CN113264583A - Process and equipment based on electric persulfate activation technology - Google Patents
Process and equipment based on electric persulfate activation technology Download PDFInfo
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- 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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- C02F1/46104—Devices therefor; Their operating or servicing
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- C02F2201/46—Apparatus for electrochemical processes
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Abstract
The invention discloses a process and equipment based on an electric persulfate activation technology, wherein the equipment comprises an anode reaction kettle, a cathode reaction kettle, an adjustable direct-current power supply and a high-precision variable resistor; the anode reaction kettle is provided with an anode electrode which can move up and down; a cathode electrode is arranged on the cathode reaction kettle; the anode electrode and the cathode electrode are respectively and electrically connected with the positive electrode and the negative electrode of the adjustable direct current power supply; the bottom inert electrodes are respectively arranged at the positions of the side walls of the anode reaction kettle and the cathode reaction kettle close to the bottom, the two bottom inert electrodes are electrically connected with each other by a lead, and a high-precision variable resistor is connected in series between the leads. The depth of the anode electrode in the medicament, the voltage of the adjustable direct current power supply and the resistance of the high-precision variable resistor are accurately controlled, so that the electric activation current can be effectively controlled, and the speed and the quality of the electric activation persulfate are further controlled.
Description
Technical Field
The invention discloses a process and equipment based on an electric persulfate activation technology, and belongs to the field of environmental remediation.
Background
The removal of toxic and harmful substances in the environment by chemical oxidation is a common environmental remediation method, and advanced oxidation is based on active free radicals OH and
the oxidation technology of (1) has high degradation efficiency on organic pollutants in the environment, and other chemical oxidation technologies do not have the advantages. Compared with the H commonly used as the oxidizing free radical source at present2O2The persulfate has the characteristics of easy storage and stability. Based on Fe2+Activated persulfate systems are becoming increasingly the focus of research because of their green-friendly nature, but Fe2+The greatest disadvantage of the activated persulfate system is the Fe formed during the activation process3+Will hydrolyze and precipitate to cause Fe in the system2+The concentration is reduced. Therefore, in order to achieve the ideal repairing effect, a large amount of Fe needs to be added in the initial stage2+However, a large amount of Fe2+The addition of (2) will generate a large amount of iron mud. Having active free radicals OH and
the existence half-life period of (A) is very short, and how to effectively improve Fe2+The efficiency of activating a persulfate system to degrade pollutants becomes the bottleneck of future application of the prior iron-persulfate technology.
Research shows that the carbon material as a cathode can catalyze the generation of persulfate during the electric activation of the persulfate
Because the carbon material has good conductivity and relatively low production cost, the carbon material can increase the mass transfer efficiency of the electrode and persulfate ions, thereby increasing the catalytic efficiency of persulfate and improving the mineralization capability of the system. The active Carbon fiber developed in the 70 s of the 20 th century has more micropores (the pore diameter is less than 2nm) of a novel Active Carbon Fiber (ACF), so that the Carbon-pi phenomenon is easier to occur due to higher specific surface area.
Chinese patent 2018105186217 discloses a device and method for producing persulfate and its activator ferrous ion simultaneously by electrolysis, but in practical operation, because the area size of the ionic membrane is difficult to adjust rapidly and possible to fail, it is almost impossible to control the persulfate in the process of activation. And because the anode is an inert electrode, a large amount of sub-ionic iron salt is added in the activation process, and the sub-ionic iron salt inevitably generates a large amount of iron mud in an acid environment.
Based on the background, the invention discloses a set of electric activation process and equipment of advanced oxidation technology based on persulfate, so that the persulfate activation process is simple, efficient and controllable, and is very important.
Disclosure of Invention
The invention aims to: provides a process and equipment based on an electric persulfate activation technology, so that the electric activation process of the persulfate-based advanced oxidation technology becomes simple, efficient and controllable.
The purpose of the invention is realized by the following technical scheme:
an apparatus based on electric persulfate activation technology comprises an anode reaction kettle, a cathode reaction kettle, an adjustable direct current power supply and a high-precision variable resistor;
the anode reaction kettle is provided with an anode electrode which can move up and down; a cathode electrode is arranged on the cathode reaction kettle; the anode electrode and the cathode electrode are respectively and electrically connected with the positive electrode and the negative electrode of the adjustable direct current power supply; the bottom inert electrodes are respectively arranged at the positions of the side walls of the anode reaction kettle and the cathode reaction kettle close to the bottom, the two bottom inert electrodes are electrically connected with each other by a lead, and a high-precision variable resistor is connected in series between the leads.
