CN113101977B - Preparation method and application of visible light response composite photocatalyst - Google Patents
Preparation method and application of visible light response composite photocatalyst Download PDFInfo
- Publication number
- CN113101977B CN113101977B CN202110322081.7A CN202110322081A CN113101977B CN 113101977 B CN113101977 B CN 113101977B CN 202110322081 A CN202110322081 A CN 202110322081A CN 113101977 B CN113101977 B CN 113101977B
- Authority
- CN
- China
- Prior art keywords
- visible light
- composite photocatalyst
- reaction
- preparation
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 230000004298 light response Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000013110 organic ligand Substances 0.000 claims abstract description 18
- 239000012043 crude product Substances 0.000 claims abstract description 14
- 230000015556 catabolic process Effects 0.000 claims abstract description 13
- 238000006731 degradation reaction Methods 0.000 claims abstract description 13
- 238000004729 solvothermal method Methods 0.000 claims abstract description 11
- 150000002505 iron Chemical class 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 9
- 239000002351 wastewater Substances 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 5
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 31
- 229910052742 iron Inorganic materials 0.000 abstract description 15
- 239000003446 ligand Substances 0.000 abstract description 11
- 239000003054 catalyst Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000011068 loading method Methods 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 21
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 14
- KHLVKKOJDHCJMG-QDBORUFSSA-L indigo carmine Chemical compound [Na+].[Na+].N/1C2=CC=C(S([O-])(=O)=O)C=C2C(=O)C\1=C1/NC2=CC=C(S(=O)(=O)[O-])C=C2C1=O KHLVKKOJDHCJMG-QDBORUFSSA-L 0.000 description 8
- 229960003988 indigo carmine Drugs 0.000 description 8
- 235000012738 indigotine Nutrition 0.000 description 8
- 239000004179 indigotine Substances 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000000593 degrading effect Effects 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- AVJBQMXODCVJCJ-UHFFFAOYSA-M 1,3-bis[2,6-di(propan-2-yl)phenyl]imidazol-1-ium;chloride Chemical compound [Cl-].CC(C)C1=CC=CC(C(C)C)=C1N1C=[N+](C=2C(=CC=CC=2C(C)C)C(C)C)C=C1 AVJBQMXODCVJCJ-UHFFFAOYSA-M 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 235000006694 eating habits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Images
Classifications
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2265—Carbenes or carbynes, i.e.(image)
- B01J31/2269—Heterocyclic carbenes
- B01J31/2273—Heterocyclic carbenes with only nitrogen as heteroatomic ring members, e.g. 1,3-diarylimidazoline-2-ylidenes
-
- 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
-
- 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
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0225—Complexes comprising pentahapto-cyclopentadienyl analogues
- B01J2531/0233—Aza-Cp ligands, i.e. [CnN(5-n)Rn]- in which n is 0-4 and R is H or hydrocarbyl, or analogous condensed ring systems
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/842—Iron
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of photocatalysis, in particular to a preparation method and application of a visible light response composite photocatalyst, which comprises the following steps: (1) adding iron salt and an organic ligand into an organic solvent under the protection of inert gas to obtain a reaction solution; (2) carrying out solvothermal reaction on the reaction solution in an oxygen-free environment, and centrifuging after the reaction is finished to obtain a crude product; (3) and washing the crude product, and drying in vacuum to obtain the visible light response composite photocatalyst. The preparation method is simple to operate, easy to control conditions and easy to industrialize; by loading a specific organic ligand (ligand A), the photoresponse range of the iron-based catalyst is expanded, so that the iron-based catalyst can be excited by visible light, and the efficient degradation of the dye under the visible light is realized.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to a preparation method and application of a visible light response composite photocatalyst.
Background
The organic dye is an important chemical product and is closely related to human clothes and eating habits. But with the rapid development of the dye industry, The produced organic wastewater also becomes one of water pollution sources. Methyl orange and indigo carmine are common water pollutants, and common treatment methods comprise physical adsorption, an electrochemical oxidation method and a membrane filtration method, but the methods have low degradation efficiency and high energy consumption and can cause secondary pollution, and photodegradation has the advantages of utilization of solar energy, cleanness, high efficiency and the like. Usually TiO 2 、WO 3 And the semiconductor photocatalyst has low sunlight utilization efficiency and high price.
