CN115228465A - 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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- B01J35/39—
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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
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention 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 invention is characterized in that in-situ hydrothermal reaction is carried out on carbon quantum dots derived from waste biomass and bismuth tungstate, and an efficient S-type heterojunction photocatalyst is constructed by chemical bond combination, so that the structure is stable, the charge separation efficiency is high, the redox capability is strong, and organic pollutants in a water environment can be effectively removed 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 construction of high-efficiency photocatalysts and restoration of environmental sewage, and has potential practical application value.
Description
Technical Field
The invention belongs to the technical field of development of novel photocatalytic materials and environmental management, and particularly relates to a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as well as a preparation method and application thereof.
Background
With the rapid development of the chemical and pharmaceutical industry, tens of thousands of chemicals are discharged into water environment in different degrees in the processes of production, use and transportation, which pose serious threats to the ecological environment and human health, wherein, the medicines and personal care products (PPCPs) are chemicals with large dosage and strong universality, and among the sources of various new organic pollutants, the environmental discharge of the PPCPs is one of the important sources of new pollutants in water. PPCPs are gathered in drinking water sources to affect the quality of drinking water, and have great influence on water environment and human life health. Because PPCPs have poor biodegradability and are difficult to degrade in durability, the traditional biochemical treatment process is difficult to economically and effectively remove. Therefore, new technologies for removing new organic pollutants in water environment need to be developed.
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 intrinsic photocatalysts have low solar utilization efficiency (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 photocatalysis efficiency is low. Therefore, designing a low-cost, green and efficient photocatalyst with a broad spectral response is a major challenge in the practical application of photocatalytic technology. The S-type heterojunction is a novel photocatalysis system and is generally constructed by a reduction type semiconductor photocatalyst with higher Fermi level and an oxidation type semiconductor photocatalyst with lower Fermi level, the built-in electric field and the bending function of an energy band promote the recombination of oxidized photoproduction electrons and reduced photoproduction holes, and simultaneously prevent the transfer of the oxidized photoproduction holes and the reduced photoproduction electrons. Finally, the electrons and the holes respectively have high reduction and oxidation capacities, and the performance of the heterojunction is superior to that of the traditional II-type heterojunction, so that 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, the material is in special relevance due to the characteristics of unique layered structure, good visible light catalytic activity, high thermal stability and photochemical stability, environmental friendliness and the likeAnd (6) note. However, the photocatalytic activity is greatly limited by limited light absorption, rapid recombination of photogenerated carriers, and the inability of low conduction band positions to effectively participate in redox reactions. At present, to Bi 2 WO 6 There have been many reports of ways to make improvements, such as the introduction of oxygen vacancies, and g-C 3 N 4 The method is complex, can be used for constructing heterojunction with other metal-containing semiconductors, can be used for loading noble metal, can be used for doping non-metal atoms and the like, but the methods have the problems of high preparation cost, complex preparation process, unstable catalyst structure and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention 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 problem of Bi 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 purpose, the invention adopts the following technical scheme to realize the purpose:
the invention 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: adding Bi (NO) 3 ) 3● 5H 2 Addition of O to HNO 3 Stirring the solution to obtain Bi (NO) 3 ) 3● 5H 2 An aqueous solution of O; mixing Na 2 WO 4● 2H 2 Adding O into ultrapure water, and performing ultrasonic treatment to obtain Na 2 WO 4● 2H 2 An aqueous solution of O;
s2: adding carbon quantum dot aqueous solution to Na 2 WO 4● 2H 2 In the O aqueous solution, performing 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, after the pH value is adjusted, a mixed solution B is obtained; and (3) 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 3 The concentration of the solution is 1 mol/L-3 mol/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 carbon quantum dot aqueous solution is:
dispersing the leaf powder in water, then carrying out hydrothermal reaction for 6h at 200-240 ℃, and cooling to obtain a reaction solution; filtering the reaction solution to obtain a reacted aqueous solution, and performing freeze drying treatment on the reacted 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.
Further, the mass percentage of the carbon quantum dots in the carbon quantum dots/bismuth tungstate S-type heterojunction is 1-7 wt%.
