CN114950488A - Photocatalyst and preparation method thereof - Google Patents
Photocatalyst and preparation method thereof Download PDFInfo
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- CN114950488A CN114950488A CN202210768592.6A CN202210768592A CN114950488A CN 114950488 A CN114950488 A CN 114950488A CN 202210768592 A CN202210768592 A CN 202210768592A CN 114950488 A CN114950488 A CN 114950488A
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- photocatalyst
- thioacetamide
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 12
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 8
- 229910021617 Indium monochloride Inorganic materials 0.000 claims abstract description 5
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 description 15
- 238000006731 degradation reaction Methods 0.000 description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 12
- 229940043267 rhodamine b Drugs 0.000 description 12
- 239000000243 solution Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 125000004122 cyclic group Chemical group 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000012463 white pigment Substances 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a photocatalyst and a preparation method thereof, which adopts cobalt nitrate and InCl 3 And thioacetamide is used as a raw material, the thioacetamide is added into a solution consisting of dimethylformamide and diethylene glycol, and the preparation method comprises the steps of stirring, reacting, centrifuging, drying and the like.
Description
Technical Field
The invention relates to a photocatalyst and a preparation method thereof, in particular to a photocatalyst for degrading rhodamine B and a preparation method thereof.
Background
Due to the rapid development of modern industry, many countries and regions are contaminated with various harmful substances, such as organic compounds, heavy metals, and pharmaceutical antibiotics. These pollutants are generally difficult to degrade by natural means, and cause serious pollution to the environment due to long-term existence, and also have serious influence on life and physical health of people. The photocatalysis technology has the advantages of high efficiency, low cost, no secondary pollution, direct utilization of natural solar energy and the likeThe method is an efficient and economic method for eliminating pollutants in the environment. Scientific researchers adopt a hydrothermal method and an impregnation method to prepare ZnIn with a Z-shaped heterostructure 2 S 4 /MoO 3 The photocatalyst is researched to degrade organic pollutants such as rhodamine B and the like under the irradiation of visible light, and is found to have higher degradation rate. However, the photocatalytic activity of a catalyst depends on its ability to generate photoinduced electron-hole pairs. For pure ZnIn 2 S 4 On the other hand, due to low separation efficiency and poor electron transport capability, effective separation of photoelectron hole pairs is inhibited, resulting in ZnIn 2 S 4 Has poor photocatalytic activity.
Disclosure of Invention
The invention provides a novel photocatalyst and a preparation method thereof, and the photocatalyst can greatly improve the degradation rate of rhodamine B.
The preparation method of the photocatalyst comprises the following steps:
mixing cobalt nitrate and InCl 3 And thioacetamide is added into the solution consisting of the dimethylformamide and the diethylene glycol, stirred to be fully dissolved, poured into a reaction kettle and fully reacted in an oven. And finally, centrifuging the white precipitate, washing with deionized water, and finally, putting the white precipitate into an oven to be completely dried to obtain the white pigment.
The invention also provides a photocatalyst prepared by the preparation method.
The photocatalytic activity of the prepared photocatalyst is evaluated by taking the rhodamine B solution as a probe, and the rhodamine B solution has higher degradation rate and excellent repeated degradation stability.
Drawings
FIG. 1 (a) degradation curve of photocatalyst prepared according to the present invention (b) kinetic curve
FIG. 2 is a schematic diagram showing the change of 4-cycle degradation performance of the photocatalyst prepared by the present invention
Detailed Description
Embodiments for carrying out the present invention will be described in detail with reference to the accompanying drawings. The present invention is not limited to the contents described in the following examples. The components described below include substantially the same components as can be easily conceived by those skilled in the art. The method steps described below can be combined as appropriate. Various omissions, substitutions, and changes in the method steps can be made without departing from the spirit of the invention.
A process for preparing photocatalyst includes such steps as mixing cobalt nitrate with InCl 3 And adding thioacetamide into a solution consisting of dimethylformamide and diethylene glycol, stirring to fully dissolve the thioacetamide, pouring the thioacetamide into a reaction kettle, fully reacting the thioacetamide and the diethylene glycol in an oven, finally centrifuging the white precipitate, washing the white precipitate with deionized water, and completely drying the white precipitate in the oven to obtain the compound.
Preferably, the cobalt nitrate or InCl is 3 And thioacetamide in a molar ratio of 1:2: 4.
Preferably, the stirring time is 20 to 40 minutes.
Preferably, the temperature for carrying out the reaction in the oven is set to be 160-200 ℃, and the reaction time is 8-12 h.
Preferably, the temperature at which the white precipitate is placed in an oven for drying is set at 60-100 ℃.
Preferably, the white precipitate is washed with deionized water and then with ethanol.
Preferably, the raw material for preparing the photocatalyst also comprises cerium nitrate.
Preferably, the content ratio of the cobalt nitrate to the cerium nitrate is 1 mol: 10-50 g.
Another aspect of the present invention is to provide a photocatalyst prepared by the above preparation method. Wherein the chemical formula of the photocatalyst without adding cerium nitrate is CoIn 2 S 4 The chemical formula of the photocatalyst added with cerium nitrate is Ce/CoIn 2 S 4 。
The photocatalyst prepared by the invention has the following catalytic activity test:
in the photocatalytic degradation experiment, a 500W mercury lamp is used as a light source for photocatalytic degradation, a rhodamine B solution is used as a probe, and the photocatalytic activity of the photocatalyst is judged by detecting the degradation of the photocatalyst on rhodamine B under the irradiation of ultraviolet light. The specific process of the experiment is as follows: 0.1g of photocatalyst is dispersed in 100 mL of rhodamine B solution (15mg/L), stirred for 30min in the dark state, and then a light source is turned on to carry out a photocatalytic degradation experiment. In the process of the photocatalytic reaction, 5mL of reaction liquid is taken out of the reactor every 10 min, then the photocatalyst in the reaction liquid is removed by a centrifuge, and the residual concentration of rhodamine B in the solution is measured by a spectrophotometer.
Before starting the photocatalytic degradation experiment, in order to avoid the reduction of the rhodamine B content in the solution due to the adsorption effect of the photocatalyst, the mixed solution is stirred for 30 minutes in the dark state, and then the light source is started to carry out the photocatalytic degradation experiment. As can be seen from FIG. 1 (a), after 30min of dark reaction, CoIn 2 S 4 ，Ce/CoIn 2 S 4 (5)，Ce/CoIn 2 S 4 (10) And Ce/CoIn 2 S 4 (20) (Note: the values 5, 10, and 20 in the parentheses indicate that the amounts of cerium nitrate were 5g, 10g, and 20g, respectively, when the amount of cobalt nitrate was 0.4mol, respectively), the absorbances of rhodamine B were 69.17%, 67.94%, 66.02%, and 63.24%, respectively. Then, the ultraviolet lamp is turned on to perform the photodegradation reaction. After 60min of UV irradiation, CoIn 2 S 4 ，Ce/CoIn 2 S 4 (5)，Ce/CoIn 2 S 4 (10) And Ce/CoIn 2 S 4 (20) The degradation rates of rhodamine B are 91.76%, 95.15%, 98.55% and 93.62% respectively. Ce/CoIn 2 S 4 (10) Shows the optimal degradation rate, and FIG. 1 (b) is the corresponding kinetic curve chart, from which it can be seen that CoIn 2 S 4 ，Ce/CoIn 2 S 4 (5)，Ce/CoIn 2 S 4 (10) And Ce/CoIn 2 S 4 (20) The kinetic curve constants of (A) are respectively 0.021, 0.026, 0.046 and 0.024 min -1 。Ce/CoIn 2 S 4 (10) The degradation rate of (a) is maximized. As can be seen, Ce/CoIn 2 S 4 (10) Has the strongest photocatalytic activity.
Cyclic degradation stability experiments:
FIG. 2 is Ce/CoIn 2 S 4 (10) Four times of cyclic degradation of the photocatalyst. After 4 times of cyclic degradation, Ce/CoIn 2 S 4 (10) The degradation rate of the catalyst is only reduced by about 2.41 percent. Probably due to the Ce/CoIn in the experiment 2 S 4 (10) The loss of the photocatalyst results in a decrease in the degradation rate. From this, it can be confirmed that Ce/CoIn 2 S 4 (10) The photocatalyst has good stability.
The present invention is not limited to the above embodiments. That is, the present invention can be implemented without departing from the scope of the present invention
Various modifications are made.
Claims (8)
1. A preparation method of a photocatalyst, cobalt nitrate and InCl are added 3 And adding thioacetamide into a solution consisting of dimethylformamide and diethylene glycol, stirring to fully dissolve the thioacetamide, pouring the thioacetamide into a reaction kettle, fully reacting the thioacetamide and the diethylene glycol in an oven, centrifuging the white precipitate, washing the white precipitate with deionized water, and completely drying the white precipitate in the oven to obtain the compound.
2. The method of claim 1, wherein the photocatalyst further comprises cerium nitrate as a raw material.
3. The method for preparing photocatalyst as claimed in claim 1, wherein the temperature for the reaction in the oven is set at 160-200 ℃ and the reaction time is 8-12 h.
4. The method for preparing a photocatalyst as claimed in claim 1, wherein the temperature at which the white precipitate is dried in an oven is set to 60 to 100 ℃.
5. The method of claim 1, wherein the white precipitate is washed with deionized water and then with ethanol.
6. The method of claim 1, wherein the raw material for preparing the photocatalyst further comprises cerium nitrate.
7. The method for preparing a photocatalyst according to claim 1, wherein the content ratio of cobalt nitrate to cerium nitrate is 1 mol: 10-50 g.
8. A photocatalyst produced by the production method described in any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210768592.6A CN114950488A (en) | 2022-07-01 | 2022-07-01 | Photocatalyst and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210768592.6A CN114950488A (en) | 2022-07-01 | 2022-07-01 | Photocatalyst and preparation method thereof |
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| CN114950488A true CN114950488A (en) | 2022-08-30 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2021100865A4 (en) * | 2021-02-12 | 2021-04-22 | Guangdong University Of Technology | Preparation and application of a series non-copper catalyst for preparing methane by electrocatalytic carbon dioxide |
| CN113078416A (en) * | 2021-03-22 | 2021-07-06 | 电子科技大学 | Nano flower-shaped CoIn2S4Granule/graphite alkene complex modification's diaphragm |
| CN113841557A (en) * | 2021-03-17 | 2021-12-28 | 丽水市农林科学研究院 | Method for increasing content of coumarins in chimonanthus salicifolius |
| CN114534745A (en) * | 2022-01-29 | 2022-05-27 | 武汉理工大学 | Zero-dimensional cerium oxide/three-dimensional porous calcium indium sulfide composite nano material and preparation method and application thereof |
-
2022
- 2022-07-01 CN CN202210768592.6A patent/CN114950488A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2021100865A4 (en) * | 2021-02-12 | 2021-04-22 | Guangdong University Of Technology | Preparation and application of a series non-copper catalyst for preparing methane by electrocatalytic carbon dioxide |
| CN113841557A (en) * | 2021-03-17 | 2021-12-28 | 丽水市农林科学研究院 | Method for increasing content of coumarins in chimonanthus salicifolius |
| CN113078416A (en) * | 2021-03-22 | 2021-07-06 | 电子科技大学 | Nano flower-shaped CoIn2S4Granule/graphite alkene complex modification's diaphragm |
| CN114534745A (en) * | 2022-01-29 | 2022-05-27 | 武汉理工大学 | Zero-dimensional cerium oxide/three-dimensional porous calcium indium sulfide composite nano material and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| FEI TIAN ET AL.: "Improving photocatalytic activity for hydrogen evolution over ZnIn2S4 under visible-light: A case study of rare earth modification", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》, vol. 39, pages 6335 - 6344, XP028835566, DOI: 10.1016/j.ijhydene.2014.01.188 * |
| 孙娟娟: "尖晶石型复合硫化物的制备与性能研究", 《万方数据》, pages 1 - 49 * |
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