CN107140716B - Equipment and method for treating dye wastewater by electrochemical-adsorption composite process - Google Patents
Equipment and method for treating dye wastewater by electrochemical-adsorption composite process Download PDFInfo
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- CN107140716B CN107140716B CN201710479443.7A CN201710479443A CN107140716B CN 107140716 B CN107140716 B CN 107140716B CN 201710479443 A CN201710479443 A CN 201710479443A CN 107140716 B CN107140716 B CN 107140716B
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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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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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
- C02F1/46104—Devices therefor; Their operating or servicing
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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
- C02F1/4674—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation with halogen or compound of halogens, e.g. chlorine, bromine
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- 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
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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- 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
- C02F2001/46133—Electrodes characterised by the material
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- 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
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4616—Power supply
- C02F2201/4617—DC only
Abstract
The invention provides equipment and a treatment method for treating dye wastewater by an electrochemical-adsorption composite process, wherein a main electrode plate of a reactor consists of a graphite plate cathode loaded with metal copper and palladium and a titanium anode coated with ruthenium, titanium and tin, and anhydrous NaCl and powdered activated carbon are filled between the main electrode plates.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to equipment and a method for treating dye wastewater by an electrochemical-adsorption composite process.
Background
Along with the rapid development of the dye production and printing and dyeing industry in China, the discharge amount of the waste water in the dye industry is also increased rapidly, and according to data provided by relevant departments, about 1.8 memory cubic meters of the waste water in the dye industry is discharged into the environment every year in China. The dye wastewater has high organic matter content, large chroma, complex components and wide PH variation range. Because the production varieties of the dye are various and develop towards the photolysis resistance, oxidation resistance and biological oxidation resistance, the treatment difficulty of the dye wastewater is further increased. The dye wastewater contains a large amount of organic pollutants, and after being discharged into a water body, dissolved oxygen in the water body is consumed, so that the balance of a water body ecological system is damaged, and the survival of fishes and other aquatic organisms is seriously threatened. In view of the above, the treatment of dye wastewater has become the focus of domestic and foreign research.
The traditional method for treating the dye wastewater comprises a physical method, a chemical method, a biological method and the like. The methods have certain effect on the treatment of the dye wastewater and have defects at the same time.
In order to find a method for solving the problem of environmental pollution caused by dye wastewater more effectively and economically, people adopt different methods and technologies to try various treatment approaches to the dye wastewater. The electrochemical water treatment technology attracts a plurality of researchers at home and abroad, and has the advantages of simple equipment, convenient operation, small secondary pollution, wide application range and the like.
Therefore, in consideration of the superiority and development trend of the composite process, the invention takes the rubigins S simulated dye wastewater as a research object, and adopts a treatment method combining an electrochemical technology and an adsorption technology to deeply research the treatment of the dye wastewater by the electrochemical-adsorption synergistic composite process.
Disclosure of Invention
The technical problem to be solved is as follows: the application mainly provides equipment and a treatment method for treating dye wastewater by an electrochemical-adsorption composite process, and solves the technical problems that carbon nitride is a powder material, stirring is needed in the use process, and the carbon nitride is not easy to recover after being used in the prior art.
The technical scheme is as follows: an apparatus for treating dye wastewater by an electrochemical-adsorption composite process comprises a direct current stabilized power supply, a graphite plate cathode loaded with metallic copper palladium, a ruthenium-tin coating titanium anode, a magnetic stirrer, a wastewater storage tank, a magnetic stirrer, a peristaltic pump, an overflow port, a water inlet valve, a water outlet valve and powdered activated carbon, wherein the graphite plate cathode loaded with metallic copper palladium and the ruthenium-tin coating titanium anode are respectively arranged at two ends of a tank body of the apparatus for treating dye wastewater by the electrochemical-adsorption composite process, the graphite plate cathode loaded with metallic copper palladium is connected with the negative electrode of the direct current stabilized power supply through a lead, the ruthenium-tin coating titanium anode is connected with the positive electrode of the direct current stabilized power supply through a lead, powdered activated carbon and anhydrous sodium chloride are filled between the graphite plate cathode loaded with metallic copper palladium and the ruthenium-tin coating titanium anode, the overflow port is arranged below a top cover of the tank body, the top cover of the tank body, the top cover of the tank body is provided with a group of openings, the bottom of the tank body is provided with a magnetic stirrer, the tank body is internally provided with a magnetic stirrer, the water inlet valve and the water outlet valve are respectively arranged at two sides of the tank body, the wastewater storage tank is connected with the water inlet valve through a peristaltic pump, when wastewater completely reacts in the tank body, the wastewater flows out from the water outlet valve, and when the wastewater in the tank body is excessive, the excessive wastewater overflows from the overflow port.
