6.5 μm, substantial amounts of nanometer sheet being interweaved forms; In2S3Nanometer sheet is of a size of 100 300nm, and thickness is 50 100nm; In2S3Nanometer sheet is wrapped in three-dimensional flower-shaped In equably2O3Surface.
A kind of three-dimensional flower-shaped In2S3/In2O3The preparation method of compound micron ball catalysis material, step is as follows:
(1) hydro-thermal method prepares three-dimensional flower-shaped In2O3: by InCl3·xH2O and sodium lauryl sulphate are dissolved in deionized water with mol ratio 1:2 1:4, and then stirring is until obtaining clear solution, wherein InCl3·xH2The concentration of O is 0.01 0.03mol/L; Adding carbamide in above-mentioned clear solution, the concentration of carbamide is 0.05 0.10mol/L, continuing stirring until dissolving, being proceeded to by above-mentioned mixed solution in politef reactor, at 115 160 DEG C of Water Under thermal response 8 16h; After being cooled to room temperature, repeatedly wash purification with ethanol and deionized water and remove unreacted reactant completely, centrifugation, collect white depositions In (OH)3, dry, by obtained white depositions In (OH)3Calcine 2h in 550 DEG C, prepare three-dimensional flower-shaped In2O3Powder.
(2) original position anion exchange reaction is adopted to prepare three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material: by three-dimensional flower-shaped In obtained in step (1)2O3Powder joins in deionized water, then ultrasonic disperse, wherein, adds flower-shaped In in every L water2O3Amount be 1.5 4.8g;Adding thioacetamide, continue stirring until thioacetyl amine solvent, obtain mixing suspension, wherein the concentration of thioacetamide is 0.6 3.0g/L.
(3) the mixing suspension of gained in step (2) is proceeded in politef reactor, carry out hydro-thermal reaction, hydrothermal temperature is 120 160 DEG C, the hydro-thermal reaction time is 6 10h, after naturally cooling to room temperature, with ethanol and deionized water cyclic washing, after being performing centrifugal separation on, collect precipitate and dry, preparing three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
The invention has the beneficial effects as follows: be prepared for a kind of three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material, the In of this method load2S3Nanometer sheet is at In2O3The surface distributed of micro-flowers is uniform; Utilize narrow-band semiconductor In2S3Nanometer sheet is to three-dimensional flower-shaped In2O3Modify, not only increase In2O3Utilization rate to visible ray, and inhibit the compound of photo-generated carrier. Additionally, the three-dimensional flower-shaped In of the method synthesis2S3/In2O3Compound micron ball catalysis material has good using value and prospect in catalytic degradation volatile organic contaminant field.
Accompanying drawing explanation
Fig. 1 (a) is the In prepared2O3Micro-flowers, In2S3Nano-particle and three-dimensional flower-shaped In2S3/In2O3The x-ray diffraction pattern of compound micron ball catalysis material. (step (2)), the three-dimensional flower-shaped In of addition in preparation process are represented respectively for IOS (I), IOS (II) and IOS (III) sample2O3The amount of powder is identical, and the addition of thioacetamide respectively 0.0192g, 0.0500g and 0.0960g.
Fig. 1 (b) is the In prepared2O3Micro-flowers and three-dimensional flower-shaped In2S3/In2O3The Raman spectrogram of compound micron ball catalysis material.
Fig. 2 (a) is scale when being 10 μm, In2O3The field emission scanning electron microscope figure of micro-flowers.
Fig. 2 (b) is scale when being 2 μm, In2O3The field emission scanning electron microscope figure of micro-flowers.
Fig. 2 (c) is scale when being 2.5 μm, three-dimensional flower-shaped In2S3/In2O3The field emission scanning electron microscope figure of compound micron ball catalysis material.
Fig. 2 (d) is scale when being 0.5 μm, three-dimensional flower-shaped In2S3/In2O3The field emission scanning electron microscope figure of compound micron ball catalysis material.
