CN111939936A - In2S3/TiO2Preparation method and application of photocatalyst - Google Patents

In2S3/TiO2Preparation method and application of photocatalyst Download PDF

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CN111939936A
CN111939936A CN202010854317.7A CN202010854317A CN111939936A CN 111939936 A CN111939936 A CN 111939936A CN 202010854317 A CN202010854317 A CN 202010854317A CN 111939936 A CN111939936 A CN 111939936A
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photocatalyst
titanium
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indium
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罗涛
马多谋
刘皖彦
陈倩
金震
张勇
黄健
张华�
彭夫敏
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Anhui Jianzhu University
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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
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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
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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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/10—Heat treatment in the presence of water, e.g. steam
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/20—Sulfiding
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—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
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

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Abstract

The present invention discloses an In2S3/TiO2The photocatalyst, the preparation method and the application thereof are characterized In that a solid titanium-oxygen cluster is taken as a titanium source, an indium source and a sulfur source are introduced, and In is prepared by a hydrothermal method2S3/TiO2A photocatalyst. The invention takes the solid titanium-oxygen cluster as the titanium source, and compared with the traditional liquid titanium source, the solid titanium-oxygen cluster is used as the precursor of titanium dioxide, thereby avoiding spontaneous hydrolysis and condensation reaction. Book (I)In of the invention2S3/TiO2The photocatalyst is a green and environment-friendly material, does not produce secondary pollution after being degraded, and has wide application range. In provided by the invention2S3/TiO2The photocatalyst is easy to synthesize, simple to operate, strong in photocatalytic degradation capacity and easy to apply to equipment and process in a large scale. The invention can be TiO2Provides a new idea for developing a base catalyst and is suitable for large-scale production of TiO2The base composite material provides a new raw material and a simple synthesis method.