As a preferred technical scheme of the invention: the loadPreparing a graphite plate cathode of metal copper palladium by an ethylene glycol reduction method, taking a graphite plate electrode, polishing the surface of the graphite plate electrode by using abrasive paper to be smooth and flat, sequentially putting the graphite plate electrode into a NaOH solution and a hydrochloric acid solution for soaking, washing and drying to prepare a prepared graphite plate electrode, putting the prepared graphite plate electrode into an ethylene glycol solution, and carrying out ultrasonic treatment for 1 h; 76mg of PdCl were weighed out272mg of CuCl2 .2H2O and 240mg of sodium citrate are put into a 250mL round bottom flask, 50mL of ethylene glycol EG is added, stirring is carried out for 1h at room temperature, then the graphite plate electrode soaked in the ethylene glycol is placed in the flask, 5wt% of KOH/EG solution is used for adjusting the pH of the reaction mixed solution to 9.5-0-10.5, stirring is carried out for 30min at room temperature, then the reaction mixed solution is put into an oil bath and reacts for 6h at 160 ℃, after the reaction is finished, the graphite plate electrode is taken out, the graphite plate electrode is washed by deionized water, and vacuum drying is carried out, thus obtaining the graphite plate cathode loaded with metal copper and palladium.
As a preferred technical scheme of the invention: the tank body of the equipment for treating the dye wastewater by the electrochemical-adsorption composite process is a cuboid, and the size of the tank body is 15cm multiplied by 10cm multiplied by 12 cm.
As a preferred technical scheme of the invention: the sizes of the graphite plate cathode loaded with metal copper palladium and the ruthenium tin coating titanium anode are both 10cm multiplied by 8cm multiplied by 0.5cm, and the distance between the two electrodes is 3.0-5.0 cm.
As a preferred technical scheme of the invention: the particle size of the powdered activated carbon particles is 0.15-2.00 mm.
As a preferred technical scheme of the invention: the overflow port is 1-5cm lower than the top end of the tank body.
The treatment method of the equipment for treating the dye wastewater by the electrochemical-adsorption composite process comprises the following steps:
the first step is as follows: boiling powdered activated carbon in distilled water for 2-4h, washing with distilled water for 5-10min, drying at 120 ℃ for 24-48h, taking out, placing between a graphite plate cathode loaded with metal copper and palladium and a ruthenium-tin coating titanium anode, and simultaneously adding 20g/L anhydrous sodium chloride;
the second step is that: turning on a direct-current power supply, adjusting the voltage range to be less than or equal to 9V, controlling the reaction intermittent time to be less than or equal to 30min, turning on a water inlet valve, starting a peristaltic pump, and enabling dye wastewater to enter a reactor from a wastewater storage tank, wherein the dye wastewater adopts alizarin S dye wastewater simulating wastewater, the initial concentration is 1000mg/L, COD =600mg/L, and the chromaticity is 4-6;
step three, effluent detection: closing the water inlet valve after reaction, opening the water outlet valve, allowing the treated dye wastewater to flow out of the water outlet valve, and discharging the treated dye wastewater after detecting that COD and chroma in the treated dye wastewater reach Integrated wastewater discharge Standard (GB 8978-1996);
the fourth step: when the concentration of the dye wastewater is increased, the concentration of the treated effluent water is increased and cannot reach the integrated wastewater discharge standard (GB 8978-1996), a water inlet valve and a peristaltic pump are closed, the voltage and the reaction intermittent time are readjusted until the effluent water reaches the standard, and then the normal treatment process is recovered.
As a preferred technical scheme of the invention: the four-step readjustment voltage and reaction pause time adjusting method comprises the steps of sequentially increasing the voltages by 1V, 3V, 5V, 7V and 9V, and adjusting the reaction pause times by 5min, 10min, 15min, 20min, 25min and 30 min.
