CN108439553B - Electrochemical oxidation device for removing chloride ions in water - Google Patents
Electrochemical oxidation device for removing chloride ions in water Download PDFInfo
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- CN108439553B CN108439553B CN201810359222.0A CN201810359222A CN108439553B CN 108439553 B CN108439553 B CN 108439553B CN 201810359222 A CN201810359222 A CN 201810359222A CN 108439553 B CN108439553 B CN 108439553B
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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
- C02F1/46—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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
Abstract
The invention provides an electrochemical oxidation device for removing chloride ions in water, which comprises a direct-current stabilized voltage supply, a constant-current pump, a storage tank, an oxidation chlorine removal tank, a gas collection tank, a drainage storage tank and a rotameter, wherein an electrode array consisting of an oxide anode of a titanium sheet substrate and a titanium mesh cathode which are connected with a power supply is arranged in the oxidation chlorine removal tank, chloride ions in water are directly oxidized on the surface of the anode to generate adsorbed chlorine atoms by virtue of the high potential and the catalytic activity of the anode through the electrode array consisting of the oxide anode of the titanium sheet substrate and the titanium mesh cathode, and then the two adsorbed chlorine atoms are chemically compounded to form chlorine molecules to be separated from the surface of the electrode, mainly electrons are used as a reagent, and other reagents are not required to be added. Due to the adoption of the structure, the invention has the advantages of no need of adding other medicaments, flexible operation, environmental protection, simple and convenient maintenance and continuous operation.
Description
Technical Field
The invention relates to the field of water and wastewater treatment, in particular to an electrochemical oxidation device for removing chloride ions in water.
Background
With the ten issues of water, the country increases the wastewater treatment strength, the environmental standards of various types of wastewater become strict, and zero discharge of wastewater of enterprises becomes a necessary development trend. The removal of chloride ions is one of the problems considered in zero discharge, and when circulating cooling water concentration discharge, reverse osmosis membrane concentration discharge and desulfurization wastewater reuse are all related to the removal of chloride ions in a water body. Because of the high chloride ion content, the method can corrode water system pipelines, various metal materials and related power equipment, and the treatment and recycling of the high-salinity wastewater are very difficult. The conventional treatment methods at present include: sedimentation, chemical precipitation, adsorption method, and zero-valent iron mixing technology; the advanced treatment method comprises the following steps: membrane process, evaporative crystallization process and flue evaporation. The traditional treatment method can not reduce the content of chloride ions in water basically, and the advanced treatment method can remove the chloride ions in the wastewater through a membrane treatment technology, but the problems of the service life of a membrane and the pollution of the membrane need to be further solved, and a small amount of concentrated wastewater after membrane treatment naturally contains a large amount of chloride ions, so that the discharge is influenced or the zero discharge of the wastewater can not be achieved.
The electrocatalytic advanced oxidation method can directly or indirectly oxidize the chloride ions in the water through electrode reaction with catalytic activity at normal temperature and normal pressure, and has the advantages of high treatment efficiency, simple and convenient operation and environmental compatibility.
In the electrochemical industry, the selection of anode materials is an extremely important problem, and when the anode is applied to wastewater treatment, the use environment is harsh, and the electrode materials with scouring resistance, stable property, strong catalytic capability and high economic benefit need to be selected.
Disclosure of Invention
The invention aims to provide an electrochemical advanced oxidation device for removing chloride ions in water, which has the advantages of simple structure, convenient operation and stable operation, and can efficiently and economically reduce the concentration of the chloride ions in the water by changing the voltage, the water retention time and the like of the device according to the water quality condition of the water.
The specific technical scheme is as follows:
an electrochemical oxidation device for removing chloride ions in water comprises a direct-current stabilized voltage supply, a constant flow pump, a storage tank, an oxidation dechlorination tank, a gas collecting tank, a drainage storage tank and a rotor flow meter, wherein the storage tank is communicated with the lower part of the oxidation dechlorination tank; a rotor flowmeter is arranged between the oxidation dechlorination tank and the gas collecting tank; an electrode array connected with a direct current stabilized voltage supply is arranged in the oxidation dechlorination tank; the electrode array comprises an oxide anode of a titanium sheet substrate and a titanium sheet cathode.
The oxide anode of the titanium sheet substrate takes titanium as a substrate, the surface of the titanium sheet substrate is sequentially modified with an intermediate layer and an oxide layer, and the intermediate layer is SnO with the thickness of 0.2-0.4mm2And Sb2O5The oxide layer is CeO2And (3) a layer.
The titanium sheet cathode is in a net shape.
