CN113209997A - Near-infrared light response CuS/S-C3N4Preparation method of heterojunction nano composite material - Google Patents
Near-infrared light response CuS/S-C3N4Preparation method of heterojunction nano composite material Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 21
- 230000004298 light response Effects 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title abstract description 16
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
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- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 230000000593 degrading effect Effects 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 claims description 2
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 239000002904 solvent Substances 0.000 abstract 2
- 229910052927 chalcanthite Inorganic materials 0.000 abstract 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 30
- 239000004098 Tetracycline Substances 0.000 description 12
- 229960002180 tetracycline Drugs 0.000 description 12
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- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- OFVLGDICTFRJMM-WESIUVDSSA-N tetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O OFVLGDICTFRJMM-WESIUVDSSA-N 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 150000003522 tetracyclines Chemical class 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
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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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
-
- 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
Abstract
The invention discloses a near-infrared light response CuS/sulfur-doped carbon nitride (S-C)3N4) The preparation method of the heterojunction nano composite material comprises the step of growing CuS in situ on S-C by a hydrothermal method3N4Preparing CuS/S-C on the surface3N4The heterojunction nano composite material comprises the following operation steps: preparing S-C by using urea and Thioacetamide (TAA) as raw materials and distilled water as a solvent by adopting a two-step heating method3N4(ii) a Then with S-C3N4、CuSO4·5H2O and TAA are taken as raw materials, distilled water is taken as a solvent, and a hydrothermal method is adopted to carry out reaction on S-C3N4Surface in situ generationGrowing CuS to produce CuS/S-C3N4A heterojunction nanocomposite. The invention has the advantages that: simple process, simple operation and low cost, and the obtained CuS/S-C3N4Heterojunction nanocomposites with greatly expanded g-C3N4The light response capability in visible and near infrared spectral regions, and the activity of degrading organic pollutants is obviously improved.
Description
Technical Field
The invention belongs to the technical field of environmental pollution treatment, and particularly relates to near-infrared light response CuS/S-C3N4A preparation method of heterojunction nano composite material.
Background
With the widespread use of antibiotics, the problem of their remaining pollution in the environment has been difficult to reasonably solve. A better solution to this problem can be provided by efficient use of solar photocatalytic degradation. With simple g-C3N4In contrast, sulfur doped carbon nitride (S-C)3N4) Has better stability and proper band gap, and enhances g-C after doping sulfur3N4The light absorption capacity is improved, and the degradation activity of the light absorption agent on pollutants is improved. At present, there are already S-C3N4Reports on improving the efficiency of pollutant degradation.
Copper sulfide (CuS) is a p-type semiconductor material with narrow band gap, easy synthesis and low cost, and has wider photoresponse range. Due to the narrow band gap, the photon-generated carriers and the photon-generated holes are easy to be combined. The semiconductor is compounded with other semiconductors to form a heterojunction, so that the separation efficiency of a photon-generated carrier is improved, the photocatalytic activity of the semiconductor is improved, and the semiconductor is one of strategies for utilizing CuS in the field of photocatalysis.
In recent years, by mixing g-C3N4Coupling with metal oxides is a common strategy to improve their electron transport path and efficiency. Therefore, we have designed a new approach to S-C3N4The process route of forming the heterojunction composite material by growing CuS on the surface in situ successfully obtains the composite material with near infrared light response. So far, no relevant process is published.
Disclosure of Invention
In order to solve the technical problem, the invention provides a near infrared light response CuS/S-C3N4A preparation method of heterojunction nano composite material.
The invention adopts the following technical scheme: near-infrared light response CuS/S-C3N4The preparation method of the heterojunction nano composite material is characterized by comprising the following steps: CuS is grown in situ on S-C by adopting a hydrothermal method3N4Surface, thereby S-C3N4The photoresponse range of the photocatalyst is successfully expanded from a visible light region to a near infrared region, and the activity of photocatalytic degradation of organic matters in the visible light region is enhanced. The preparation method comprises the following steps:
(1) weighing a certain amount of urea, stirring and dissolving the urea in a certain amount of secondary distilled water at a constant temperature, adding a certain amount of thioacetamide after the urea is fully dissolved, and continuously stirring until the thioacetamide is fully dissolved.
