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 PDF

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CN105664973A
CN105664973A CN201610108957.7A CN201610108957A CN105664973A CN 105664973 A CN105664973 A CN 105664973A CN 201610108957 A CN201610108957 A CN 201610108957A CN 105664973 A CN105664973 A CN 105664973A
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dimensional flower
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李新勇
张菲
肇启东
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Dalian University of Technology
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8659Removing halogens or halogen compounds
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/51Spheres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
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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

A kind of three-dimensional flower-shaped In2S3/In2O3Compound micron ball catalysis material and preparation method thereof
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.
CN201610108957.7A 2016-02-26 2016-02-26 Three-dimensional flower-like In2S3/In2O3 composite microsphere photocatalytic material and preparation method thereof Pending CN105664973A (en)

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CN108126689A (en) * 2017-12-20 2018-06-08 江苏大学 A kind of Bi rich in oxygen defect2WO6/In2O3The Preparation method and use of heterojunction composite photocatalyst
CN108455709A (en) * 2018-04-11 2018-08-28 北京工业大学 A kind of preparation method of three indium oxides modifying titanium dioxide nanometer pipe array electrode
CN109338391A (en) * 2018-10-18 2019-02-15 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of substrate for optical electro-chemistry hydrogen production by water decomposition and products thereof and application
CN109589961A (en) * 2018-12-17 2019-04-09 江苏大学 One kind is for restoring CO2In2O3/CeO2The preparation method of/HATP composite photo-catalyst
CN109759082A (en) * 2019-02-21 2019-05-17 黑龙江大学 A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide
CN109999836A (en) * 2019-04-28 2019-07-12 大连工业大学 A kind of preparation of indium oxide/indium sulfide heterojunction semiconductor material and photochemical catalyst purposes and solar energy fixed nitrogen application
CN110038594A (en) * 2019-05-13 2019-07-23 东北师范大学 A kind of preparation method of porous oxidation indium/indium sulfide heterojunction material
CN110282653A (en) * 2019-08-08 2019-09-27 东北师范大学 A kind of oxidation phosphide material and preparation method for gas detection
CN110436514A (en) * 2018-05-05 2019-11-12 北京化工大学 The preparation method and application of transition metal element doped flower-shaped indium oxide gas sensitive
CN110937653A (en) * 2019-12-18 2020-03-31 扬州大学 Method for treating hexavalent chromium-containing wastewater through indium oxide-indium sulfide-titanium dioxide composite photocatalytic reduction
CN112023943A (en) * 2020-03-06 2020-12-04 商丘师范学院 Flower-shaped porous In2S3/In2O3Preparation method and application of composite catalyst
CN112264045A (en) * 2020-12-04 2021-01-26 福州大学 One-step synthesis method of one-dimensional indium oxide/indium sulfide composite semiconductor nanofiber
CN112316954A (en) * 2020-11-02 2021-02-05 江苏师范大学 Preparation of In having a hollow dodecahedron shape2O3-In2S3Method for preparing composite photocatalyst
CN112337491A (en) * 2020-11-17 2021-02-09 北华大学 Preparation method and application of nickel phosphide/indium oxide nanocomposite material applied to bifunctional photocatalysis
CN112588300A (en) * 2020-12-16 2021-04-02 江苏大学 Lattice distortion-based heterojunction photocatalyst and preparation method and application thereof
CN112774659A (en) * 2021-01-25 2021-05-11 中国计量大学 Graphene/indium oxide hydride composite photocatalyst and preparation method thereof
CN114471620A (en) * 2022-03-09 2022-05-13 淮北师范大学 a-SnWO4/In2S3Composite photocatalyst
CN114534746A (en) * 2022-02-28 2022-05-27 浙江理工大学 Photocatalytic hydrogen production system based on heterojunction photocatalyst and formaldehyde aqueous solution

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101508462A (en) * 2009-03-11 2009-08-19 长沙理工大学 Process for producing flower shaped indium hydroxide powder having high specific surface area
CN104588039A (en) * 2014-12-31 2015-05-06 山东玉皇新能源科技有限公司 Indium sulfide photocatalyst with hierarchical structures and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101508462A (en) * 2009-03-11 2009-08-19 长沙理工大学 Process for producing flower shaped indium hydroxide powder having high specific surface area
CN104588039A (en) * 2014-12-31 2015-05-06 山东玉皇新能源科技有限公司 Indium sulfide photocatalyst with hierarchical structures and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIA YANG 等: "Synthesis of In2O3-In2S3 core-shell nanorods with inverted type-I structure for photocatalytic H2 generation", 《PHYS. CHEM. CHEM. PHYS.》 *
康灵 等: "沿[100]晶向择优生长的花状In(OH)3晶体的合成与表征", 《长沙理工大学学报(自然科学版)》 *