And the lower part of the oxidation dechlorination pool is provided with a slot for plugging the power supply electrode.
The oxide anode of the titanium sheet substrate takes titanium as a substrate, and SnO is respectively and sequentially obtained on the surface of the titanium sheet substrate by coating a thermal decomposition oxidation method2And Sb2O5Then depositing CeO by an electrochemical method2To obtain Ti- (Sn, Sb) -CeO2Of (2) an anode.
The preparation steps of the oxide anode are as follows: (1) pretreatment of the titanium sheet: polishing a titanium sheet by using sand paper to show bright color, soaking the titanium sheet for 30 to 40 minutes by using hydrochloric acid with the concentration of 12 to 18 percent, and then washing the titanium sheet by using deionized water;
(2) coating an ethanol solution prepared by antimony trichloride and stannic chloride on the surface of the treated titanium sheet, controlling the molar ratio of tin to antimony to be 12:1-6:1, wherein the addition amount of the ethanol is that the antimony trichloride and the stannic chloride can be dissolved; after being coated evenly on the two sides, the two sides are dried at the temperature of 80-90 ℃, and then are calcined for 10 minutes at the temperature of 550-600 ℃ after being taken out; repeating the steps for 5-8 times, wherein the calcination time of the last time is 2 hours, and obtaining the electrode with the middle layer for later use;
(3) dissolving yellowish cerium oxide and copper nitrate in water and nitric acid, and controlling the pH value to be 1.5 to obtain an electrolyte; the concentration of cerium oxide in the electrolyte is 6-12 g/L; the concentration of the copper nitrate is 12-24 g/L;
(4) and (3) placing the electrode with the intermediate layer prepared in the step (2) into the electrolyte in the step (3), electrifying by taking two stainless steel sheets as cathodes at the temperature of 80-85 ℃, controlling the current to be 1.2-1.5A, stirring, and electrolyzing for 4-4.5 hours to obtain the oxide anode.
The core of the electrochemical oxidation device is the preparation technology of the anode in the oxidation dechlorination pool, the anode takes a titanium sheet as a substrate, an intermediate layer containing Sn and Sb is brushed by a hot coating and brushing method, and Ti-Sb, Sn-CeO is prepared by an electrodeposition method2An electrode; the cathode is a durable titanium sheet net, and the net design enables water to effectively flow in the oxidation dechlorination tank 4, so that the oxidation efficiency of the water is improved; thirdly, the design of water inlet at the bottom and exhaust at the upper part of the oxidation dechlorination tank 4 is shown in figure 2, and the retention time of water can be ensured by the design of water inlet at the bottom of the electrolytic bath.
The invention has the following beneficial technical effects:
1. the oxidation rate of the chloride ions can be effectively controlled by adjusting the voltage and the residence time of the water;
2. in the water treatment process, anodic oxidation mainly occurs, chlorine ions in water are oxidized into chlorine atoms, and two adsorbed chlorine atoms are chemically compounded to form chlorine molecules to be separated from the surface of the electrode;
3. the anode material prepared by the method has high mechanical strength, is not easy to corrode in the electrolytic process, has stable electrode surface or coating, is not easy to crack and is not easy to react with reactants and products; the corrosion resistance is strong, and the deposit is not easy to form on the surface of the electrode. The electrode material is easy to process, disassemble and replace, and can be made into different sizes and shapes according to requirements.
4. The oxidation device adopting the anode can effectively remove chloride ions in water, is flexible in assembly, can design the size of the anode according to actual needs, is easy to prepare and maintain, is low in cost and long in service life, and has good environmental and economic benefits;
5. the prepared titanium @ tin dioxide @ iridium oxide electrode has high chlorine evolution potential, high catalytic activity and high stability. The basic principle is that by utilizing an anode electrocatalytic oxidation technology, chlorine ions in the wastewater are firstly oxidized on the surface of an anode to generate adsorbed chlorine atoms, and then the two adsorbed chlorine atoms are chemically compounded to form chlorine molecules to be separated from the surface of the electrode, so that the aim of removing the chlorine ions in the water is fulfilled;
6. the method utilizes the high potential and catalytic activity of the anode to directly oxidize the chloride ions in the water, the chloride ions in the water are firstly oxidized on the surface of the anode to generate adsorbed chlorine atoms, and then the two adsorbed chlorine atoms are chemically compounded to form chlorine molecules to be separated from the surface of the electrode, mainly takes electrons as a reagent, and does not need to add other medicaments; due to the adoption of the structure, the invention has the advantages of no need of adding other medicaments, flexible operation, environmental protection, simple and convenient maintenance and continuous operation.
