CN112371147A - Fe3O4Quantum dot modified Bi2O4/g-C3N4Preparation method and application of composite photocatalyst - Google Patents
Fe3O4Quantum dot modified Bi2O4/g-C3N4Preparation method and application of composite photocatalyst Download PDFInfo
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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
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- B01J35/33—
-
- 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
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the technical field of preparation of environmental materials, and relates to Fe3O4Quantum dot modified Bi2O4/g‑C3N4A preparation method and application of the composite photocatalyst; the method comprises the following steps: first of all, g-C3N4Nanosheets and Bi/CN; then dissolving the Bi/CN photocatalyst in deionized water, and adding FeCl3·6H2O and FeCl2·4H2O, stirring at 60-80 ℃, and thenDropping NH3·H2O, stirring again; after stirring, collecting a sample by using a magnet, washing by using deionized water and ethanol, and drying to obtain a composite photocatalyst; the invention uses g-C3N4And Bi2O4Visible light is used as excitation, and through the interaction with the interface of organic pollutant molecules, surrounding oxygen and water molecules are excited into free negative ions with strong oxidizing power, so that the aim of degrading harmful organic substances is fulfilled, and the method is a green, environment-friendly, efficient and stable treatment technology.
Description
Technical Field
The invention belongs to the technical field of preparation of environmental materials, and particularly relates to Fe3O4Quantum dot modified Bi2O4/g-C3N4A preparation method and application of the composite photocatalyst.
Background
In this year, the deterioration of environmental quality is a serious concern in the imbalance of ecological balance internationally, and human beings are facing the most serious environmental crisis from history. Among the environmental pollution, the majority is directly related to the pollution of industrial and industrial products. The dye wastewater is one of the main harmful industrial wastewater, and mainly comes from the dye and dye intermediate production industry. The dye has various types, brings bright and colorful colors for the life of people and generates great economic benefit, but also generates a great amount of dye wastewater to be discharged into environmental water, thus causing pollution to natural water. The main hazards are as follows:
(1) the dye in the chromaticity wastewater of the dye can absorb light, reduce the transparency of a water body, consume a large amount of oxygen in the water, cause the oxygen deficiency of the water body, influence the growth of aquatic organisms and microorganisms, destroy the self-purification of the water body, and easily cause visual pollution. (2) The dye is aromatic halide, aromatic nitro compound, aromatic amine chemical, biphenyl and other polyphenyl ring substituted compounds generated after the hydrogen on the benzene ring of the organic aromatic compound is substituted by halogen, nitro and amino, and has larger biological toxicity, and some are 'three-dimensional' substances. (3) The heavy metal salts such as chromium, lead, mercury, arsenic and zinc in the heavy metal wastewater in the dye cannot be biodegraded, can exist in the natural environment for a long time, and can be continuously transmitted through a food chain to be accumulated in a human body. (4) The waste water has high organic matter content, complex components and high content of harmful substances. In general, materials such as acid, alkali and salt and detergents such as soap are relatively harmless, but have certain influence on the environment. In recent years, a lot of nitrogen and phosphorus containing compounds are used as cleaning agents, and urea is also commonly used in each printing and dyeing process, so that the total phosphorus and the total nitrogen content in the wastewater are increased, and the water body is eutrophicated after the wastewater is discharged. If the dye wastewater is directly discharged without treatment, the dye wastewater will pose a great threat to increasingly tense drinking water sources. The dye that is more common among dyes is rhodamine b (rhodamine b).
The rhodamine B is an artificially synthesized dye with fresh peach red color, and is found through a mouse test that the rhodamine B can cause sarcoma of subcutaneous tissues, is suspected to be a carcinogen, has strong fluorescence in a solution, and can be used as a cell fluorescent coloring agent in experiments, colored glass, special fireworks and crackers and other industries. Although the dye brings gorgeous life to human beings, the harm is not small and varied. Therefore, complete eradication of dyes in the environment has become a significant problem for researchers to urgently need to solve. Currently, the dye processing technology has advanced greatly and many methods have been developed, such as: physical, chemical, biological, etc., each having advantages and features. However, with these conventional methods for treating dye waste water, there is still usually a certain amount of dye residue discharged into the environment, which is difficult to eradicate completely, with obvious limitations.