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CN108126689A (en) * 2017-12-20 2018-06-08 江苏大学 A kind of Bi rich in oxygen defect2WO6/In2O3The Preparation method and use of heterojunction composite photocatalyst
CN108455709A (en) * 2018-04-11 2018-08-28 北京工业大学 A kind of preparation method of three indium oxides modifying titanium dioxide nanometer pipe array electrode
CN110436514A (en) * 2018-05-05 2019-11-12 北京化工大学 The preparation method and application of transition metal element doped flower-shaped indium oxide gas sensitive
CN109338391A (en) * 2018-10-18 2019-02-15 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of substrate for optical electro-chemistry hydrogen production by water decomposition and products thereof and application
CN109589961B (en) * 2018-12-17 2021-08-03 江苏大学 For reducing CO2In (2) of2O3/CeO2Preparation method of HATP composite photocatalyst
CN109589961A (en) * 2018-12-17 2019-04-09 江苏大学 One kind is for restoring CO2In2O3/CeO2The preparation method of/HATP composite photo-catalyst
CN109759082A (en) * 2019-02-21 2019-05-17 黑龙江大学 A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide
CN109999836A (en) * 2019-04-28 2019-07-12 大连工业大学 A kind of preparation of indium oxide/indium sulfide heterojunction semiconductor material and photochemical catalyst purposes and solar energy fixed nitrogen application
CN110038594A (en) * 2019-05-13 2019-07-23 东北师范大学 A kind of preparation method of porous oxidation indium/indium sulfide heterojunction material
CN110282653A (en) * 2019-08-08 2019-09-27 东北师范大学 A kind of oxidation phosphide material and preparation method for gas detection
CN110937653A (en) * 2019-12-18 2020-03-31 扬州大学 Method for treating hexavalent chromium-containing wastewater through indium oxide-indium sulfide-titanium dioxide composite photocatalytic reduction
CN110937653B (en) * 2019-12-18 2022-03-25 扬州大学 Method for treating hexavalent chromium-containing wastewater through indium oxide-indium sulfide-titanium dioxide composite photocatalytic reduction
CN112023943A (en) * 2020-03-06 2020-12-04 商丘师范学院 Flower-shaped porous In2S3/In2O3Preparation method and application of composite catalyst
CN112316954A (en) * 2020-11-02 2021-02-05 江苏师范大学 Preparation of In having a hollow dodecahedron shape2O3-In2S3Method for preparing composite photocatalyst
CN112337491A (en) * 2020-11-17 2021-02-09 北华大学 Preparation method and application of nickel phosphide/indium oxide nanocomposite material applied to bifunctional photocatalysis
CN112337491B (en) * 2020-11-17 2023-04-07 北华大学 Preparation method and application of nickel phosphide/indium oxide nanocomposite material applied to bifunctional photocatalysis
CN112264045B (en) * 2020-12-04 2021-08-31 福州大学 One-step synthesis method of one-dimensional indium oxide/indium sulfide composite semiconductor nanofiber
CN112264045A (en) * 2020-12-04 2021-01-26 福州大学 One-step synthesis method of one-dimensional indium oxide/indium sulfide composite semiconductor nanofiber
CN112588300A (en) * 2020-12-16 2021-04-02 江苏大学 Lattice distortion-based heterojunction photocatalyst and preparation method and application thereof
CN112774659A (en) * 2021-01-25 2021-05-11 中国计量大学 Graphene/indium oxide hydride composite photocatalyst and preparation method thereof
CN114534746A (en) * 2022-02-28 2022-05-27 浙江理工大学 Photocatalytic hydrogen production system based on heterojunction photocatalyst and formaldehyde aqueous solution
CN114534746B (en) * 2022-02-28 2023-12-05 浙江理工大学 Photocatalytic hydrogen production system based on heterojunction photocatalyst and formaldehyde aqueous solution
CN114471620A (en) * 2022-03-09 2022-05-13 淮北师范大学 a-SnWO4/In2S3Composite photocatalyst

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