CN105964275B - CuS/CdIn2S4/ZnIn2S4Microwave-assisted one-step synthesis method of composite photocatalyst - Google Patents
CuS/CdIn2S4/ZnIn2S4Microwave-assisted one-step synthesis method of composite photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- 238000001308 synthesis method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 5
- 230000005855 radiation Effects 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 17
- 239000001257 hydrogen Substances 0.000 abstract description 17
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 12
- 229940012189 methyl orange Drugs 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000006303 photolysis reaction Methods 0.000 abstract description 6
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Chemical compound [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 abstract description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
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- 238000010586 diagram Methods 0.000 description 3
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- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 241001556567 Acanthamoeba polyphaga mimivirus Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
- B01J27/045—Platinum group metals
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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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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- 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
- C02F2101/40—Organic compounds containing sulfur
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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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a CuS/CdIn2S4/ZnIn2S4A microwave-assisted one-step synthesis method of a composite photocatalyst belongs to the technical field of chemical industry. By Zn (NO)3)3·6H2O、In(NO3)3·4.5H2O、Cd(NO3)2·4H2O、Cu(NO3)2·3H2O、C2H5NS five chemical reagent raw materials are mixed according to the mass ratio, put into deionized water and stirred uniformly, reacted by microwave radiation in a microwave reactor, repeatedly washed by deionized water and absolute ethyl alcohol respectively, and dried to obtain a final product CuS/CdIn2S4/ZnIn2S4A composite photocatalyst is provided. The surface appearance, microstructure and photocatalytic activity of the photocatalyst are measured, and the product performance is greatly improved in the aspects of degrading organic pollutants methyl orange and photocatalytic hydrogen production by water photolysis. The microwave-assisted one-step synthesis method has the characteristics of short reaction time, uniform generated product, simple and practical production process and the like, and the performance of the sample and the batch production is stable and reliable.
Description
Technical Field
The invention relates to CuS/CdIn2S4/ZnIn2S4Microwave of composite photocatalystAn auxiliary one-step synthesis method belongs to the technical field of chemical industry.
Background
Since 1972 professor Fujishima and Honda discovered the use of TiO2Since the electrode can decompose water to generate hydrogen and oxygen under the irradiation of ultraviolet light, the photocatalysis technology has attracted wide attention of scientists in various countries. However, most of the existing photocatalysts can only be excited by ultraviolet light which only accounts for 3% -5% of sunlight, and most of visible light in the sunlight cannot be effectively utilized, so that research on preparing the high-efficiency photocatalytic material with visible light response is very significant in the aspects of photocatalytic degradation of organic pollutants methyl orange and hydrogen production by water photolysis.
Disclosure of Invention
In order to solve the above problems, the present invention provides a CuS/CdIn2S4/ZnIn2S4The microwave-assisted one-step synthesis method of the composite photocatalyst comprises the steps of, on one hand, ZnIn2S4、CdIn2S4And both the CuS and the composite material have narrower forbidden bandwidth, so that the absorption of the composite material in a visible light region can be effectively improved, and higher sunlight utilization rate can be achieved. On the other hand, ZnIn2S4With CdIn2S4The composite material is compounded with CuS, so that the migration path of photo-generated electrons of the composite material is increased, the multi-path migration of the photo-generated electrons substantially reduces the recombination rate of photo-generated electron-hole pairs, and the photocatalytic reaction efficiency of the composite material is improved. By Zn (NO)3)3·6H2O、In(NO3)3·4.5H2O、Cd(NO3)2·4H2O、Cu(NO3)2·3H2O、C2H5NS five chemical reagent raw materials are mixed according to the mass ratio, put into deionized water and stirred uniformly, reacted by microwave radiation in a microwave reactor, repeatedly washed by deionized water and absolute ethyl alcohol respectively, and dried to obtain a final product CuS/CdIn2S4/ZnIn2S4A composite photocatalyst is provided. The product manufacturing process is simple and practical, the product performance is stable and reliable, and the visible light response is high.
