CN115400768A - Heterojunction CdIn 2 S 4 /Bi 2 WO 6 Application of piezoelectric-optical composite catalyst in piezoelectric photodegradation of organic matters - Google Patents

Heterojunction CdIn 2 S 4 /Bi 2 WO 6 Application of piezoelectric-optical composite catalyst in piezoelectric photodegradation of organic matters Download PDF

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CN115400768A
CN115400768A CN202211089067.8A CN202211089067A CN115400768A CN 115400768 A CN115400768 A CN 115400768A CN 202211089067 A CN202211089067 A CN 202211089067A CN 115400768 A CN115400768 A CN 115400768A
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马江权
孙桂芳
李楠
吴棉棉
沈文静
史明豪
李庆飞
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Changzhou University
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Abstract

The invention belongs to the field of piezoelectric photocatalysts, and particularly relates to heterojunction CdIn 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in the piezoelectric photodegradation of organic matters. A CIS/BWO composite catalyst is synthesized by a simple impregnation method, and rhodamine B is subjected to piezoelectric photocatalysis degradation under the synergistic effect of sunlight irradiation and ultrasonic vibration. CdIn 2 S 4 And Bi 2 WO 6 Can be well combined to form a typical type II heterojunction, thereby accelerating the separation speed of electrons and holes. Meanwhile, the method is green and pollution-free, and the prepared catalyst has the characteristics of rich active sites, no secondary pollution and the like.