Description

In2S3/TiO2Preparation method and application of photocatalyst
Technical Field
The present invention relates to an In2S3/TiO2Photocatalyst, preparation method and application thereof.
Background
Titanium dioxide (TiO)2) Has the advantages of high chemical stability, no toxicity, low cost and the like, and is widely used in the field of photocatalysis. However, single component TiO2Still limited by the wide band gap and the rapid recombination of electrons and holes. Thus, TiO with visible light response2The development of the base composite catalyst becomes a research hotspot. TiO 22Coupling with other semiconductors to create heterostructures is an effective strategy to improve photocatalytic performance, e.g. g-C3N4/TiO2，CuO/ZrO2-TiO2，Ag3PO4/TiO2And the like. In2S3Has good photosensitivity and stable physicochemical properties, and is widely used in the field of photocatalysis. In3+The toxicity of the compound is far lower than that of Cd2+And thus has less risk of secondary pollution to water. By using In2S3And TiO2The coupling of (a) as a photocatalyst,degradation of organic contaminants in water under visible light is a viable approach.
Titanium alcoholates and titanium chlorides are commonly used for preparing TiO2The liquid titanium source can be rapidly hydrolyzed when meeting water. Thus, for TiO2The synthesis of functional materials, how to control the hydrolysis of the titanium source is a difficult problem, especially for TiO2For composites, this is in combination with TiO2The crystal size and the dispersion in the heterostructure are related. Typically, to control hydrolysis, surfactants are introduced into the synthesis system. However, the introduction of surfactants makes the production process complicated and difficult to control. In addition, the removal of surfactants in the collection and purification of samples is also a challenge. TiOx clusters have the advantages of definite crystal structure, high stability, and good solubility in water and various organic solvents, and thus, the TiOx clusters can be used as building blocks to assemble TiO having a highly ordered structure2Networking or building TiO2The composite photocatalyst avoids the problem of rapid hydrolysis of the traditional titanium source.
Disclosure of Invention
In view of the problems of the prior art, the present invention provides an In2S3/TiO2Photocatalyst, preparation method and application thereof.
In for achieving the above object, the present invention employs an In2S3/TiO2The preparation method of the photocatalyst comprises the steps of taking a solid titanium-oxygen cluster as a titanium source, introducing an indium source and a sulfur source, and preparing In by a hydrothermal method2S3/TiO2A photocatalyst.
As an improvement, the In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) adding solid titanium oxide clusters into water according to a solid-to-liquid ratio of 1g (400-500 ml), and carrying out ultrasonic treatment to obtain an aqueous solution of the titanium oxide clusters;
2) respectively adding indium salt and a sulfur source into an aqueous solution of the titanium oxide cluster, magnetically stirring, and adjusting the pH value to 1-3; wherein the molar ratio of the added indium salt to the titanium oxide clusters is 1-4: 1, and the molar ratio of the added sulfur source to the indium salt is 1-5: 1;
3) obtaining In from the solution prepared In the step 2) by a hydrothermal method2S3/TiO2A photocatalyst.
Among these, reference may be made to chem.sci.,2015,6, 3926-; Angew.chem.Int.Ed.2018,57, 14852-14856; solid titanyl clusters were synthesized by the method disclosed in j.mater.chem.a,2019,7, 19161-.
As an improvement, the titanium-oxygen cluster adopts Ti6O6(OiPr)6(abz)6、Ti11O13(OiPr)18、Ti6O6(OiPr)6(t-BA)6、Ti6(μ3-O)6(OiPr)6(NA)6、Ti8O8(OOCCH2But)16、Ti12O4(PgC3)(OiPr)28、Ti8O6(OBz)20、Ti8(μ2-O)8(μ2-OMc)16、Ti7O4(OEt)20、Ti10O12(CAT)8(PY)8、Ti16O16(OEt)32At least one of (1).
In a refinement, the indium salt is at least one of indium acetate, indium nitrate, or indium chloride.
In the improvement, the sulfur source is at least one of sodium sulfide, thiourea or thioacetamide.
As an improvement, the reaction temperature of the hydrothermal method is 150-200 ℃, and the heating time is 14-20 h.
In addition, the invention also provides In2S3/TiO2The photocatalyst is prepared by the preparation method.
Finally, the invention also provides the In2S3/TiO2The application of the photocatalyst in catalyzing and degrading tetracycline in wastewater under the irradiation of visible light.
The principle of the invention is as follows: under hydrothermal conditions, solid titanium oxide clusters are gradually converted into TiO2Small crystal grainIn is formed by the simultaneous reaction of a sulfur source and an indium source In the same reaction system2S3Small crystal grain, TiO2And In2S3The small crystal grains are mutually interwoven to form In2S3/TiO2The heterostructure photocatalyst of (1).
The invention has the beneficial effects that:
1. the invention takes the solid titanium-oxygen cluster as the titanium source, and compared with the traditional liquid titanium source, the solid titanium-oxygen cluster is used as the precursor of titanium dioxide, thereby avoiding spontaneous hydrolysis and condensation reaction.
2. In of the invention2S3/TiO2The photocatalyst is a green and environment-friendly material, does not produce secondary pollution after being degraded, and has wide application range.
3. In provided by the invention2S3/TiO2The photocatalyst is easy to synthesize, simple to operate, strong in photocatalytic degradation capacity and easy to apply to equipment and process in a large scale.
4. In2S3/TiO2In the photocatalyst, In2S3With TiO2Uniform slow nucleation of formed In2S3And TiO2The small crystal grains are mutually interwoven to form a heterogeneous structure with uniform distribution.
5. The invention can be TiO2Provides a new idea for developing a base catalyst and is suitable for large-scale production of TiO2The base composite material provides a new raw material and a simple synthesis method.
Drawings
FIG. 1 shows In prepared by the present invention2S3/TiO2An X-ray diffraction pattern of the photocatalyst;
FIG. 2 shows In prepared by the present invention2S3/TiO2Transmission electron micrographs of the photocatalyst;
FIG. 3 shows In prepared by the present invention2S3/TiO2High resolution electron microscopy of the photocatalyst;
FIG. 4 shows In prepared by the present invention2S3/TiO2Photo-degradation performance diagram of the photocatalyst to TC.
Detailed Description
The following examples are further illustrative of the present invention as to the technical content of the present invention, but the essence of the present invention is not limited to the following examples, and one of ordinary skill in the art can and should understand that any simple changes or substitutions based on the essence of the present invention should fall within the protection scope of the present invention.
Example 1
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti6O6(OiPr)6(t-BA)6(corresponding solid TiOx clusters were prepared beforehand as disclosed in references chem.Sci.,2015,6, 3926-3930; Angew. chem.Int.Ed.2018,57, 14852-14856; J.Mater. chem.A., 2019,7, 19161-19172, the same applies hereinafter) into a beaker containing 50mL of deionized water and after sonication for 60 minutes Ti was formed6O6(OiPr)6(t-BA)6An aqueous solution;
