CN113042102A - Preparation method of CdS-PDA-RGO photoelectric catalytic material and application of CdS-PDA-RGO photoelectric catalytic material in degradation of organic pollutants - Google Patents
Preparation method of CdS-PDA-RGO photoelectric catalytic material and application of CdS-PDA-RGO photoelectric catalytic material in degradation of organic pollutants Download PDFInfo
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
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- B01J35/33—
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- B01J35/39—
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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
-
- 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
Abstract
A preparation method of a CdS-PDA-RGO photoelectric catalytic material and application thereof in degrading organic pollutants. Firstly, preparing a CdS precursor reaction solution by adopting a mixed solution of cadmium nitrate, thiourea and glutathione, and then preparing a CdS film by utilizing a hydrothermal reaction; then immersing the CdS film into a solution of tris (hydroxymethyl) aminomethane and dopamine, and loading a Polydopamine (PDA) organic semiconductor polymer prepared at room temperature onto the CdS film; and finally, ultrasonically dispersing Reduced Graphene Oxide (RGO) in water and grafting the RGO on the surface layer of the CdS-PDA film by an electrodeposition method to obtain the CdS-PDA-RGO photoelectric catalytic material. The prepared CdS-PDA-RGO photoelectric catalyst has the advantages of simple preparation process, mild reaction conditions, no toxicity and no pollution, and the degradation rate of methylene blue within 5 hours is 96% under the irradiation of 1.1V external bias and simulated sunlight, and is improved by 1.75 times compared with the degradation rate of unmodified CdS.
Description
Technical Field
The invention belongs to the field of hydrogen production by using a photoelectric catalytic material, and particularly relates to a preparation method of a CdS-PDA-RGO photoelectric catalytic material and application of the CdS-PDA-RGO photoelectric catalytic material in degradation of organic pollutants.
Background
With the economic development and the acceleration of the global industrialization process, the environmental pollution, especially the water pollution, is increasingly serious, and the realization of the efficient recycling of sewage and water resources at low cost is urgent. The semiconductor photoelectrocatalysis technology combines photocatalysis and electrochemistry, and a double-electrode system is constructed, so that toxic and harmful pollutants are changed into carbon dioxide, water and other harmless substances by using an oxidation-reduction reaction to realize the treatment of organic sewage. The technology has the advantages of mild reaction conditions, low energy consumption, simple and convenient operation and no secondary pollution. However, the current photoelectrocatalysis efficiency and degradation rate are still lower, the cost is higher, and a great gap is still left between the photoelectrocatalysis efficiency and the degradation rate and the photoelectrocatalysis rate is used for industrial production. Therefore, a novel high-efficiency photoelectrode material is developed, surface modification and modification are carried out on the material to increase the separation and transfer efficiency of photon-generated carriers, the real application of a photoelectrocatalysis technology is realized, and the photoelectrode material has important practical significance for treating organic pollutants in water.
Cadmium sulfide (CdS) is favored by people due to its appropriate forbidden bandwidth (-2.4 eV), wide visible light absorption range and high photocatalytic activity, making it possible to apply to industrial production in large quantities in the future. However, the CdS still has the following two defects to limit the application of the CdS: (1) the recombination probability of photo-generated electrons and holes generated by CdS is high, so that the photoelectrocatalysis performance of the CdS is limited; (2) the sulfur ions in ZnS are easy to react with photo-generated holes under the action of water and oxygen in the solution to generate a photo-corrosion phenomenon, so that the light stability of the ZnS is poor. In view of the defects, researchers adopt modification approaches such as morphology control, element doping, surface modification and heterostructure construction on semiconductors, and improve the stability of the semiconductors on the basis of improving the photoelectric catalytic activity of the semiconductors.
Meanwhile, the organic semiconductor material becomes a research hotspot of the photoelectric catalytic composite material due to the characteristics of better flexibility, low price, stable chemical performance and the like. However, most organic semiconductors have complicated preparation processes, long reaction time and pollution to the environment, so that the search for an organic semiconductor catalytic material which has a simple preparation process, low price and no pollution to the environment is very important. The semiconductor loaded by the adsorbent is a new idea for improving the catalytic activity of the semiconductor, and the adsorbent serving as a carrier generally has the advantages of large specific surface area, strong adsorption performance, high stability, low price and the like. The adsorbent carrier is modified by compounding the CdS-based photoelectric catalytic material, more carbon materials are adopted, the active carbon loads the CdS-based photoelectrode, reactants are adsorbed on the carbon materials and then are transmitted to the CdS surface through an interface, and the active carbon and the CdS-based photoelectrode generate a synergistic effect, so that the photoelectric catalytic activity is improved.