Has the advantages that: compared with the prior art, the equipment and the treatment method for treating the dye wastewater by the electrochemical-adsorption composite process have the following technical effects:
1. aiming at the improvement of the traditional three-dimensional electrode, a novel electrode pair is introduced, a graphite plate loaded with metal copper palladium and a ruthenium tin titanium anode are loaded, and powdered activated carbon and anhydrous NaCl are added between the electrodes to serve as electrolytes, so that a dye wastewater treatment device and process which are high in current efficiency, strong in oxidation capacity, low in energy consumption, good in COD removal and decoloration effects, convenient to operate and wide in application range are formed, and the dye wastewater treatment device and process have positive significance for treating dye wastewater;
2. a new electrode pair is adopted, graphite plate loaded metal copper palladium is used as a cathode, and a titanium anode with a ruthenium-tin coating is adopted. Then the electrode and powdered activated carbon in the reactor form a three-dimensional electrode reactor, thereby greatly improving the specific surface area of the electrode and enhancing the electrolysis effect;
3. an electrochemical-adsorption composite process is adopted, and a treatment process with electrochemistry as the main part and an adsorption method as the auxiliary part is skillfully combined, so that time and energy are saved, and the effect of treating the dye wastewater is greatly improved;
4. powdered activated carbon is used as filler, which can be used as electrolyte and adsorbent. The top cover of the reactor can be uncovered, and a hole is formed in the top cover, so that the assembly of the reactor and the replacement of the filler are facilitated, and the gas is conveniently discharged in the reaction process;
5. by utilizing a series of electrochemical reactions of electrolyte sodium chloride, intermediates such as HClO, OCl, HClO3 and the like with extremely strong oxidizability can be generated, and organic matters are subjected to oxidative degradation, so that the chromaticity removal effect on dye wastewater is very good;
6. the two ends of the reactor are connected with a power supply, the activated carbon becomes charged particles in an electric field and can serve as a carrier for electrochemical oxidation reduction, organic molecules which are difficult to degrade complete the process of getting lost charges on the carrier, the molecules are broken and decomposed into small molecules, and part of the molecules can be directly oxidized and decomposed into H2O and CO2The powdery active carbon serves as a third electrode in the electrochemical-adsorption composite process, so that the specific surface area of the electrode is greatly improved, and the electrolytic effect is enhanced;
7. after the raw wastewater (200 mg/L, 600mg/L and 1000 mg/L) with different concentrations is treated, the removal rates of COD and chromaticity in the wastewater reach 85-90%, which shows that the process has very high efficiency on the treatment effect of the dye wastewater.
Description of the drawings:
FIG. 1 is a schematic structural diagram of a reactor for treating dye wastewater by the electrochemical-adsorption composite process.
Description of reference numerals: 1. the device comprises a direct current stabilized power supply, 2, a graphite plate cathode loaded with metal copper palladium, 3, a ruthenium-tin coating titanium anode, 4, a magnetic stirrer, 5, a wastewater storage tank, 6, a magnetic stirrer, 7, a peristaltic pump, 8, an overflow port, 9-1 water outlet valve, 9-2 water inlet valve, 10 and powdered activated carbon.
Detailed Description
The following detailed description of embodiments of the invention is provided in conjunction with the accompanying drawings: in the examples, ruthenium-tin coated titanium anodes were purchased from Shanxi Bao chicken Medium-color Special metals, LLC.
