CN113231081A - Flower-shaped CDs-ZnIn2S4Composite photocatalyst and preparation method and application thereof - Google Patents

Flower-shaped CDs-ZnIn2S4Composite photocatalyst and preparation method and application thereof Download PDF

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CN113231081A
CN113231081A CN202110557854.XA CN202110557854A CN113231081A CN 113231081 A CN113231081 A CN 113231081A CN 202110557854 A CN202110557854 A CN 202110557854A CN 113231081 A CN113231081 A CN 113231081A
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cds
znin
flower
composite photocatalyst
preparation
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延旭
毛艳丽
康海彦
施伟龙
宋忠贤
刘彪
闫晓乐
潘龙
胡泊
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Henan University of Urban Construction
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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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04—Sulfides
    • 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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

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Abstract

The invention discloses a flower-shaped CDs-ZnIn2S4A composite photocatalyst and a preparation method thereof belong to the field of catalyst preparation. According to the invention, after CDs are introduced, the light absorption capacity of the CDs-ZIS composite photocatalyst is obviously enhanced, but the integral photocatalytic activity is not obviously improved, so that the CDs-ZnIn is considered2S4Persulfate (PS) is introduced into the composite photocatalytic system, and the excellent electron transfer characteristic of CDs is fully utilized, so that the composition and yield of active oxidation components in the reaction system are improved, and the catalytic performance of the CDs-ZIS composite photocatalyst is further improved. The invention has simple preparation process, low production cost, easy operation and abundant raw material sourcesThe composite photocatalyst has high photocatalytic activity by combining the advantages of an advanced oxidation process, so that the CDs-ZIS composite photocatalyst has great potential in the aspect of practical application.

Description

Flower-shaped CDs-ZnIn2S4Composite photocatalyst and preparation method and application thereof
Technical Field
The invention belongs to the field of catalyst preparation, relates to the combination of photocatalysis and advanced oxidation technology, and particularly relates to flower-shaped CDs-ZnIn2S4Preparation of the composite photocatalyst and application of the composite photocatalyst in activating persulfate.
Background
The photocatalytic technology attracts attention as an energy-saving and green technology. The core of the photocatalysis technology is a semiconductor photocatalyst which generates electrons and holes under the irradiation of ultraviolet/visible/sunlight to further generate oxidation active species with strong oxidation reduction capability, so that pollutants in a water body can be effectively degraded and converted into small molecular substances, and the effect of purifying the water body is achieved.
Sulfur indium zinc (ZnIn)2S4) Is a ternary chalcogenide compound with the forbidden band width of 2.4-2.6(eV) and shows strong visible light absorption, which enables ZnIn to be formed2S4Is considered to be a good visible light driving photocatalyst. However, pure phase ZnIn2S4The short life-span of the photo-generated electron-hole pair has high recombination rate, which limits the application of the photo-generated electron-hole pair in the field of photocatalysis. Therefore, how to achieve efficient separation and migration of photogenerated charges to enhance ZnIn2S4Is the focus of current research.
Carbon quantum dots (CDs) are a novel carbon nanomaterial and are unique due to their low biotoxicityThe ability to transfer photo-induced electrons is of great interest. Many researches have found that CDs can effectively promote the separation efficiency of photo-generated charges in the photocatalyst as a cocatalyst. Therefore, ZnIn is considered2S4The nanosheets are compounded with CDs to improve the visible light response of the composite material and the separation efficiency of the photoexcited electron-hole pairs.
Although CDs-ZnIn is available at present2S4Reports of visible light degradation of pollutants in composite materials, however, ZnIn2S4The composite material with CDs has limited effect on improving the photocatalytic performance of the material, and has slow rate of oxidative degradation of organic pollutants.
Therefore, how to prepare the CDs-ZnIn with excellent catalytic performance and high stability2S4The composite catalyst material is a technical problem to be solved in the field.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to overcome the defects of the prior art and to provide a flower-shaped CDs-ZnIn2S4A preparation method of a composite photocatalyst.