The technical scheme adopted by the invention for solving the technical problems is as follows: CuS/CdIn2S4/ZnIn2S4Microwave-assisted one-step synthesis method of composite photocatalyst, weighing Zn (NO)3)3·6H2O, mass 0.134. + -. 0.001g, In (NO)3)3·4.5H2O, mass 0.382 +/-0.002 g, Cd (NO)3)2·4H2O, mass 0.015. + -. 0.001g, Cu (NO)3)2·3H2O, mass 0.001. + -. 0.0002g and C2H5NS with a mass of 0.225 + -0.002 g. Mixing the above five chemical reagents, adding into 20 + 2mL deionized water, stirring for 20 + 2min, pouring into 100 mL microwave reactor with polytetrafluoroethylene lining, setting microwave hydrothermal reaction temperature at 160 + -2 deg.C, and reaction time at 1.5 + 0.05 h. After the microwave radiation reaction is finished, the generated brown precipitate is repeatedly washed for 4-5 times by using deionized water and absolute ethyl alcohol respectively. Putting the precipitate into a drying box, setting the drying temperature at 60 +/-2 ℃ and the drying time at 12 + 0.1h, and taking out to obtain the final product CuS/CdIn2S4/ZnIn2S4A composite photocatalyst is provided.
The invention has the beneficial effects that: CuS/CdIn with high visible light response is synthesized by adopting microwave-assisted one-step method2S4/ZnIn2S4A composite photocatalyst is provided. The composite material is made of heterogeneous ZnIn2S4Cubic phase CdIn2S4And hexagonal phase CuS, and CdIn2S4And the introduction of CuS improves the absorption of the photocatalyst in the visible light region. CuS/CdIn2S4/ZnIn2S4Maintains a better flower ball-shaped structure and has larger specific surface area. Compared with P25, the composite photocatalyst has a better photodegradation effect on organic pollutant methyl orange under simulated sunlight and visible light. In addition, when Pt is used as a cocatalyst, the composite catalyst is in Na2S-Na2SO3The solution has higher hydrogen production rate under the irradiation of visible light due to CdIn2S4And CuS are introduced, the visible light response range of the composite material is expanded,simultaneously increases the migration path of photo-generated electrons, and inhibits CuS/CdIn2S4/ZnIn2S4The photo-generated electron-hole pair is recombined, so that the photo-catalytic activity is improved. Meanwhile, the microwave-assisted one-step synthesis method has the characteristics of short reaction time, uniform generated product, simple and practical production process and the like, and the performance of the sample and the batch production is stable and reliable.
Drawings
The invention is further described with reference to the following figures and detailed description.
FIG. 1 is a graph of CuS/CdIn2S4/ZnIn2S4A graph of the surface topography of the composite photocatalyst.
FIG. 2 is a graph of CuS/CdIn2S4/ZnIn2S4A second graph of the surface topography of the composite photocatalyst.
FIG. 3 is a graph of CuS/CdIn2S4/ZnIn2S4A diagram of the microstructure of the composite photocatalyst.
FIG. 4 is a graph of CuS/CdIn2S4/ZnIn2S4A second figure of the microstructure of the composite photocatalyst.
FIG. 5 is a graph of CuS/CdIn2S4/ZnIn2S4One of the HRTEM photographs of the composite photocatalyst.
FIG. 6 is a graph of CuS/CdIn2S4/ZnIn2S4HRTEM photograph of the composite photocatalyst.
FIG. 7 direct photodegradation, P25, ZnIn2S4、CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4And (3) simulating a reaction rate graph of sunlight catalytic degradation of methyl orange.
FIG. 8 direct photodegradation, P25, ZnIn2S4、CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4Reaction rate chart of visible light catalytic degradation of methyl orange.
FIG. 9 direct photodegradation, P25, ZnIn2S4、CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4The dynamic result chart of the visible light catalytic degradation of methyl orange is shown.
FIG. 10 shows P25 and ZnIn2S4、CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4In Na2And (3) a hydrogen production rate diagram by photolysis of water in S solution.
FIG. 11 is a 0.2% wt Pt promoter loaded CuS/CdIn2S4/ZnIn2S4In Na2S-Na2SO3An experimental diagram for hydrogen production by photolysis of water in solution.
FIG. 12 is a 0.2% wt Pt promoter loaded CuS/CdIn2S4/ZnIn2S4With Na2S-Na2SO3As a sacrificial agent, the stability results of the catalyst for hydrogen production by photolysis of water under visible light irradiation of more than 420 nm.