Further, in S2, the carbon quantum dot aqueous solution and Na 2 WO 4● 2H 2 The dosage ratio of the O aqueous solution is 1; the ultrasonic treatment time is 10 min-30 min.
Further, in S3, na is contained in the mixed solution A 2 WO 4● 2H 2 O and aqueous solution Bi (NO) 3 ) 3● 5H 2 The molar ratio of O is 1:2; and adjusting the pH value to 2-4 by adopting an alkaline solution.
In S3, the temperature of the hydrothermal reaction is 160-200 ℃, and the time of the hydrothermal reaction is 24 hours.
The invention discloses a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the preparation method.
The invention also discloses an application of the carbon quantum dot/bismuth tungstate S-shaped heterojunction photocatalyst, and the S-shaped heterojunction photocatalyst is used as a catalyst for a photocatalytic reaction for removing organic pollutants in a water environment.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a carbon quantum dot/bismuth tungstate (CQDs/Bi) 2 WO 6 ) The preparation method of the S-type heterojunction photocatalyst adopts an in-situ hydrothermal method to carry out hydrothermal reaction on Carbon Quantum Dots (CQDs) to form Bi 2 WO 6 In-situ growth of Bi 2 WO 6 On the surface of the nanosheet, the two nano materials are stably combined through chemical bonds, so that an efficient S-shaped heterojunction photocatalyst is constructed, and organic pollutants in a water environment can be effectively removed under the action of visible light and near infrared light; the preparation process is simple in process (one-step hydrothermal method), low in cost (waste biomass derived carbon quantum dots), environment-friendly and high in efficiency;
the invention also discloses a carbon quantum dot/bismuth tungstate S-type 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; in situ hydrothermal treatment of Bi 2 WO 6 CQDs are loaded on the surface of the nano-sheet to construct an efficient S-type heterojunction, CQDs and Bi 2 WO 6 Are combined by a chemical bond Bi-O-C, are favorable for the rapid transmission of photo-generated charges, and improve CQDs/Bi 2 WO 6 Stability of (2). Meanwhile, the separation efficiency of photo-generated charges and the redox capability of a conduction band valence band can be enhanced, and the response range of sunlight to near infrared light can be greatly enhanced by utilizing the up-conversion performance of the carbon quantum dots.
The invention also discloses the application of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and the related experiment results prove that 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 species; the performance of photocatalytic degradation of pollutants can be obviously improved by loading a very small amount of CQDs; the light is only used as energy, and the nascent organic pollutants PPCPs can be degraded into carbon dioxide, water and non-toxic organic small 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 has good degradation potential under outdoor actual sunlight, and is a high-efficiency and low-cost catalyst for photocatalytic degradation of organic pollutants.
Drawings
FIG. 1 is a TEM photograph of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the present invention;
wherein: a-100nm; b-20nm; c-5nm;
FIG. 2 is an XRD spectrum and an XPS energy spectrum of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the invention;
wherein: a-is an XRD spectrogram of the catalyst prepared by compounding different amounts of CQDs; b-comparison of pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS full spectrum of (a); c-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of middle W; d-comparison of pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of middle Bi; e-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of middle O; f-comparative pure Bi 2 WO 6 And CQDs/Bi 2 WO 6 XPS fine spectrum of medium C;
FIG. 3 is a diagram showing the absorption spectrum and charge separation characterization of the prepared carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst for light;
wherein: a-compounding CQDs with different amounts to prepare an ultraviolet-visible absorption spectrum chart of the catalyst; b-compounding CQDs with different quantities to prepare a photocurrent response diagram of the catalyst; c-compounding CQDs with different amounts to prepare a photoluminescence graph of the catalyst; d-compounding CQDs with different quantities 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 present invention with respect to Tetracycline (TC);
wherein: a-is a tetracycline removal performance curve of the catalyst prepared by compounding different amounts of CQDs under visible light; b-is the reaction rate of the correspondence fit of a; c-a curve of an ultraviolet-visible absorption spectrum of the carbon quantum dot/bismuth tungstate S-type heterojunction for removing tetracycline under visible light; d-is a performance curve of the carbon quantum dot/bismuth tungstate S-type heterojunction for removing tetracycline under near infrared light; e-is the reaction rate of the fit of d; a graph of ultraviolet-visible absorption spectrum of the f-carbon quantum dot/bismuth tungstate S-type heterojunction for tetracycline removal under near-infrared;
FIG. 5 is a schematic diagram of the present invention, which analyzes the work function of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst by using UPS technology, and plots the process of forming S-type heterojunction;
FIG. 6 is a graph showing the performance of tetracycline removal by the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared in example 2 of the present invention;
wherein: a-a performance curve of the carbon quantum dot/bismuth tungstate S-type heterojunction for tetracycline removal under outdoor sunlight; b-a tetracycline removal performance curve of the carbon quantum dot/bismuth tungstate S-type heterojunction in actual water (tap water, river water and lake water); c-a cycle experiment performance curve of the carbon quantum dot/bismuth tungstate S-type heterojunction on tetracycline removal; XRD spectrograms of the d-carbon quantum dot/bismuth tungstate S-type heterojunction before and after use;
Detailed Description
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, 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 invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are provided for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.