(2) Transferring the mixed solution obtained in the step (1) into a semi-sealed crucible and then sending the mixed solution into a rapid heating furnace, setting a program to heat to a certain temperature and keep the temperature for a period of time, heating to another temperature again and keeping the temperature for a period of time, and naturally cooling to obtain a yellow product, namely S-C3N4。
(3) A certain amount of S-C3N4Adding into secondary distilled water, stirring and dispersing. Then weighing a certain amount of copper sulfate pentahydrate and thioacetamide, and adding into the solution step by step under the condition of stirring.
(4) Stirring, transferring to a reaction kettle with polytetrafluoroethylene lining, keeping the temperature in an oven at a certain temperature for a certain period of time, naturally cooling, washing for 3 times, and vacuum drying at a certain temperature for a certain period of timeObtaining yellow green powder which is CuS/S-C3N4A composite material.
Preferably, the adding amount of the urea in the step (1) is 5-40 g, the adding amount of the water is 10-100 ml, the adding amount of the thioacetamide is 5-180 mg, and the stirring temperature is 20-60 ℃.
Preferably, in the step (2), the first temperature programming is performed at a temperature setting rate of 5-30 ℃/min, a temperature keeping temperature of 200-; the second temperature programming is carried out with the temperature-raising rate set to be 2-25 ℃/min, the heat-preservation temperature set to be 250-650 ℃ and the heat-preservation time set to be 0.5-3 h.
Preferably, S-C in said step (3)3N4The dosage of the compound is 500-4000 mg, the dosage of the blue copperas is 30-200 mg, and the dosage of the thioacetamide is 45-300 mg.
Preferably, in the step (4), the reaction kettle is dried in a vacuum drying oven at the temperature of 100 ℃ and 300 ℃ for 5-20 h, washed with water and ethanol, and dried in the vacuum drying oven at the temperature of 60 ℃ for 8 h.
Compared with the prior art, the invention has the following outstanding advantages: 1. the near-infrared light response heterojunction composite photocatalyst CuS/S-C prepared by the technical scheme of the invention3N4CuS is loaded at S-C3N4After the method is adopted, the separation efficiency of photo-generated electrons and holes is improved, the utilization efficiency of visible light is improved, and the photoresponse capability of the photo-generated electrons and holes in a near infrared light region is expanded, so that CuS/S-C3N4Has light response capability in the visible light to near infrared light region. 2. The method has the advantages of simple preparation and low cost, can effectively improve the absorption of visible light and near infrared light, realizes the efficient degradation of organic pollutants in a wide spectral range, and has important significance for photocatalytic degradation of pollutants.
Drawings
FIG. 1 is an XRD pattern of a sample prepared by the method of the present invention.
FIG. 2 is a diffuse reflectance plot of a sample prepared by the method of the present invention.
FIG. 3 is a graph showing the degradation rate of Tetracycline (TC) under visible light for samples prepared by the method of the present invention.
FIG. 4 is a graph showing the degradation rate of Tetracycline (TC) under visible light and near-infrared light in a sample prepared by the method of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in order to make the advantages and features of the present invention more comprehensible to those skilled in the art, and to clearly define the scope of the present invention.
Example one
Near-infrared light response CuS/S-C3N4The preparation method of the heterojunction nano composite material comprises the following preparation steps:
(1) 10 g of urea is weighed out and dissolved in 15 ml of secondary distilled water at 50 ℃ under stirring, after full dissolution, 100mg of thioacetamide is added and stirring is continued until complete dissolution.
(2) Transferring the mixed solution obtained in the step (1) into a semi-sealed crucible and then sending the semi-sealed crucible into a rapid heating furnace, setting a program to heat from room temperature to 300 ℃ at a speed of 10 ℃/min and keeping the temperature for 0.5 h, then heating to 400 ℃ at a speed of 10 ℃/min and keeping the temperature for 1 h, and then naturally cooling to obtain a yellow product, namely S-C3N4。
(3) 1.28 g S-C3N4Adding into 80 ml secondary distilled water, stirring and dispersing evenly. 50 mg of copper sulfate pentahydrate and 100mg of thioacetamide were weighed out and added to the above solution stepwise with stirring.