Example 1
As shown in figure 1, the device for treating dye wastewater by an electrochemical-adsorption composite process comprises a direct current stabilized power supply 1, a graphite plate cathode 2 loaded with metal copper and palladium, a ruthenium-tin coated titanium anode 3, a magnetic stirrer 4, a wastewater storage tank 5, a magnetic stirrer 6, a peristaltic pump 7, an overflow port 8, a water outlet valve 9-1, a water inlet valve 9-2 and powdered activated carbon 10, wherein the graphite plate cathode 2 loaded with metal copper and palladium is prepared by an ethylene glycol reduction method, a graphite plate electrode is taken, the surface of the graphite plate electrode is polished to be smooth and flat by abrasive paper, the graphite plate electrode is sequentially soaked in NaOH solution and hydrochloric acid solution, washed and dried to prepare a prepared graphite plate electrode, and the prepared graphite plate electrode is placed in the ethylene glycol solution and subjected to ultrasonic treatment for 1 hour; 76mg of PdCl were weighed out272mg of CuCl2 .2H2O and 240mg of sodium citrate are put in a 250mL round bottom flask, 50mL of ethylene glycol EG is added, stirring is carried out for 1h at room temperature, then the graphite plate electrode soaked in the ethylene glycol is placed in the flask, 5wt% of KOH/EG solution is used for adjusting the pH of reaction mixed solution to 9.5-0-10.5, stirring is carried out for 30min at room temperature continuously, then the reaction mixed solution is placed in an oil bath, reaction is carried out for 6h at 160 ℃, after the reaction is finished, the graphite plate electrode is taken out, the graphite plate electrode is washed by deionized water and dried in vacuum, a graphite plate cathode loaded with metallic copper and palladium is obtained, a tank body of equipment for treating dye wastewater by an electrochemical-adsorption composite process is a cuboid anode with the size of 15cm × 10cm × 12cm, the graphite plate cathode 2 loaded with the metallic copper and palladium and the ruthenium tin-coated titanium anode 3 are respectively arranged at two ends of the equipment for treating the dye wastewater by the electrochemical-adsorption composite process, the graphite plate cathode 2 and the tin-coated titanium anode with the ruthenium are respectively arranged between 10cm × 8cm × 0.5cm ruthenium and the anode of a stabilized voltage power supply, the graphite plate anode is connected with the cathode of the anode loaded metallic copper-ruthenium-tin-supported by a stabilized voltage power supply direct current lead wire with the cathode of which is a cathode of 10.8 mm, the graphite plate anode of the graphite plate anode with the cathode of the anode of the cathode of the anode ofUnder the cover. The overflow port 8 is 1cm lower than the top end of the tank body, the top cover of the tank body is movably connected with the tank body, the top cover is provided with a group of openings, the bottom of the tank body is provided with a magnetic stirrer 4, the tank body is internally provided with a magnetic stirrer 6, the water outlet valve and the water inlet valve 9-2 are respectively arranged at two sides of the tank body, the wastewater storage tank 5 is connected with the water inlet valve 9-2 through a peristaltic pump 7, when the wastewater completely reacts in the tank body, the wastewater flows out through the water outlet valve 9-1, and when the wastewater in the tank body is excessive.
The treatment method specifically comprises the following steps:
the first step is as follows: the powdery active carbon 10 is put into distilled water to be boiled for 2h, then is washed by distilled water for 5min to remove water-soluble and volatile substances in the active carbon, is dried for 24h at 120 ℃ after being washed, is taken out, is put between a graphite plate cathode 2 loaded with metal copper palladium and a ruthenium tin coating titanium anode 3, the distance between two electrode plates is 3.0cm, and 20g/L NaCl is added between the electrode plates.
The second step is that: turning on a direct-current power supply 1, adjusting voltage to 5V, controlling reaction pause time to be 5min, turning on a water inlet valve 9-2, turning on a peristaltic pump 7, and enabling dye wastewater to enter a reactor from a wastewater storage tank 5, wherein the dye wastewater is alizarin S dye wastewater simulating wastewater, the initial concentration is 200mg/L, COD =600mg/L, and the chromaticity is 4.
Step three, effluent detection: after the reaction, closing the water inlet valve 9-2, opening the water outlet valve 9-1, allowing the treated dye wastewater to flow out of the water outlet valve 9-1, detecting COD and chroma in the treated dye wastewater, and after the reaction is carried out for 15 minutes, removing rates of the COD and the chroma of the treated original wastewater respectively reach 98% and 90%, so that obvious comparison is formed between the removing rates and the original wastewater.
The fourth step: when the concentration of the dye wastewater is increased, so that the treated effluent cannot reach the integrated wastewater discharge standard (GB 8978-1996), closing the water inlet valve 9-2 and the peristaltic pump 7, adjusting the voltage and the reaction pause time until the effluent reaches the standard and then recovering the normal treatment process, wherein the method for re-adjusting the voltage and the reaction pause time comprises the steps of sequentially increasing the voltage by 1V, 3V, 5V, 7V and 9V, and adjusting the reaction pause time by 5min, 10min, 15min, 20min, 25min and 30 min.
Example 2
As shown in the figure1, the equipment for treating dye wastewater by an electrochemical-adsorption composite process comprises a direct current stabilized power supply 1, a graphite plate cathode 2 loaded with metal copper palladium, a ruthenium-tin coating titanium anode 3, a magnetic stirrer 4, a wastewater storage tank 5, a magnetic stirrer 6, a peristaltic pump 7, an overflow port 8, a water outlet valve 9-1, a water inlet valve 9-2 and powdered activated carbon 10, wherein a tank body of the equipment for treating dye wastewater by the electrochemical-adsorption composite process is a cuboid, the size of the tank body is 15cm x 10cm x 12cm, the graphite plate cathode 2 loaded with metal copper palladium and the ruthenium-tin coating titanium anode 3 are respectively arranged at two ends of the tank body of the equipment for treating dye wastewater by the electrochemical-adsorption composite process, the graphite plate cathode 2 loaded with metal copper palladium is prepared by an ethylene glycol reduction method, a graphite plate electrode is taken, the surface of sand paper is polished to be smooth and flat, sequentially putting the graphite electrode into NaOH solution and hydrochloric acid solution for soaking, washing and drying to prepare a prepared graphite plate electrode, putting the prepared graphite plate electrode into ethylene glycol solution, and carrying out ultrasonic treatment for 1 h; 76mg of PdCl were weighed out272mg of CuCl2 .2H2O and 240mg of sodium citrate are put in a 250mL round bottom flask, 50mL of ethylene glycol EG is added, stirring is carried out for 1h at room temperature, then the graphite plate electrode soaked in the ethylene glycol is placed in the flask, 5wt% of KOH/EG solution is used for adjusting the pH of the reaction mixed solution to 9.5-0-10.5, stirring is carried out for 30min at room temperature, then the reaction mixed solution is put in an oil bath and reacts for 6h at 160 ℃, after the reaction is finished, the graphite plate electrode is taken out, deionized water is used for washing, vacuum drying is carried out, the graphite plate cathode loaded with metallic copper palladium is obtained, the size of the graphite plate cathode 2 loaded with the metallic copper palladium and the size of the ruthenium tin coating titanium anode 3 are both 10cm x 8cm x 0.5cm, the distance between the two electrodes is 4.0cm, the graphite plate cathode 2 loaded with the metallic copper palladium is connected with the cathode of a direct current stabilized voltage power supply 1 through a lead, the ruthenium tin coating titanium anode 3 is connected with the anode of the, powdered activated carbon 10 and anhydrous sodium chloride are filled between a graphite plate cathode 2 loaded with metal copper palladium and a ruthenium tin coating titanium anode 3, the particle size of the powdered activated carbon 10 is 0.170mm, and an overflow port 8 is arranged below a top cover of the tank body. The overflow port 8 is lower than the top end of the tank body by 3cm, the top cover of the tank body is movably connected with the tank body, a group of openings are arranged on the top cover, a magnetic stirrer 4 is arranged at the bottom of the tank body, and magnetic stirring is arranged in the tank bodyAnd 6, the water outlet valve 9-1 and the water inlet valve 9-2 are respectively arranged at two sides of the tank body, the waste water storage tank 5 is connected with the water inlet valve 9-2 through the peristaltic pump 7, when the waste water completely reacts in the tank body, the waste water flows out through the water outlet valve (9-1), and when the waste water in the tank body is excessive, the excessive waste water overflows from the overflow port (8).
The treatment method specifically comprises the following steps:
the first step is as follows: the powdery active carbon 10 is put into distilled water to be boiled for 3h, then the distilled water is used for washing for 8min to remove water-soluble and volatile substances in the active carbon, the active carbon is dried for 36h at 120 ℃ after the washing is finished, the active carbon is taken out, the active carbon is put between a graphite plate cathode 2 loaded with metal copper palladium and a ruthenium tin coating titanium anode 3, the distance between two electrode plates is 3.0cm, and 20g/L NaCl is added between the electrode plates.
The second step is that: turning on a direct-current power supply 1, adjusting the voltage to be 5V, controlling the reaction intermittent time to be 15min, turning on a water inlet valve 9-2, turning on a peristaltic pump 7, and enabling dye wastewater to enter a reactor from a wastewater storage tank 5, wherein the dye wastewater is alizarin S dye wastewater simulating wastewater, the initial concentration is 600mg/L, COD =600mg/L, and the chromaticity is 5.
The third step: and (3) effluent detection: after the reaction, closing the water inlet valve 9-2, opening the water outlet valve 9-1, allowing the treated dye wastewater to flow out of the water outlet valve 9-1, and discharging the treated dye wastewater after detecting that COD and chroma in the treated dye wastewater reach the Integrated wastewater discharge Standard (GB 8978-1996); after the reaction is carried out for 25 minutes, the removal rate of COD and chromaticity in the treated wastewater reaches 90 percent.
The fourth step: when the concentration of the dye wastewater is increased, the concentration of the treated effluent water is increased and cannot reach the integrated wastewater discharge standard (GB 8978-1996), the water inlet valve 9-2 and the peristaltic pump 7 are closed, the voltage and the reaction intermittent time are readjusted, and the normal treatment process is recovered until the effluent water reaches the standard. The method for readjusting voltage and reaction pause time comprises sequentially increasing voltage 1V, 3V, 5V, 7V and 9V, and adjusting reaction pause time 5min, 10min, 15min, 20min, 25min and 30 min.
Example 3
As shown in figure 1, the equipment for treating dye wastewater by an electrochemical-adsorption composite process comprises a direct current stabilized voltage power supply 1 and a graphite plate cathode loaded with metal copper2. The device comprises a ruthenium-tin coating titanium anode 3, a magnetic stirrer 4, a wastewater storage tank 5, a magnetic stirrer 6, a peristaltic pump 7, an overflow port 8, a water outlet valve 9-1, a water inlet valve 9-2 and powdered activated carbon 10, wherein a tank body of the equipment for treating dye wastewater by the electrochemical-adsorption composite process is a cuboid with the size of 15cm 10cm 12cm, a graphite plate cathode 2 loaded with metallic copper and palladium and the ruthenium-tin coating titanium anode 3 are respectively arranged at two ends of the tank body of the equipment for treating dye wastewater by the electrochemical-adsorption composite process, the graphite plate cathode 2 loaded with metallic copper and palladium is prepared by an ethylene glycol reduction method, a graphite plate electrode is taken, the surface of the graphite plate electrode is polished to be smooth and flat, the graphite plate electrode is sequentially soaked in NaOH solution and hydrochloric acid solution, then washed and dried to prepare the graphite plate electrode, the prepared graphite plate electrode is placed in the ethylene glycol solution, performing ultrasonic treatment for 1 h; 76mg of PdCl were weighed out272mg of CuCl2 .2H2O and 240mg of sodium citrate are put in a 250mL round bottom flask, 50mL of ethylene glycol EG is added, stirring is carried out for 1h at room temperature, then the graphite plate electrode soaked in the ethylene glycol is placed in the flask, 5wt% of KOH/EG solution is used for adjusting the pH of the reaction mixed solution to 9.5-0-10.5, stirring is carried out for 30min at room temperature, then the reaction mixed solution is put in an oil bath and reacts for 6h at 160 ℃, after the reaction is finished, the graphite plate electrode is taken out, the graphite plate electrode is washed by deionized water and dried in vacuum, a graphite plate cathode loaded with metallic copper palladium is obtained, the sizes of the graphite plate cathode 2 loaded with the metallic copper palladium and the graphite plate anode 3 loaded with the metallic copper palladium are both 10cm x 8cm x 0.5cm, the distance between the two electrodes is 5.0cm, the graphite plate cathode 2 loaded with the metallic copper palladium is connected with the cathode of a direct current stabilized voltage power supply 1 through a lead, the ruthenium tin coating titanium anode 3 is connected with the positive, powdered activated carbon 10 and anhydrous sodium chloride are filled between a graphite plate cathode 2 loaded with metal copper palladium and a ruthenium tin coating titanium anode 3, the particle size of the powdered activated carbon 10 is 2.00mm, and an overflow port 8 is arranged below a top cover of the tank body. An overflow port 8 is lower than the top end of the tank body by 5cm, a top cover of the tank body is movably connected with the tank body, a group of openings are arranged on the top cover, a magnetic stirrer 4 is arranged at the bottom of the tank body, a magnetic stirrer 6 is arranged in the tank body, a water outlet valve 9-1 and a water inlet valve 9-2 are respectively arranged at two sides of the tank body, a waste water storage tank 5 is connected with the water inlet valve 9-2 through a peristaltic pump 7, and when waste water isAfter the internal reaction is completed, the wastewater flows out from the water outlet valve 9-1, and when the wastewater in the tank body is excessive, the excessive wastewater overflows from the overflow port 8.
The treatment method specifically comprises the following steps:
the first step is as follows: the powdered activated carbon 10 is put into distilled water to be boiled for 4h, then the distilled water is used for washing for 10min to remove water-soluble and volatile substances in the activated carbon, the activated carbon is dried for 48h at 120 ℃ after the washing is finished, the activated carbon is taken out, the activated carbon is put between a graphite plate cathode 2 which supports metal copper palladium and a ruthenium tin coating titanium anode 3, the distance between two electrode plates is 3.0cm, and 20g/L NaCl is added between the electrode plates.
The second step is that: turning on a direct-current power supply 1, adjusting voltage 9V, controlling reaction pause time for 30min, turning on a water inlet valve 9-2, turning on a peristaltic pump 7, and enabling dye wastewater to enter a reactor from a wastewater storage tank 5, wherein the dye wastewater is alizarin S dye wastewater simulating wastewater, and the initial concentration is 1000mg/L, COD =600mg/L chromaticity 6.
Step three, effluent detection: after the reaction, closing the water inlet valve 9-2, opening the water outlet valve 9-1, allowing the treated dye wastewater to flow out of the water outlet valve 9-1, and detecting COD (chemical oxygen demand) and chromaticity in the treated dye wastewater; after the reaction is carried out for 50 minutes, the removal rate of COD and chroma in the wastewater after the reaction reaches 85 percent, and the wastewater can be discharged after reaching the integrated wastewater discharge standard (GB 8978-1996).
The fourth step: when the concentration of the dye wastewater is increased, so that the treated effluent cannot reach the integrated wastewater discharge standard (GB 8978-1996), closing the water inlet valve 9-2 and the peristaltic pump 7, adjusting the voltage and the reaction pause time until the effluent reaches the standard and then recovering the normal treatment process, wherein the method for re-adjusting the voltage and the reaction pause time comprises the steps of sequentially increasing the voltage by 1V, 3V, 5V, 7V and 9V, and adjusting the reaction pause time by 5min, 10min, 15min, 20min, 25min and 30 min.
High current efficiency, strong oxidation capacity, low energy consumption, good COD removal and decoloration effects, convenient operation and wide application range.
The embodiments of the present invention have been described in detail with reference to the drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.
Claims (7)
1. The equipment for treating dye wastewater by the electrochemical-adsorption composite process is characterized in that: the device comprises a direct current stabilized voltage power supply (1), a graphite plate cathode (2) loaded with metallic copper palladium, a ruthenium tin coating titanium anode (3), a magnetic stirrer (4), a wastewater storage tank (5), a magnetic stirrer (6), a peristaltic pump (7), an overflow port (8), a water outlet valve (9-1), a water inlet valve (9-2) and powdered activated carbon (10), wherein the graphite plate cathode (2) loaded with metallic copper palladium and the ruthenium tin coating titanium anode (3) are respectively arranged at two ends of a tank body of the device for treating dye wastewater by an electrochemical-adsorption composite process, the graphite plate cathode (2) loaded with metallic copper palladium is connected with the negative electrode of the direct current stabilized voltage power supply (1) through a lead, the powdered activated carbon (10) and anhydrous sodium chloride are filled between the graphite plate cathode (2) loaded with metallic copper palladium and the ruthenium tin coating titanium anode (3), the overflow port (8) is arranged below the top cover of the tank body, the top cover of the tank body is movably connected with the tank body, the top cover of the tank body is provided with a group of open holes, the bottom of the tank body is provided with a magnetic stirrer (4), a magnetic stirrer (6) is arranged in the tank body, the water outlet valve (9-1) and the water inlet valve (9-2) are respectively arranged at two sides of the tank body, the waste water storage tank (5) is connected with the water inlet valve (9-2) through a peristaltic pump (7), when the waste water completely reacts in the tank body, the waste water flows out from the water outlet valve (9-1), and when the waste water in the tank body is excessive; the graphite plate cathode (2) loaded with the metal copper palladium is prepared by an ethylene glycol reduction method, a graphite plate electrode is taken, the surface of the graphite plate electrode is polished to be smooth and flat by abrasive paper, the graphite plate electrode is sequentially placed into NaOH solution and hydrochloric acid solution for soaking, then is washed and dried to prepare a prepared graphite plate electrode, and the prepared graphite plate electrode is placed into ethylene glycol solution and is subjected to ultrasonic treatment for 1 hour; 76mg of PdCl were weighed out272mg of CuCl2.2H2O and 240mg of sodium citrate in a 250mL round-bottom flask, and 50mL of ethylene glycol was added, stirred at room temperature for 1h, and then the graphite plate electrode soaked in ethylene glycol was placed therein with 5wt% KOH/ethylene glycolAnd (3) regulating the pH value of the reaction mixed solution to 9.5-10.5 by using the solution, continuously stirring at room temperature for 30min, then placing the reaction mixed solution in an oil bath kettle, reacting at 160 ℃ for 6h, taking out a graphite plate electrode after the reaction is finished, washing with deionized water, and drying in vacuum to obtain the metal copper-palladium loaded graphite plate cathode.