In this document, unless otherwise specified, "comprising," including, "" having, "or similar terms, shall encompass the meaning of" consisting of 8230, 8230%, "consisting of" and "consisting essentially of 8230; \8230, consist of," e.g., "A comprising a" shall encompass the meaning of "A comprising a and the other" and "A comprising only a".
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, as long as there is no contradiction between combinations of these technical features, any combinations of the technical features in the respective embodiments or examples may be made, and all possible combinations should be considered as the scope of the present specification.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The following examples use instrumentation conventional in the art. Experimental procedures without specific conditions noted in the following examples, generally according to conventional conditions, or according to conditions recommended by the manufacturer. The various starting materials used in the examples which follow, unless otherwise indicated, are conventional commercial products having specifications which are conventional in the art. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.
Example 1
A preparation method of a 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 HNO with the concentration of 1mol/L 3 Stirring the solution continuously to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous solution of O; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 Dissolving O in 15mL of ultrapure water, and then carrying out ultrasonic treatment for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous solution of O;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder into 60mL of water, then reacting for 6h 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 water solution; freezing and drying the obtained water solution after reaction to obtain CQDs powder; dissolving 0.0105g of CQDs powder in 15mL of water to obtain a carbon quantum dot aqueous solution; 15mL of this carbon quantum dot aqueous solution was added to 15mL of Na 2 WO 4 ·2H 2 Performing ultrasonic treatment for 20min in the O aqueous solution to obtain a mixed solution A;
and step 3: adding the mixed solution A into the Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In O aqueous solution, and adjusting the pH to be =3 by using 1mol/L NaOH solution to obtain mixed solution B; and (3) putting the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction for 24h at 160 ℃, collecting the obtained solid product, washing the solid product with pure water and ethanol for 3 times respectively, and drying the solid product to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dot being 1 wt%.
Example 2
A preparation method of a 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 HNO with the concentration of 1mol/L 3 Stirring the solution continuously to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous solution of O; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 Dissolving O in 15mL of ultrapure water, and then carrying out ultrasonic treatment for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous solution of O;
and 2, step: collecting waste peach leaves, cleaning, drying, grinding into powder, dispersing 0.6g of leaf powder in 60mL of water, reacting at 240 ℃ in a 100mL hydrothermal kettle for 6h, and coolingFiltering the obtained reaction solution by using a 50nm filter membrane to obtain a reacted water solution; freezing and drying the obtained water solution after reaction to obtain CQDs powder; dissolving 0.0315g CQDs powder in 15mL water to obtain carbon quantum dot water solution; 15mL of this carbon quantum dot aqueous solution was added to 15mL of Na 2 WO 4 ·2H 2 Performing ultrasonic treatment for 20min in the O aqueous solution to obtain a mixed solution A;
and step 3: adding the mixed solution A into the Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In O aqueous solution, and adjusting the pH to be =3 by using 1mol/L NaOH solution to obtain mixed solution B; and (3) putting the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction for 24h at 160 ℃, collecting the obtained solid product, washing the solid product with pure water and ethanol for 3 times respectively, and drying the washed solid product to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the carbon quantum dot mass percentage of 3 wt%.