Detailed Description
CuS/CdIn2S4/ZnIn2S4The microwave-assisted one-step synthesis method of the composite photocatalyst comprises weighing 99.0% of Zn (NO) purchased from Tianjin City of Tongli district chemical reagent factory3)3·6H2O, 0.1339g In (NO) 99.5% by mass of chemical reagent group, Inc. of Shanghai city3)3·4.5H2O, Cd (NO) with a mass of 0.3819 g and a purity of 99.0% of Mimi chemical reagent available in Tianjin3)2·4H2O, Cu (NO) 0.0154g in mass and 99.5% in Tianjin from Natural chemical reagents, Inc3)2·3H2O, 0.001g by mass and 99.0% C available from Kemiou Chemicals Co., Ltd, Tianjin2H5NS with a mass of 0.2254 g. The five chemical reagent raw materials are mixed and put into 20mL of deionized water, the mixture is fully stirred for 20min and then poured into a 100 mL microwave reactor with a polytetrafluoroethylene lining, an MDS-8G type microwave reactor of Shanghai New Instrument microwave chemistry Co., Ltd is selected, the microwave hydrothermal reaction temperature is set to be 160 ℃, and the reaction time is 1.5 h. Microwave radiationAfter the completion of the irradiation reaction, the resulting brown precipitate was repeatedly washed with deionized water and absolute ethanol for 4 times, respectively. Filtering the precipitate, putting the precipitate into a drying box, setting the drying temperature to be 60 ℃, drying for 12h, taking out to obtain the final product of CuS/CdIn2S4/ZnIn2S4A composite photocatalyst is provided.
CuS/CdIn2S4/ZnIn2S4And (3) measuring the structure and the performance of the composite photocatalyst:
surface topography and microstructure
CuS/CdIn2S4/ZnIn2S4The results of the surface topography and microstructure analysis of the samples are shown in FIGS. 1-6. As clearly seen from fig. 1 and 2, the sample showed a more regular petal-like spherical structure, and the spheres had a diameter of about 600 nm and had good dispersibility between the spheres. Meanwhile, TEM results of the images in the figures 3 and 4 show that the microstructure of the sample is mainly formed by uniformly stacking irregular blocky crystals and rod-shaped crystals with the length of 100-200 nm, and a large number of nanoparticles with the diameter of 5 nm are distributed on the surfaces of the blocky crystals and the long rod-shaped crystals. FIG. 5 and FIG. 6 show the CuS/CdIn sample2S4/ZnIn2S4Inset is a Fast Fourier Transform (FFT) image of the selected region.
Secondly, measuring the photocatalytic performance
Commercial P25, elemental ZnIn2S4Double CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4The photocatalytic activity of the organic compound is subjected to photocatalytic experiments for degrading organic pollutants methyl orange and producing hydrogen by photolyzing water.
1. The degradation of organic pollutant methyl orange is shown in figure 7 and figure 8, and CuS/CdIn2S4/ZnIn2S4The composite material shows the highest photocatalytic activity on the degradation of methyl orange under simulated sunlight and visible light, and far exceeds the commercial P25. In addition, the effect of different samples on the rate of degradation of methyl orange is shown in FIG. 9. According to the formula and experimental data-ln(C t /C 0 )=kt+bA calculation is performed in which, among other things,C t is a dye intConcentration at time (mg. L)-1)，C 0 Is the initial concentration of the dye (mg. L)-1)，kIs the rate constant (min)-1)，bIs the intercept. As can be seen from the view in figure 9,-ln(C t /C 0 )with reaction timetThe relationship is basically linear, which shows that the degradation of the dye methyl orange follows the quasi-first order reaction kinetics. Calculated, direct photodegradation, P25, ZnIn2S4、CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4The apparent reaction rate constants of the visible light photocatalytic degradation of methyl orange are respectively 5.67 multiplied by 10-5、4.95×10-4、5.34×10-3、6.20×10-3And 8.96X 10-3 min-1。