Among the numerous sewage treatment methods, the photocatalytic degradation technology emerging in recent years has the advantages of high efficiency, stability, low energy consumption and less secondary pollution, and enters the field of researchers, so that the photocatalytic degradation technology becomes a promising wastewater purification technology at present. Thus, the photocatalytic technology is utilized to mineralize and decompose the difficult-to-degrade dye pollutants into H2O、CO2And other small molecular substances, is expected to become a new high-efficiency energy-saving environmental pollution treatment technology, and is also a research hotspot in the field of current environmental science and technology. The simultaneous improvement of the yield of electron-hole pairs in photocatalytic semiconductors and the acceleration of carrier separation are the key points of research in this technology.
Among the numerous semiconductor photocatalysts, g-C3N4As a novel photocatalytic material, the photocatalyst is stable in chemical property, non-toxic and suitable in band gap (about 2.7 eV). But a single photocatalytic semiconductorThe light absorption of the body is weak, and the defects of easy recombination of carriers, few reactive active sites and the like are possessed. Therefore, a rational design is required to obtain high photocatalytic activity and stability. For example, metal or nonmetal doping, surface organic modification, heterojunction formation and the like are carried out on a semiconductor catalyst, wherein the heterojunction generally consists of two semiconductors and an electronic medium (metal or carbon material), and compared with the original ii-type heterojunction, the z-type heterojunction maintains higher photocarrier redox capability and good photo-corrosion resistance. In addition, the emerging bismuth-based semiconductor bismuth oxide (Bi)2O4) The visible light responsive photocatalytic material has a narrow band gap of about 2.0 eV. Therefore, the two semiconductors with proper band gaps are selected to be compounded to prepare the photocatalyst, so that the carrier separation is accelerated, the specific surface area is increased, and more reactive active sites are provided. However, the conventional powder photocatalyst is not easy to collect and reuse after being dispersed in a solution. Then by introducing the magnetic material ferroferric oxide (Fe)3O4) Thus, the problem is further solved by adopting a convenient and direct magnetic separation process for recovery. In the present discovery application, a magnetic Z-type heterojunction Fe is prepared3O4-QDs/Bi2O4/g-C3N4The preparation of the photocatalyst overcomes the traditional g-C3N4And Bi2O4The above disadvantages of photocatalysts.
Disclosure of Invention
The invention aims to overcome the technical defects in the prior art, solve the problems of easy recombination of a single photocatalyst carrier, low reactive site and the like, and greatly improve the degradation of a pollutant rhodamine B.
The invention is realized by the following technical scheme:
fe synthesis by using calcination method and hydrothermal method as technical means3O4-QQs/Bi2O4/g-C3N4The heterojunction composite photocatalyst is prepared according to the following steps:
step (1), preparation of g-C3N4Nano-flake:
taking out urea, grinding, and calcining for the first time to obtain a sample; subsequently, the sample was ground again to a powder and subjected to secondary calcination to give g-C3N4Nanosheets;
step (2) of preparing Bi2O4/g-C3N4(Bi/CN) photocatalyst:
g-C prepared in the step (1)3N4And NaBiO3Adding the mixture into deionized water, and stirring at room temperature to obtain a mixed solution; then transferring the sample to a polytetrafluoroethylene stainless steel autoclave for reaction and synthesis to obtain a sample, finally cleaning the sample by using deionized water and ethanol, and then putting the sample into a drying oven for drying to obtain Bi2O4/g-C3N4A photocatalyst;
step (3) preparation of Fe3O4-QDs/Bi2O4/g-C3N4(FeQDs/Bi/CN) composite photocatalysts;
firstly, Bi prepared in the step (2)2O4/g-C3N4Dissolving a photocatalyst in deionized water to obtain a solution C; then adding FeCl3·6H2O and FeCl2·4H2O, stirring for the first time at a certain temperature to obtain a mixed solution D; then NH is introduced3·H2O is dripped into the solution D to obtain a solution E, and the solution E is stirred for the second time; collecting sample with magnet, washing with deionized water and ethanol, and drying to obtain Fe3O4-QDs/Bi2O4/g-C3N4A photocatalyst.
Preferably, in the step (1), the two calcinations are performed under the condition of 550 ℃ for 4 hours, and the heating rate is 5 ℃/min.