Example 3
A preparation method of a 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 HNO with the concentration of 1mol/L 3 Stirring the solution continuously to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous solution of O; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 Dissolving O in 15mL of ultrapure water, and then carrying out ultrasonic treatment for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous solution of O;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder into 50mL of water, then reacting for 6 hours at 240 ℃ in a 100mL hydrothermal kettle, and filtering the reaction solution obtained after cooling by using a 50nm filter membrane to obtain a reacted water solution; freezing and drying the obtained water solution after reaction to obtain CQDs powder; 0.0525g of CQDs powder is dissolved in 15mL of water to obtain a carbon quantum dot aqueous solution; 15mL of this carbon quantum dot aqueous solution was added to 15mL of Na 2 WO 4 ·2H 2 Performing ultrasonic treatment for 20min in the O aqueous solution to obtain a mixed solution A;
step (ii) of3: adding the mixed solution A into the Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In O aqueous solution, and adjusting the pH to be =3 by using 1mol/L NaOH solution to obtain mixed solution B; and (3) putting the mixed solution B into a 50mL hydrothermal kettle, carrying out hydrothermal reaction for 24h at 180 ℃, collecting the obtained solid product, washing with pure water and ethanol for 3 times respectively, and drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dot being 5 wt%.
Example 4
A preparation method of a 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 HNO with the concentration of 1mol/L 3 Stirring the solution continuously to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous solution of O; 1.5mmol (0.4948 g) of Na 2 WO 4 ·2H 2 Dissolving O in 15mL of ultrapure water, and then carrying out ultrasonic treatment for 15min to obtain Na 2 WO 4 ·2H 2 An aqueous solution of O;
and 2, step: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.6g of leaf powder into 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 water solution; freezing and drying the obtained water solution after reaction to obtain CQDs powder; dissolving 0.0735g of CQDs powder in 15mL of water to obtain a carbon quantum dot aqueous solution; 15mL of this carbon quantum dot aqueous solution was added to 15mL of Na 2 WO 4 ·2H 2 Performing ultrasonic treatment for 20min in an O aqueous solution to obtain a mixed solution A;
and step 3: adding the mixed solution A into the Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In O aqueous solution, and adjusting the pH to be =3 by using 1mol/L NaOH solution to obtain mixed solution B; putting the mixed solution B into a 50mL hydrothermal kettle, reacting at 180 ℃ for 24h, collecting the obtained solid product, washing with pure water and ethanol for 3 times respectively, and drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dot being 7wt%An oxidizing agent.
Example 5
A preparation method of a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: adding 6mmol of Bi (NO) 3 ) 3 ·5H 2 O is slowly added into 60mL of HNO with the concentration of 3mol/L 3 Stirring the solution continuously to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous solution of O; adding 3mmol of Na 2 WO 4 ·2H 2 Dissolving O in 30mL of ultrapure water, and then carrying out ultrasonic treatment for 20min to obtain Na 2 WO 4 ·2H 2 An aqueous solution of O;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.4g of leaf powder into 40mL of water, then reacting for 6 hours in a 100mL hydrothermal kettle at 200 ℃, and filtering the reaction liquid obtained after cooling by using a 50nm filter membrane to obtain a reacted water solution; freezing and drying the obtained water solution after reaction to obtain CQDs powder; 0.1655g of CQDs powder was dissolved in 30mL of water to obtain a carbon quantum dot aqueous solution; 30mL of the carbon quantum dot aqueous solution was added to 20mL of Na 2 WO 4 ·2H 2 Performing ultrasonic treatment on the O aqueous solution for 30min to obtain a mixed solution A;
and step 3: adding the mixed solution A into the Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In an O aqueous solution, adjusting the pH value to be =4 by using a 1mol/L NaOH solution to obtain a mixed solution B; and (3) putting the mixed solution B into a 50mL hydrothermal kettle, reacting for 24h at 200 ℃, collecting the obtained solid product, washing for 3 times by using pure water and ethanol respectively, and drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dot being 7wt%.