Drawings
FIG. 1 is a process flow of an oxide anode fabrication of a titanium plate substrate;
FIG. 2 is a schematic diagram of a process flow;
FIG. 3 is a design diagram of an oxidation dechlorination tank;
FIG. 4 is a view showing a microstructure of the prepared electrode;
wherein: a power supply-1, a constant flow pump-2, a storage tank-3, an oxidation dechlorination tank-4, a gas collection tank-5, a drainage storage tank-6 and a rotameter-7.
Detailed Description
The present invention will be further described with reference to the following examples.
An electrochemical oxidation device for removing chloride ions in water comprises a direct-current stabilized voltage supply 1, a constant-flow pump 2, a storage tank 3, an oxidation dechlorination tank 4, a gas collecting tank 5, a drainage storage tank 6 and a rotor flow meter 7, wherein the storage tank 3 and the drainage storage tank 6 are respectively connected with the oxidation dechlorination tank 4, the constant-flow pump 2 is arranged between the storage tank 3 and the oxidation dechlorination tank 4, a gas outlet is formed in the top of the oxidation dechlorination tank 4, and the oxidation dechlorination tank 4 is communicated with the gas collecting tank 5 through the gas outlet; a rotor flowmeter 7 is arranged between the oxidation dechlorination tank 4 and the gas collecting tank 5; an electrode array connected with a direct current stabilized voltage power supply 1 is arranged in the oxidation dechlorination tank 4; the electrode array comprises an oxide anode of a titanium sheet substrate and a titanium sheet cathode. The oxide anode of the titanium sheet substrate takes titanium as a substrate, the surface of the titanium sheet substrate is sequentially modified with an intermediate layer and an oxide layer, and the intermediate layer is SnO with the thickness of 0.2-0.4mm2And Sb2O5The oxide layer is CeO2And (3) a layer.
The titanium sheet cathode is in a net shape.
And the lower part of the oxidation dechlorination pool 4 is provided with a slot for plugging the power supply electrode.
The oxide anode of the titanium sheet substrate takes titanium as a substrate, and SnO is respectively and sequentially obtained on the surface of the titanium sheet substrate by coating a thermal decomposition oxidation method2And Sb2O5Then depositing CeO by an electrochemical method2To obtain Ti- (Sn, Sb) -CeO2Of (2) an anode.
The preparation steps of the oxide anode are as follows: (1) pretreatment of the titanium sheet: polishing a titanium sheet by using sand paper to show bright color, soaking the titanium sheet for 40 minutes by using hydrochloric acid with the concentration of 12 percent, and then washing the titanium sheet by using deionized water;
(2) adding antimony trichloride and stannic chloride into an ethanol solution to dissolve the antimony trichloride and the stannic chloride, and controlling the molar ratio of tin to antimony to be 12: 1; obtaining an ethanol solution of antimony trichloride and stannic chloride; coating an ethanol solution prepared by antimony trichloride and stannic chloride on the surface of the treated titanium sheet; after being coated evenly on the two sides, the two sides are dried at the temperature of 80-90 ℃, and then are calcined for 10 minutes at the temperature of 550-600 ℃ after being taken out; repeating the steps for 5-8 times, wherein the calcination time of the last time is 2 hours, and obtaining the electrode with the middle layer for later use;
(3) dissolving yellowish cerium oxide and copper nitrate in water and nitric acid, and controlling the pH value to be 1.5 to obtain an electrolyte; the concentration of cerium oxide in the electrolyte is 6 g/L; the concentration of the copper nitrate is 12 g/L;
(4) and (3) placing the electrode with the intermediate layer prepared in the step (2) into the electrolyte in the step (3), taking two stainless steel sheets as cathodes, electrifying under the condition of 80-85 ℃, controlling the current to be 1.2A, stirring, and electrolyzing for 4-4.5 hours to obtain the oxide anode.
Example 2
The specific structure is the same as the embodiment, and the difference is the preparation condition of the oxide anode;
the preparation steps of the oxide anode are as follows: (1) pretreatment of the titanium sheet: polishing a titanium sheet by using sand paper to show bright color, soaking the titanium sheet for 30 minutes by using hydrochloric acid with the concentration of 18 percent, and then washing the titanium sheet by using deionized water;
(2) adding antimony trichloride and stannic chloride into an ethanol solution to dissolve the antimony trichloride and the stannic chloride, coating the ethanol solution prepared by mixing the antimony trichloride and the stannic chloride on the surface of the treated titanium sheet, and controlling the molar ratio of tin to antimony to be 6: 1; after being coated evenly on the two sides, the two sides are dried at the temperature of 80-90 ℃, and then are calcined for 10 minutes at the temperature of 550-600 ℃ after being taken out; repeating the steps for 5-8 times, wherein the calcination time of the last time is 2 hours, and obtaining the electrode with the middle layer for later use;
(3) dissolving yellowish cerium oxide and copper nitrate in water and nitric acid, and controlling the pH value to be 1.5 to obtain an electrolyte; the concentration of cerium oxide in the electrolyte is 12 g/L; the concentration of the copper nitrate is 24 g/L;
(4) and (3) placing the electrode with the intermediate layer prepared in the step (2) into the electrolyte in the step (3), taking two stainless steel sheets as cathodes, electrifying under the condition of 80-85 ℃, controlling the current to be 1.5A, stirring, and electrolyzing for 4-4.5 hours to obtain the oxide anode.
Fig. 1 shows an anode fabrication process flow.
According to the figure 2, the oxidation dechlorination pond is provided with voltage by a direct current stabilized voltage supply, and the efficiency and time for reducing the chloride ions in the treated water are controlled by adjusting the output voltage. The constant flow pump can continuously input water to be treated to the oxidation dechlorination tank 4, the drainage storage tank is used for storing the treated water, and the treatment effect of the oxidation dechlorination tank 4 on the chloride ions in the water can be analyzed by sampling through the tank.
According to the figure 3, the oxidation dechlorination tank 4 is a closed organic glass cylinder container, an electrode socket is designed at the bottom, the water inlet direction is parallel to the electrode, so that the wastewater can smoothly circulate in the oxidation dechlorination tank 4, the lower ends of the anode and the cathode are respectively connected to the anode and the cathode of a direct current stabilized voltage power supply through leads, the water enters from the bottom of the oxidation dechlorination tank 4 and is oxidized and degraded through a period of retention time of the oxidation dechlorination tank 4, the upper part of the water is discharged to a water discharge storage tank, and chlorine generated after chlorine ions lose electrons enters a gas collection tank after being measured by a flowmeter.
The SEM of fig. 4, 5 provides the microstructure of the prepared electrode.
The working process of the invention is as follows:
1. and installing and fixing the anode and the cathode in an oxidation dechlorination tank, and connecting a lead.
2. And (3) injecting a certain amount of wastewater into the storage tank, and opening the constant flow pump to ensure that the wastewater stably enters the oxidation dechlorination tank.
3. Preparing chlorine absorption liquid, and adopting 10% sodium hydroxide as absorption liquid.
4. And connecting a power supply with the cathode and the anode, and starting the electrochemical reaction by turning on the direct-current stabilized voltage power supply.
The first embodiment is as follows: the required anode is prepared by the preparation method, and sewage drainage of the Olympic technologies of Hubei Jin is treated, wherein the quality of the sewage drainage is as follows: 625.7mg/L of chloride ions, 5.42mmol/L of hardness and 1.877 mg.L of ammonia nitrogen-1The pH value is 6.2-6.5, and the volume of the treatment pool is 3L by design; 138cm2(four), cathode area: 138cm2(four blocks).
The device is filled with 3L of wastewater (without adjusting pH), is electrified under different conditions, is statically treated for 3 hours firstly, ensures that the chloride ions in the 3L of wastewater in the treatment pool are reduced by 80 percent, then the constant flow pump is opened, the water inlet flow and the water outlet flow and the retention time are controlled, the treatment is carried out according to different conditions, the sampling is carried out once per hour, the chloride ion concentration of the water sample in the drainage pool is monitored, the test is continuously operated each time, the chloride ions in the outlet water are stabilized at 60.1-67.28mg/L, and the removal rate is about 89.24-90.4 percent.
The second embodiment: the ion exchange resin regeneration wastewater of Shenhua Funeng (Fujian Yanshi) generating Limited liability company is treated by the device, and the wastewater quality is as follows: 1683.7mg/L of chloride ions, 4.09mmol/L of hardness, 1.82-2.05 of pH and 3L of designed treatment tank volume; area of the anode: 138cm2(four), cathode area: 138cm2(four blocks).
At a current density of 45.0mA/cm2Under the condition of (3), the chloride ions in the acid-base wastewater are reduced from 1683.70mg/L to 505.70mg/L, and the removal rate is 70.0 percent; the hardness is reduced from 4.09mmol/L to 2.94mmol/L, which is reduced by 28.11%.
It should be understood that parts of the specification not set forth in detail are well within the prior art.