2. Photolysis of water to produce P25 and ZnIn2S4、CdIn2S4/ZnIn2S4And CuS/CdIn2S4/ZnIn2S4Different samples are in Na2The results of the hydrogen production rate in the S solution are shown in fig. 10. The results show that CuS/CdIn2S4/ZnIn2S4The composite material has the best hydrogen production capacity, and the hydrogen production rate is 15 times of that of P25. The inset shows that CuS/CdIn2S4/ZnIn2S4In Na2S-Na2SO3The hydrogen production rate in the solution is higher than that of Na2S or Na2SO3A single solution of (A), demonstrates Na2S and Na2SO3There is a synergistic effect in the photocatalytic process. In order to further improve the hydrogen production capability of the photocatalyst, Pt is taken as a cocatalyst and is loaded on the sample CuS/CdIn by a photoreduction method2S4/ZnIn2S4The results are shown in fig. 11. 0.2% wt Pt loaded, CuS/CdIn2S4/ZnIn2S4The hydrogen production rate reaches 358.4 mu mol.h-1·g-1The efficiency is improved by 6 times compared with that before the load. Pt loaded CuS/CdIn after use of a 420 nm cut-off filter2S4/ZnIn2S4The hydrogen production rate can still reach 233.9 mu mol.h-1·g-1Indicating that the sample has a higher visible response. To investigate Pt-loaded CuS/CdIn2S4/ZnIn2S4Photocatalytic stability of (1) with Na2S-Na2SO3As a sacrificial agent, the hydrogen is continuously produced for 24 hours under the irradiation of visible light with the wavelength of more than 420 nm. Fig. 12 shows that the sample still maintains certain photocatalytic stability after 24 h of hydrogen production, the crystal structure before and after photocatalytic reaction is not greatly changed, and the inset shows the XRD spectrogram of the sample before and after reaction.
Claims (2)
1. CuS/CdIn2S4/ZnIn2S4The microwave-assisted one-step synthesis method of the composite photocatalyst is characterized by comprising the following steps of: weighing Zn (NO)3)3·6H2O, mass 0.134. + -. 0.001g, In (NO)3)3·4.5H2O, mass 0.382 +/-0.002 g, Cd (NO)3)2·4H2O, mass 0.015. + -. 0.001g, Cu (NO)3)2·3H2O, mass 0.001. + -. 0.0002g and C2H5NS with the mass of 0.225 plus or minus 0.002 g; mixing the five chemical reagent raw materials, putting the mixture into 20 +/-2 mL of deionized water, fully stirring the mixture for 20 +/-2 min, pouring the mixture into a 100 mL of microwave reactor with a polytetrafluoroethylene lining, setting the microwave hydrothermal reaction temperature to be 160 +/-2 ℃ and the reaction time to be 1.5 +/-0.05 h; after the microwave radiation reaction is finished, repeatedly washing the generated brown precipitate for 4-5 times by using deionized water and absolute ethyl alcohol respectively; putting the precipitate into a drying box, setting the drying temperature to be 60 +/-2 ℃, drying for 12 +/-0.1 h, and taking out to obtain a final product CuS/CdIn2S4/ZnIn2S4A composite photocatalyst is provided.
2. The CuS/CdIn of claim 12S4/ZnIn2S4The microwave-assisted one-step synthesis method of the composite photocatalyst is characterized by comprising the following steps of: zn (NO)3)3·6H2O, mass 0.1339g、In(NO3)3·4.5H2O, mass 0.3819 g, Cd (NO)3)2·4H2O, mass 0.0154g, Cu (NO)3)2·3H2O, mass 0.001g and C2H5NS with the mass of 0.2254 g; mixing, putting into 20mL of deionized water, fully stirring for 20min, and pouring into a 100 mL microwave reactor, wherein the reaction temperature is 160 ℃, and the reaction time is 1.5 h; after the reaction is finished, repeatedly washing the product for 4 times by using deionized water and absolute ethyl alcohol respectively; and (4) filtering and putting the precipitate into a drying box, setting the drying temperature to be 60 ℃, and drying for 12 h.
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| CN109847781A (en) * | 2019-01-30 | 2019-06-07 | 太原理工大学 | A kind of CdIn2S4/g-C3N4The preparation method and applications of composite photo-catalyst |
| CN109821562B (en) * | 2019-04-09 | 2021-08-24 | 淮北师范大学 | MoP-Zn3In2S6Preparation method of composite nano material |
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| ZnIn2S4光催化剂的制备及光催化分解硫化氢的研究;单雯妍;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20101115(第11期);第58页 * |
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