CN108033522B - Electrocatalysis coupling advanced oxidation system - Google Patents
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- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
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Abstract
The invention provides an electrocatalytic coupling advanced oxidation system which can degrade organic pollutants into carbon dioxide and synchronously electrocatalytic reduce the carbon dioxide into hydrocarbons. In the catalytic system, three-dimensional hexagonally-star-shaped Co3O4And nanosheet stacked flower-shaped CuO are respectively used as anode and cathode materials, and the two electrode materials are prepared by a solvothermal method. In a three-electrode system electrocatalytic process, Co3O4The electric anode can completely mineralize the p-nitrophenol into CO2And H2O, CuO cathodes can simultaneously reduce the carbon dioxide produced to useful hydrocarbons. When the external bias is-0.8V vs Ag/AgCl, the catalytic effect of the material is the best. The removal rate of the p-nitrophenol can reach more than 98 percent, and the yield of the methanol and the yield of the ethanol respectively reach 49.145 and 20.475 micromoles/liter/hour.
Description
Technical Field
The invention relates to an electrocatalysis coupling advanced oxidation system, and belongs to the field of sewage treatment.
Background
The rapid development of industrialization and urbanization brings highly developed material civilization to human beings, and also brings serious problems of non-negligible environmental pollution, resource shortage and the like. The continuously increasing pollution not only causes serious problems like global warming, but also threatens our lives. Wherein a large amount of industrial wastewater is discharged and a large amount of CO is generated after fossil energy is combusted2Of particular interest. At present, the water environment pollutants are not only simple inorganic pollutants, but also more and more components are more and more complex, and the problem of organic pollution with higher and higher concentration is more and more severe. How to deeply treat the organic pollutants harmful to human beings, which have high concentration, difficult degradation and easy accumulation and reduce the greenhouse effect gas CO2Has become a focus of social attention. Common organic pollutant treating methods include photocatalysis, electrocatalysis, advanced oxidation technology, traditional physical and chemical methods and the like, but in the methods, organic pollutants can be mineralized into CO2However, the problems of low quantum efficiency, low energy utilization rate, difficult catalyst recovery and the like still exist. On the other hand, CO2Reports of catalytic reduction to other hydrocarbons have been extensively studied, common CO2Catalytic reduction approaches include photocatalytic, electrocatalytic and photoelectrocatalytic methods, etc., and problems of low faraday efficiency, selectivity of reduced products, etc. are still urgently needed to be solved, although there are a large number of problems related to organic pollutant removal and CO removal at present2And (5) reporting reduction. But at the same time, all the current treatment methods do not consider realizing CO while efficiently removing organic pollutants2And (4) catalytic reduction. This not only solvesThe problem of environmental pollution is solved, the resource utilization of organic pollutants can be realized, and the negative effects brought by greenhouse gases are overcome while the organic pollutants in the water body are solved.
In recent years, sulfate radicals (SO) have been used4The advanced oxidation technologies (AOPs) based on. cndot. -) and hydroxyl radicals (. OH) are rapidly developing and becoming an emerging technology for the efficient treatment of organic pollutants. There is currently a large body of information on SO production by Peroxymonosulfate (PMS) or Peroxydisulfate (PDS) activation4The removal of organic contaminants by-and OH was reported. The method mainly comprises the following categories: (1) ultrasonic, heating and ultraviolet light; (2) valence-variable metal ions in the homogeneous catalysis process: co2+，Mn2+，Fe2+Etc.; (3) heterogeneous catalysts containing a variable valence metal: co3O4，MnO2，Fe2O3And the like. The system of Shiying Yang et al discusses the degradation of acid orange-7 by ultraviolet light and PMS activation under heating conditions to generate sulfate radicals and hydroxyl radicals. Jing Deng obtains ordered mesoporous Co by template method3O4Relative to Co3O4The nano particles have higher stability, and the mechanism process of activating PMS to degrade chloramphenicol is explored. Meanwhile, the technology for removing organic pollutants through electro-catalysis draws extensive attention of researchers, and the technology is developed from the early simple removal of organic pollutants through anodic oxidation to the application of electro-Fenton to organic wastewater. Comninella, C by doped SnO2As an anode electrocatalytic oxidation of phenol, TOC removal could reach 90%, and the oxidation of phenol to CO was confirmed by analysis of the intermediates of the reaction and the equilibrium of carbon2The process of (1). Although there are currently many electrocatalytic oxidations and SO-based4Report of advanced oxidative removal of organic contaminants with electrocatalytic reduction of CO2There are also few reports of organic compounds. However, no system for the electrocatalytic coupled advanced oxidative degradation of organic pollutants to carbon dioxide and simultaneous electrocatalytic reduction to hydrocarbons has been reported so far. Therefore, it is not uncommon to create a novel electrocatalytic system to test these two goals. Thus, the method is not only beneficial to environmental management, but also beneficial to relieving energy crisis and simultaneously beneficial to environmental managementProvides a new idea.