Preferably, in step (2), said g-C3N4、NaBiO3And deionized water in a ratio of 0.1g to 0.131 g: 60 mL.
Preferably, in the step (2), the reaction synthesis temperature is 160 ℃, and the synthesis time is 8 h.
Preferably, in the step (3), in the C solution, the Bi is2O4/g-C3N4The dosage ratio of the photocatalyst to the deionized water is 0.1g to 20 mL.
Preferably, in the step (3), in the mixed solution D, the deionized water and FeCl3·6H2O、FeCl2·4H2O、NH3·H2The dosage ratio of O is 20 mL: 0.0467g, 0.0172 g:2 mL.
Preferably, in the step (3), in the E solution, the mixed solution D and NH3·H2The dosage ratio of O is 20 mL: 2 mL.
Preferably, in the step (3), the first stirring is carried out at a certain temperature for 60-80 ℃ for 30-60 min; the time of the second stirring is 30-60 min.
Preferably, in steps (2) to (3), the drying conditions are all 60 ℃ and 12 h.
Prepared Fe3O4-QDs/Bi2O4/g-C3N4The composite photocatalyst is used for degrading rhodamine B in wastewater.
Evaluation of photocatalytic activity: irradiating with visible light lamp in DW-01 type photochemical reactor (purchased from teaching instrument factory of Yangzhou university), adding 100mL rhodamine simulation wastewater into the reactor, measuring initial value, adding composite photocatalyst, magnetically stirring, starting aeration device, introducing air to keep the catalyst in suspension or floating state, sampling and analyzing at 10min interval in the irradiation process, centrifuging, collecting supernatant, and placing in spectrophotometer lambdamaxThe absorbance was measured at 553nm and determined by the formula: DR ═ [ (A)0-Ai)/A0]X 100% calculating the degradation rate, wherein A0Absorbance of rhodamine B solution to equilibrium adsorption, AiThe absorbance of the rhodamine B solution was determined for timed sampling.
NH used in the invention3·H2O,FeCl3·6H2O,FeCl2·4H2O,NaBiO3·2H2O,terephthalic acid(TA),p-Benzoquinone(99.0%,AR),triethanolamine(TEOA,AR),isopropanol(IPA,AR)and 5,5-dimethyl-1-pirroline N-Oxide(DMPO) The equal grade is reagent grade and is purchased from Shanghai chemical reagent company Limited; rhodamine B, urea and ethanol, purchased from national drug control, GmbH.
Has the advantages that:
the invention realizes the purpose of using Fe3O4-QDs/Bi2O4/g-C3N4The photocatalyst is used for degrading dye wastewater. g-C3N4And Bi2O4The two semiconductor materials are used as photocatalysts, visible light is used as excitation, a special catalysis or conversion effect is realized through the interface interaction with organic pollutant molecules, and surrounding oxygen and water molecules are excited into free negative ions with strong oxidizing power, so that the aim of degrading harmful organic substances in the environment is fulfilled.
The innovation of the invention is as follows: among the numerous semiconductor photocatalysts, two emerging semiconductor carbon nitrides (g-C) were selected3N4) And bismuth (Bi) tetraoxide2O4) Forming a Z-type heterojunction composite photocatalyst different from a ii-type heterojunction, and introducing magnetic quantum dot ferroferric oxide for convenient recovery; formed Fe3O4-QDs/Bi2O4/g-C3N4The photocatalyst is used for photocatalytic degradation of environmental pollutants; at the same time, the fine dosage ratio of Bi in the synthetic series2O4/g-C3N4In the photocatalyst, Bi is selected through a photocatalytic performance test for degrading rhodamine B2O4/g-C3N4The optimal proportion of the binary photocatalyst is 1:1, marked as Bi/CN, therefore, the proportion of 1:1 is not randomly selected and is the optimal proportion selected by creative experiments; then taking Bi/CN as a substrate to load Fe3O4-QDs, Fe produced3O4-QDs/Bi2O4/g-C3N4The photocatalyst has excellent effect, and the degradation rate of the photocatalyst on rhodamine B reaches 98.6% within 160 min.
Drawings
FIG. 1 shows g-C3N4(a),Bi2O4(c) And SEM image of Bi/CN (e), g-C3N4(b)、Bi2O4(d) The TEM image of (a), (b), (C), (d), (.
