CN115228465B - Carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and preparation method and application thereof - Google Patents
Carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and preparation method and application thereof Download PDFInfo
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- 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
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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
- 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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- 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
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02F2101/30—Organic compounds
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- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The application discloses a preparation method and application of a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and belongs to the technical field of development of novel photocatalytic materials and environmental management. The preparation method disclosed by the application is that the waste biomass-derived carbon quantum dots and bismuth tungstate are subjected to in-situ hydrothermal reaction, and the high-efficiency S-type heterojunction photocatalyst is constructed through chemical bond combination, has the advantages of stable structure, high charge separation efficiency and strong redox capacity, and can effectively remove organic pollutants in water environment under the action of visible light and near infrared light. The preparation process is simple to operate, low in cost and environment-friendly, provides a low-cost green strategy for constructing a high-efficiency photocatalyst and repairing environmental sewage, and has potential practical application value.
Description
Technical Field
The application belongs to the technical field of development of novel photocatalytic materials and environmental treatment, and particularly relates to a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and a preparation method and application thereof.
Background
With the rapid development of the chemical and medical industry, tens of thousands of chemicals are discharged into the water environment in different degrees in the production, use and transportation processes, and serious threats are caused to the ecological environment and human health, wherein medicines and personal care products (PPCPs) are large-dosage and strong-universality chemicals, and among the sources of various new organic pollutants, the environmental emission of the PPCPs is one of the important sources of new pollutants in water bodies. PPCPs are converged in a drinking water source to influence the quality of drinking water, and have great influence on water environment and human life and health. Because PPCPs have poor biodegradability and persistent degradation, the traditional biochemical treatment process is difficult to economically and effectively remove. Thus, there is a need to develop new technologies for the removal of nascent organic contaminants in aqueous environments.
The photocatalysis provides a new technology for removing PPCPs pollutants in water environment, and the photocatalysis technology has the advantages of surface enrichment, high oxidation-reduction capability, strong removal capability, small secondary pollution, clean energy, low energy consumption, simplicity, practicability and the like. However, most of the intrinsic photocatalysts have low solar light utilization rate (only ultraviolet light and a small part of visible light can be utilized), and the recombination of photo-generated electrons and holes is serious, so that the photocatalyzing efficiency is low. Therefore, designing a low cost, green and efficient photocatalyst with a broad spectral response is a major challenge for practical application of photocatalytic technology. The S-type heterojunction is used as a novel photocatalysis system, and is generally constructed by a reduced semiconductor photocatalyst with higher fermi energy level and an oxidized semiconductor photocatalyst with lower fermi energy level, and the built-in electric field and the function of energy band bending promote the recombination of oxidized photo-generated electrons and reduced photo-generated holes and simultaneously prevent the transfer of the oxidized photo-generated holes and the reduced photo-generated electrons. Finally, the electrons and the holes respectively have high reduction and oxidation capacities, the performance of the heterojunction is superior to that of the traditional II type heterojunction, and the heterojunction has a huge application prospect in the fields of organic pollutant degradation and the like.
Bismuth tungstate (Bi) 2 WO 6 ) As a typical layered perovskite material, attention is paid to the characteristics of unique layered structure, good visible light catalytic activity, high thermal stability, photochemical stability, environmental friendliness and the like. However, limited light absorption, rapid recombination of photogenerated carriers, and low conduction band position do not effectively participate in redox reactions, greatly limiting their photocatalytic activity. Currently, for Bi 2 WO 6 There have been many reports on ways of making improvements, such as the introduction of oxygen vacancies, and g-C 3 N 4 Compounding, constructing heterojunction with other metal-containing semiconductors, loading noble metals, doping nonmetallic atoms and the like, but the problems of high preparation cost, complex preparation process, unstable catalyst structure and the like exist in the modes.
Disclosure of Invention
In order to overcome the defects in the prior art, the application aims to provide a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and a preparation method and application thereof, so as to solve the problems ofBi 2 WO 6 The preparation process of the base photocatalytic material is complex, the cost is high, the stability of the catalyst is poor, and the response range to sunlight is narrow.