Disclosure of Invention
The invention aims to provide an electrocatalysis coupling advanced oxidation system, in particular relates to a novel coupling electrocatalysis method and a preparation scheme of a novel electrode material thereof, and provides a new idea and a new material for solving the current pollution and energy problems.
One aspect of the present invention provides an electrocatalytic coupled advanced oxidation system in which three-dimensional hexagonally-shaped Co3O4And nanosheet-stacked flower-shaped CuO as anode and cathode materials, respectively.
According to the invention, an advanced oxidation technique is coupled with electrocatalysis at the anode, Co3O4The electric anode can activate persulfate to generate sulfate radicals and hydroxyl radicals and can also generate hydroxyl radicals through electrocatalysis, so that organic pollutants are efficiently and thoroughly mineralized into CO2And H2O。
According to the invention, the organic pollutants are completely mineralized in the anode to generate CO2Introduced into the cathode through the exhaust pipe and then reduced to hydrocarbons on the CuO cathode.
According to the invention, both electrode materials are prepared by a solvothermal method.
Another aspect of the invention provides three-dimensional hexagonally-star-shaped Co3O4And a synthesis method of the nano-sheet stacked flower-shaped CuO electrode material.
The invention also provides an application method of the electrocatalytic coupling advanced oxidation system and an application of the electrocatalytic coupling advanced oxidation system in the field of sewage treatment.
The invention has the advantages that: 1. the catalyst can degrade organic pollutants and reduce carbon dioxide into green chemical energy source-hydrocarbon fuel; 2. the organic pollutants harmful to the environment are removed by an electrocatalysis coupling advanced oxidation technology, so that the organic pollutants are efficiently removed, and a new idea is provided for the environmental management; 3. the invention grows the target catalyst on the conductive glass substrate in situ by a one-step solvothermal method, and obtains a new appearance by regulating and synthesizing by adding different urea. 4. The catalyst of the invention has good stability, easy recovery and good catalytic effect; 5. the material of the invention is cheap and easy to obtain, the synthesis method is simple, the synthesized yield and purity are high, the experimental repeatability is good, and the invention is suitable for the requirement of expanded production
Drawings
FIG. 1 shows Co0.5 catalyst and pure Co before and after the reaction of the present invention3O4And x-ray powder diffraction contrast plots with co0.2, co1.0, and co1.5;
FIG. 2 is a graph comparing diffraction of CuO catalyst of the present invention with pure CuOX radiation powder;
FIG. 3 shows Co of the present invention3O4Scanning electron micrographs of the catalyst;
FIG. 4 is a scanning electron micrograph of a CuO catalyst of the present invention;
FIG. 5 Co of the present invention3O4The rate of degrading p-nitrophenol in the advanced oxidation process and the rate of degrading p-nitrophenol by Co0.5 electrocatalytic oxidation;
FIG. 6 shows the rate of degradation of p-nitrophenol in an electrocatalytic oxidation coupled advanced oxidation process of Co0.5 of the present invention;
FIG. 7 illustrates that the Co0.5 electric anode and the CuO electric cathode of the present invention degrade p-nitrophenol and reduce carbon dioxide to methanol and ethanol at different voltages;
FIG. 8 is a UV-visible full-wave band diagram of the Co0.5 catalyst of the present invention in electrocatalytic coupling advanced oxidative degradation of p-nitrophenol for 1 hour.
Detailed Description
One aspect of the present invention provides an electrocatalytic coupled advanced oxidation system in which three-dimensional hexagonally-shaped Co3O4And nanosheet-stacked flower-shaped CuO as anode and cathode materials, respectively.
Preferably, the advanced oxidation technique is coupled with electrocatalysis at the anode, Co3O4The electric anode can activate persulfate to generate sulfate radicals and hydroxyl radicals and can also generate hydroxyl radicals through electrocatalysis, so that organic pollutants are efficiently and thoroughly mineralized into CO2And H2O。
Preferably, the organic contaminants completely mineralize the CO produced at the anode2Introduced into the cathode through the exhaust pipe and then reduced to hydrocarbons on the CuO cathode.