The iron element is rich in source, cheap and nontoxic, and the iron-based photocatalyst has a narrow forbidden band width and has better light absorption and excitation characteristics compared with other metals. Chinese patent literature discloses 'application of iron-based composite photocatalyst in burst decomposition of low-concentration dye wastewater', and application publication number of the application is CN 110818013A, the invention takes iron-based oxide as a matrix, and the iron-based oxide is reacted with g-C 3 N 4 And Ce is loaded by means of intermolecular interaction force, the forbidden bandwidth of the iron-based catalyst is widened by the loading ligand, the photoresponse range of the iron-based catalyst to visible light is expanded, the iron-based catalyst can be excited by the visible light, and efficient visible light response is realized. However, the iron-based composite photocatalyst is only used for degrading low-concentration dye wastewater, and has low degradation efficiency on high-concentration dye wastewater.
Disclosure of Invention
The invention provides a preparation method of a visible-light response composite photocatalyst in order to overcome the problems in the prior art, and the preparation method is simple to operate, easy to control conditions and easy to industrialize.
The invention also provides application of the visible light response composite photocatalyst prepared by the preparation method in degradation of dye wastewater.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a visible light response composite photocatalyst comprises the following steps:
(1) adding iron salt and an organic ligand into an organic solvent under the protection of inert gas to obtain a reaction solution;
(2) carrying out solvothermal reaction on the reaction solution in an oxygen-free environment, and centrifuging after the reaction is finished to obtain a crude product;
(3) washing the crude product, and drying in vacuum to obtain the visible light response composite photocatalyst;
in the step (1), the structural formula of the organic ligand (ligand A) is as follows:
according to the invention, a specific organic ligand (ligand A) is loaded, so that the photoresponse range of the iron-based catalyst is expanded, the iron-based catalyst can be excited by visible light, and the efficient degradation of the dye under the visible light is realized. The specific mechanism is as follows: the electron donating ability of Nitrogen Heterocyclic Carbene (NHC) is combined with the photocatalysis ability of the iron-based catalyst. The composite photocatalyst can be fully excited by light to generate electron-hole pairs, and lone electrons on NHC can be rapidly compounded with holes, so that the service life of photo-generated electrons is prolonged, and the photocatalytic efficiency is improved.
Preferably, in the step (1), the iron salt is one selected from iron oxide, a hydrate of iron oxide, iron sulfate and a hydrate of iron sulfate.
Preferably, in step (1), the organic solvent consists of N-N dimethylformamide and ethanol in a volume ratio of 1: 1. The organic solvent combination has the effects of easily dissolving ferric salt and ligand and promoting crystallization.
Preferably, in step (1), the organic solvent consists of N-N dimethylformamide and ethanol in a volume ratio of 1: 1.
Preferably, in the step (1), the concentration of the organic ligand in the reaction solution is 0.01 to 1 mol/L.
Preferably, in the step (2), the temperature of the solvothermal reaction is 175-210 ℃, and the reaction time is 12-20 h.
Preferably, in the step (3), washing is performed 3-5 times by sequentially adopting N-N dimethylformamide and ethanol.
Preferably, in the step (3), the vacuum drying temperature is 75-85 ℃ and the time is 5-10 h.
An application of a visible light response composite photocatalyst in degradation of dye wastewater.
Preferably, the concentration of the dye wastewater is 5-20 mg/L, and the dosage of the visible light response composite photocatalyst is 0.005-1 mg/mL.
Therefore, the invention has the following beneficial effects:
(1) The preparation method is simple to operate, easy to control conditions and easy to industrialize;
(2) by loading a specific organic ligand (ligand A), the photoresponse range of the iron-based catalyst is expanded, so that the iron-based catalyst can be excited by visible light, and the efficient degradation of the dye under the visible light is realized.
Drawings
FIG. 1 is a UV diffuse reflectance spectrum of the visible-light-responsive composite photocatalyst prepared in example 1.