In order to achieve the above purpose, the invention provides the following technical scheme:
flower-shaped CDs-ZnIn2S4The preparation method of the composite photocatalyst specifically comprises the following steps:
(1) weighing a certain amount of carbon quantum dots (CDs) and zinc acetate dihydrate (Zn (CH)3COO)2·2H2O), indium chloride tetrahydrate (InCl)3·4H2O) and Thioacetamide (TAA) are added into a mixed solution containing ethanol and water at room temperature to be uniformly mixed by ultrasonic waves, and the mixed solution is transferred into a high-pressure reaction kettle to be heated, then cooled to room temperature and centrifugally collected to obtain precipitates;
(2) washing the precipitate with deionized water and ethanol alternately for several times, and vacuum drying to obtain the flower-shaped CDs-ZnIn2S4A composite photocatalyst is provided.
Preferably, in the step (1), Zn (CH)3COO)2·2H2O、InCl3·4H2The molar ratio of O to TAA is 1: 2ZnIn obtained by theory of adding 4 CDs2S4The ultrasonic treatment time is 0.5-1 hour (0.3-3%) of the mass.
Further preferably, in the step (1), the heating reaction temperature is 180 ℃, and the reaction time is 22-24 hours.
Preferably, in the step (2), the vacuum drying temperature is 50-60 ℃, and the drying time is 12-18 h.
The invention also claims the flower-shaped CDs-ZnIn prepared by the method2S4A composite photocatalyst, the flower-like CDs-ZnIn2S4The composite photocatalyst is prepared from zinc acetate dihydrate (Zn (CH)3COO)2·2H2O), indium chloride tetrahydrate (InCl)3·4H2O), Thioacetamide (TAA) and carbon quantum dots (CDs) are synthesized by a hydrothermal method.
In addition, the invention also requests to protect the flower-shaped CDs-ZnIn2S4The application of the composite photocatalyst in the field of photocatalysis.
In particular, the flower-like CDs-ZnIn2S4The application of the composite photocatalyst in activating persulfate to carry out photocatalytic degradation on tetracycline under the condition of visible light.
It is noted that the present invention contemplates CDs-ZnIn2S4Persulfate (PS) is introduced into the composite photocatalytic system, so that the excellent electron transfer characteristic of CDs is fully utilized, the composition and yield of active oxidation components in the reaction system are improved, and the content of CDs-ZnIn is further improved2S4The photocatalytic performance of the composite photocatalyst.
According to the technical scheme, the invention discloses and provides flower-shaped CDs-ZnIn2S4Compared with the prior art, the composite photocatalyst and the preparation method and the application thereof have the following excellent effects:
(1) the preparation method has the advantages of simple preparation process, low production cost, easy operation, sufficient raw material sources and flower-shaped CDs-ZnIn2S4The composite photocatalyst has high stability and great potential in the aspect of practical application;
(2) prepared by the present inventionFlower-like CDs-ZnIn2S4The composite photocatalyst has obviously enhanced light absorption capacity under visible light, and improves the separation efficiency of photo-generated electron hole pairs. In addition, in order to fully utilize the excellent electron transfer characteristics of CDs, in CDs-ZnIn2S4PS is introduced into a photocatalysis system, and photo-generated electrons are extracted from ZnIn2S4The conduction band is enriched on CDs, PS can be effectively activated, and the photocatalytic activity of the whole reaction system is further improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 shows flower-like CDs-ZnIn in example 2 of the present invention2S4Composite photocatalyst and ZnIn2S4XRD pattern of (a).
FIG. 2 shows flower-like CDs-ZnIn in example 2 of the present invention2S4Composite photocatalyst and ZnIn2S4FTIR spectra of (1).
FIG. 3 shows the flower-like CDs-ZnIn of example 2 of the present invention2S4Composite photocatalyst and ZnIn2S4High resolution transmission electron microscope images of (a); wherein, FIG. 3(a-b) shows ZnIn2S4SEM of (5), FIG. 3(c-d) is CDs-ZnIn2S4TEM and HRTEM of (1).
