CN115571947A - Photoelectric catalytic reactor for inactivating microorganisms in water - Google Patents
Photoelectric catalytic reactor for inactivating microorganisms in water Download PDFInfo
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- CN115571947A CN115571947A CN202211339704.2A CN202211339704A CN115571947A CN 115571947 A CN115571947 A CN 115571947A CN 202211339704 A CN202211339704 A CN 202211339704A CN 115571947 A CN115571947 A CN 115571947A
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- 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
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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
- C02F1/72—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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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Abstract
The invention belongs to the technical field of photoelectrocatalysis, and particularly relates to a photoelectrocatalysis reactor for inactivating microorganisms in water. The photoelectrocatalysis reactor consists of a sunlight simulator, a photoelectrocatalysis reactor and an aeration device; the solar simulator is positioned at the upper part of the photoelectrocatalysis reactor and provides light irradiation for the photoelectrocatalysis reactor; the aeration device is arranged beside the photoelectrocatalysis reactor and provides dissolved oxygen for the photoelectrocatalysis reactor; an air outlet end opening of an aeration pipe in the aeration device is arranged near a cathode in the photoelectrocatalysis reactor; after the reactor is operated, the dissolved oxygen is reduced to hydrogen peroxide at the cathode, and the efficient microorganism inactivation in water is realized by the cooperation of the photo-anode photoelectrocatalysis effect. The invention combines the photo-anode photoelectrocatalysis effect with the cathode electrochemical reduction to generate hydrogen peroxide, utilizes clean energy, improves the microorganism inactivation efficiency, does not generate secondary pollution and harmful byproducts, and is an environment-friendly water treatment device.
Description
Technical Field
The invention belongs to the technical field of photoelectrocatalysis, and particularly relates to a photoelectrocatalysis reactor for inactivating microorganisms in water.
Background
Water disinfection technology is essential to inactivate water-borne pathogens and reduce global public health risks. However, the conventional disinfection methods such as chlorine/chloramine disinfection, ultraviolet disinfection, ozone disinfection and the like have the problems of long reaction time, carcinogenic disinfection by-products, high energy consumption, high chemical consumption and the like. In addition, water treatment infrastructure and pipelines are restricted by regional positions, population distribution, economic development and potential natural disaster damage, and the development of cheap and efficient distributed water treatment devices has wide application prospects.
The photoelectrocatalysis water treatment has high purification efficiency, the photocatalyst is anchored on the conductive substrate to be used as an electrode, so that the catalyst can be easily recovered, the oxidation-reduction reaction can be controlled by applying voltage, and the separation of photon-generated carriers is improved. The invention selects a self-made bismuth oxyiodide-molybdenum disulfide electrode as a photo-anode to provide anodic oxidation capability. In addition, hydrogen peroxide is an environment-friendly disinfectant, can attack cell membranes and diffuse into cells, and reacts with free iron ions or iron-sulfur clusters to destroy microbial DNA. The hydrogen peroxide can be further converted into OH with higher oxidation-reduction potential through electro-catalysis and photocatalysis, and pollutants can be rapidly and nonselectively degraded. The additional addition of hydrogen peroxide may be accompanied by additional transportation costs and safety concerns for chemical storage. However, electrochemically generating hydrogen peroxide in situ at the cathode may circumvent the above limitations. The carbon cathode can inhibit the cracking of O-O bonds and meet the kinetic requirement of oxygen for generating hydrogen peroxide through a double-electron approach. The reticular glassy carbon electrode has high pore volume and specific surface area, and is particularly suitable for generating hydrogen peroxide. However, no studies have been reported so far on the synergistic disinfection by photoanode oxidation and in situ generation of hydrogen peroxide.
Disclosure of Invention
The invention aims to provide a high-efficiency, quick and low-cost photoelectrocatalysis reactor for inactivating microorganisms in water.
The invention provides a photoelectrocatalysis reactor for inactivating microorganisms in water, which comprises a solar simulator, a photoelectrocatalysis reactor and an aeration device; wherein:
the solar simulator is positioned at the upper part of the photoelectrocatalysis reactor and provides light irradiation for the photoelectrocatalysis reactor; the aeration device is arranged beside the photoelectrocatalysis reactor and is used for providing dissolved oxygen for the photoelectrocatalysis reactor; an air outlet end opening of an aeration pipe in the aeration device is arranged near a cathode in the photoelectrocatalysis reactor;
the photoelectrocatalysis reactor comprises a photo-anode, a cathode and a sodium sulfate electrolyte, wherein the area ratio of the photo-anode to the cathode is 1-1 (1: 1-2)), and the electrode is arranged in the sodium sulfate electrolyte;
the solar simulator is a commercial product.
The cathode material is a commercial reticulated vitreous carbon electrode; the anode is a bismuth oxyiodide-molybdenum disulfide electrode; the reactor can effectively remove 10 percent of the waste water after oxygen introduction and electrification for 50 min under the irradiation of sunlight 6 CFU/mL E.coli.
In the invention, the photo-anode is prepared by the following steps:
(1) Ultrasonically dissolving bismuth nitrate pentahydrate and potassium iodide into ethylene glycol, and then placing the mixture into a reaction kettle for hydrothermal reaction at the temperature of 160-200 ℃ for 12-18h; filtering, drying to obtain bismuth oxyiodide; wherein the mass ratio of the bismuth nitrate pentahydrate to the potassium iodide is 3;
(2) Dissolving sodium molybdate and thioacetamide in deionized water, adding the prepared bismuth oxyiodide, placing the mixture in a liner of a reaction kettle, and carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 12-18h; filtering, drying to obtain bismuth oxyiodide-molybdenum disulfide powder; wherein the mass ratio of the sodium molybdate to the thioacetamide is 1-1 (1-2)), the mass ratio of the total mass of the sodium molybdate and the thioacetamide to the added bismuth oxyiodide is 1;
(3) And (2) loading the prepared bismuth oxyiodide-molybdenum disulfide powder on indium tin oxide conductive glass by adopting a point coating method, then calcining in a tube furnace under the protection of nitrogen, wherein the calcining temperature is 200-500 ℃ (preferably 400-500 ℃), and the holding time is 30-100min (preferably 30-60 min), thus obtaining the required electrode.
In the photoelectrocatalysis reactor for inactivating microorganisms in water, a photoanode is connected with a positive electrode of a power supply, a glassy carbon cathode is connected with a negative electrode of the power supply, the constant current for stabilizing voltage is 0-100mA (preferably 10-100 mA), the irradiation light intensity at the liquid level is controlled to be 0-1000W (5-1000W, more preferably 100-800W), the distance between counter electrodes is 0-3cm (preferably 1-3 cm), and the electrolyte is 0-1mol/L (preferably 0.4-1 mol/L) of sodium sulfate. When the reaction starts, the solar simulator and the power supply are turned on, and the aeration device is turned on.
The photoelectrocatalysis reactor for inactivating microorganisms in water promotes separation of photon-generated carriers by applying external bias voltage to a photoanode under illumination so as to react with dissolved oxygen in water to generate a series of strong oxidizing free radicals; on the other hand, the hydrogen peroxide generated by the dissolved oxygen in the water on the carbon cathode through the double-electron path can also be sterilized cooperatively, so that the sterilization efficiency of the device is improved.
The invention has the following beneficial effects:
(1) The external bias voltage is applied to the photo-anode, so that the recombination of photon-generated carriers can be effectively inhibited, and the photoelectrocatalysis efficiency is improved; the hydrogen peroxide generated in situ by the reduction of the cathode oxygen has strong oxidizing property and can assist the photoelectrocatalysis action of the photoanode to sterilize. Hydrogen peroxide is generated in situ by coupling photoelectrocatalysis of the photoanode and the cathode, and the device can efficiently kill microorganisms in water and ensure the safety of drinking water;
(2) The device has the advantages of low cost, high disinfection efficiency, good repeatability, no secondary pollutant, energy conservation, environmental protection and wide application prospect;
(3) The invention can kill colibacillus in water effectively and kill various microbes, such as staphylococcus aureus, bacillus subtilis, etc. The application of the material in raw water shows that the material can effectively reduce the total number of bacteria and the number of heterotrophic bacteria.
Drawings
FIG. 1 is a schematic view of a photoelectrocatalytic reactor for inactivation of microorganisms in water according to the present invention.
FIG. 2 is a graph showing the disinfection performance of the photoelectrocatalysis reactor of the present invention on Escherichia coli under different applied currents in examples 1-3.
FIG. 3 is a graph showing the disinfection performance of the photoelectrocatalysis reactor of the present invention on Escherichia coli with different applied light intensities in examples 1-3.
FIG. 4 is a graph showing the sterilization performance of the photoelectrocatalytic reactor of the present invention for various bacteria in example 1.
Reference numbers in the figures: the device comprises a solar simulator 1, a photoelectrocatalysis reactor 2, an aeration device 3, a photoanode 4, a cathode 5, an electrolyte 6 and an oxygen bottle 7.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the scope of the present invention is not limited thereto. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available products.
Example 1:
1.5g of bismuth nitrate pentahydrate and 0.5g of potassium iodide were weighed out and dissolved in 35 mL of ethylene glycol, respectively. The potassium iodide solution was added dropwise to the stirred bismuth nitrate solution. Sonication for 10min ensured that the mixture was homogeneous, then transferred to a 100mL autoclave and heated at 160 ℃ for 16h. Naturally cooling the autoclave to room temperature, filtering and collecting bismuth oxyiodide solid through a 0.22 mu m microporous membrane, washing with deionized water and absolute ethyl alcohol for multiple times, and drying for later use. Similarly, 0.2g of sodium molybdate and 0.2g of thioacetamide were completely dissolved in 100mL of deionized water, and 2g of the bismuth oxyiodide prepared above was added to the resulting mixture, which was then placed in a 150mL autoclave, heated at 160 ℃ for 16 hours, and cooled to obtain a bismuth oxyiodide-molybdenum disulfide solid, which was similar to the bismuth oxyiodide, and was filtered, washed, and dried for future use. Dispersing 40 mg of bismuth oxyiodide-molybdenum disulfide solid in 20 mL of ethanol, and dropwise adding the bismuth oxyiodide-molybdenum disulfide solid into the solution with the surface area of 20 cm by a point coating method 2 The indium tin oxide conductive glass is placed in a 300 ℃ tube furnace for 60 min under the protection of nitrogen to obtain the photo-anode.
The photoanode and a commercial reticulated vitreous carbon cathode with the same area are vertically and parallelly placed in a beaker at the interval of 2cm, electrolyte is 0.01mol/L sodium sulfate, the photoanode is connected with a power supply anode, the vitreous carbon cathode is connected with a power supply cathode, a constant current of 20 mA is set by a stabilized voltage power supply, and an aeration conduit connected with an oxygen bottle continuously aerates near the cathode. And (5) opening the sunlight simulator, and controlling the irradiation light intensity at the liquid level to be 500W.
Example 2:
1.5g of bismuth nitrate pentahydrate and 0.5g of potassium iodide were weighed out and dissolved in 35 mL of ethylene glycol, respectively. The potassium iodide solution was added dropwise to the stirred bismuth nitrate solution. Sonication for 10min ensured that the mixture was homogeneous, then transferred to a 100mL autoclave and heated at 160 ℃ for 16h. Naturally cooling the autoclave to room temperature, filtering and collecting bismuth oxyiodide solid through a 0.22 mu m microporous membrane, washing with deionized water and absolute ethyl alcohol for multiple times, and drying for later use. Similarly, 0.2g of sodium molybdate and 0.2g of thioacetamide were completely dissolved in 100mL of deionized water, 2g of the bismuth oxyiodide prepared above was added to the resulting mixture, and then the mixture was placed in a 150mL autoclave, heated at 160 ℃ for 16 hours, and cooled to obtain a bismuth oxyiodide-molybdenum disulfide solid, which was similar to the bismuth oxyiodide, and was filtered, washed, and dried for future use. Dispersing 40 mg of bismuth oxyiodide-molybdenum disulfide solid in 20 mL of ethanol, and dropwise adding the bismuth oxyiodide-molybdenum disulfide solid to the surface area of 20 cm by a point coating method 2 The indium tin oxide conductive glass is placed in a 300 ℃ tube furnace for 60 min under the protection of nitrogen to obtain the photo-anode.
The photoanode and a commercial reticular glassy carbon cathode with the same area are vertically and parallelly placed in a beaker, the distance is 2cm, electrolyte is 0.01mol/L sodium sulfate, the photoanode is connected with a power supply anode, the glassy carbon cathode is connected with a power supply cathode, a constant voltage power supply is respectively provided with constant currents of 10 mA, 20 mA, 30 mA, 40 mA and 50 mA, and an aeration conduit connected with an oxygen bottle continuously aerates near the cathode. And (5) opening the sunlight simulator, and controlling the irradiation light intensity at the liquid level to be 500W.
Example 3:
1.5g of bismuth nitrate pentahydrate and 0.5g of potassium iodide were weighed out and dissolved in 35 mL of ethylene glycol, respectively. The potassium iodide solution was added dropwise to the stirred bismuth nitrate solution. Sonication for 10min ensured that the mixture was homogeneous, then transferred to a 100mL autoclave and heated at 160 ℃ for 16h. Naturally cooling the autoclave to room temperature, filtering the obtained product through a 0.22 mu m microporous membrane to collect bismuth oxyiodide solid, and filtering the obtained product through a filterWashing deionized water and absolute ethyl alcohol for many times, and drying for later use. Similarly, 0.2g of sodium molybdate and 0.2g of thioacetamide were completely dissolved in 100mL of deionized water, and 2g of the bismuth oxyiodide prepared above was added to the resulting mixture, which was then placed in a 150mL autoclave, heated at 160 ℃ for 16 hours, and cooled to obtain a bismuth oxyiodide-molybdenum disulfide solid, which was similar to the bismuth oxyiodide, and was filtered, washed, and dried for future use. Dispersing 40 mg of bismuth oxyiodide-molybdenum disulfide solid in 20 mL of ethanol, and dropwise adding the bismuth oxyiodide-molybdenum disulfide solid into the solution with the surface area of 20 cm by a point coating method 2 The indium tin oxide conductive glass is placed in a 300 ℃ tube furnace for 60 min under the protection of nitrogen to obtain the photo-anode.