FIG. 2 is an XRD pattern of the prepared sample, wherein (a) is a pattern of g-C3N4,Bi2O4XRD patterns of Bi/4CN, Bi/2CN, 3Bi/4CN, Bi/CN, and 4Bi/3 CN; (b) the XRD patterns of 7FeQDs/Bi/CN, 10FeQDs/Bi/CN, 20FeQDs/Bi/CN and 30FeQDs/Bi/CN are shown respectively.
FIG. 3 is a solid ultraviolet image of the prepared sample, wherein g-C are shown in the image (A)3N4、Bi2O4Solid UV diagrams of Bi/4CN, Bi/2CN, 3Bi/4CN, Bi/CN and 4Bi/3 CN; (B) solid ultraviolet images of 7FeQDs/Bi/CN, 10FeQDs/Bi/CN, 20FeQDs/Bi/CN and 30FeQDs/Bi/CN are shown in the figure respectively.
Wherein g-C in FIGS. 1 to 33N4The sample prepared in example 1.
Detailed Description
The invention is further illustrated by the following examples.
Comparative example:
(1)Bi2O4preparing a nanorod photocatalyst:
1.31g of NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain single Bi2O4A photocatalyst.
(2)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.0327g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 0.25: 1, denoted as Bi/4 CN.
(3)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.0655g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 0.5: 1, denoted as Bi/2 CN.
(4)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.0982g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 0.75: 1, and 3Bi/4 CN.
(5)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.75g g-C3N4And 0.131g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 1: the quantitative ratio of the substances was 0.75, and was designated 4Bi/3 CN.
(6)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.131g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 1:1, denoted as Bi/CN.
Bi obtained in comparative example2O4/g-C3N4The photocatalyst is used for carrying out a photocatalytic performance experiment for degrading rhodamine B, and the Bi/CN performance is found to be the best and is obviously superior to Bi/4CN, Bi/2CN, 3Bi/4CN and 4Bi/3CN, so that Bi/CN is selected for carrying out the next step of magnetic quantum dot Fe3O4The load of (2).
Example 1:
(1)g-C3N4preparing nano flakes:
taking out 10g of urea, grinding and then putting into a crucible; placing the sample in a muffle furnace, keeping the temperature at 550 ℃ for 4h, and heating at the rate of 5 ℃/min to obtain a sample A; subsequently, sample A was transferred to a mortar and ground into powder, and placed in a muffle furnace to be subjected to secondary calcination under the same conditions to obtain g-C3N4Nanosheets.
(2)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.131g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 1:1, denoted as Bi/CN.
(3) 0.0233g of FeCl3·6H2O and 0.0085g FeCl2·4H2O is dissolved in Bi2O4/g-C3N4Stirring the sample in 20mL of solution at 80 ℃ for 30min to obtain a mixed solution C; then NH is introduced3·H2O is quickly dropped into the solution C and stirred for 30 min; collecting sample with magnet, washing with deionized water and ethanol, and drying to obtain Fe3O4-QDs/Bi2O4/g-C3N4A composite photocatalyst is provided. Obtaining Fe3O4-QDs/Bi2O4/g-C3N4The photocatalyst contains 10% Fe3O4QDs, labeled 10 FeQDs/Bi/CN.
Example 2:
(1)g-C3N4preparing nano flakes:
taking out 10g of urea, grinding and then putting into a crucible; placing the sample in a muffle furnace, keeping the temperature at 550 ℃ for 4h, and heating at the rate of 5 ℃/min to obtain a sample A; subsequently, sample A was transferred to a mortar and ground into powder, and placed in a muffle furnace to be subjected to secondary calcination under the same conditions to obtain g-C3N4Nanosheets.
(2)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.131g NaBiO3Added to a beaker containing 60mL of deionized water and vigorously stirred at room temperatureStirring for 30min to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 1:1, denoted as Bi/CN.
(3) 0.0467g FeCl3·6H2O and 0.0172g FeCl2·4H2O is dissolved in Bi2O4/g-C3N4Stirring the sample in 20mL of solution at 80 ℃ for 30min to obtain a mixed solution C; then NH is introduced3·H2O is quickly dropped into the solution C and stirred for 30 min; collecting sample with magnet, washing with deionized water and ethanol, and drying to obtain Fe3O4-QDs/Bi2O4/g-C3N4A composite photocatalyst;
obtaining Fe3O4-QDs/Bi2O4/g-C3N4The photocatalyst contains 20% of Fe3O4QDs, labeled 20 FeQDs/Bi/CN.