FIG. 4 shows flower-like CDs-ZnIn in examples 1-4 of the present invention2S4Composite photocatalyst and ZnIn2S4The solid ultraviolet spectrum of (1).
FIG. 5 shows flower-like CDs-ZnIn in example 2 of the present invention2S4Composite photocatalyst and ZnIn2S4A fluorescence spectrum of (a).
FIG. 6 shows flower-like CDs-ZnIn in example 2 of the present invention2S4Composite photocatalyst and ZnIn2S4A photocurrent map of (a).
FIG. 7 shows flower-like CDs-ZnIn in example 2 of the present invention2S4Composite photocatalyst and ZnIn2S4And a performance diagram of degrading tetracycline by photocatalysis of PS.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings of the specification, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a flower-shaped CDs-ZnIn with simple preparation process, low production cost, easy operation and sufficient raw material source2S4A preparation method of a composite photocatalyst.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1
0.0002g of CDs, 0.0439g of Zn (CH) at room temperature3COO)2·2H2O、0.1173gInCl3·4H2Adding O and 0.0601g TAA into a mixed solution of 15mL of ethanol and 15mL of deionized water, performing ultrasonic treatment for 1 hour, uniformly mixing, and transferring the mixed solution into a 50mL high-pressure reaction kettle with a polytetrafluoroethylene lining, and storing for 24 hours at 180 ℃; cooling to room temperature, centrifuging and collecting precipitate; finally, the precipitate is dried for 12 hours in vacuum at the temperature of 60 ℃ to obtain the flower-shaped CDs-ZnIn2S4A composite photocatalyst, designated 0.3% CDs-ZIS.
Example 2
At room temperature0.0008g CDs、0.0439g Zn(CH3COO)2·2H2O、0.1173gInCl3·4H2O and 0.0601g TAA are added into a mixed solution of 15mL ethanol and 15mL deionized water and are uniformly mixed by ultrasonic for 1h, and the preparation step is the same as the above and is marked as 1% CDs-ZIS.
Example 3
0.0017g CDs, 0.0439g Zn (CH) were added at room temperature3COO)2·2H2O、0.1173gInCl3·4H2O and 0.0601g TAA are added into a mixed solution of 15mL ethanol and 15mL deionized water and are uniformly mixed by ultrasonic for 1h, and the preparation step is the same as the above and is marked as 2% CDs-ZIS.
Example 4
0.0017g CDs, 0.0439g Zn (CH) were added at room temperature3COO)2·2H2O、0.1173gInCl3·4H2O and 0.0601g TAA are added into a mixed solution of 15mL ethanol and 15mL deionized water and are uniformly mixed by ultrasonic for 1h, and the preparation step is the same as the above and is marked as 3% CDs-ZIS.
In order to further verify the flower-shaped CDs-ZnIn prepared by the invention2S4The inventor respectively pairs flower-shaped CDs-ZnIn with the effect of a composite photocatalyst2S4The composite photocatalyst is characterized and tested in performance, and the characteristics are as follows:
(1) for the flower-shaped CDs-ZIS composite photocatalyst and flower-shaped ZnIn in example 22S4XRD characterization was performed as follows:
the crystalline phase of the sample was measured using a Bruker-AXSSM D8 advanced XRD diffractometer of germany with Cu ka (λ ═ 0.15418nm) radiation, and data collection was done with a 2 θ scan pattern, with continuous scanning in the range of 10 ° to 70 ° at a scan speed of 8 °/min.