In order to achieve the above purpose, the application is realized by adopting the following technical scheme:
the application discloses a preparation method of a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, which is characterized by comprising the following steps of:
s1: bi (NO) 3 ) 3● 5H 2 O is added to HNO 3 Stirring the solution to obtain Bi (NO) 3 ) 3● 5H 2 An aqueous O solution; na is mixed with 2 WO 4● 2H 2 Adding O into ultrapure water, and performing ultrasonic treatment to obtain Na 2 WO 4● 2H 2 An aqueous O solution;
s2: adding the aqueous solution of the carbon quantum dots to Na 2 WO 4● 2H 2 In the O aqueous solution, carrying out ultrasonic treatment to obtain a mixed solution A;
s3: adding the mixed solution A to Bi (NO) 3 ) 3● 5H 2 In the O aqueous solution, regulating the pH value to obtain a mixed solution B; and (3) after carrying out hydrothermal reaction on the mixed solution B, collecting a solid product after the reaction, and washing and drying the solid product to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst.
Further, in S1, the Bi (NO 3 ) 3● 5H 2 O and HNO 3 The dosage ratio of the solution is (2-6) mmol: (20-60) mL; the HNO is 3 The concentration of the solution is 1mol/L to 3mol/L.
Further, in S1, the Na 2 WO 4● 2H 2 The dosage ratio of O to ultrapure water is (1-3) mmol: (10-30) mL; the ultrasonic treatment time is 10 min-30 min.
Further, in S2, the preparation method of the aqueous solution of carbon quantum dots includes:
dispersing leaf powder in water, performing hydrothermal reaction at 200-240 ℃ for 6h, and cooling to obtain reaction liquid; filtering the reaction solution to obtain a post-reaction aqueous solution, and performing freeze drying treatment on the post-reaction aqueous solution to obtain carbon quantum dot powder; mixing carbon quantum dot powder with water to obtain a carbon quantum dot aqueous solution; the dosage ratio of the leaf powder to the water is 1:100g/mL.
Further, the mass percentage of the carbon quantum dots in the carbon quantum dot/bismuth tungstate S-type heterojunction is 1-7wt%.
Further, in S2, the aqueous solution of carbon quantum dots and Na 2 WO 4● 2H 2 The dosage ratio of the O aqueous solution is 1:1; the ultrasonic treatment time is 10 min-30 min.
Further, in S3, na in the mixed solution A 2 WO 4● 2H 2 O and aqueous Bi (NO) 3 ) 3● 5H 2 The molar ratio of O is 1:2; and regulating the pH value to 2-4 by adopting alkaline solution.
Further, in S3, the temperature of the hydrothermal reaction is 160-200 ℃, and the time of the hydrothermal reaction is 24 hours.
The application discloses a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the preparation method.
The application also discloses application of the carbon quantum dot/bismuth tungstate S-shaped heterojunction photocatalyst, wherein the S-shaped heterojunction photocatalyst is used as a catalyst for removing photocatalytic reaction of organic pollutants in water environment.
Compared with the prior art, the application has the following beneficial effects:
the application discloses a carbon quantum dot/bismuth tungstate (CQDs/Bi) 2 WO 6 ) Preparation method of S-type heterojunction photocatalyst, in which in-situ hydrothermal method is adopted to form Bi by hydro-thermal reaction of Carbon Quantum Dots (CQDs) 2 WO 6 In-situ growth in Bi 2 WO 6 The two nano materials are stably combined through chemical bonds on the surface of the nano sheet, so that a high-efficiency S-shaped heterojunction photocatalyst is constructed, and organic pollutants in water environment can be effectively removed under the action of visible light and near infrared light; the preparation process has the advantages of simple process (one-step hydrothermal method), low cost (waste biomass derived carbon quantum dots), environmental friendliness and high efficiency;
the application also discloses the carbon quantum dot/bismuth tungstate S-shaped heterojunction photocatalyst prepared by the preparation method, and compared with the improvement strategy of the existing semiconductor photocatalyst, the carbon quantum dot derived from the loaded waste biomass is green, low in cost and small in secondary pollution; bi in situ by hydrothermal 2 WO 6 CQDs is loaded on the surface of the nanosheet, and an efficient S-shaped heterojunction is constructed, and CQDs and Bi are formed 2 WO 6 The combination of the two components through chemical bond Bi-O-C is beneficial to the rapid transmission of photo-generated charges and improves CQDs/Bi 2 WO 6 Is stable. Meanwhile, the separation efficiency of photo-generated charges and the oxidation-reduction capability of a conduction band valence band can be enhanced, and the response range to sunlight can be greatly enhanced to near infrared light by utilizing the up-conversion performance of the carbon quantum dots.