Description

Heterojunction CdIn 2 S 4 /Bi 2 WO 6 Application of piezoelectric-optical composite catalyst in piezoelectric photodegradation of organic matters
Technical Field
The invention belongs to the field of piezoelectric photocatalysts and application thereof, and particularly relates to a II-type heterojunction CdIn for degrading rhodamine B by piezoelectric light 2 S 4 /Bi 2 WO 6 (CIS/BWO) composite catalyst and a method for preparing the same.
Background
In recent years, the problems of ecological environment pollution and energy resource shortage are becoming more and more serious, and the pollution caused by organic dyes in industrial wastewater cannot be ignored, so that the application of the organic pollutant problem solving through the electro-optical photocatalysis is receiving wide attention. The piezoelectric catalysis means that an electric field is formed on the surface of catalyst particles under the induction of mechanical vibration energy of a piezoelectric material to generate an active substance with redox capability, and then the dye is subjected to redox reaction to achieve the purpose of degrading organic pollutants. On the one hand, many factors influence the piezo-catalytic efficiency, such as catalyst morphology, internal carrier separation efficiency, and active species, among others. On the other hand, the piezoelectric catalysis and the photocatalysis are combined, so that the piezoelectric catalytic degradation performance can be greatly improved. However, the construction of a high efficiency piezoelectric photocatalyst has remained a great problem so far.
Recently, bi 2 WO 6 The photocatalyst is an oxide with a layered structure, has good photocatalytic performance under the irradiation of visible light, has a band gap of about 2.7eV, and has the advantages of no toxicity, high light stability, thermal stability and environmental friendliness. The pure BWO has higher recombination rate of photo-generated electrons and holes, thus hindering the catalytic activity and limiting the large-scale application on the catalytic performance. The catalytic performance can be effectively improved by constructing a II type heterojunction composite material with abundant electron capture as an active site of the oxidation-reduction reaction. In semiconductor photocatalysts, metal sulfides are of interest because of their appropriate band gap and good coefficients. Firstly, the methodTernary sulfides with strong visible absorption and narrow forbidden bands are becoming the focus of research. CdIn 2 S 4 Nanomaterials are used in many applications such as light emitting diodes, photocatalysts, solar cells, photovoltaic applications, and the like. CdIn 2 S 4 Is AB 2 C 4 The family members of the ternary compound have direct band gaps (1.95-2.4 eV), and show good photocatalytic activity under visible light.
Therefore, the invention adopts a hydrothermal method to prepare the excellent II-type heterojunction CIS/BWO composite material. The electron transfer rate of BWO and CIS can be more efficiently promoted by constructing a type II heterojunction. Further explores the degradation efficiency of the CIS/BWO composite material on organic pollutants in photocatalysis, piezoelectric catalysis and piezoelectric-photocatalysis. The result shows that the CIS/BWO composite material shows remarkable piezoelectric photocatalytic efficiency and strong stability in the aspect of degrading organic pollutants, and the excellent II-type heterojunction composite material is proved to have good application prospect in treating pollutants.
Disclosure of Invention
The invention aims to provide a CIS/BWO composite catalyst and a preparation method thereof, and the CIS/BWO composite catalyst is applied to piezoelectric light to degrade rhodamine B and has high catalytic activity and better stability.
The technical scheme of the invention is as follows: the preparation method of the CIS/BWO composite catalyst provided by the invention comprises the following steps:
(1)Bi 2 WO 6 preparation: adding a bismuth source and a tungsten source into deionized water, stirring and dissolving at room temperature, transferring the mixed solution into a reaction kettle lined with polytetrafluoroethylene, and carrying out hydrothermal reaction in an oven; cooling to room temperature, filtering, washing, drying and grinding to obtain white powder, namely Bi 2 WO 6 A catalyst (BWO);
Bi(NO 3 ) 3 ·5H 2 o as a bismuth source; na (Na) 2 WO 4 ·2H 2 O is used as a tungsten source; wherein Bi (NO) 3 ) 3 ·5H 2 O and Na 2 WO 4 ·2H 2 The mass ratio of O is 2.9:1, the hydrothermal reaction temperature is 190 ℃, and the reaction time is 2h.
(2)CdIn 2 S 4 Preparation: adding thiourea, cadmium chloride and indium (III) chloride tetrahydrate into deionized water, carrying out ultrasonic treatment for 0.5h to completely dissolve the thiourea, the cadmium chloride and the indium (III) chloride tetrahydrate, transferring the obtained transparent solution into a reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction in an oven; after cooling to room temperature, filtering, washing, drying and grinding to finally obtain yellow powder, namely the CdIn 2 S 4 A catalyst;
mixing thiourea, cadmium chloride and indium (III) chloride tetrahydrate at a molar ratio of 4:1:2; the hydrothermal reaction temperature is 150-220 ℃, preferably 180 ℃ and the reaction time is 48h.
(3) Preparing a CIS/BWO composite catalyst: cdIn is mixed with 2 S 4 Dissolving the catalyst and the BWO catalyst in absolute ethyl alcohol, stirring and mixing for 10-12 h at room temperature until the absolute ethyl alcohol is volatilized, filtering, washing, drying for 10-12 h at 60 ℃ in a vacuum drying oven, and grinding into powder to finally obtain brown powder, namely the CIS/BWO composite catalyst. CdIn added 2 S 4 Mass is Bi 2 WO 6 5 to 15 percent of the mass.
The CIS/BWO composite catalyst prepared by the method has a nanosheet integrated flower-ball-shaped structure.
The invention has the advantages that:
(1) The catalyst provided by the invention is a CIS/BWO composite catalyst, and has the characteristics of simple synthesis conditions, easy operation, high speed, high efficiency, energy conservation, environmental protection, good stability and the like; cdIn 2 S 4 The introduction of the catalyst does not change the crystal structure of BWO, and other diffraction peaks do not appear, indicating that the CIS/BWO composite material has excellent crystallinity and purity. The CIS is added to change the piezoelectricity of the compound, and meanwhile, a II-type heterojunction is formed between the CIS and BWO, so that the degradation capability under the piezoelectric-optical action is obviously improved.
(2) 10% of the CIS/BWO composite catalyst was able to degrade most of the organic substances within 15min under the synergistic effect of pure photocatalysis, pure piezoelectric catalysis and piezoelectricity-photocatalysis, the degradation ability was strong, the efficiency of degrading RhB was higher than that of pure BWO, indicating that CdIn 2 S 4 Loading on BWO can improve degradation efficiency,the catalyst is shown to have obvious effect of degrading RhB under the piezoelectric-optical synergistic effect.
Description of the drawings:
FIG. 1 is an XRD pattern of synthesized CIS/BWO catalyst and BWO in different ratios.
FIG. 2 is a scanning electron micrograph of the BWO catalyst synthesized in example 1.