Wherein, figure 1 shows a flower-shaped 1 percent CDs-ZIS composite photocatalyst and pure ZnIn2S4XRD spectrum of (1). All samples had distinct characteristic diffraction peaks at 15.5 °, 21.6 °, 27.7 °, 30.4 °, 39.9 °, 47.2 °, 52.4 ° and 55.6 °, corresponding to ZnIn, respectively2S4The (002), (006), (102), (104), (108), (110), (116) and (022) crystal planes, which are consistent with the hexagonal patterns that have been reportedZnIn2S4The characteristic diffraction peaks (JCPDS No.72-0773) of the two-dimensional diffraction pattern were identical. Furthermore, in ZnIn2S4No additional characteristic peak of CDs was observed at 26 ° after introduction of CDs, mainly because the amount of CDs added was relatively limited.
(2) Infrared testing of the flower-like CDs-ZIS composite photocatalyst of example 2 was conducted
In which, fig. 2 shows FTIR spectra of the flower-like CDs-ZIS composite photocatalyst prepared in example 2 and CDs. And 1241, 1403, 1631, 3430cm-1There are distinct diffraction peaks corresponding to C-OH, C ═ C, C ═ O, and O — H bonds, respectively. The presence of these peaks can also be observed in the infrared image of 1% CDs-ZIS, demonstrating the successful incorporation of CDs into the 1% CDs-ZIS composite.
(3) SEM topography determination of the flower-shaped CDs-ZIS composite photocatalyst in example 2
FIG. 3 shows ZnIn2S4The same flower-shaped CDs-ZnIn as in example 22S4The morphology of the composite photocatalyst; wherein FIG. 3(a-b) clearly shows pure ZnIn2S4Is a cluster flower-like structure formed by the aggregation of nanosheets, and ZnIn can be observed after CDs are introduced in figure 3(c)2S4Still sheet-like structure, but the presence of CDs was not observed due to its too small size; while HRTEM of 1% CDs-ZIS in FIG. 3(d) clearly shows the successful incorporation of CDs into ZnIn2S4In (1).
(4) The flower-like CDs-ZIS composite photocatalyst and pure ZnIn in examples 1-42S4Performing ultraviolet visible diffuse reflection characterization
It can be observed from fig. 4 that all composite samples show a significant red-shift after the introduction of CDs, which is advantageous for enhancing the visible light absorption capacity of the material. Moreover, as the amount of the introduced CDs increases, the color of the sample gradually deepens, and the light absorption of the corresponding composite photocatalyst also gradually increases, which means that the CDs-ZIS composite material is purer than ZnIn under the irradiation of visible light2S4More photo-generated charge may be generated.
(5) To implementationFlower-like CDs-ZIS composite photocatalyst and flower-like ZnIn in example 22S4Performing PL test
As shown in FIG. 5, at an excitation wavelength of 325nm, it can be seen that the fluorescence intensity of 1% CDs-ZIS is significantly lower than that of pure ZnIn2S4It is shown that interface electrons are transferred more effectively due to the introduction of CDs in the CDs-ZIS system, so that the excellent electron transfer characteristics of CDs are fully utilized, PS can be activated effectively, and the photocatalytic activity of the whole reaction system is further improved.
(6) FIG. 6 shows the flower-like CDs-ZIS composite photocatalyst and flower-like ZnIn in example 22S4Transient photocurrent response for several switching cycles under visible light illumination. It is clear that 1% CDs-ZIS is more pure ZnIn2S4The method has higher photocurrent signals, and the combination rate of photo-generated electron-hole pairs is greatly reduced by introducing CDs which are used as storage and transmission centers of electrons.
And, for further validation of the flower-like CDs-ZnIn2S4The inventor also performs the following tests on the application effect of the composite photocatalyst in the field of photocatalysis:
FIG. 7 shows a graph of the photocatalytic degradation of TC by the flower-like CDs-ZIS composite photocatalyst combined with PS under the irradiation of visible light in example 2.
The photocatalytic properties of the already prepared samples, as well as their ability to activate PS, were examined by degradation of TC under visible light irradiation (λ >420 nm).