It should be understood that the above description of the preferred embodiments is given for clarity and not for any purpose of limitation, and that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (3)
1. The application of the electrochemical oxidation device for removing the chloride ions in the water is characterized in that: the electrochemical oxidation device comprises a direct-current stabilized voltage power supply (1), a constant-flow pump (2), a storage tank (3), an oxidation dechlorination tank (4), a gas collecting tank (5), a drainage storage tank (6) and a rotor flow meter (7), wherein the storage tank (3) and the drainage storage tank (6) are respectively connected with the oxidation dechlorination tank (4), the constant-flow pump (2) is arranged between the storage tank (3) and the oxidation dechlorination tank (4), a gas outlet is formed in the top of the oxidation dechlorination tank (4), and the oxidation dechlorination tank (4)Is communicated with the gas collecting tank (5) through a gas outlet; a rotameter (7) is arranged between the oxidation dechlorination tank (4) and the gas collecting tank (5); an electrode array connected with a direct current stabilized voltage power supply (1) is arranged in the oxidation dechlorination tank (4); the electrode array comprises an oxide anode of a titanium sheet substrate and a titanium sheet cathode; the oxide anode of the titanium sheet substrate takes titanium as a substrate, the surface of the titanium sheet substrate is sequentially modified with an intermediate layer and an oxide layer, and the intermediate layer is SnO with the thickness of 0.2-0.4mm2And Sb2O5The oxide layer is CeO2A layer; the preparation steps of the oxide anode are as follows: (1) pretreatment of the titanium sheet: polishing a titanium sheet by using sand paper to show bright color, soaking the titanium sheet for 30 to 40 minutes by using hydrochloric acid with the concentration of 12 to 18 percent, and then washing the titanium sheet by using deionized water;
(2) uniformly coating an ethanol solution prepared from antimony trichloride and stannic chloride on the surface of the treated titanium sheet, controlling the molar ratio of tin to antimony to be 12:1-6:1, wherein the addition amount of ethanol can dissolve the antimony trichloride and the stannic chloride; after being coated evenly on the two sides, the two sides are dried at the temperature of 80-90 ℃, and then are calcined for 10 minutes at the temperature of 550-600 ℃ after being taken out; repeating the steps for 5-8 times, wherein the calcination time of the last time is 2 hours, and obtaining the electrode with the middle layer for later use;
(3) dissolving yellowish cerium oxide and copper nitrate in water and nitric acid, and controlling the pH =1.5 to obtain an electrolyte; the concentration of cerium oxide in the electrolyte is 6-12 g/L; the concentration of the copper nitrate is 12-24 g/L;
(4) and (3) placing the electrode with the intermediate layer prepared in the step (2) into the electrolyte in the step (3), electrifying by taking two stainless steel sheets as cathodes at the temperature of 80-85 ℃, controlling the current to be 1.2-1.5A, stirring, and electrolyzing for 4-4.5 hours to obtain the oxide anode.
2. The use of claim 1, wherein: the titanium sheet cathode is in a net shape.
3. The use of claim 1, wherein: and the lower part of the oxidation dechlorination pool (4) is provided with a slot for plugging the power supply electrode.
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| CN109534709B (en) * | 2018-11-20 | 2022-05-31 | 中国京冶工程技术有限公司 | Equipment for quickly removing chloride ions in sea sand |
| CN110357220B (en) * | 2019-07-01 | 2021-12-03 | 太原理工大学 | Method and device for removing chloride ions in desulfurization wastewater through electrochemical coupling |
| CN110642339B (en) * | 2019-09-19 | 2021-01-01 | 武汉大学 | Porous Ti/IrO2-Nb2O5-Bi2O3Preparation method and application of electrode |
| CN114054483B (en) * | 2021-11-03 | 2023-04-11 | 浙江坤德创新岩土工程有限公司 | Large-volume alkaline residue in-situ electric dechlorination and dehydration method |
| CN114082769B (en) * | 2021-11-03 | 2023-03-17 | 浙江坤德创新岩土工程有限公司 | Large-volume alkaline residue electric dechlorination method |
| CN114044696B (en) * | 2021-11-10 | 2022-06-17 | 河海大学 | Device for removing chloride ions, preparation method and application |
| CN114409146A (en) * | 2022-01-18 | 2022-04-29 | 中石化节能技术服务有限公司 | Device and method for electrochemically catalyzing and degrading total nitrogen in high-salinity wastewater |
| CN115520941B (en) * | 2022-11-10 | 2023-05-30 | 中建安装集团有限公司 | Hydraulic self-adaptive electrochemical semi-flexible reaction device |
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