Example 6
A preparation method of a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst comprises the following steps:
step 1: 2mmol of Bi (NO) 3 ) 3 ·5H 2 O is slowly added into 20mL of HNO with the concentration of 2mol/L 3 Stirring the solution continuously to obtain Bi (NO) 3 ) 3 ·5H 2 An aqueous solution of O; 1m is to bemol of Na 2 WO 4 ·2H 2 Dissolving O in 10mL of ultrapure water, and then subjecting to ultrasonic treatment for 10min to obtain Na 2 WO 4 ·2H 2 An aqueous solution of O;
step 2: collecting waste peach leaves, cleaning, drying and grinding the waste peach leaves into powder, dispersing 0.5g of leaf powder into 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 water solution; freezing and drying the obtained water solution after reaction to obtain CQDs powder; dissolving 0.035g CQDs powder in 10mL water to obtain carbon quantum dot water solution; 10mL of this carbon quantum dot aqueous solution was added to 20mL of Na 2 WO 4 ·2H 2 Performing ultrasonic treatment on the O aqueous solution for 30min to obtain a mixed solution A;
and step 3: adding the mixed solution A into the Bi (NO) obtained in the step 1 3 ) 3 ·5H 2 In an O aqueous solution, adjusting the pH value to be =2 by using a 1mol/L NaOH solution to obtain a mixed solution B; and (3) putting the mixed solution B into a 50mL hydrothermal kettle, reacting for 24h at 200 ℃, collecting the obtained solid product, washing the solid product with pure water and ethanol for 3 times respectively, and drying to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst with the mass percent of the carbon quantum dots being 3 wt%.
Comparative example 1
Unlike example 1, CQDs are not added in this example, and the procedure is the same as example 1, and pure Bi is finally obtained 2 WO 6 。
Application example 1
The application of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst in removing antibiotics comprises the following steps:
step 1: the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared in the examples 1, 2, 3 and 4 and pure Bi 2 WO 6 Respectively adding into tetracycline solution with concentration of 20mg/L, with concentration of catalyst of 0.5g/L, and continuously stirring in dark for 30min to reach adsorption balance;
and 2, step: then taking a sample every 10min under the irradiation of visible light (420-780 nm) or (more than 800 nm) near infrared light or outdoor sunlight, filtering out the catalyst by using a 0.22um filter, and measuring the absorbance of the obtained solution by using an ultraviolet-visible spectrophotometer;
and 3, step 3: and calculating the degradation rate according to the change of the absorbance of the degradation liquid at 357 nm.
And 4, step 4: the method is completely the same as the steps 1, 2 and 3, except that the solvent for preparing the tetracycline solution in the step 1 is respectively changed from pure water to tap water, lake water and river water, and the using effect of the prepared carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is evaluated in an actual water sample.
FIG. 1 shows TEM picture of the prepared carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst, and it can be seen from the TEM picture that carbon quantum dots with 5nm size are loaded on Bi 2 WO 6 The S-shaped heterojunction can be seen from the CQDs and Bi on the surface of the nano sheet through a high-resolution TEM picture 2 WO 6 And (4) forming.
FIG. 2 shows XRD spectrum and XPS spectrum of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the present invention, from which CQDs/Bi loaded with different amounts of CQDs can be seen 2 WO 6 Retains Bi 2 WO 6 The S-type heterojunction consists of four elements of C, bi, O and W, and CQDs and Bi 2 WO 6 The combination of the two components is combined by a chemical bond Bi-O-C, which is not only beneficial to the rapid transmission of photo-generated charges, but also improves CQDs/Bi 2 WO 6 Stability of (2).
FIG. 3 shows the absorption spectrum and charge separation characterization diagram of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the invention for light, and as can be seen from FIGS. 3a to 3d, the combination of CQDs significantly enhances the sunlight absorption range of the S-type heterojunction, and simultaneously significantly improves the charge separation efficiency.