2) then 0.3mmol indium nitrate and 0.9mmol sodium sulfide were added to the above solution under stirring, and the pH of the solution was adjusted to 3.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 180 deg.C for 16h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
In prepared by the above method2S3/TiO2The photocatalyst is subjected to performance tests, and the results are as follows:
FIG. 1 shows the X-ray diffractometer (XRD) vs. In2S3/TiO2The photocatalyst was characterized, and the figure demonstrates that the synthesized target product is made of anatase TiO2And In2S3And (4) forming.
FIG. 2 shows In vs. In using a Transmission Electron Microscope (TEM)2S3/TiO2The photocatalyst was characterized and showed a target product as small as about 20nm in sizeAggregates of rice particles.
FIG. 3 shows the In contrast with a High Resolution Transmission Electron Microscope (HRTEM)2S3/TiO2The photocatalyst was characterized and the figure shows that the target product is In2S3And TiO2The grains are uniformly combined.
Example 2
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti11O13(OiPr)18Adding into a beaker filled with 40mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti11O13(OiPr)18An aqueous solution;
2) then 0.1mmol indium nitrate and 0.3mmol thiourea were added to the above solution under stirring, and the pH of the solution was adjusted to 2.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 150 deg.C for 20h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 3
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti7O4(OEt)20Adding into a beaker filled with 45mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti7O4(OEt)20An aqueous solution;
2) then 0.5mmol indium nitrate and 1.5mmol thioacetamide were added to the above solution under stirring, and the pH of the solution was adjusted to 1.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 160 deg.C for 18h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 4
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti6O6(OiPr)6(abz)6Adding into a beaker filled with 40mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti6O6(OiPr)6(abz)6An aqueous solution;
2) then 0.3mmol indium chloride and 0.6mmol sodium sulfide were added to the above solution under stirring, and the pH of the solution was adjusted to 3.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 170 deg.C for 20h, naturally cooling to room temperature, washing with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 5
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti8O8(OOCCH2But)16Adding into a beaker filled with 50mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti8O8(OOCCH2But)16An aqueous solution;
2) then 0.3mmol indium chloride and 1.2mmol thiourea were added to the above solution under stirring, and the pH of the solution was adjusted to 2.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 150 deg.C for 20h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 6
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti8O6(OBz)20Adding into a beaker filled with 45mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti8O6(OBz)20An aqueous solution;
2) then 0.3mmol indium chloride and 1.5mmol thioacetamide were added to the above solution under stirring, and the pH of the solution was adjusted to 1.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 190 deg.C for 15h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 7
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti12O4(PgC3)(OiPr)28Adding into a beaker filled with 40mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti12O4(PgC3)(OiPr)28An aqueous solution;
2) then 0.2mmol indium acetate and 0.6mmol sodium sulfide were added to the above solution under stirring, and the pH of the solution was adjusted to 3.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 200 deg.C for 14h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 8
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti6(μ3-O)6(OiPr)6(NA)6Adding into a beaker filled with 50mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti6(μ3-O)6(OiPr)6(NA)6An aqueous solution;
2) then 0.4mmol indium acetate and 1.2mmol thiourea were added to the above solution under stirring, and the pH of the solution was adjusted to 2.0 with dilute nitric acid;
3) the solution was transferred to a teflon liner and heated at 160 deg.CHeating for 19h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 9
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti8(μ2-O)8(μ2-OMc)16Adding the mixture into a beaker filled with 40mL of deionized water, and carrying out ultrasonic treatment for 1h to form a white solution;
2) then 0.2mmol of indium acetate and 0.8mmol of thioacetamide were added to the above suspension with stirring, and the pH of the solution was adjusted to 1.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 180 deg.C for 17h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 10
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti10O12(CAT)8(PY)8Adding into a beaker filled with 40mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti10O12(CAT)8(PY)8An aqueous solution;
2) then 0.2mmol of indium acetate and 1.0mmol of thioacetamide were added to the above solution under stirring, and the pH of the solution was adjusted to 3.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 180 deg.C for 17h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 11
In2S3/TiO2The preparation method of the photocatalyst comprises the following steps:
1) 100mg of Ti16O16(OEt)32Adding into a beaker filled with 40mL of deionized water, and carrying out ultrasonic treatment for 1h to form Ti16O16(OEt)32An aqueous solution;
2) then 0.3mmol of indium acetate and 1.2mmol of thioacetamide were added to the above solution under stirring, and the pH of the solution was adjusted to 2.0 with dilute nitric acid;
3) transferring the solution into polytetrafluoroethylene lining, heating at 150 deg.C for 17h, naturally cooling to room temperature, washing the product with distilled water and ethanol for 3 times, and vacuum drying to obtain In2S3/TiO2A photocatalyst.
Example 12
In2S3/TiO2The application of the photocatalyst in catalyzing and degrading tetracycline in wastewater under the irradiation of visible light comprises the following steps:
1) preparing 50ml of 40ppm tetracycline aqueous solution;
2) collecting 10mg of the prepared In2S3/TiO2Adding a photocatalyst into the aqueous solution;
3) stirring the mixed solution prepared in the step 2) for 1 hour in the absence of light to achieve adsorption and desorption balance, carrying out photoreaction for 1 hour, and measuring the absorbance of the solution every 10min for six times.
FIG. 4 shows In under visible light2S3/TiO2The degradation performance of the photocatalyst on tetracycline shows that the target product has better photocatalytic performance than pure In2S3And TiO2And the degradation efficiency of 40ppm tetracycline reaches 78.1% after 1h of photocatalysis.
The above description is only exemplary of the invention, and should not be taken as limiting the invention, as any modification, equivalent replacement or improvement made within the spirit and principle of the invention should be included in the protection scope of the invention.