First, the prepared photocatalyst was placed in 100mL of TC solution (50mg L-1) In the dark, the mixture was stirred for 60 minutes to reach the equilibrium of adsorption and desorption. Subsequently, PS (0.75g L-1) And transferred to a xenon lamp to be stirred for 120 minutes, during which time samples are taken every 20 minutes to be tested and recorded, and finally, the TC degradation rate is calculated at each time point. Under the condition of not adding a catalyst, the degradation effect of pure visible light irradiation on TC is negligible, and the degradation rate of pure PS on TC under the condition of no light irradiation reaches 8%.
In addition, the degradation rate of pure PS to TC under the condition of illumination reaches 20%, which indicates that the visible light can activate the PS. Thus, the degradation capability of 1 percent of CDs-ZIS to tetracycline under the irradiation of visible light is higher than that of pure ZnIn2S4Slightly increased, and the introduction of CDs reduced its adsorption capacity to TC, but this did not affect the increase of the photocatalytic performance of the material.
Further, compared to ZnIn2S4The efficiency of degrading TC by activating PS under the irradiation of visible light can be found to be as high as 84% when 1% of CDs-ZIS is used for activating PS under the irradiation of visible light after CDs are introduced, which indicates that photogenerated electrons are generated from ZnIn2S4The conduction band is enriched on CDs, PS can be effectively activated, and active species of the reaction system are increased, so that the catalytic activity of the whole reaction system is further improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (7)

1. Flower-shaped CDs-ZnIn2S4The preparation method of the composite photocatalyst is characterized by comprising the following steps:
(1) weighing a certain amount of carbon quantum dots (CDs) and zinc acetate dihydrate (Zn (CH)3COO)2·2H2O), indium chloride tetrahydrate (InCl)3·4H2O) and Thioacetamide (TAA) are added into a mixed solution containing ethanol and water at room temperature to be uniformly mixed by ultrasonic waves, and the mixed solution is transferred into a high-pressure reaction kettle to be heated, then cooled to room temperature and centrifugally collected to obtain precipitates;
(2) washing the precipitate with deionized water and ethanol alternately for several times, and vacuum dryingDrying to obtain the flower-shaped CDs-ZnIn2S4A composite photocatalyst is provided.
2. A flower-like CDs-ZnIn according to claim 12S4The preparation method of the composite photocatalyst is characterized in that in the step (1), Zn (CH)3COO)2·2H2O、InCl3·4H2The molar ratio of O to TAA is 1: 2: 4, the amount of CDs added is the ZnIn theoretically obtained2S4The mass is 0.3-3%, and the ultrasonic time is 0.5-1 h.
3. A flower-like CDs-ZnIn according to claim 22S4The preparation method of the composite photocatalyst is characterized in that in the step (1), the heating reaction temperature is 180 ℃, and the reaction time is 22-24 hours.
4. The method for preparing the flower-shaped CDs-ZnIn2S4 composite photocatalyst according to claim 1, wherein in the step (2), the vacuum drying temperature is 50-60 ℃ and the drying time is 12-18 h.
5. A flower-like CDs-ZnIn prepared by the method of claim 12S4The composite photocatalyst is characterized in that the flower-shaped CDs-ZnIn is2S4The composite photocatalyst is prepared from zinc acetate dihydrate (Zn (CH)3COO)2·2H2O), indium chloride tetrahydrate (InCl)3·4H2O), Thioacetamide (TAA) and carbon quantum dots (CDs) are synthesized by a hydrothermal method.
6. A flower-like CDs-ZnIn prepared by the method of claim 12S4Composite photocatalyst or flower-like CDs-ZnIn as claimed in claim 52S4The application of the composite photocatalyst in the field of photocatalysis.
7. The use of claim 6, further comprisingComprises the following steps: the flower-shaped CDs-ZnIn2S4The application of the composite photocatalyst in activating persulfate to carry out photocatalytic degradation on tetracycline under the condition of visible light.
CN202110557854.XA 2021-05-21 2021-05-21 Flower-shaped CDs-ZnIn2S4Composite photocatalyst and preparation method and application thereof Pending CN113231081A (en)

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Application publication date: 20210810