Fig. 3 (a) is the three-dimensional flower-shaped In prepared2S3/In2O3The transmission electron microscope picture of compound micron ball catalysis material.
Fig. 3 (b) is the three-dimensional flower-shaped In prepared2S3/In2O3The high-resolution-ration transmission electric-lens figure of compound micron ball catalysis material.
Fig. 4 (a) is the three-dimensional flower-shaped In prepared2S3/In2O3The full spectrogram of XPS of compound micron ball catalysis material.
Fig. 4 (b) is the XPS spectrum figure of In3d.
Fig. 4 (c) is the XPS spectrum figure of S2p.
Fig. 4 (d) is the XPS spectrum figure of O1s.
Fig. 5 (a) is the In prepared2O3Micro-flowers and three-dimensional flower-shaped In2S3/In2O3The uv-visible absorption spectra figure of compound micron ball catalysis material.
Fig. 5 (b) is (α h ν)2The graph of a relation of corresponding photon energy.
Fig. 6 is the In prepared2O3Micro-flowers and three-dimensional flower-shaped In2S3/In2O3The fluorescence spectrum figure of compound micron ball catalysis material.
Fig. 7 (a) is the In prepared2O3Micro-flowers, commercially available TiO2And three-dimensional flower-shaped In (P25)2S3/In2O3Compound micron ball catalysis material degradation efficiency to gas phase o-dichlorohenzene under visible light illumination.
Fig. 7 (b) is the kinetics matched curve figure in the degraded of radiation of visible light condition therapeutic method to keep the adverse QI flowing downwards phase o-dichlorohenzene.
Detailed description of the invention
The specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing and technical scheme.
Embodiment 1
Hydro-thermal method is adopted to prepare three-dimensional flower-shaped In2O3
By 0.7mmolInCl3·xH2O and 2.1mmol sodium lauryl sulphate is dissolved in 42mL deionized water, and then stirring is until obtaining clear solution;In above-mentioned solution, adding 3.5mmol carbamide, continuing stirring until dissolving; Above-mentioned mixed solution is proceeded in politef reactor, at 120 DEG C of Water Under thermal response 16h; After being cooled to room temperature, repeatedly wash purification with ethanol and deionized water and remove unreacted reactant completely, after centrifugation, collect white depositions (In (OH)3), dry, by obtained In (OH)3Powder calcines 2h in 550 DEG C, finally obtains three-dimensional flower-shaped In2O3。
Embodiment 2
According to the preparation method in embodiment 1, hydrothermal temperature is 160 DEG C, reacts 8h, and other parameters remain unchanged, and prepares three-dimensional flower-shaped In2O3。
Embodiment 3
According to the preparation method in embodiment 1, hydrothermal temperature is 140 DEG C, reacts 12h, and other parameters remain unchanged, and prepares three-dimensional flower-shaped In2O3。
Embodiment 4
According to the preparation method in embodiment 1, the consumption of carbamide increases to 4.2mmol, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2O3。
Embodiment 5
According to the preparation method in embodiment 1, the consumption of carbamide reduces to 2.1mmol, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2O3。
Embodiment 6
According to the preparation method in embodiment 1, InCl3·xH2The consumption of O and sodium lauryl sulphate reduces respectively to 0.42mmol and 1.26mmol, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2O3。
Embodiment 7
According to the preparation method in embodiment 1, InCl3·xH2The consumption of O and sodium lauryl sulphate increases respectively to 1.26mmol and 3.78mmol, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2O3。
Embodiment 8
According to the preparation method in embodiment 1, by InCl3·xH2The consumption of O and sodium lauryl sulphate increases respectively to 1.4mmol and 5.6mmol, joins in the deionized water of 84mL, and then stirring is until obtaining clear solution; Adding 8.4mmol carbamide in above-mentioned solution, other raw material dosage and experimental procedure remain unchanged, final prepared three-dimensional flower-shaped In2O3. Obtained In2O3Field emission scanning electron microscope figure see Fig. 2.