FIG. 2 is a graph showing the degradation curves of the visible light response composite photocatalyst prepared in example 1 for methyl orange solution (MO) and indigo carmine solution (IC).
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
The synthesis method of the organic ligand (ligand A) comprises the following steps:
potassium tert-butoxide (4.60g,41.0mmol) was added in portions to a solution of 1, 3-bis (2, 6-diisopropylphenyl) imidazolium chloride (15.5g,36.4mmol) in THF (185 mL). After the reaction mixture was stirred at 238 ℃ for 2h, all volatiles were removed in vacuo and the residue was extracted with hot toluene (2X 40mL) and filtered through celite. Toluene was removed by rotary evaporation to give a pale yellow solid, which was designated ligand A.
Example 1
(1) In an argon glove box, mixing iron salt and an organic ligand (ligand A) according to a mass ratio of 2: 1, adding into a mixed solution containing DMF and EtOH (V: V ═ 1:1) to obtain a reaction solution, wherein the concentration of an organic ligand in the reaction solution is 0.01 mol/L;
(2) transferring the reaction solution to a reaction kettle in an oxygen-free environment for solvothermal reaction, wherein the solvothermal reaction temperature is 200 ℃, the reaction time is 15 hours, and centrifuging after the reaction is finished to obtain a crude product;
(3) and washing the crude product by sequentially adopting N-N dimethylformamide and ethanol for 3 times, and drying the crude product in vacuum at the temperature of 80 ℃ for 8 hours to obtain the visible light response composite photocatalyst.
The ultraviolet diffuse reflection characterization is performed on the visible-light-responsive composite photocatalyst prepared in the example, and the result is shown in fig. 1, and it can be seen that the forbidden bandwidth Eg of the visible-light-responsive composite photocatalyst is 1.99eV, which indicates that the visible-light-responsive composite photocatalyst has visible-light-responsive performance.
The visible-light-responsive composite photocatalyst prepared in the example is used for respectively degrading methyl orange solution (MO) and indigo carmine solution (IC) under the irradiation of visible light (the light source is a Newport 3A-level solar simulator). The volume of each dye is 20ml, the concentration is 10mg/L, the dosage of the visible light response composite photocatalyst is 10mg, and the visible light catalytic degradation curve graph is shown in figure 2.
As can be seen from FIG. 2, the degradation rates after 60min for methyl orange solution (MO) and indigo carmine solution (IC) were 98% and 99%, respectively.
Example 2
(1) In an argon glove box, mixing iron salt and an organic ligand (ligand A) according to a mass ratio of 3: 1, adding the mixture into a mixed solution containing DMF and EtOH (V: V ═ 1:1) to obtain a reaction solution, wherein the concentration of an organic ligand in the reaction solution is 1 mol/L;
(2) transferring the reaction solution to a reaction kettle in an oxygen-free environment for solvothermal reaction, wherein the temperature of the solvothermal reaction is 175 ℃, the reaction time is 12 hours, and centrifuging after the reaction is finished to obtain a crude product;
(3) and washing the crude product by sequentially adopting N-N dimethylformamide and ethanol for 5 times, and drying at 85 ℃ for 5 hours in vacuum to obtain the visible light response composite photocatalyst.
The visible-light-responsive composite photocatalyst prepared in the example is used for respectively degrading methyl orange solution (MO) and indigo carmine solution (IC) under the irradiation of visible light (the light source is a Newport 3A-level solar simulator). The volume of each dye is 20ml, the concentration is 5mg/L, the dosage of the visible light response composite photocatalyst is 20mg, and the degradation rate of the methyl orange solution (MO) and the indigo carmine solution (IC) after 60min is 98.2% and 99.7% respectively.