The application also discloses application of the carbon quantum dot/bismuth tungstate S-shaped heterojunction photocatalyst, and the related experimental results prove that the carbon quantum dot/bismuth tungstate S-shaped heterojunction photocatalyst can remove 90% of antibiotic solution within 40 minutes under visible light without adding additional active species; the performance of photocatalytic degradation of pollutants can be remarkably improved by loading a very small amount of CQDs; the light is taken as energy only, and the renewable organic pollutant PPCPs are degraded into carbon dioxide, water and nontoxic small organic molecules. The method has great application potential in actual water environments such as river water, lake water, tap water and the like; and the catalyst can be well degraded in the outdoor actual sunlight, and the catalyst is high-efficiency and low-cost for photocatalytic degradation of organic pollutants.
Drawings
FIG. 1 is a TEM photograph of a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the application;
wherein: a-100nm; b-20nm; c-5nm;
FIG. 2 is an XRD spectrum and an XPS spectrum of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the application;
wherein: a-is XRD spectrum of the catalyst prepared by compounding CQDs with different amounts; b-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS spectrogram of (b); c-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of W; d-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrogram of middle Bi; e-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of medium O; f-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of medium C;
FIG. 3 is a graph showing the absorption spectrum and charge separation characteristics of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the application;
wherein: a-compounding CQDs with different amounts to prepare an ultraviolet-visible absorption spectrum of the catalyst; b-compounding different amounts of CQDs to prepare a photocurrent response diagram of the catalyst; c-compounding CQDs with different amounts to prepare a photoluminescence chart of the catalyst; d-compounding CQDs with different amounts to prepare an impedance diagram of the catalyst;
FIG. 4 is a graph showing the removal performance of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the application on Tetracycline (TC);
wherein: a-is a removal performance curve of the catalyst prepared by compounding CQDs with different amounts on tetracycline under visible light; b-is a response rate corresponding to the fit; c-ultraviolet-visible absorption spectrum curve of the carbon quantum dot/bismuth tungstate S-type heterojunction for removing tetracycline under visible light; d-is a removal performance curve of the carbon quantum dot/bismuth tungstate S-type heterojunction on tetracycline under near infrared light; e-is the reaction rate of d corresponding fit; an ultraviolet-visible absorption spectrum graph of f-carbon quantum dot/bismuth tungstate S-type heterojunction for removing tetracycline under near infrared;
FIG. 5 is a schematic diagram showing the formation process of the S-type heterojunction by analyzing the work function of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst by utilizing the UPS technology;
FIG. 6 is a graph showing the evaluation performance of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared in example 2 of the present application for removing tetracycline;
wherein: a performance curve of the a-carbon quantum dot/bismuth tungstate S-type heterojunction for removing tetracycline under outdoor sunlight; b-carbon quantum dot/bismuth tungstate S-type heterojunction in actual water (tap water, river water and lake water) to remove the tetracycline; c-cyclic experimental performance curve of carbon quantum dot/bismuth tungstate S-type heterojunction on tetracycline removal; XRD spectra before and after d-carbon quantum dot/bismuth tungstate S-type heterojunction is used;
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present application, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the application in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present application and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 3mmol (1.4553 g) of Bi (NO) 3 ) 3 ·5H 2 Slowly adding O into 30mL of HNO with concentration of 1mol/L 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 O is dissolved in 15mL of ultrapure water and then treated by ultrasonic for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder in 60mL of water, then reacting for 6 hours at 240 ℃ in a 100mL hydrothermal kettle, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a reacted aqueous solution; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; 0.0105g of CQDs powder is dissolved in 15mL of water to obtain an aqueous solution of carbon quantum dots; 15mL of the aqueous carbon quantum dot solution was added to 15mL of Na 2 WO 4 ·2H 2 In O aqueous solution, carrying out ultrasonic treatment for 20min,obtaining a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, regulating the pH value to be=3 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; and (3) filling the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction for 24 hours at 160 ℃, collecting the obtained solid product, washing for 3 times by using pure water and ethanol respectively, and then drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of 1wt% of carbon quantum dots.