Embodiment 9
According to the preparation method in embodiment 8, reducing the consumption of sodium lauryl sulphate to 2.8mmol, other raw material dosage and experimental procedure remain unchanged, and prepare three-dimensional flower-shaped In2O3。
Embodiment 10
According to the preparation method in embodiment 8, by less for the consumption of carbamide to 4.2mmol, other raw material dosage and experimental procedure remain unchanged, and prepare three-dimensional flower-shaped In2O3。
Embodiment 11
Original position anion exchange reaction is adopted to prepare three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material
By the three-dimensional flower-shaped In of 0.1g obtained in embodiment 12O3Powder joins in 32mL deionized water, then ultrasonic disperse 60min, and ultrasonic power is 60W; Add 0.05g thioacetamide, continue stirring until thioacetyl amine solvent, obtain mixing suspension. Then proceeding in politef reactor by mixing suspension, carry out hydro-thermal reaction, reaction temperature is 150 DEG C, and the response time is 8h. After naturally cooling to room temperature, with ethanol and deionized water cyclic washing, after being performing centrifugal separation on, collect precipitate, dry, final prepared three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material. Obtained three-dimensional flower-shaped In2S3/In2O3The Raman spectrum of compound micron ball catalysis material is shown in that Fig. 1 (b), field emission scanning electron microscope figure are shown in that Fig. 2, transmission electron microscope picture are shown in that Fig. 3, x-ray photoelectron spectroscopy are shown in that Fig. 4, uv-visible absorption spectra are shown in Fig. 5, and fluorescence spectrum is shown in Fig. 6.
Embodiment 12
According to the preparation method in embodiment 11, hydrothermal temperature is 120 DEG C, and the response time is 10h, and other parameters remain unchanged, and prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 13
According to the preparation method in embodiment 11, hydrothermal temperature is 160 DEG C, and the response time is 6h, and other parameters remain unchanged, and prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 14
According to the preparation method in embodiment 11, the consumption of thioacetamide reduces to 0.0192g, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 15
According to the preparation method in embodiment 11, the consumption of thioacetamide increases to 0.0960g, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material. The three-dimensional flower-shaped In that method described in embodiment 11,14 and 15 prepares2S3/In2O3The X-ray diffracting spectrum of compound micron ball catalysis material is shown in Fig. 1 (a).
Embodiment 16
According to the preparation method in embodiment 11, three-dimensional flower-shaped In2O3The addition of powder reduces to 0.0480g, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 17
According to the preparation method in embodiment 11, three-dimensional flower-shaped In2O3The addition of powder increases to 0.1536g, and other raw material dosage and experimental procedure remain unchanged, and prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 18
According to the preparation method in embodiment 11, ultrasonic disperse time lengthening is to 90min, and ultrasonic power is decreased to 40W, and he remains unchanged at parameter, prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 19
According to the preparation method in embodiment 11, the ultrasonic disperse time foreshortens to 30min, and ultrasonic power increases to 80W, and he remains unchanged at parameter, prepares three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
Embodiment 20
Three-dimensional flower-shaped In2S3/In2O3The degrading activity of o-dichlorohenzene is investigated by compound micron ball catalysis material under visible light illumination
First, three-dimensional flower-shaped In obtained in 0.03g embodiment 11 is taken2S3/In2O3Compound micron ball catalysis material, being pressed into thickness is 0.5mm, and diameter is the disk of 13mm. Disk is fixed on the sample holder of infrared quartz reaction tank (volume is 120mL), disk and horizontal level angle at 45 °, then quartz reaction pond is sealed. Secondly, the o-dichlorohenzene liquid measuring 5 μ L with microsyringe is injected in quartz reaction pond, through the dark adsorption of 2h so that o-dichlorohenzene volatilizees fully, and reaches adsorption-desorption balance on the surface of catalyst. Then, opening light source and start o-dichlorohenzene of degrading, the light source used is the xenon lamp of 500W, xenon lamp distance catalyst disk 30cm, filters the wavelength ultraviolet portion less than 400nm with filter lens. Fourier transform infrared spectrometer is all adopted to gather the infrared spectrum of o-dichlorohenzene in real time in absorption and degradation period, finally according to the three-dimensional flower-shaped In of the change calculations of o-dichlorohenzene characteristic peak area2S3/In2O3The compound micron ball catalysis material degradation rate to o-dichlorohenzene, active testing result is shown in Fig. 7.