Another aspect of the invention provides three-dimensional hexagonally-star-shaped Co3O4And a synthesis method of the nano-sheet stacked flower-shaped CuO electrode material.
Preferably, both electrode materials are prepared by a solvothermal method.
Preferably, three-dimensional hexagonally-star-shaped Co3O4The synthesis method of the material comprises the steps of dissolving 0.5-1 g of cobalt nitrate in 40 ml of mixed solution of ethylene glycol and water, stirring, adding 0.5-1.5 g of urea after the cobalt nitrate is completely dissolved, stirring uniformly, adding 30-50 mg of hexadecyl trimethyl ammonium bromide and 1-2 g of ammonium fluoride, stirring for 30-45 minutes at normal temperature to form uniform and transparent colorless solution, transferring the solution to a 100 ml of polytetrafluoroethylene reaction kettle lining, placing a piece of cleaned conductive glass (1.5 cm × 4.0.0 cm) in a reaction kettle in an inclined mode, enabling the conductive surface of the conductive glass to face upwards, transferring the reaction kettle to a drying box to react at 100-120 ℃ for 10-12 hours to obtain a purple precursor, placing the conductive glass in a muffle furnace, calcining at 350-550 ℃ for 2-4 hours, cooling to room temperature to obtain the three-dimensional hexagram-shaped Co3O4。
Preferably, the synthesis method of the nanosheet-stacked flower-shaped CuO material is characterized by sequentially dissolving 5-6 g of sodium hydroxide, 1-1.2 g of ammonium persulfate and 0.2-0.4 g of sodium tungstate in 30-40 ml of deionized water, stirring for 30-45 minutes at normal temperature to form a uniform and transparent colorless solution, then adding 0.4-0.6 g of sodium dodecyl sulfate into the solution to form a uniform white solution, after the sodium dodecyl sulfate is completely dissolved, transferring into a stainless steel autoclave with a polytetrafluoroethylene lining, immersing a cleaned copper net (1.5 cm × 4.0.0 cm) into the solution, reacting for 24 hours at 100-150 ℃ under the condition that the autoclave is sealed, then cooling to room temperature, taking out the copper net, and cleaning with deionized water to obtain black nanosheet-stacked flower-shaped CuO.
The invention also provides an application method of the electrocatalysis coupling advanced oxidation system, and Co is in a three-dimensional hexagram shape in a conventional H-shaped electrolytic cell reaction system3O4And nano-sheet stacked flower-shaped CuO are respectively used as anode and cathode materials, 0.1 mol/L sodium sulfate solution is added into an anode chamber, 0.1 mol/L potassium bicarbonate solution is added into a cathode chamber, then 0.5 g/L persulfate and 10 mg/L p-nitrophenol solution are added into anolyte, and electrolysis and advanced oxidation coupling reaction are carried out by electrifying.
Preferably, the volumes of the sodium sulfate solution of 0.1 mol/l added to the anode chamber and the potassium bicarbonate solution of 0.1 mol/l added to the cathode chamber are 60 ml.
The invention also provides application of the electrocatalysis coupling advanced oxidation system in the field of sewage treatment, which is used for removing organic pollutants in wastewater, wherein the organic pollutants are mineralized at the anode to generate CO2Introduced into the cathode through the exhaust pipe and then reduced to hydrocarbons at the cathode.
The invention is further illustrated by the following examples, which are not intended to be limiting thereof.
Example 1
Three-dimensional hexagonal star shaped Co3O4Synthesis of the electric anode material:
0.582 g of cobalt nitrate 2 mmol is dissolved in 10 ml of ethylene glycol and 30 ml of water and stirred, after complete dissolution, 0.5g of urea is added and stirred uniformly, then 0.05g of hexadecyl trimethyl ammonium bromide and 1.455g of ammonium fluoride are added, stirring is carried out for 30 minutes at 25 ℃ to form a uniform and transparent colorless solution, the solution is transferred to a lining of a 100 ml polytetrafluoroethylene reaction kettle, a piece of cleaned conductive glass (1.5 cm × 4.0.0 cm) is obliquely placed in the reaction kettle, the conductive surface of the conductive glass faces upwards, finally the reaction kettle is transferred to a drying box for reaction at 120 ℃ for 12 hours to obtain a purple precursor, the conductive glass is placed in a muffle furnace, pre-calcined at 350 ℃ for 2 hours, then calcined at 550 ℃ for 2 hours, and then cooled to room temperature to obtain Co3O4. The urea is added in amounts of 0.2g, 0.5g, 1.0g and 1.5gCo3O4Designated as Co0.2, Co0.5, Co1.0 and Co1.5 electrodes.