FIG. 3 is a scanning electron micrograph of the 10% CIS/BWO catalyst synthesized in example 7.
FIG. 4 is a graph of rhodamine B degradation performance of CIS/BWO catalysts and BWO at different ratios under sunlight irradiation.
FIG. 5 is a diagram of the performance of different proportions of CIS/BWO catalyst and BWO in degrading rhodamine B under ultrasonic vibration.
FIG. 6 is a performance diagram of degraded rhodamine B of CIS/BWO catalysts and BWO in different proportions under the effects of sunlight irradiation and ultrasonic vibration.
FIG. 7 is a hysteresis curve diagram of 10% CIS/BWO catalyst and BWO.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The degradation efficiency is calculated according to the following formula:
R＝(C-C 0 )/C 0 *100％
r degradation efficiency
C 0 Initial concentration
C concentration after degradation reaction
Example 1
Weighing 1.94g Bi (NO) 3 ) 3 ·5H 2 Dissolving O in 50ml deionized water, stirring to dissolve, adding 0.66g Na 2 WO 4 ·2H 2 O is added to the mixture and stirred vigorously for 1h at room temperature. Transferring the mixed solution into a 100ml reaction kettle lined with polytetrafluoroethylene, heating in an oven at 190 ℃ for 2h, cooling to room temperature, filtering, washing, drying and grinding to finally obtain white powder, namely BWO powder.
Weighing 10mg BWO powder catalyst and 30ml 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under sunlight irradiation, taking a sample every 5min, calculating degradation efficiency by measuring absorbance, and analyzing to obtain the degradation efficiency of 31.8%.
Weighing 10mg BWO powder catalyst and 30ml 10mol/L rhodamine B, stirring for 30min under dark condition to reach adsorption-desorption balance, degrading for 15min under ultrasonic vibration (240W, 40 kHz), sampling every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 19.8%.
Example 2
CdIn 2 S 4 Preparation: adding 0.3045g of thiourea, 0.2283g of cadmium chloride and 0.5864g of indium (III) chloride tetrahydrate into 30mL of deionized water, carrying out ultrasonic treatment for 0.5h to completely dissolve the thiourea, transferring the obtained transparent solution into a reaction kettle with a polytetrafluoroethylene lining, and carrying out hydrothermal reaction in an oven at 180 ℃ for 48h; after cooling to room temperature, filtering, washing, drying and grinding to finally obtain yellow powder, namely CdIn 2 S 4 A catalyst;
the photocatalyst conditions were the same as in example 1: weighing 10mg CdIn 2 S 4 Stirring a powder catalyst and 30ml of 10mol/L rhodamine B for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under the irradiation of sunlight, taking a sample every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 15.8%.
The ultrasonic vibration conditions were the same as in example 1: weighing 10mg CdIn 2 S 4 The powder catalyst and 30ml of 10mol/L rhodamine B are stirred for 30min under the dark state condition to reach adsorption-desorption balance, the degradation is carried out for 15min under the ultrasonic vibration (240W, 40kHz), samples are taken every 5min, the degradation efficiency is calculated by measuring the absorbance, and the degradation efficiency is 8.2% by analysis.
Example 3
Otherwise, the same procedure as in example 1 was repeated to obtain a white powder, i.e., BWO powder.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, simultaneously degrading for 15min under sunlight irradiation and ultrasonic vibration, taking a sample every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 66%.
Example 4
Otherwise, the same procedure as in example 1 was repeated to obtain a white powder, i.e., BWO powder. Thiourea (4 mmol), cadmium chloride (1 mmol) and indium (III) chloride tetrahydrate (2 mmol) were added to 30mL of deionized water and sonicated for 0.5h to dissolve completely. Transferring the mixed solution into a 100ml reaction kettle with a polytetrafluoroethylene lining, heating in an oven at 180 ℃ for 48h, cooling to room temperature, filtering, washing, drying and grinding to obtain yellow powder, namely CdIn 2 S 4 A catalyst. Then, 1g BWO and 0.05g CdIn were weighed out 2 S 4 Dissolving in certain amount of anhydrous ethanol, vigorously stirring the above mixture at room temperature overnight (12H), filtering at room temperature, washing, drying at 60 deg.C overnight (12H), and grinding to obtain 5%1T/2H MS/BWO brown powder.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under sunlight irradiation, sampling every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 39.9%.
Example 5
Otherwise, in the same manner as in example 4, 5% of a CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under ultrasonic vibration, taking samples every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 23.6%.
Example 6
Otherwise, in the same manner as in example 4, 5% of a CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, simultaneously degrading for 15min under sunlight irradiation and ultrasonic vibration, taking a sample every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 87%.
Example 7
Weighing 1g BWO and 0.1g CdIn 2 S 4 Otherwise, the same procedure as in example 4 was repeated, except that 10% of CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under sunlight irradiation, taking samples every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 57.6%.
Example 8
Otherwise, in the same manner as in example 7, 10% of a CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under ultrasonic vibration, sampling every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 32.4%.
FIG. 7 is a hysteresis loop diagram of the 10-percent CIS/BWO catalyst and BWO; it can be seen that the incorporation of CIS changes the piezoelectricity of the composite.
Example 9
Otherwise, in the same manner as in example 7, 10% of a CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, simultaneously degrading for 15min under sunlight irradiation and ultrasonic vibration, taking a sample every 5min, calculating degradation efficiency by measuring absorbance, and obtaining the degradation efficiency of 99.9% by analysis, thereby basically realizing complete degradation.
Stability test: after repeating the stability experiment for four times, the degradation effect in piezoelectric photocatalysis for 15min can reach 99%, and the stability is excellent.
Example 10
Weighing 1g of Bi 2 WO 6 And 0.15g of CdIn 2 S 4 The other same as example 4, 15% CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under sunlight irradiation, taking samples every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 35.2%.
Example 11
The same procedure as in example 10 was repeated, except that 15% of CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, degrading for 15min under ultrasonic vibration, taking samples every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 22.5%.
Example 12
The same procedure as in example 10 was repeated, except that 15% of CIS/BWO brown powder was obtained.
Weighing 10mg of catalyst and 30ml of 10mol/L rhodamine B, stirring for 30min under a dark state condition to achieve adsorption-desorption balance, simultaneously degrading for 15min under sunlight irradiation and ultrasonic vibration, taking a sample every 5min, measuring absorbance, calculating degradation efficiency, and analyzing to obtain the degradation efficiency of 81.1%.
The best rate of 10% from the degradation efficiency was obtained, CIS/BWO.