(4) Stirring thoroughly, transferring into a reaction kettle with polytetrafluoroethylene lining, keeping the temperature in an oven at 150 deg.C for 5 h, naturally cooling, washing for 3 times, and vacuum drying at 60 deg.C for 8 h to obtain yellowish green powder as CuS/S-C3N4A composite material.
Example two
Near-infrared light response CuS/S-C3N4The preparation method of the heterojunction nano composite material comprises the following preparation steps:
(1) 15 g of urea is weighed out and dissolved in 20 ml of redistilled water under stirring at 50 ℃, after full dissolution, 150 mg of thioacetamide is added and stirring is continued until complete dissolution.
(2) Transferring the mixed solution obtained in the step (1) into a semi-sealed crucible and then sending the mixed solution into a rapid heating furnace, setting a program to heat up from room temperature to 400 ℃ at a speed of 15 ℃/min and preserving heat for 1 h, heating up to 500 ℃ at a speed of 15 ℃/min twice and preserving heat for 2 h, and naturally cooling to obtain a yellow product, namely S-C3N4。
(3) 2.28 g S-C3N4Adding into 80 ml secondary distilled water, stirring and dispersing evenly. 75 mg of copper sulfate pentahydrate and 115 mg of thioacetamide were weighed out and added to the above solution stepwise with stirring.
(4) Stirring thoroughly, transferring into a reaction kettle with polytetrafluoroethylene lining, keeping the temperature in an oven at 180 deg.C for 8 h, naturally cooling, washing for 3 times, and vacuum drying at 60 deg.C for 8 h to obtain yellowish green powder as CuS/S-C3N4A composite material.
EXAMPLE III
Near-infrared light response CuS/S-C3N4The preparation method of the heterojunction nano composite material comprises the following preparation steps:
(1) 20 g of urea is weighed out and dissolved in 30 ml of secondary distilled water at 50 ℃ with stirring, after complete dissolution, 180 mg of thioacetamide is added and stirring is continued until complete dissolution.
(2) Transferring the mixed solution obtained in the step (1) into a semi-sealed crucible and then sending the semi-sealed crucible into a rapid heating furnace, setting a program to heat up from room temperature to 500 ℃ at a speed of 20 ℃/min for 2 h, heating up to 600 ℃ at a speed of 20 ℃/min for two times, keeping the temperature for 3 h, and naturally cooling to obtain a yellow product, namely S-C3N4。
(3) 3.28 g S-C3N4Adding into 80 ml secondary distilled water, stirring and dispersing evenly. 100mg of copper sulfate pentahydrate and 150 mg of thioacetamide were weighed out and added to the above solution stepwise with stirring.
(4) Stirring thoroughly, transferring into a reaction kettle with polytetrafluoroethylene lining, keeping the temperature in an oven at 200 deg.C for 10 h, naturally cooling, washing for 3 times, and vacuum drying at 60 deg.C for 8 h to obtain yellowish green powderThe powder is CuS/S-C3N4A composite material.
FIG. 1 shows a near-infrared light response CuS/S-C prepared by the method of the present invention3N4Heterojunction nanocomposite sample and CuS, S-C3N4XRD contrast pattern of (a).
FIG. 2 shows a near-infrared light response CuS/S-C prepared by the method of the present invention3N4Heterojunction nano composite material sample with different solubility and CuS and S-C3N4Diffuse reflectance contrast plot of (1).
As can be seen from FIGS. 1 and 2, CuS/S-C was successfully synthesized3N4The nano composite material has better near infrared light response performance.
Photocatalytic Performance test
The technical scheme is adopted to respond the prepared near infrared light CuS/S-C3N4Carrying out photocatalytic performance test on the heterojunction nano composite material, preparing a TC solution with the concentration of 50 mg/l, and responding 100mg of near infrared light to the heterojunction composite photocatalyst CuS/S-C3N4Adding into 100 ml TC solution, standing in dark place, reaching adsorption-desorption balance within 30 min, performing photocatalytic experiment under 300W full spectrum light source, controlling incident light wavelength by filter plate, selecting visible light and near infrared light, sampling every 10-15 min, and performing photocatalytic degradation performance test.