Example 2
The synthesis of the nano-sheet stacked flower-shaped CuO electric cathode comprises the steps of sequentially dissolving 6.4g of sodium hydroxide, 1.0954g of ammonium persulfate and 0.211g of sodium tungstate in 32 ml of deionized water, stirring for 30 minutes at 25 ℃ to form a uniform and transparent colorless solution, then adding 0.4614g of sodium dodecyl sulfate into the solution to form a uniform white solution, after the sodium dodecyl sulfate is completely dissolved, transferring the solution into a polytetrafluoroethylene-lined stainless steel autoclave, immersing a cleaned copper net (1.5 cm × 4.0.0 cm) into the solution, reacting for 24 hours at 130 ℃ under the condition of the autoclave being sealed, cooling to room temperature, taking out the copper net, and cleaning with the deionized water to obtain a black sample CuO.
As shown in fig. 1-8, the X-ray powder diffraction test results show that:
diffraction patterns of a series of Co0.2, Co0.5, Co, 1.0 and Co1.5 catalysts of the invention were compared to standard card Co3O4Indicates that the addition of different amounts of urea does not affect Co3O4And the crystal form is not changed after the reaction. Raman analysis, XPS and EDS analysis show that the Co0.5 catalyst material is made of Co3O4And (4) compounding. From a scanning electron microscope image, the appearance of the catalyst Co0.5 is greatly influenced by adding different amounts of urea. When the urea is less than 0.5, the catalyst has a flower-shaped structure formed by nano particles, when the urea is more than 0.5, the surface becomes smooth, and the appearance is further converted into a hexagram-shaped structure.
According to the CuO, the CuO is in a flower-like structure stacked by nano sheets in the appearance seen by a scanning electron microscope. From the linear cyclic voltammogram, it can be found that the CuO catalyst of the present invention has high activity for carbon dioxide reduction.
Example 3
In a conventional H-shaped electrolytic cell reaction system, Co is respectively in a three-dimensional hexagonal star shape3O4And nano-sheet stacked flower-shaped CuO are respectively used as anode and cathode materials, 0.1 mol/L sodium sulfate solution (volume is 60 ml) is added into an anode chamber, and a cathode is filled with the sodium sulfate solutionAdding 0.1 mol/L potassium bicarbonate solution (the volume is 60 ml) into the polar chamber, then adding 0.5 g/L persulfate and 10 mg/L p-nitrophenol solution into the anolyte, and electrifying to carry out electrolysis and advanced oxidation coupling reaction.
Co when applied bias was-0.8V vs Ag/AgCl3O4The removal rate of the paranitrophenol of the anode can reach more than 98 percent, and the yield of the CuO anode which can synchronously reduce the carbon dioxide into the methanol and the ethanol respectively reaches 49.145 micromoles/liter/hour and 20.475 micromoles/liter/hour. The Co of the invention can be proved by full-wave band degradation data0.5The catalyst can mineralize p-nitrophenol into CO2And H2O。
The catalyst is prepared by a solvothermal method, the material is cheap and easy to obtain, the synthesis method is simple, the synthesis yield is high, the purity is high, the repeatability is good, and the catalyst is suitable for the requirement of enlarged production. The catalyst of the invention is coupled with electrocatalytic oxidation technology and electrocatalytic reduction technology through electrocatalytic oxidation technology, and simultaneously the electrocatalytic oxidation technology is coupled with advanced oxidation, so that the aims of effectively mineralizing organic pollutants in water and simultaneously converting carbon dioxide into simple and useful chemical products (such as methane, methanol, ethanol and the like) are fulfilled. The electrocatalyst can efficiently remove organic pollutants and convert carbon dioxide into green energy, is beneficial to environmental management and energy crisis alleviation, and provides a new idea for environmental management.