Disclosure of Invention
In view of the above, the present invention aims to provide a preparation method of a CdS-PDA-RGO photoelectrocatalysis material and an application thereof in degrading organic pollutants, wherein the prepared photoelectrocatalysis material has high catalytic activity and degradation rate.
In order to achieve the above object, the CdS-PDA-RGO photoelectrocatalysis material and the preparation method thereof provided by the invention comprise the following steps in sequence:
(1) dissolving cadmium nitrate tetrahydrate in deionized water to prepare a cadmium nitrate solution, dissolving thiourea in the deionized water to prepare a thiourea solution, dissolving glutathione in the deionized water to prepare a glutathione solution, and then slowly dropping the thiourea solution and the glutathione solution into a zinc acetate solution to prepare a CdS precursor reaction solution.
(2) Putting clean FTO glass into a hydrothermal kettle inner container, adding a proper amount of CdS precursor reaction liquid, carrying out hydrothermal reaction for a certain time at a certain temperature, taking out a sample after the reaction, and air-drying to obtain the CdS/FTO film.
(3) Dissolving a certain amount of trihydroxymethyl aminomethane and dopamine in deionized water, mechanically stirring at room temperature, reacting for a period of time to obtain Polydopamine (PDA) copolymer, immersing the CdS/FTO film in the solution, and continuously stirring for a period of time to obtain the CdS photoelectrode with PDA loaded on the surface.
(4) Dissolving a certain amount of Reduced Graphene Oxide (RGO) prepared by a Hummers method in deionized water, performing ultrasonic treatment for a period of time to prepare an RGO solution, and adding a certain amount of Na2SO4Adding into the above mixed solution to obtain RGO and Na2SO4The mixed solution of (1). It was transferred to a quartz electrolytic cell as an electrolyte. And adopting an electrochemical deposition method, and taking the CdS-PDA as a working electrode, Pt as a counter electrode and Ag/AgCl as a reference electrode. Depositing for a period of time under a certain voltage, and loading RGO on the surface of the PDA layer to obtain the CdS-PDA-RGO photoelectric catalytic material.
In the step (1), the solubilities of the cadmium nitrate, the thiourea and the glutathione are respectively 0.01-0.05M, 0.01-0.05M and 0.016-0.020M.
In the step (2), the temperature and the time of the hydrothermal reaction are respectively 100-140 ℃ and 6-10 h.
In the step (3), the concentrations of the tris and the dopamine are 0.010-0.030M and 0.024-0.028M respectively, and the stirring time is 4-12 hours after the tris and the dopamine are immersed in the CdS electrode.
In step (4), the RGO solution has a concentration of 100mg/L, and the Na is2SO4The concentration of the solution is 0.5M, and the time for loading RGO by the electrodeposition method is 5-15 min.
The CdS-PDA-RGO photoelectric catalytic material and the preparation method thereof provided by the invention select PDA as an organic semiconductor catalyst, and have the advantages of simple preparation process, mild reaction condition, low price and low requirement on instruments and equipment. Meanwhile, the electrochemical deposition method has low manufacturing cost and simple and convenient operation, can ensure that RGO is uniformly distributed on the CdS-PDA film surface layer, and effectively improves the photoelectric catalytic activity. The degradation rate of the prepared CdS-PDA-RGO photoelectric catalytic material to methylene blue within 5h under the irradiation of simulated sunlight is 96%, and compared with the degradation rate of unmodified CdS, the degradation rate is improved by 1.75 times.
Drawings
FIG. 1 is a graph comparing the photo-catalytic degradation curves of CdS and CdS-PDA-RGO.