Example 2
The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 3mmol (1.4553 g) of Bi (NO) 3 ) 3 ·5H 2 Slowly adding O into 30mL of HNO with concentration of 1mol/L 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 O is dissolved in 15mL of ultrapure water and then treated by ultrasonic for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder in 60mL of water, then reacting for 6 hours at 240 ℃ in a 100mL hydrothermal kettle, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a reacted aqueous solution; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; 0.0315g of CQDs powder is dissolved in 15mL of water to obtain an aqueous solution of carbon quantum dots; 15mL of the aqueous carbon quantum dot solution was added to 15mL of Na 2 WO 4 ·2H 2 Carrying out ultrasonic treatment in the O aqueous solution for 20min to obtain a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, regulating the pH value to be=3 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; filling the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction for 24 hours at 160 ℃, collecting the obtained solid product, washing for 3 times respectively by pure water and ethanol, and then drying to obtain the carbon contentThe mass percentage of the sub-dots is 3wt% of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst.
Example 3
The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 3mmol (1.4553 g) of Bi (NO) 3 ) 3 ·5H 2 Slowly adding O into 30mL of HNO with concentration of 1mol/L 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 O is dissolved in 15mL of ultrapure water and then treated by ultrasonic for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder in 50mL of water, then reacting for 6 hours at 240 ℃ in a 100mL hydrothermal kettle, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a reacted aqueous solution; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; 0.0525g of CQDs powder is dissolved in 15mL of water to obtain an aqueous solution of carbon quantum dots; 15mL of the aqueous carbon quantum dot solution was added to 15mL of Na 2 WO 4 ·2H 2 Carrying out ultrasonic treatment in the O aqueous solution for 20min to obtain a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, regulating the pH value to be=3 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; and (3) filling the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction for 24 hours at 180 ℃, collecting the obtained solid product, respectively washing with pure water and ethanol for 3 times, and then drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of carbon quantum dots of 5 wt%.
Example 4
The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 3mmol (1.4553 g) of Bi (NO) 3 ) 3 ·5H 2 O is slowly added into 30mL of the mixture with the concentration of 1mol/LHNO of (F) 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 O is dissolved in 15mL of ultrapure water and then treated by ultrasonic for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder in 50mL of water, then reacting for 6 hours at 240 ℃ in a 100mL hydrothermal kettle, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a reacted aqueous solution; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; 0.0735g of CQDs powder is dissolved in 15mL of water to obtain an aqueous solution of carbon quantum dots; 15mL of the aqueous carbon quantum dot solution was added to 15mL of Na 2 WO 4 ·2H 2 Carrying out ultrasonic treatment in the O aqueous solution for 20min to obtain a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, regulating the pH value to be=3 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; and (3) filling the mixed solution B into a 50mL hydrothermal kettle, reacting at 180 ℃ for 24 hours, collecting the obtained solid product, washing for 3 times by using pure water and ethanol respectively, and then drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dots of 7wt%.