FIGS. 4 a-4 f show that the composition of CQDs significantly increases Bi 2 WO 6 The photocatalytic antibiotic removal performance is good, 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 that ofThe 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 the total weight of the powder.
CQDs and Bi can be seen in FIG. 5 2 WO 6 The interface charge transfer efficiency is promoted through the action of a built-in electric field, and the S-shaped heterojunction catalytic material with enhanced oxidation-reduction capability is constructed.
Fig. 6a to 6d show that the carbon quantum dot/bismuth tungstate S-type heterojunction prepared in example 2 can effectively remove biological contaminants under outdoor sunlight and in actual water (tap water, lake water and river water), has high stability, does not significantly degrade after being recycled for 5 times, and does not significantly change the chemical structure.
The invention evaluates the actual use effect of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst through tetracycline, proves that the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is an efficient photocatalyst, and can be popularized and applied to removal of other pollutants.
The invention relates to CQDs and Bi derived from waste biomass 2 WO 6 And the high-efficiency carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is constructed by combining. The catalyst only takes light as energy, can degrade new organic pollutants into carbon dioxide, water and nontoxic organic micromolecules, and provides a low-cost, high-efficiency, green and safe purification technology for environmental sewage remediation.
The above contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention should not be limited thereby, and any modification made on the basis of the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is characterized by comprising the following steps:
s1: adding Bi (NO) 3 ) 3● 5H 2 Addition of O to HNO 3 Stirring the solution to obtain Bi (NO) 3 ) 3● 5H 2 An aqueous solution of O; 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 solution of O;
s2: adding carbon quantum dot aqueous solution to Na 2 WO 4● 2H 2 In the O aqueous solution, obtaining a mixed solution A after ultrasonic treatment;
s3: adding the mixed solution A to Bi (NO) 3 ) 3● 5H 2 In the O aqueous solution, after the pH value is adjusted, a mixed solution B is obtained; and carrying out hydrothermal reaction on the mixed solution B to obtain a solid product, and then washing and drying the solid product to obtain the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst.
2. The method for preparing the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein in S1, bi (NO) is added 3 ) 3● 5H 2 O and HNO 3 The dosage ratio of the solution is (2.0-6.0) mmol: (20-60) mL; the HNO 3 The concentration of the solution is 1.0 mol/L-3.0 mol/L.
3. The method for preparing the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein in S1, na is added 2 WO 4● 2H 2 The dosage ratio of O to ultrapure water is (1.0-3.0) mmol: (10-30) mL; the ultrasonic treatment time is 10 min-30 min.
4. The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein in S2, the preparation method of the carbon quantum dot aqueous solution is as follows:
dispersing the leaf powder in water, then carrying out hydrothermal reaction for 6h at 200-240 ℃, and cooling to obtain a reaction solution; filtering the reaction solution to obtain a reacted aqueous solution, and performing freeze drying treatment on the reacted 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.
5. The preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein the mass percentage of the carbon quantum dot in the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst is 1-7 wt%.
6. The method for preparing the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein in S2, the carbon quantum dot aqueous solution and Na 2 WO 4● 2H 2 The dosage ratio of the O aqueous solution is 1; the ultrasonic treatment time is 10 min-30 min.
7. The method for preparing the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein in S3, na is contained in the mixed solution A 2 WO 4● 2H 2 O and aqueous solution Bi (NO) 3 ) 3● 5H 2 The molar ratio of O is 1:2; and adjusting the pH value to 2-4 by adopting an alkaline solution.
8. The method for preparing the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 1, wherein in S3, the temperature of the hydrothermal reaction is 160-200 ℃, and the time of the hydrothermal reaction is 24h.
9. The carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst prepared by the preparation method of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in any one of claims 1 to 8.
10. The application of the carbon quantum dot/bismuth tungstate S-type heterojunction photocatalyst as claimed in claim 9, wherein the S-type heterojunction photocatalyst is used as a catalyst for a photocatalytic reaction for removing organic pollutants in a water environment.
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