Example 3:
(1)g-C3N4preparing nano flakes:
taking out 10g of urea, grinding and then putting into a crucible; placing the sample in a muffle furnace, keeping the temperature at 550 ℃ for 4h, and heating at the rate of 5 ℃/min to obtain a sample A; subsequently, sample A was transferred to a mortar and ground into powder, and placed in a muffle furnace to be subjected to secondary calcination under the same conditions to obtain g-C3N4Nanosheets.
(2)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.131g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and placingDrying at 60 deg.C for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 1:1, denoted as Bi/CN.
(3) 0.0700g FeCl3·6H2O and 0.0257g FeCl2·4H2O is dissolved in Bi2O4/g-C3N4Stirring the sample in 20mL of solution at 80 ℃ for 30min to obtain a mixed solution C; then NH is introduced3·H2O is quickly dropped into the solution C and stirred for 30 min; collecting sample with magnet, washing with deionized water and ethanol, and drying to obtain Fe3O4-QDs/Bi2O4/g-C3N4Compounding photocatalyst to obtain Fe3O4-QDs/Bi2O4/g-C3N4The photocatalyst contains 30% Fe3O4QDs, labeled 30 FeQDs/Bi/CN.
Example 4:
(1)g-C3N4preparing nano flakes:
taking out 10g of urea, grinding and then putting into a crucible; placing the sample in a muffle furnace, keeping the temperature at 550 ℃ for 4h, and heating at the rate of 5 ℃/min to obtain a sample A; subsequently, sample A was transferred to a mortar and ground into powder, and placed in a muffle furnace to be subjected to secondary calcination under the same conditions to obtain g-C3N4Nanosheets.
(2)Bi2O4/g-C3N4Preparation of (Bi/CN) photocatalyst:
0.1g g-C3N4And 0.131g NaBiO3Adding the mixture into a beaker containing 60mL of deionized water, and violently stirring the mixture for 30min at room temperature to obtain a mixed solution B; then transferring the solution B into a 100mL polytetrafluoroethylene stainless steel autoclave, keeping the temperature at 160 ℃, and keeping the temperature for 8 hours; finally, washing the sample by deionized water and ethanol, and drying the sample in a drying box at 60 ℃ for 12h to obtain Bi2O4/g-C3N4A photocatalyst; due to Bi2O4And g-C3N4Is 1:1, denoted as Bi/CN.
(3) 0.0163g FeCl3·6H2O and 0.0060g FeCl2·4H2O is dissolved in Bi2O4/g-C3N4Stirring the sample in 20mL of solution at 80 ℃ for 30min to obtain a mixed solution C; then NH is introduced3·H2O is quickly dropped into the solution C and stirred for 30 min; collecting sample with magnet, washing with deionized water and ethanol, and drying to obtain Fe3O4-QDs/Bi2O4/g-C3N4Compounding photocatalyst to obtain Fe3O4-QDs/Bi2O4/g-C3N4The photocatalyst contains 7% of Fe3O4QDs, labeled 7 FeQDs/Bi/CN.
Degradation experiments:
the 20FeQDs/Bi/CN composite photocatalyst prepared in example 2 is used for degradation experiments, samples are taken for photocatalytic degradation experiments in a photochemical reactor, and the degradation rate of the photocatalyst to rhodamine B is measured to reach 98.6% within 160 min.
FIG. 1 shows g-C3N4,Bi2O4TEM and HRTEM images of the Bi/CN and 20FeQDs/Bi/CN composite photocatalyst can further confirm the successful preparation of the 20FeQDs/Bi/CN composite photocatalyst through the material morphology observed from the TEM image and the lattice spacing of the HETEM.
FIG. 2 is an XRD pattern of the prepared sample, wherein (a) is a pattern of g-C3N4,Bi2O4Bi/4CN, Bi/2CN, 3Bi/4CN, Bi/CN, and 4Bi/3 CN; (b) the graphs are respectively 7FeQDs/Bi/CN, 10FeQDs/Bi/CN, 20FeQDs/Bi/CN and 30FeQDs/Bi/CN, which proves that the sample prepared by the application is g-C indeed3N4Bi/CN and 20FeQDs/Bi/CN composite photocatalyst.