Example 5
The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 6mmol of Bi (NO) 3 ) 3 ·5H 2 Slowly adding O into 60mL of HNO with the concentration of 3mol/L 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; 3mmol of Na 2 WO 4 ·2H 2 O was dissolved in 30mL of ultrapure water, and then sonicated for 20min to give Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, oven drying, grinding into powder, dispersing 0.4g of leaf powder in 40mIn L water, then reacting for 6 hours at 200 ℃ in a 100mL hydrothermal kettle, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a water solution after reaction; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; 0.1655g of CQDs powder is dissolved in 30mL of water to obtain an aqueous solution of carbon quantum dots; 30mL of the aqueous carbon quantum dot solution was added to 20mL of Na 2 WO 4 ·2H 2 Carrying out ultrasonic treatment in the O aqueous solution for 30min to obtain a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, adjusting the pH value to be 4 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; and (3) filling the mixed solution B into a 50mL hydrothermal kettle, reacting for 24 hours at 200 ℃, collecting the obtained solid product, respectively washing for 3 times by using pure water and ethanol, and then drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dots of 7wt%.
Example 6
The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 2mmol of Bi (NO) 3 ) 3 ·5H 2 Slowly adding O into 20mL of HNO with concentration of 2mol/L 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; 1mmol of Na 2 WO 4 ·2H 2 O was dissolved in 10mL of ultrapure water, and then sonicated for 10min to give Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.5g of leaf powder in 60mL of water, then reacting for 6 hours at 220 ℃ in a 100mL hydrothermal kettle, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a reacted aqueous solution; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; 0.035g of CQDs powder was dissolved in 10mL of water to obtain an aqueous solution of carbon quantum dots; 10mL of the aqueous carbon quantum dot solution was added to 20mL of Na 2 WO 4 ·2H 2 Carrying out ultrasonic treatment in the O aqueous solution for 30min to obtain a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, regulating the pH value to be 2 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; and (3) filling the mixed solution B into a 50mL hydrothermal kettle, reacting for 24 hours at 200 ℃, collecting the obtained solid product, respectively washing for 3 times by using pure water and ethanol, and then drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of 3wt% of carbon quantum dots.
Comparative example 1
Unlike example 1, in this example, CQDs were not added, and the rest of the procedure was the same as in example 1, to finally obtain pure Bi 2 WO 6 。
Application example 1
The application of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst for removing antibiotics comprises the following steps:
step 1: carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared in examples 1, 2, 3 and 4 and pure Bi 2 WO 6 Respectively adding the catalyst into tetracycline solution with the concentration of 20mg/L, and continuously stirring for 30min under dark condition, wherein the concentration of the catalyst is 0.5g/L, so as to reach adsorption equilibrium;
step 2: then taking samples every 10min under the irradiation of visible light (420-780 nm) or near infrared light (more than 800 nm) or outdoor sunlight, filtering out the catalyst by using a 0.22um filter head, and measuring the absorbance of the obtained solution by using an ultraviolet-visible spectrophotometer;
step 3: the degradation rate was calculated from the change in absorbance of the degradation solution at 357 nm.
Step 4: and (3) the method is completely the same as the steps (1), 2 and 3, except that the solvent of the tetracycline solution prepared in the step (1) is changed from pure water to tap water, lake water and river water respectively, and the use effect of the prepared carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is evaluated in an actual water sample.
FIG. 1 shows TEM image of prepared carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and from the image, it can be seen that carbon quantum dot with the size of 5nm is loaded on Bi 2 WO 6 On the surface of the nano-sheet, the S-type heterojunction can be seen by high-resolution TEM image from CQDs and Bi 2 WO 6 Composition is prepared.
FIG. 2 shows XRD spectra and XPS energy spectra of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the method, and the CQDs/Bi loaded with different amounts of CQDs can be seen from the figures 2 WO 6 Bi is maintained 2 WO 6 The S-type heterojunction is composed of C, bi, O, W four elements, and CQDs and Bi 2 WO 6 The combination of the two components through chemical bond Bi-O-C is not only beneficial to the rapid transmission of photo-generated charges, but also improves CQDs/Bi 2 WO 6 Is stable.