Detailed Description
The present invention will be described in detail with reference to the following specific examples:
the first embodiment is as follows:
(1) dissolving cadmium nitrate tetrahydrate in deionized water to prepare 0.01M cadmium nitrate solution, dissolving thiourea in deionized water to prepare 0.01M thiourea solution, dissolving glutathione in deionized water to prepare 0.016M glutathione solution, and then slowly dripping the thiourea solution and the glutathione solution into zinc acetate solution to prepare CdS precursor reaction liquid.
(2) And (3) putting the clean FTO glass into a hydrothermal kettle inner container, adding a proper amount of CdS precursor reaction liquid, carrying out hydrothermal reaction for 6 hours at 100 ℃, taking out a sample after the reaction, and air-drying to obtain the CdS/FTO film.
(3) Dissolving trihydroxymethyl aminomethane and dopamine in deionized water to prepare 0.010M trihydroxymethyl aminomethane and 0.024M dopamine solution, mechanically stirring at room temperature, reacting for 0.5h to obtain Polydopamine (PDA) copolymer, immersing the CdS/FTO film in the solution, and continuously stirring for 4h to obtain the CdS photoelectrode modified by PDA.
(4) Dissolving RGO in deionized water, ultrasonic treating for 1 hr to obtain RGO solution, adding Na2SO4Adding into the above mixed solution to obtain 100mg/L RGO and 0.5M Na2SO4The mixed solution adopts an electrochemical deposition method, and the CdS-PDA is taken as a working electrode, Pt is taken as a counter electrode, and Ag/AgCl is taken as a reference electrode. Depositing for 5min under the voltage of 1.1V, and loading RGO on the surface of the PDA layer to obtain the CdS-PDA-RGO photoelectric catalytic material.
Example two:
(1) dissolving cadmium nitrate tetrahydrate in deionized water to prepare 0.03M cadmium nitrate solution, dissolving thiourea in deionized water to prepare 0.03M thiourea solution, dissolving glutathione in deionized water to prepare 0.018M glutathione solution, and then slowly dripping the thiourea solution and the glutathione solution into zinc acetate solution to prepare CdS precursor reaction liquid.
(2) And (3) putting the clean FTO glass into a hydrothermal kettle inner container, adding a proper amount of CdS precursor reaction liquid, carrying out hydrothermal reaction for 8 hours at 120 ℃, taking out a reacted sample, and air-drying to obtain the CdS/FTO film.
(3) Dissolving trihydroxymethyl aminomethane and dopamine in deionized water to prepare 0.020M trihydroxymethyl aminomethane and 0.026M dopamine solution, mechanically stirring at room temperature, reacting for 0.5h to obtain Polydopamine (PDA) copolymer, immersing the CdS/FTO film in the solution, and continuously stirring for 8h to obtain the CdS photoelectrode modified by PDA.
(4) Dissolving RGO in deionized water, ultrasonic treating for 1 hr to obtain RGO solution, adding Na2SO4Adding into the above mixed solution to obtain 100mg/L RGO and 0.5M Na2SO4The mixed solution adopts an electrochemical deposition method, and the CdS-PDA is taken as a working electrode, Pt is taken as a counter electrode, and Ag/AgCl is taken as a reference electrode. Depositing for 10min under the voltage of 1.1V, and loading RGO on the surface of the PDA layer to obtain the CdS-PDA-RGO photoelectric catalytic material.
Example three:
(1) dissolving cadmium nitrate tetrahydrate in deionized water to prepare 0.05M cadmium nitrate solution, dissolving thiourea in deionized water to prepare 0.05M thiourea solution, dissolving glutathione in deionized water to prepare 0.022M glutathione solution, and then slowly dripping the thiourea solution and the glutathione solution into zinc acetate solution to prepare CdS precursor reaction liquid.
(2) And (3) putting the clean FTO glass into a hydrothermal kettle inner container, adding a proper amount of CdS precursor reaction liquid, carrying out hydrothermal reaction for 10 hours at 140 ℃, taking out a reacted sample, and air-drying to obtain the CdS/FTO film.
(3) Dissolving trihydroxymethyl aminomethane and dopamine in deionized water to prepare 0.030M trihydroxymethyl aminomethane and 0.028M dopamine solution, mechanically stirring at room temperature, reacting for 0.5h to obtain Polydopamine (PDA) copolymer, immersing the CdS/FTO film in the solution, and continuously stirring for 12h to obtain the CdS photoelectrode modified by PDA.