Claims (6)

1. Typical type II heterojunction CdIn 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in the piezoelectric photodegradation of organic matters is characterized in that: preparation of Bi separately 2 WO 6 、CdIn 2 S 4 Mixing CdIn 2 S 4 And Bi 2 WO 6 Dissolving in absolute ethyl alcohol, stirring, mixing, filtering at room temperature, washing, drying, and grinding to obtain CdIn 2 S 4 /Bi 2 WO 6 And (3) compounding a catalyst.
2. The typical type II heterojunction CdIn of claim 1 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in the piezoelectric photodegradation of organic matters is characterized in that: the stirring condition is that the mixture is stirred for 10 to 12 hours at room temperature until the absolute ethyl alcohol solvent is volatilized.
3. The typical type II heterojunction CdIn of claim 1 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in the piezoelectric photodegradation of organic matters is characterized in that: the drying condition is that the drying is carried out for 10 to 12 hours at the temperature of 60 ℃.
4. The typical type II heterojunction CdIn of claim 1 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in the piezoelectric photodegradation of organic matters is characterized in that: cdIn 2 S 4 Is Bi 2 WO 6 5 to 15 percent of the mass.
5. The typical type II heterojunction CdIn of claim 4 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in the piezoelectric photodegradation of organic matters is characterized in that: cdIn 2 S 4 Mass is Bi 2 WO 6 10% by mass.
6. A typical type II heterojunction CdIn as claimed in any one of claims 1 to 5 2 S 4 /Bi 2 WO 6 The application of the piezoelectric-optical composite catalyst in piezoelectric photodegradation of organic matters is characterized in that the catalyst is weighed and added into organic pollutants, stirred under a dark condition to achieve adsorption-desorption balance, and degraded under sunlight irradiation and ultrasonic vibration.
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