The foregoing is only a preferred embodiment of the invention. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (4)
1. Electrocatalytic couplingAn advanced oxidation system characterized by: in this system, three-dimensional hexagonally-star-shaped Co3O4And nano-sheet stacked flower-shaped CuO are respectively used as anode and cathode materials; coupling advanced oxidation technology with electrocatalysis at the anode, Co3O4The electric anode can activate persulfate to generate sulfate radicals and hydroxyl radicals and can also generate hydroxyl radicals through electrocatalysis, so that organic pollutants are efficiently and thoroughly mineralized into CO2And H2O; wherein: CO generated by thorough mineralization of organic pollutants at anode2Is introduced into the cathode through an exhaust pipe and then is reduced into hydrocarbon on the CuO cathode;
the two electrode materials are both prepared by a solvothermal method;
the three-dimensional hexagonally-shaped Co3O4The synthesis method of the material comprises the following steps: dissolving 0.5-1 g of cobalt nitrate in 40 ml of mixed solution of ethylene glycol and water, stirring, adding 0.5-1.5 g of urea after the cobalt nitrate is completely dissolved, uniformly stirring, then adding 30-50 mg of hexadecyl trimethyl ammonium bromide and 1-2 g of ammonium fluoride, stirring for 30-45 minutes at normal temperature to form uniform and transparent colorless solution, and transferring the solution to the inner liner of a 100 ml of polytetrafluoroethylene reaction kettle; then placing a piece of cleaned conductive glass in a reaction kettle in an inclined mode, enabling the conductive surface of the conductive glass to face upwards, finally transferring the reaction kettle to a drying box to react at the temperature of 100-120 ℃, and reacting for 10-12 hours to obtain a purple precursor on the conductive glass; putting the conductive glass into a muffle furnace, calcining for 2-4 hours at 350-550 ℃, and then cooling to room temperature to obtain three-dimensional hexagram-shaped Co3O4；
The synthesis method of the nanosheet stacked flower-shaped CuO material comprises the following steps: sequentially dissolving 5-6 g of sodium hydroxide, 1-1.2 g of ammonium persulfate and 0.2-0.4 g of sodium tungstate in 30-40 ml of deionized water, and stirring for 30-45 minutes at normal temperature to form a uniform and transparent colorless solution; then 0.4-0.6 g of sodium dodecyl sulfate is added into the solution to form a uniform white solution, after the sodium dodecyl sulfate is completely dissolved, the solution is moved into a stainless steel autoclave with a polytetrafluoroethylene lining, and a cleaned copper mesh is immersed into the solution; and (3) reacting for 24 hours at 100-150 ℃ under the closed condition of the high-pressure kettle, cooling to room temperature, taking out the copper mesh, and washing with deionized water to obtain black nanosheet-stacked flower-shaped CuO.
2. A method of using the electrocatalytic coupled advanced oxidation system of claim 1, wherein: in a conventional H-shaped electrolytic cell reaction system, Co takes a three-dimensional hexagonal star shape3O4And nano-sheet stacked flower-shaped CuO are respectively used as anode and cathode materials, 0.1 mol/L sodium sulfate solution is added into an anode chamber, 0.1 mol/L potassium bicarbonate solution is added into a cathode chamber, then 0.5 g/L persulfate and 10 mg/L p-nitrophenol solution are added into anolyte, and electrolysis and advanced oxidation coupling reaction are carried out by electrifying.
3. The method of application of claim 2, wherein: the volumes of the sodium sulfate solution of 0.1 mol/l added to the anode chamber and the potassium bicarbonate solution of 0.1 mol/l added to the cathode chamber were 60 ml.
4. The application of the electrocatalytic coupled advanced oxidation system as set forth in claim 1 in the field of sewage treatment, characterized in that: for removing organic pollutants in wastewater, the organic pollutants being mineralized at the anode to generate CO2Introduced into the cathode through the exhaust pipe and then reduced to hydrocarbons at the cathode.
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| WO2020257218A1 (en) * | 2019-06-19 | 2020-12-24 | Evoqua Water Technologies Llc | Electrochemically activated persulfate for advanced oxidation processes |
| CN110526343B (en) * | 2019-09-06 | 2021-10-12 | 南昌航空大学 | Electrocatalysis coupling advanced oxidation system and application thereof |
| CN112320895A (en) * | 2020-09-21 | 2021-02-05 | 北京科技大学 | Device and method for producing methane by coupling printing and dyeing wastewater treatment through three-dimensional electrode |
| CN114132999B (en) * | 2021-11-26 | 2023-07-25 | 宁波职业技术学院 | Method for treating printing and dyeing wastewater by anode electrochemical activation persulfate |
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