(4) Dissolving RGO in deionized water, ultrasonic treating for 1 hr to obtain RGO solution, adding Na2SO4Adding into the above mixed solution to obtain 100mg/L RGO and 0.5M Na2SO4The mixed solution adopts an electrochemical deposition method, and the CdS-PDA is taken as a working electrode, Pt is taken as a counter electrode, and Ag/AgCl is taken as a reference electrode. Depositing for 15min under the voltage of 1.1V, and loading RGO on the surface of the PDA layer to obtain the CdS-PDA-RGO photoelectric catalytic material.
To verify the effect of the present invention, the inventors have shown the photo-catalytic degradation curves of CdS and CdS-PDA-RGO prepared in example 1 above, as shown in FIG. 1.
Claims (5)
1. A preparation method of CdS-PDA-RGO photoelectric catalytic material and its application in degrading organic pollutant are characterized by the following: the preparation method comprises the following steps which are carried out in sequence:
(1) dissolving cadmium nitrate tetrahydrate in deionized water to prepare a cadmium nitrate solution, dissolving thiourea in the deionized water to prepare a thiourea solution, dissolving glutathione in the deionized water to prepare a glutathione solution, and then slowly dropping the thiourea solution and the glutathione solution into a zinc acetate solution to prepare a CdS precursor reaction solution.
(2) Putting clean FTO glass into a hydrothermal kettle inner container, adding a proper amount of CdS precursor reaction liquid, carrying out hydrothermal reaction for a certain time at a certain temperature, taking out a sample after the reaction, and air-drying to obtain the CdS/FTO film.
(3) Dissolving a certain amount of trihydroxymethyl aminomethane and dopamine in deionized water, mechanically stirring at room temperature, reacting for a period of time to obtain Polydopamine (PDA) copolymer, immersing the CdS/FTO film in the solution, and continuously stirring for a period of time to obtain the CdS photoelectrode with PDA loaded on the surface.
(4) Dissolving a certain amount of Reduced Graphene Oxide (RGO) prepared by a Hummers method in deionized water, performing ultrasonic treatment for a period of time to prepare an RGO solution, and adding a certain amount of Na2SO4Adding into the above mixed solution to obtain RGO and Na2SO4The mixed solution of (1). It was transferred to a quartz electrolytic cell as an electrolyte. And adopting an electrochemical deposition method, and taking the CdS-PDA as a working electrode, Pt as a counter electrode and Ag/AgCl as a reference electrode. Depositing for a period of time under a certain voltage, and loading RGO on the surface of the PDA layer to obtain the CdS-PDA-RGO photoelectric catalytic material.
2. The preparation method of the CdS-PDA-RGO photoelectrocatalytic material as set forth in claim 1 and application thereof in degrading organic pollutants are characterized in that: in the step (1), the concentrations of the cadmium nitrate tetrahydrate, the thiourea and the glutathione solution are 0.01-0.05M, 0.01-0.05M and 0.016-0.020M respectively.
3. The preparation method of the CdS-PDA-RGO photoelectrocatalytic material as set forth in claim 1 and application thereof in degrading organic pollutants are characterized in that: in the step (2), the temperature and the time of the hydrothermal reaction are respectively 100-140 ℃ and 6-10 h.
4. The preparation method of the CdS-PDA-RGO photoelectrocatalytic material as set forth in claim 1 and application thereof in degrading organic pollutants are characterized in that: in the step (3), the concentrations of the trihydroxymethyl aminomethane and the dopamine solution are respectively 0.010-0.030M and 0.024-0.028M, and the stirring time is 4-12 h after the trihydroxymethyl aminomethane and the dopamine solution are immersed in the CdS electrode.
5. The preparation method of the CdS-PDA-RGO photoelectrocatalytic material as set forth in claim 1 and application thereof in degrading organic pollutants are characterized in that: in step (4), the RGO solution has a concentration of 100mg/L, and the Na is2SO4The concentration of the solution is 0.5M, and the time for loading RGO by the electrodeposition method is 5-15 min.
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| CN116651514A (en) * | 2023-04-14 | 2023-08-29 | 南京信息工程大学 | Photocatalytic composite film and preparation method thereof |
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