Example 3
(1) In an argon glove box, iron salt and an organic ligand (ligand A) are mixed according to a mass ratio of 2.5: 1, adding into a mixed solution containing DMF and EtOH (V: V ═ 1:1) to obtain a reaction solution, wherein the concentration of an organic ligand in the reaction solution is 0.5 mol/L;
(2) transferring the reaction solution to a reaction kettle in an oxygen-free environment for solvothermal reaction, wherein the solvothermal reaction temperature is 210 ℃, the reaction time is 12 hours, and centrifuging after the reaction is finished to obtain a crude product;
(3) and washing the crude product by sequentially adopting N-N dimethylformamide and ethanol for 4 times, and drying the crude product in vacuum at 75 ℃ for 10 hours to obtain the visible light response composite photocatalyst.
The visible-light-responsive composite photocatalyst prepared in the example is used for respectively degrading methyl orange solution (MO) and indigo carmine solution (IC) under the irradiation of visible light (the light source is a Newport 3A-level solar simulator). The volume of each dye is 20ml, the concentration is 20mg/L, the dosage of the visible light response composite photocatalyst is 0.1mg, and the degradation rate of the methyl orange solution (MO) and the indigo carmine solution (IC) after 60min is 95.9% and 97.5% respectively.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (8)
1. The preparation method of the visible light response composite photocatalyst is characterized by comprising the following steps of:
(1) adding iron salt and an organic ligand into an organic solvent under the protection of inert gas to obtain a reaction solution;
(2) carrying out solvothermal reaction on the reaction solution in an oxygen-free environment, wherein the temperature of the solvothermal reaction is 175-210 ℃, the reaction time is 12-20 h, and the mass ratio of the iron salt to the organic ligand is (2-3): 1, centrifuging after the reaction is finished to obtain a crude product;
(3) washing the crude product, and drying in vacuum to obtain the visible light response composite photocatalyst;
in the step (1), the structural formula of the organic ligand is as follows:
2. the method according to claim 1, wherein in the step (1), the iron salt is one selected from iron sulfate and a hydrate of iron sulfate.
3. The method according to claim 1, wherein in the step (1), the organic solvent is composed of N-N dimethylformamide and ethanol in a volume ratio of 1: 1.
4. The method according to claim 1, wherein in the step (1), the concentration of the organic ligand in the reaction solution is 0.01 to 1 mol/L.
5. The method according to claim 1, wherein in the step (3), the washing is performed 3 to 5 times by using N-N dimethylformamide and ethanol in this order.
6. The preparation method according to claim 1, wherein in the step (3), the vacuum drying temperature is 75-85 ℃ and the time is 5-10 h.
7. Use of the visible-light-responsive composite photocatalyst prepared by the preparation method as claimed in any one of claims 1 to 6 in degradation of dye wastewater.
8. The application of claim 7, wherein the concentration of the dye wastewater is 5-20 mg/L, and the dosage of the visible-light-responsive composite photocatalyst is 0.005-1 mg/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110322081.7A CN113101977B (en) | 2021-03-25 | 2021-03-25 | Preparation method and application of visible light response composite photocatalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110322081.7A CN113101977B (en) | 2021-03-25 | 2021-03-25 | Preparation method and application of visible light response composite photocatalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113101977A CN113101977A (en) | 2021-07-13 |
| CN113101977B true CN113101977B (en) | 2022-07-29 |
Family
ID=76712182
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110322081.7A Active CN113101977B (en) | 2021-03-25 | 2021-03-25 | Preparation method and application of visible light response composite photocatalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113101977B (en) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525266B (en) * | 2014-12-30 | 2017-04-12 | 河南理工大学 | Preparation method of metal-organic framework material photocatalyst and application |
| CN105268479B (en) * | 2015-11-10 | 2017-09-05 | 安徽理工大学 | The preparation method of high efficiency photocatalyst based on iron and Phen |