FIG. 3 is a solid ultraviolet image of the prepared sample, wherein (A) is g-C3N4,Bi2O4Bi/4CN, Bi/2CN, 3Bi/4CN, Bi/CN, and 4Bi/3 CN; (B) the graphs are 7FeQDs/Bi/CN, 10FeQDs/Bi/CN, 20FeQDs/Bi/CN, respectively. From graph A g-C3N4Has an absorption edge of about 450nm and Bi2O4The visible light absorption performance of the composite material is also better, and an adsorption edge is arranged at the position of 670 nm. With Bi in the binary composite material2O4The increase of the mass ratio results in red shift of the Bi/CN absorption edge within the range of 450-800 nm. As can be seen from the graph B, the visible light absorption capability of FeQDs/Bi/CN in the range of 200-600 nm is better than that of Bi/CN, and the absorption capability is stronger than that of Bi/CN. With the absorption edge of 30FeQDs/Bi/CN being the largest. This is probably due to Fe3O4The quantum effect of-QDs can effectively accelerate visible light absorption. The excellent visible light absorption capability can help the composite photocatalyst to generate more carriers to participate in photocatalytic degradation, so that the photocatalytic activity of the photocatalyst is improved.
It can be seen that pure FeQDs/Bi/CN have a narrow band gap and have good absorption in the visible region, with Fe3O4The loading of QDs is gradually increased, and the absorption of the composite catalyst in the visible light range is gradually enhanced.
Description of the drawings: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; thus, while the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention and protected by the following claims.
Claims (10)
1. Fe3O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized by comprising the following steps:
step (1), taking out urea, grinding, and then carrying out primary calcination to obtain a sample; subsequently, the sample was ground again to a powder and subjected to secondary calcination to give g-C3N4Nanosheets;
step (2) of mixing the g-C prepared in step (1)3N4And NaBiO3Adding the mixture into deionized water, and stirring at room temperature to obtain a mixed solution; then transferred to a polytetrafluoroethylene stainless steel autoclaveReacting and synthesizing to obtain a sample, finally cleaning the sample by using deionized water and ethanol, and then drying the sample in a drying box to obtain Bi2O4/g-C3N4A photocatalyst;
step (3) preparation of Fe3O4-QDs/Bi2O4/g-C3N4A composite photocatalyst;
firstly, Bi prepared in the step (2)2O4/g-C3N4Dissolving a photocatalyst in deionized water to obtain a solution C; then adding FeCl3·6H2O and FeCl2·4H2O, stirring for the first time at a certain temperature to obtain a mixed solution D; then NH is introduced3·H2O is dripped into the solution D to obtain a solution E, and the solution E is stirred for the second time; collecting sample with magnet, washing with deionized water and ethanol, and drying to obtain Fe3O4-QDs/Bi2O4/g-C3N4A photocatalyst.
2. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (1), the conditions of the two times of calcination are all 550 ℃ for 4 hours, and the heating rate is 5 ℃/min.
3. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (2), g-C is adopted3N4、NaBiO3And deionized water in a ratio of 0.1g to 0.131 g: 60 mL.
4. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (2), the reaction synthesis temperature is 160 ℃, and the synthesis time is 8 hours.
5. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (3), in the solution C, Bi is added2O4/g-C3N4The dosage ratio of the photocatalyst to the deionized water is 0.1g to 20 mL.
6. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (3), the deionized water and FeCl are added into the mixed solution D3·6H2O、FeCl2·4H2O、NH3·H2The dosage ratio of O is 20 mL: 0.0467g, 0.0172 g:2 mL.
7. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (3), in the solution E, the mixed solution D and NH3·H2The dosage ratio of O is 20 mL: 2 mL.
8. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (3), the first stirring is carried out at a certain temperature for 60-80 ℃ for 30-60 min; the time of the second stirring is 30-60 min.
9. Fe of claim 13O4Quantum dot modified Bi2O4/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the steps (2) to (3), the drying conditions are all at the temperature of 60 ℃ for 12 hours.
10. Preparation of Fe by the method of any one of claims 1 to 93O4-QDs/Bi2O4/g-C3N4The composite photocatalyst is used for photocatalytic degradation of rhodamine B.
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