2. The apparatus for treating dye wastewater by electrochemical-adsorption composite process according to claim 1, wherein: the tank body of the equipment for treating the dye wastewater by the electrochemical-adsorption composite process is a cuboid, and the size of the tank body is 15cm multiplied by 10cm multiplied by 12 cm.
3. The apparatus for treating dye wastewater by electrochemical-adsorption composite process according to claim 1, wherein: the sizes of the graphite plate cathode (2) loaded with metal copper palladium and the ruthenium tin coating titanium anode (3) are both 10cm multiplied by 8cm multiplied by 0.5cm, and the distance between the two electrodes is 3.0cm-5.0 cm.
4. The apparatus for treating dye wastewater by electrochemical-adsorption composite process according to claim 1, wherein: the particle diameter of the powdered activated carbon (10) is 0.15mm to 2.00 mm.
5. The apparatus for treating dye wastewater by electrochemical-adsorption composite process according to claim 1, wherein: the overflow port (8) is 1cm-5cm lower than the top end of the tank body.
6. A treatment method of an apparatus for treating dye wastewater by an electrochemical-adsorption composite process as claimed in any one of claims 1 to 5, wherein: the method comprises the following steps: the first step is as follows: putting the powdered activated carbon (10) into distilled water to boil for 2-4h, then washing with distilled water for 5-10min, drying at 120 ℃ for 24-48h after washing, taking out, putting between a graphite plate cathode (2) loaded with metal copper palladium and a ruthenium tin coating titanium anode (3), and simultaneously adding 20g/L anhydrous sodium chloride; the second step is that: opening a direct current stabilized voltage supply (1), adjusting the voltage range to be less than or equal to 9V, controlling the reaction intermittent time to be less than or equal to 30min, opening a water inlet valve (9-2), starting a peristaltic pump (7), enabling dye wastewater to enter a reactor from a wastewater storage tank (5), wherein the dye wastewater adopts alizarin S dye wastewater simulating wastewater, the initial concentration is 200-; step three, effluent detection: after the reaction, closing the water inlet valve (9-2), opening the water outlet valve (9-1), allowing the treated dye wastewater to flow out of the water outlet valve (9-1), and discharging the treated dye wastewater after detecting that COD and chroma in the treated dye wastewater reach the Integrated wastewater discharge Standard (GB 8978-1996); the fourth step: when the concentration of the dye wastewater is increased, the concentration of the treated effluent water is increased and cannot reach the integrated wastewater discharge standard (GB 8978-1996), the water inlet valve (9-2) and the peristaltic pump (7) are closed, the voltage and the reaction intermittent time are readjusted until the effluent water reaches the standard, and the normal treatment process is recovered.
7. The treatment method of the apparatus for treating dye wastewater by electrochemical-adsorption composite process according to claim 6, characterized in that: and the fourth step of readjusting the voltage and the reaction pause time comprises the steps of sequentially increasing the voltage by 1V, 3V, 5V, 7V and 9V, and adjusting the reaction pause time by 5min, 10min, 15min, 20min, 25min and 30 min.
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