| CN109422620B (en) * | 2017-08-25 | 2021-08-24 | 浙江工业大学 | Method for highly selectively reducing alkyne into Z-type olefin |
| US11103861B2 (en) * | 2017-09-14 | 2021-08-31 | The Board Of Trustees Of The University Of Alabama | Light driven metal pincer photocatalysts for carbon dioxide reduction to carbon monoxide |
| CN108080028B (en) * | 2017-12-22 | 2020-11-03 | 安徽工业大学 | Preparation method of 8-hydroxyquinoline iron organic dye photodegradation catalyst |
| CN109794293B (en) * | 2019-01-24 | 2021-09-21 | 杭州师范大学 | Iron-based photocatalyst and application thereof in degrading rhodamine B |
| CN110449187B (en) * | 2019-07-25 | 2022-07-12 | 中山大学 | Preparation method and application of perovskite-metal complex composite material |
| EP3822281A1 (en) * | 2019-11-18 | 2021-05-19 | Wärnmark, Kenneth | Iron n-heterocyclic carbene compounds |
-
2021
- 2021-03-25 CN CN202110322081.7A patent/CN113101977B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113101977A (en) | 2021-07-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xiao et al. | Synthesis of EDTA-bridged CdS/g-C3N4 heterostructure photocatalyst with enhanced performance for photoredox reactions | |
| Yuan et al. | Visible-light-driven hydrogen production from water in a noble-metal-free system catalyzed by zinc porphyrin sensitized MoS2/ZnO | |
| CN103801294B (en) | A kind of activated carbon-loaded cuprous oxide photocatalyst and method thereof | |
| CN102274739B (en) | Copper-nitrogen double-doped titanium dioxide photocatalytic material | |
| CN104437589B (en) | A kind of silver/graphene oxide/carbonitride composite photocatalyst material and preparation method thereof | |
| CN111453804B (en) | Preparation method of iron-doped graphite-like phase carbon nitride/graphene multifunctional nano composite material | |
| CN101711988B (en) | NaBiO3/BiOCl heterojunction photocatalyst and preparation method thereof | |
| Gao et al. | Novel nitrogen-rich g-C3N4 with adjustable energy band by introducing triazole ring for cefotaxime removal | |
| CN106865685B (en) | Treatment method for photocatalytic degradation of rhodamine B dye wastewater | |
| CN105148983B (en) | Photochemical catalyst of dyestuff and preparation method thereof in a kind of degrading waste water | |
| CN102513135A (en) | BiOI (bismuth oxyiodide)/AgX (silver halide) visible light response photocatalyst, preparation methods for same and application thereof | |
| Essawy et al. | A novel photocatalytic system consists of Co (II) complex@ ZnO exhibits potent antimicrobial activity and efficient solar-induced wastewater remediation | |
| Li et al. | Constructing porous intramolecular donor–acceptor integrated carbon nitride doped with m-aminophenol for boosting photocatalytic degradation and hydrogen evolution activity | |
| Chen et al. | Construction of surface oxygen vacancies by bimetallic doping combined with ellagic acid modification to enhance the photocatalytic degradation of ethinyl estradiol by TiO2 | |
| Tong et al. | Cobalt doped nitrogen-vacancies-rich C3N5 with optimizing local electron distribution boosts peroxymonsulfate activation for tetracycline degradation: Multiple electron transfer mechanisms | |
| Cui et al. | A recyclable photocatalyst Cu2O/Fe3O4@ C/Cu nanocomposite for efficient photocatalytic reduction of 4-nitrophenol | |
| Zhu et al. | Selective oxidation of aniline contaminants via a hydrogen-abstraction pathway by Bi2· 15WO6 under visible light and alkaline conditions | |
| CN113101977B (en) | Preparation method and application of visible light response composite photocatalyst | |
| CN110586141A (en) | Preparation method of Ag-Bi solid solution composite photocatalyst for treating oil field waste liquid | |
| CN108816283B (en) | Metal-loaded composite photocatalyst, and preparation method and application thereof | |
| CN113117752B (en) | Preparation method and application of iron-based photocatalyst | |
| CN110038636B (en) | AgI/Ag-Ce-2MI composite photocatalyst and preparation and application thereof | |
| CN110368926B (en) | Preparation method of double-Bi defect photocatalyst | |
| CN113680363B (en) | Polyethyleneimine doped tremella integrated graphite-phase carbon nitride photocatalyst, preparation method and application thereof | |
| Zhang et al. | Benzotrithiophene-based sp2 carbon-conjugated microporous polymers for green light-triggered oxidation of amines to imines |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |