CN107162161B - Separated venturi tube type hybrid electrocatalytic ozonization method and device - Google Patents
Separated venturi tube type hybrid electrocatalytic ozonization method and device Download PDFInfo
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- 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
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Abstract
A separation type Venturi tube type hybrid electrocatalysis ozonization method and a device belong to the technical field of water treatment and environmental protection. The invention relates to a novel pollutant removal process combining efficient ozone dissolution with a carbon material three-dimensional penetrating electrode. The invention is economic and efficient, has higher removal capability on novel pollutants (such as drugs and personal care products pollutants PPCPs (pharmaceutical and personal care products) such as antibiotics, Endocrine Disruptors (EDCs), Drinking water Disinfection By-products drining-water Disinfection By-products (DBPs), perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) which are representative compounds of perfluorinated organic compounds, brominated flame retardants such as polybrominated diphenyl ethers (PBDEs) and the like) which are difficult to degrade, and can be completely removed. The mineralization removal rate of target pollutants in the treated effluent is higher than 90%, and the safety of water quality can be guaranteed.
Description
Technical Field
The invention belongs to the technical field of water treatment and environmental protection, and particularly relates to a separated venturi tube type hybrid electrocatalytic ozonization method and a device.
Background
Advanced Oxidation Processes (AOPs) were proposed by Glaze in 1987, and are defined as a method for removing organic substances by generating a large amount of hydroxyl radicals (· OH) to oxidize and destroy the structure of macromolecular organic substances. The currently common methods are: fenton method, O3And combined oxidation processes thereof (e.g. O)3Catalyst process, O3UV method, O3UV/catalyst method, O3/H2O2Method, O3/UV/H2O2Methods, etc.), photochemical oxidation (e.g., UV method, UV/catalyst method, UV/H)2O2Method, UV/H2O2Catalyst method, etc.), electrochemical oxidation methods, and other advanced oxidation methods.
O3The mechanism for oxidizing organic matters is complex, and the reaction types are mainly divided into direct oxidation and indirect oxidation. The direct oxidation is O dissolved in water environment3The molecules react directly with the organic matter. O is3Is a strong oxidant with strong oxidizing power and oxidation potential of E02.07V. But O is3The molecule has stronger selectivity, is generally easier to react with substituted aromatic compounds and is not easy to react with other organic compoundsWhen the target organic matter is degraded in a water environment through the reaction of the substances, a plurality of intermediate products are often generated and cannot be completely mineralized into the inorganic matter. The indirect oxidation is that ozone generates hydroxyl radical (OH) through decomposition or reaction, and the oxidizing property of OH is stronger than that of O3Molecular, oxidation potential E02.86V, without selectivity, can react with almost all organics.
Weiss's experiment demonstrates O3The oxidation mechanism of (a) will vary with the pH. O dissolved in water under acidic conditions3The molecule is relatively stable, and when the pH value rises, O3 is easily decomposed into OH.
Furthermore, the mechanism of ozonolysis can also be summarized by the free radical chain reaction proposed by Staehelin, Hoigne and Bader, i.e., the SBH mode.
O3The reaction with organic matter features fast reaction with unsaturated bond containing compound to form aldehyde, ketone, carboxylic acid and other reaction products. Ozone not only can effectively degrade toxic substances, but also can be decomposed into oxygen in the oxidation process, so that secondary pollution is not caused. At the same time, due to O3The selectivity of molecules is strong, the molecules are generally easy to react with substituted aromatic compounds and are not easy to react with other organic matters, when target organic matters are degraded in a water environment, a plurality of intermediate products are generated and cannot be completely mineralized into inorganic matters, the ecological safety of the intermediate products is not completely tested, and the hidden danger is undoubtedly brought to the whole ecological safety. Therefore, if the generation of intermediate products when the target organic matters are degraded can be controlled, and the mineralization rate is improved, the application of the ozone advanced oxidation technology in the aspect of removing environmental endocrine disruptors is certainly promoted.
In order to improve the mineralization degree of the organic pollutants and further improve the degradation efficiency, O is added3In combination with other methods, to make O3More OH can be produced. The ozone combined oxidation method comprises the following steps: o is3Catalyst process, O3UV method, O3UV/catalyst method, O3Method of/H2O 2, O3/UV/H2O2Methods, and the like. Catalytic ozonation (catalytic ozonation) is the use of ozone in catalysisThe OH generated by the agent can be quickly oxidized and decomposed by most organic compounds (including some organic compounds with high stability and difficult degradation). The research aims to adopt the carbon nano tube as a catalyst to carry out catalytic ozonization research.
The catalytic ozonation method is also a hot research problem for removing organic pollutants by utilizing the characteristics and adsorption capacity of a catalyst and combining the strong oxidizing property of ozone. Catalysts can be classified into homogeneous catalysts and heterogeneous catalysts according to the phase state of the catalyst. The heterogeneous catalyst is mostly solid phase catalyst, and the catalyst in the catalytic ozone method is divided into transition metal catalyst (such as Mn, Fe, Cu and the like) and transition metal oxide catalyst (such as TiO2, MnO2Etc.) and activated carbon. Nahum a et al compare O3/AC、O3/H2O2And O3Three methods remove diethyl phthalate (DEP), and it is believed that the most effective method for removing diethyl phthalate is O3Activated carbon method. The activated carbon can catalyze O3OH is generated by decomposition, so that the removal amount of diethyl phthalate is increased.
The carbon material has wide sources, different shapes and wide application, and particularly, the carbon nano material has the characteristics of high specific surface area, high electron conduction speed, easy modification and the like, and the properties of the carbon nano material, such as mechanics, chemistry, electrons and the like, can be further optimized by modifying the carbon nano material by chemical doping and other methods. The nitrogen-doped carbon nanotube has wide application prospect in the fields of nano electronic devices, energy storage materials, catalysts and the like. Nitrogen doping of carbon materials can cause the structure of the material to become disordered and thereby change the mechanical properties thereof. The graphene doped with nitrogen atoms can induce the formation of high local charge/spin density on the surface of the graphene so as to improve the chemical activity of the graphene. The doping of nitrogen can increase the density of carriers and the rate of electron transfer, which makes the oxygen reduction reaction of the doped carbon nanomaterial easier to perform. The introduction of nitrogen can change the local charge density of the material, so that more active sites are generated, and the nitrogen doping generates pyridine, pyrrole and graphite type nitrogen functional groups in the carbon crystal lattice. The pyridine type nitrogen functionality increases the redox reaction (ORR) activity, and the pyrrole type functionality represents only a small percentage of the total nitrogen functionality. The pyridine type nitrogen function has a lone pair electron besides the electron which contributes to the conjugated pi system, so that an electron-rich nitrogen site can be provided, and the conjugation effect of the nitrogen lone pair electron and the carbon pi system promotes n type conductivity, and the material is caused to show a method of various metals. In general, nitrogen doping results in high chemical activity, high electron density in localized areas, and defects caused by doping can further enhance the activity of the material and promote the electrocatalysis of the redox reaction. Theoretical calculations show that nitrogen doping decreases the activation energy and dissociation energy of oxygen on the carbon-based material, i.e., nitrogen doping the carbon-based material favors the activation dissociation of oxygen. Therefore, the nitrogen-doped carbon nano material is used as a catalyst to carry out catalytic ozonization, and a more efficient catalytic effect should be obtained theoretically.
Ozone and electrolysis are combined to be one of advanced oxidation technologies, and Takusagawa et al firstly report the advanced oxidation effect of ozone electrolysis in 1976, (2005) Kishimoto et al propose the following advanced oxidation mechanism, wherein (1) is a cathode reaction:
·O3 -+H2O→·OH+O2+OH-(2)
few ozone electrolysis reactors are currently known to be developed, the earliest being a sequencing batch single compartment reactor in which the electrodes are inserted directly into the ozone bubble column. The second generation reactor is a flow type two-chamber reactor, which is divided into an anode chamber and a cathode chamber by a glass filter or an ion exchange membrane, and ozone is directly injected into the cathode chamber. However, ozone depletion efficiency in these reactors is relatively low due to the short gas-liquid contact time.
The invention considers that the hydroxyl radical generated by the ozone decomposition reaction is the fundamental power of the ozone advanced oxidation reaction, the carbon material is used as the cathode, the catalyst is subjected to cathode protection by an external electric field in the carbon catalytic ozonation process, the service life of the catalyst is prolonged, the process cost is reduced, and meanwhile, the single-electron reduction reaction of the ozone is realized by controlling the electron supply of the cathode reaction to generate the hydroxyl radical, and the reaction formula is as follows:
HO3·→HO·+O2(5)
water pollution has been a non-competitive fact, and the prior art has not been able to effectively treat a variety of specific pollutants in water, and the present invention has been made in an effort to solve this key technical problem. Emerging carbon nano materials and the traditional ozone advanced oxidation technology are combined to form a set of electro-catalytic ozonation technology system which is characterized by nonselective oxidation, green and efficient, and can efficiently degrade target pollutants. The specific idea is as follows:
various carbon materials are used as catalysts to carry out electrocatalytic ozonization reaction, and the electron supply of cathode reaction is controlled to promote the single-electron reduction reaction of ozone so as to generate a large amount of hydroxyl radicals, form strong oxidizing atmosphere, selectively oxidize target pollutants and intermediate products without generating secondary pollutants, and achieve the final purposes of thoroughly eliminating pollution and ensuring ecological safety. The catalyst is subjected to cathode protection by an external electric field in the catalytic ozonation process, and the aims of prolonging the service life of the catalyst and reducing the process cost can be achieved.
Disclosure of Invention
The invention aims to provide a separation type Venturi tube type hybrid electrocatalysis ozonization method and a device which are rapid, efficient, wide in application range and convenient to use aiming at the technical analysis and problems, and the method can be used for conveniently and rapidly removing novel pollutants in water; the device for the separated venturi tube type hybrid electrocatalytic ozonization method is simple in structure and low in investment cost.
The technical scheme of the invention is as follows:
a separation type Venturi tube type hybrid electrocatalytic ozonization method comprises the following steps:
1) firstly, a sewage pump is started, and sewage containing target pollutants is pumped into a tubular reactor through a venturi tube by using the sewage pump;
2) secondly, turning on an ozone generator, adjusting the flow and the pressure to be proper, sucking ozone by negative pressure generated at the throat part of a Venturi tube, mixing in a diffusion zone, and entering a carbon material three-dimensional electrode chamber after passing through a tubular mixing reaction unit;
3) thirdly, turning on a direct current power supply, applying 0-32v of voltage to the separated carbon material three-dimensional electrode chamber, and performing electric filtration on sewage;
4) fourthly, the sewage flows through a separated carbon material three-dimensional electrode chamber, is subjected to electro-filtration to generate electro-catalytic ozonization reaction, and target pollutants are oxidized and removed and then return to a water storage tank;
5) and fifthly, setting a proper circulation ratio according to the residual concentration of the target pollutant in the reaction effluent, and circularly performing the reaction process. Or the processes are connected in series in N stages, N is 1-10, and the target pollutants are completely removed finally.
The invention also provides a device for the separated venturi tube type hybrid electrocatalysis ozonization method, which comprises a sewage storage tank, a water pump, a venturi tube, an ozone generator, a spiral tube type reactor, a carbon material three-dimensional electrode chamber and a water storage pool, wherein the sewage storage tank is connected with the inlet of the water pump through a pipeline and is provided with a flowmeter, the outlet of the water pump is connected with the inlet of the venturi tube, the outlet of the venturi tube is connected with the inlet of the spiral tube type reactor, the ozone generator is connected with the throat pipe of the venturi tube through a pipeline and is provided with a gas-liquid separator, the outlet of the spiral tube type reactor is connected with the inlet of the carbon material three-dimensional electrode reaction chamber through a pipeline and is provided with a valve, the outlet of the carbon material three-dimensional electrode chamber is connected with the.
The working mechanism of the device is as follows:
the sewage containing the target pollutant enters a venturi tube at a high speed through a water pump, negative pressure is generated at the throat part of the venturi tube to suck ozone, the ozone and the sewage containing the target pollutant are mixed in a diffusion zone, the sewage passes through a tubular mixing reaction unit and then enters a separated carbon material three-dimensional electrode chamber with voltage of 0-32v to be subjected to electrocatalytic ozonization reaction, the target pollutant is oxidized and removed and then enters a water storage tank, and the reaction process is circularly performed. And determining the circulation times according to the residual concentration of the target pollutants in the reaction effluent, or performing N-stage series connection (taking N as 1-10) on the Venturi tube, the tubular reactor and the carbon material three-dimensional electrode chamber, and finally completely removing the target pollutants.
The invention has the beneficial effects that:
the invention combines ozone and electrolysis, uses carbon material as catalyst to carry out electrocatalytic ozonization reaction, promotes the single electron reduction reaction of ozone by controlling the electron supply of cathode reaction so as to generate a large amount of hydroxyl free radicals, forms strong oxidizing atmosphere, does not selectively oxidize target pollutants and intermediate products, does not generate secondary pollutants, and achieves the final purposes of thoroughly eliminating pollution and ensuring ecological safety; the catalyst is subjected to cathode protection by an external electric field in the catalytic ozonation process, and the aims of prolonging the service life of the catalyst and reducing the process cost can be achieved.
Drawings
FIG. 1 is a schematic view of a reaction apparatus of the present invention.
1. The device comprises a sewage storage tank, 2 flow meters, 3 sewage pumps, 4 venturi tubes, 5 ozone generators, 6 spiral tube reactors, 7 carbon material three-dimensional electrode chambers, 8 water storage tanks, 9 gas-liquid separators and 10 valves.
Detailed Description
The device for the separated venturi tube type hybrid electrocatalytic ozonization method comprises a sewage storage tank 1, a water pump 2 and a venturi tube 3, the device comprises an ozone generator 4, a spiral tube type reactor 5, a carbon material three-dimensional electrode chamber 6 and a water storage pool 7, wherein a sewage storage tank 1 is connected with an inlet of a water pump 2 through a pipeline and is provided with a flowmeter 8, an outlet of the water pump 2 is connected with an inlet of a Venturi tube 3, an outlet of the Venturi tube 3 is connected with an inlet of the spiral tube type reactor 5, the ozone generator 4 is connected with a throat pipe of the Venturi tube 3 through a pipeline and is provided with a gas-liquid separator 9, an outlet of the spiral tube type reactor 5 is connected with an inlet of the carbon material three-dimensional electrode chamber 6 through a pipeline and is provided with a valve 10, an outlet of the carbon material three-dimensional electrode chamber 6 is connected with the water storage pool 7.
The specific implementation method of the invention is that a water pump is started, sewage containing target pollutants is pumped into a tubular reactor through a venturi tube at a high speed, water flow generates negative pressure at the throat part of the venturi tube, an ozone generator is started, output ozone is connected into the throat opening of the venturi tube, the ozone is brought into fluid by the negative pressure, mixing is carried out in a diffusion zone, the fluid passes through a tubular mixing reaction unit and then enters a separation type carbon material three-dimensional electrode chamber with proper voltage for electric filtration, electric catalytic ozonation reaction is carried out in the electric filtration process, the target pollutants are oxidized and removed, and then the fluid returns to a water storage pool, and the reaction process is carried out in a circulating mode. And determining the cycle times according to the residual concentration of the target pollutant in the reaction effluent, or performing N-stage series connection on the processes, so that the target pollutant is completely removed finally.
The present invention is described in detail below with reference to examples:
example 1.
500ml of sewage containing 10mg/L of bisphenol A (BPA) is prepared, a self-made nitrogen-doped carbon nano tube membrane electrode is used as a cathode, a counter electrode is a titanium sheet, the direct current voltage is 3V, the initial pH of the reaction is 10.2, the initial current is 15mA, the ozone generation concentration is 8 percent, and the flow rate is 0.5L/min. The reaction apparatus of FIG. 1 was used. Determining the removal rate of effluent TOC:
| time (min) | TOC(mg/l) | Removal rate |
| 0 | 7.692 | 0 |
| 5.00 | 6.526 | 15.16％ |
| 15.00 | 4.186 | 45.58％ |
| 30.00 | 3.585 | 53.39％ |
| 60.00 | 2.618 | 65.96％ |
| 120.00 | 1.389 | 81.94％ |
| 180.00 | 1.186 | 84.58％ |
Example 2.
500ml of sewage containing 10mg/L of bisphenol A (BPA) is prepared, a self-made nitrogen-doped carbon nano tube membrane electrode is used as an anode, a counter electrode is a titanium sheet, the direct current voltage is 3V, the initial pH of the reaction is 10.2, the initial current is 15mA, the ozone generation concentration is 8 percent, and the flow rate is 0.5L/min. The reaction apparatus of FIG. 1 was used. Determining the removal rate of effluent TOC:
| time (min) | TOC(mg/l) | Removal rate |
| 0 | 7.776 | 0 |
| 5.00 | 4.609 | 40.73％ |
| 15.00 | 3.28 | 57.82％ |
| 30.00 | 2.815 | 63.80％ |
| 60.00 | 1.899 | 75.58％ |
| 120.00 | 1.175 | 84.89％ |
| 180.00 | 1.054 | 86.45％ |
Example 3.
500ml of sewage containing 10mg/L of bisphenol A (BPA) is prepared, a self-made multi-wall carbon nano tube membrane electrode is used as a cathode, a counter electrode is a titanium sheet, the direct current voltage is 3V, the initial reaction pH is 10.2, the initial current is 15mA, the ozone generation concentration is 8%, and the flow rate is 0.5L/min. The reaction apparatus of FIG. 1 was used. Determining the removal rate of effluent TOC:
| time (min) | TOC(mg/l) | Removal rate |
| 0 | 7.654 | 0 |
| 15.00 | 2.443 | 68.08％ |
| 30.00 | 1.001 | 86.92％ |
| 60.00 | 0.723 | 90.55％ |
| 120.00 | 0.692 | 90.96％ |
| 180.00 | 0.67 | 91.25％ |
Example 4.
500ml of sewage containing 10mg/L of bisphenol A (BPA) is prepared, a self-made multi-walled carbon nanotube membrane electrode is used as an anode, a counter electrode is a titanium sheet, the direct current voltage is 3V, the initial reaction pH is 10.2, the initial current is 15mA, the ozone generation concentration is 8%, and the flow is 0.5L/min. The reaction apparatus of FIG. 1 was used. Determining the removal rate of effluent TOC:
| time (min) | TOC(mg/l) | Removal rate |
| 0 | 7.654 | 0 |
| 15.00 | 3.462 | 54.77％ |
| 30.00 | 2.632 | 65.61％ |
| 60.00 | 1.646 | 78.49％ |
| 120.00 | 1.415 | 81.51％ |
| 180.00 | 1.511 | 80.26％ |
Example 5.
The oil extraction wastewater contains various pollutants, is diluted to about 10mg/L of TOC, takes a self-made multi-walled carbon nanotube membrane electrode as an anode, takes a titanium sheet as a counter electrode, has direct current voltage of 3V, initial reaction pH of 10.2, initial current of 15mA, ozone generation concentration of 8 percent and flow of 0.5L/min. The reaction apparatus of FIG. 1 was used. Determining the removal rate of effluent TOC:
| time (min) | TOC(mg/l) | Removal rate |
| 0 | 10.37 | 0.00％ |
| 30 | 6.3 | 39.25％ |
| 60 | 4.38 | 57.76％ |
| 90 | 3.21 | 69.05％ |
| 150 | 1.933 | 81.36％ |
| 200 | 1.021 | 90.15％ |
Example 6.
The oil extraction wastewater contains various pollutants, is diluted to about 10mg/L of TOC, takes a self-made multi-walled carbon nanotube membrane electrode as a cathode, takes a titanium sheet as a counter electrode, has direct current voltage of 3V, initial reaction pH of 10.2, initial current of 15mA, ozone generation concentration of 8 percent and flow of 0.5L/min. The reaction apparatus of FIG. 1 was used. Determining the removal rate of effluent TOC:
| time (min) | TOC(mg/l) | Removal rate |
| 0 | 10.37 | 0.00％ |
| 15 | 6.588 | 36.47％ |
| 30 | 4.661 | 55.05％ |
| 60 | 3.374 | 67.46％ |
| 90 | 2.354 | 77.30％ |
| 180 | 1.384 | 86.65％ |
Claims (5)
1. A separated venturi tube type hybrid electrocatalytic ozonization method is characterized by comprising the following steps:
1) firstly, a sewage pump is started, and sewage containing target pollutants is pumped into a tubular reactor through a venturi tube by using the sewage pump;
2) secondly, turning on an ozone generator, adjusting the flow and the pressure to be proper, sucking ozone by negative pressure generated at the throat part of a Venturi tube, mixing in a diffusion zone, and entering a carbon material three-dimensional electrode chamber after passing through a tubular mixing reaction unit;
3) thirdly, turning on a direct current power supply, applying 3-32v of voltage to the separated carbon material three-dimensional electrode chamber, and performing electric filtration on sewage;
4) fourthly, the sewage flows through a separated carbon material three-dimensional electrode chamber, is subjected to electro-filtration to generate electro-catalytic ozonization reaction, and target pollutants are oxidized and removed and then return to a water storage tank;
5) fifthly, setting a circulation ratio according to the residual concentration of the target pollutant in the reaction effluent, and circularly performing the reaction process; or the processes are connected in series in N stages, N is 1-10, and the target pollutants are completely removed finally.
2. The method of claim 1, wherein the contaminated water is a liquid mixture having a target contaminant dissolved therein.
3. The method according to claim 1, characterized in that the ozone concentration is 8-20%.
4. An apparatus using the separated venturi tube type hybrid electrocatalytic ozonization method as claimed in claim 1, characterized by comprising a sewage storage tank, a water pump, a venturi tube, an ozone generator, a spiral tube reactor, a carbon material three-dimensional electrode chamber and a water storage tank, wherein the sewage storage tank is connected with an inlet of the water pump through a pipeline and provided with a flow meter, an outlet of the water pump is connected with an inlet of the venturi tube, an outlet of the venturi tube is connected with an inlet of the spiral tube reactor, the ozone generator is connected with a throat of the venturi tube through a pipeline and provided with a gas-liquid separator, an outlet of the spiral tube reactor is connected with an inlet of the carbon material three-dimensional electrode reaction chamber through a pipeline and provided with a valve, an outlet of the carbon material three-dimensional electrode chamber is connected with the water storage tank through a.
5. The apparatus of claim 4, wherein the venturi tube is manufactured by using a phenomenon that a low pressure is generated near a fluid flowing at a high speed to generate an adsorption effect, and an opening is formed at a throat negative pressure position of the venturi tube to introduce ozone.
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