Fig. 3 shows the absorption spectrum and the charge separation characterization diagram of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the method, and it can be seen from fig. 3 a-3 d that the recombination of CQDs significantly enhances the absorption range of the S-type heterojunction to sunlight, and meanwhile, the charge separation efficiency is significantly improved.
FIGS. 4 a-4 f show that the compounding of CQDs significantly improves Bi 2 WO 6 The photocatalytic antibiotic removal performance, and the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst has excellent performance under visible light and near infrared light; the reaction rate constant of the S-type heterojunction photocatalyst prepared in example 2 under visible light is pure Bi 2 WO 6 4.0 times of the reaction rate constant of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst under near infrared light is pure Bi 2 WO 6 4.4 times of (a).
FIG. 5 shows CQDs and Bi 2 WO 6 The interfacial charge transfer efficiency is promoted by the action of a built-in electric field, and the S-type heterojunction catalytic material with enhanced oxidation-reduction capability is constructed.
Fig. 6a to 6d can show that the carbon quantum dot/bismuth tungstate S-type heterojunction prepared in example 2 can effectively remove the anti-biological pollutants under outdoor sunlight and in actual water (tap water, lake water and river water), has higher stability, has no obvious reduction of performance after being recycled for 5 times, and has no obvious change of chemical structure.
The tetracycline antibiotics are one of the main sources of PPCPs, and the practical use effect of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is evaluated through tetracycline, so that the carbon quantum dot/bismuth tungstate S-type heterojunction is proved to be an efficient photocatalyst and can be popularized and applied to the removal of other pollutants.
The application leads the CQDs and Bi derived from the waste biomass 2 WO 6 And combining to construct the high-efficiency carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst. The catalyst only takes light as energy, can degrade new organic pollutants into carbon dioxide, water and nontoxic small organic molecules, and provides a low-cost, high-efficiency, green and safe purification technology for environmental sewage restoration.
The above is only for illustrating the technical idea of the present application, and the protection scope of the present application is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present application falls within the protection scope of the claims of the present application.
Claims (1)
1. The application of the carbon quantum dot/bismuth tungstate S-shaped heterojunction photocatalyst is characterized in that the S-shaped heterojunction photocatalyst is used as a catalyst for removing photocatalysis reaction of antibiotics in water environment;
the preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 3mmol, 1.4553g Bi (NO 3 ) 3 ·5H 2 Slowly adding O into HNO with concentration of 30mL of 1mol/L 3 Continuously stirring the solution to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous O solution; na of 1.5mmol, 0.4948g 2 WO 4 ·2H 2 O is dissolved in 15mL ultrapure water and then treated by ultrasonic for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous O solution;
step 2: collecting waste peach leaves, cleaning, oven drying, grinding into powder, dispersing 0.6. 0.6g leaf powder in 60mL water, reacting at 240 deg.C in 100mL hydrothermal kettle for 6h, cooling, filtering the obtained reaction solution with 50nm filter membrane to obtain the final productA post aqueous solution; freeze-drying the obtained aqueous solution after the reaction to obtain CQDs powder; CQDs powder of 0.0315 and g is dissolved in 15mL water to obtain a carbon quantum dot aqueous solution; adding 15mL of the aqueous solution of the carbon quantum dots described in 15mL to 15mL of Na 2 WO 4 ·2H 2 Carrying out ultrasonic treatment in the O aqueous solution for 20min to obtain a mixed solution A;
step 3: adding the mixed solution A to Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In the O aqueous solution, regulating the pH value to be=3 by using a NaOH solution with the concentration of 1mol/L to obtain a mixed solution B; filling the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction at 160 ℃ for 24h, collecting to obtain a solid product, washing with pure water and ethanol for 3 times respectively, and then drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with 3wt% of carbon quantum dots;
the CQDs and Bi 2 WO 6 The two are combined through chemical bond Bi-O-C;
the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst can remove 90% of antibiotic solution within 40 minutes under visible light without adding additional active substances.
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