Claims (8)

1. In2S3/TiO2The preparation method of the photocatalyst is characterized in that the photocatalyst is prepared by taking solid titanium-oxygen clusters as raw materialsIntroducing an indium source and a sulfur source into a titanium source, and preparing In by a hydrothermal method2S3/TiO2A photocatalyst.
2. An In according to claim 12S3/TiO2The preparation method of the photocatalyst is characterized by comprising the following steps:
1) adding solid titanium oxide clusters into water according to a solid-to-liquid ratio of 1g (400-500 ml), and carrying out ultrasonic treatment to obtain an aqueous solution of the titanium oxide clusters;
2) respectively adding indium salt and a sulfur source into an aqueous solution of the titanium oxide cluster, magnetically stirring, and adjusting the pH value to 1-3; wherein the molar ratio of the added indium salt to the titanium oxide clusters is 1-4: 1, and the molar ratio of the added sulfur source to the indium salt is 1-5: 1;
3) obtaining In from the solution prepared In the step 2) by a hydrothermal method2S3/TiO2A photocatalyst.
3. An In according to claim 1 or 22S3/TiO2The preparation method of the photocatalyst is characterized in that the titanium-oxygen cluster adopts Ti6O6(OiPr)6(abz)6、Ti11O13(OiPr)18、Ti6O6(OiPr)6(t-BA)6、Ti6(μ3-O)6(OiPr)6(NA)6、Ti8O8(OOCCH2But)16、Ti12O4(PgC3)(OiPr)28、Ti8O6(OBz)20、Ti8(μ2-O)8(μ2-OMc)16、Ti7O4(OEt)20、Ti10O12(CAT)8(PY)8、Ti16O16(OEt)32At least one of (1).
4. An In according to claim 1 or 22S3/TiO2The preparation method of the photocatalyst is characterized in that the indium salt adopts at least one of indium acetate, indium nitrate or indium chloride.
5. An In according to claim 1 or 22S3/TiO2The preparation method of the photocatalyst is characterized in that the sulfur source adopts at least one of sodium sulfide, thiourea or thioacetamide.
6. An In according to claim 1 or 22S3/TiO2The preparation method of the photocatalyst is characterized in that the reaction temperature of the hydrothermal method is 150-200 ℃, and the heating is carried out for 14-20 hours.
7. In2S3/TiO2A photocatalyst produced by the production method according to any one of claims 1 to 6.
8. An In according to any one of claims 1 to 72S3/TiO2The application of the photocatalyst in catalyzing and degrading tetracycline in wastewater under the irradiation of visible light.
CN202010854317.7A 2020-08-24 2020-08-24 In2S3/TiO2Preparation method and application of photocatalyst Pending CN111939936A (en)

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