The photoanode and a commercial reticulated vitreous carbon cathode with the same area are vertically and parallelly placed in a beaker at the interval of 2cm, electrolyte is 0.01mol/L sodium sulfate, the photoanode is connected with a power supply anode, the vitreous carbon cathode is connected with a power supply cathode, a constant current of 20 mA is set by a stabilized voltage power supply, and an aeration conduit connected with an oxygen bottle continuously aerates near the cathode. The sunlight simulator is turned on, and the irradiation light intensity at the liquid level is controlled to be 300W, 500W, 700W and 900W respectively.
FIG. 1 is a schematic diagram of a photoelectrocatalysis reactor for the inactivation of microorganisms in water prepared in examples 1-3, which has a simple structure and is convenient to operate and suitable for a distributed water treatment system;
FIG. 2 is the disinfection performance of the apparatus of examples 1-3 on Escherichia coli with different applied currents, which shows that the photoelectrocatalysis reactor has good disinfection effect under different applied currents;
FIG. 3 is the disinfection performance of the apparatus of examples 1-3 on Escherichia coli with different applied light intensities, which shows that the photoelectrocatalytic reactor has good disinfection effect under different applied light intensities;
FIG. 4 is the disinfection performance of the device in example 1 on different bacteria, which shows that the photoelectrocatalysis reactor has a wide sterilization range and a wide application range.
The external bias voltage is applied to the photo-anode, so that the recombination of photo-generated carriers can be effectively inhibited, and the photoelectric catalysis efficiency is improved; and photo-generated electrons are transferred to the cathode to assist dissolved oxygen reduction, and strong-oxidizing hydrogen peroxide is generated in situ and can assist the photo-anode photoelectrocatalysis to disinfect. By coupling the photoelectrocatalysis of the photoanode and in-situ generation of hydrogen peroxide of the cathode, the device can efficiently kill microorganisms in water, and the drinking water safety of distributed water treatment is ensured.
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent structures or equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are also included in the scope of the present invention.
Claims (3)
1. A photoelectrocatalysis reactor for inactivating microorganisms in water is characterized by comprising a solar simulator, a photoelectrocatalysis reactor and an aeration device; wherein:
the solar simulator is positioned at the upper part of the photoelectrocatalysis reactor and provides light irradiation for the photoelectrocatalysis reactor; the aeration device is arranged beside the photoelectrocatalysis reactor and is used for providing dissolved oxygen for the photoelectrocatalysis reactor; an air outlet end opening of an aeration pipe in the aeration device is arranged near a cathode in the photoelectrocatalysis reactor;
the photoelectrocatalysis reactor comprises a photo-anode, a cathode and a sodium sulfate electrolyte, the area ratio of the photo-anode to the cathode is 1-1;
the cathode material is a reticular glassy carbon electrode; the anode is a bismuth oxyiodide-molybdenum disulfide electrode.
2. The photoelectrocatalytic reactor for inactivation of microorganisms in water of claim 1, wherein the photoanode is prepared by:
(1) Ultrasonically dissolving bismuth nitrate pentahydrate and potassium iodide into ethylene glycol, and then placing the mixture into a reaction kettle for hydrothermal reaction at 160-200 ℃ for 12-18h; filtering, drying to obtain bismuth oxyiodide; wherein the mass ratio of the bismuth nitrate pentahydrate to the potassium iodide is (3);
(2) Dissolving sodium molybdate and thioacetamide in deionized water, adding the prepared bismuth oxyiodide, placing the mixture in a liner of a reaction kettle, and carrying out hydrothermal reaction at 160-200 ℃ for 12-18h; filtering, drying to obtain bismuth oxyiodide-molybdenum disulfide powder; wherein the mass ratio of the sodium molybdate to the thioacetamide is 1-1;
(3) Loading the prepared bismuth oxyiodide-molybdenum disulfide powder on indium tin oxide conductive glass by adopting a point coating method, and then calcining in a tubular furnace under the protection of nitrogen, wherein the calcining temperature is 200-500 ℃, and the holding time is 30-100min, thus obtaining the required electrode.
3. The photoelectrocatalysis reactor for in-water microorganism inactivation according to claim 1, wherein the photoanode is connected with a positive electrode of a power supply, the glassy carbon cathode is connected with a negative electrode of the power supply, the constant current of the stabilized voltage is 10-100mA, the irradiation light intensity at the liquid level is controlled to be 5-1000W, the distance between counter electrodes is 1-3cm, and the electrolyte is 0.4-1mol/L of sodium sulfate.
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