Embodiment 21
According to the investigation method in embodiment 20, to three-dimensional flower-shaped In obtained in embodiment 12O3Photocatalytic activity investigate.
Claims (9)
1. a three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material, it is characterised in that this three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material includes In2S3Nanometer sheet and three-dimensional flower-shaped In2O3;Three-dimensional flower-shaped In2O3Diameter be 3.0 6.5 μm, nanometer sheet being interweaved forms; In2S3Nanometer sheet is of a size of 100 300nm, and thickness is 50 100nm; In2S3Nanometer sheet is wrapped in three-dimensional flower-shaped In equably2O3Surface.
2. a three-dimensional flower-shaped In2S3/In2O3The preparation method of compound micron ball catalysis material, it is characterised in that step is as follows:
(1) hydro-thermal method prepares three-dimensional flower-shaped In2O3: by InCl3·xH2O and sodium lauryl sulphate are dissolved in deionized water with mol ratio 1:2 1:4, and then stirring is until obtaining clear solution, wherein InCl3·xH2The concentration of O is 0.01 0.03mol/L; Adding carbamide in above-mentioned clear solution, the concentration of carbamide is 0.05 0.10mol/L, continuing stirring until dissolving, being proceeded to by above-mentioned mixed solution in politef reactor, at 115 160 DEG C of Water Under thermal response 8 16h; After being cooled to room temperature, repeatedly wash purification with ethanol and deionized water and remove unreacted reactant completely, centrifugation, collect white depositions In (OH)3, dry, by obtained white depositions In (OH)3Calcine 2h in 550 DEG C, prepare three-dimensional flower-shaped In2O3Powder;
(2) original position anion exchange reaction is adopted to prepare three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material: by three-dimensional flower-shaped In obtained in step (1)2O3Powder joins in deionized water, then ultrasonic disperse, wherein, adds flower-shaped In in every L water2O3Amount be 1.5 4.8g; Adding thioacetamide, continue stirring until thioacetyl amine solvent, obtain mixing suspension, wherein the concentration of thioacetamide is 0.6 3.0g/L;
(3) the mixing suspension of gained in step (2) is proceeded in politef reactor, carry out hydro-thermal reaction, hydrothermal temperature is 120 160 DEG C, the hydro-thermal reaction time is 6 10h, after naturally cooling to room temperature, with ethanol and deionized water cyclic washing, after being performing centrifugal separation on, collect precipitate and dry, preparing three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material.
3. preparation method according to claim 2, it is characterised in that in step (1), hydrothermal temperature is 140 DEG C, the response time is 12h.
4. the preparation method according to Claims 2 or 3, it is characterised in that add flower-shaped In in every L water in step (2)2O3Amount be 3.125g.
5. the preparation method according to Claims 2 or 3, it is characterised in that to three-dimensional flower-shaped In in step (2)2O3The ultrasonic disperse time of powder suspension is 30 90min, and ultrasonic power is 40 80W.
6. preparation method according to claim 4, it is characterised in that to three-dimensional flower-shaped In in step (2)2O3The ultrasonic disperse time of powder suspension is 30 90min, and ultrasonic power is 40 80W.
7. the preparation method according to claim 2,3 or 6, it is characterised in that in step (3), hydrothermal temperature is 150 DEG C, and the hydro-thermal reaction time is 8h.
8. preparation method according to claim 4, it is characterised in that in step (3), hydrothermal temperature is 150 DEG C, the hydro-thermal reaction time is 8h.
9. preparation method according to claim 5, it is characterised in that in step (3), hydrothermal temperature is 150 DEG C, the hydro-thermal reaction time is 8h.
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