FIG. 3 shows a near-infrared light response CuS/S-C prepared by the method of the present invention3N4Heterojunction nano composite material sample with different concentrations and CuS and S-C3N4Graph of the degradation rate of Tetracycline (TC) under visible light.
FIG. 4 shows a near-infrared light response CuS/S-C prepared by the method of the present invention3N4Heterojunction nano composite material sample with different concentrations and CuS and S-C3N4Graph of the degradation rate of Tetracycline (TC) under visible and near infrared light.
As can be seen from FIGS. 3 and 4, 2% of CuS/S-C3N4The sample has better visible and near infrared light catalytic degradation TC performance, wherein the photocatalytic degradation TC performance under visible and near infrared light is more pure than that under visible and near infrared lightThe performance under visible light is better.
Without being limited thereto, any changes or substitutions that are not thought of through the inventive work should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (5)
1. Near-infrared light response CuS/S-C3N4The preparation method of the heterojunction nano composite material is characterized by comprising the following steps: by hydrothermal method in S-C3N4The surface of the substrate grows CuS in situ to obtain CuS/S-C3N4Compared with S-C, the composite material has the activity of degrading organic matters through photocatalysis3N4Has great promotion with CuS and expands S-C3N4Light response in the visible and near infrared regions; the specific preparation process comprises the following steps:
(1) weighing a certain amount of urea, stirring and dissolving the urea in a certain amount of secondary distilled water at a constant temperature, adding a certain amount of thioacetamide, and continuously stirring until the thioacetamide is completely dissolved after the urea is fully dissolved;
(2) transferring the mixed solution obtained in the step (1) into a semi-sealed crucible and then sending the mixed solution into a rapid heating furnace, setting a program to heat to a certain temperature and keep the temperature for a period of time, heating to another temperature again and keeping the temperature for a period of time, and naturally cooling to obtain a yellow product, namely S-C3N4；
(3) A certain amount of S-C3N4Adding into secondary distilled water, stirring and dispersing uniformly; weighing a certain amount of copper sulfate pentahydrate (CuSO)4▪5H2O) and thioacetamide are added into the solution step by step under the stirring condition, the solution is transferred into a reaction kettle with a polytetrafluoroethylene lining after being fully stirred, the solution is kept warm for a period of time at a certain temperature in a drying oven, the solution is washed for 3 times after being naturally cooled, and the solution is dried in vacuum for a period of time at a certain temperature to obtain yellow green powder which is CuS/S-C3N4A composite material.
2. The near-infrared light-responsive CuS/S-C of claim 13N4The preparation method of the heterojunction nano composite material is characterized by comprising the following steps: in the step (1), the dosage of urea is 5-40 g, the dosage of thioacetamide is 5-180 mg, and the stirring temperature is 20-60 ℃.
3. The near-infrared light-responsive CuS/S-C of claim 13N4The preparation method of the heterojunction nano composite material is characterized by comprising the following steps: in the step (2), the temperature rise rate is set to be 5-30 ℃/min for the first time of temperature programming, the heat preservation temperature is set to be 200-600 ℃, and the heat preservation time is 0.5-3 h; the second temperature programming is carried out with the temperature-raising rate set to be 2-25 ℃/min, the heat-preservation temperature set to be 250-650 ℃ and the heat-preservation time set to be 0.5-3 h.
4. The near-infrared light-responsive CuS/S-C of claim 13N4The preparation method of the heterojunction nano composite material is characterized by comprising the following steps: S-C in the step (3)3N4The dosage of the compound is 500-4000 mg, the dosage of the blue copperas is 30-200 mg, and the dosage of the thioacetamide is 45-300 mg.
5. The near-infrared light-responsive CuS/S-C of claim 13N4The preparation method of the heterojunction nano composite material is characterized by comprising the following steps: and (3) keeping the temperature of the reaction kettle in an oven at 100-300 ℃ for 5-20 h, washing with water and ethanol, and drying in a vacuum drying oven at 60 ℃ for 1-8 h.
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