Further, the anode electrode material is transition metal, including iron, copper, zinc, manganese, silver and cobalt;
further, the cathode electrode material comprises activated carbon fiber, graphene, graphite, platinum and gold.
Furthermore, the inert electrodes at the bottom are insulated from the reaction kettle and are inserted into the reaction kettle in a sealed manner; the inert electrode material comprises graphite, activated carbon fiber, platinum and gold.
Furthermore, the minimum stepping value of the high-precision variable resistor is less than or equal to 0.1 omega.
Furthermore, the adjustable direct current power supply is an adjustable phase-shifted full-bridge direct current power supply.
A process based on an electrokinetic persulfate activation technology comprises the following steps:
(1) adding persulfate solution with the concentration of 20% into the anode reaction kettle and the cathode reaction kettle respectively to enable the solution to submerge the anode electrode and the cathode electrode respectively, and starting a stirrer to start stirring;
(2) adjusting the pH value of the solution in the anode reaction kettle to 5 by using 10% HCl, and adjusting the pH value of the solution in the cathode reaction kettle to 9 by using 20% NaOH;
(3) adjusting the resistance value of the high-precision variable resistor, switching on the adjustable direct-current power supply and slowly boosting the voltage; if the concentration of liquid ions in the initial reaction kettle is low and the resistance of the liquid is high, the voltage of the adjustable direct current power supply needs to be increased and the resistance value of the high-precision variable resistor needs to be reduced;
(4) HCl or NaOH is dripped to keep the pH value in the reaction kettle unchanged and stirred for 10min, and then acidic activated and alkaline activated persulfate solutions are obtained.
Further, during the reaction process, the anode electrode undergoes an oxidation reaction, and the transition metal of the anode electrode is oxidized into transition metal ions, so that the anode electrode needs to be moved downwards continuously to stabilize the transition metal of the anode electrode in the liquid. Further, the persulfate solution includes a sodium persulfate solution.
Has the advantages that:
the invention discloses a process and equipment based on an electric persulfate activation technology, which can simultaneously obtain acidic activated persulfate and alkaline activated persulfate, greatly improve the activation effect and reduce the activation cost; the depth of the anode electrode in the medicament, the voltage of the adjustable phase-shifting direct current power supply and the resistance of the high-precision variable resistor are accurately controlled, so that the electric activation current can be effectively controlled, and the speed and the quality of the electric activation persulfate are further controlled. The activated medicinal preparation is contacted with the medicinal preparation by anode movement during application, so as to maintain activation current and make the medicinal preparation
Can not be lost quickly, further improves the oxidation effect of the medicament, has simple operation and wide engineering and market prospects.
Drawings
FIG. 1 is a block diagram of the apparatus of the present invention.
The figure is as follows: 1. an anode reaction kettle; 2. a cathode reaction kettle; 3. a high-precision variable resistor; 4. an adjustable DC power supply;
11. a first stirrer; 12. a first acidic agent control valve; 13. a first basic agent control valve; 14. an anode electrode; 15. a first pH sensor; 16. a first drug discharge control valve; 17. a first medicament detection sampling port; 18. a first bottom inert electrode; 19. a first drug injection control valve;
21. a second agitator; 22. a second acidic agent control valve; 23. a second basic agent control valve; 24. a cathode electrode; 25. a second pH sensor; 26. a second drug discharge control valve; 27. a second medicament detection sampling port; 28. a second bottom inert electrode; 29. a second medicament injection control valve.
Detailed Description
The invention is further illustrated with reference to fig. 1.
The specific implementation method of the invention comprises the following steps: the process and equipment based on the electric persulfate activation technology can control the electric activation current very effectively by accurately controlling the depth of an anode electrode 14 in a medicament, the voltage of an adjustable direct current power supply 4 and the resistance of a high-precision variable resistor 3, and further control the speed and quality of the electric persulfate activation.
An apparatus based on electric persulfate activation technology comprises an anode reaction kettle 1, a cathode reaction kettle 2, a high-precision variable resistor 3 and an adjustable direct-current power supply 4;
the anode reaction kettle 1 is provided with an anode electrode 14 which can move up and down; the anode electrode 14 is made of transition metal, including iron, copper, zinc, manganese, silver and cobalt. A cathode electrode 24 is arranged on the cathode reaction kettle 2; the cathode electrode 24 material comprises activated carbon fiber, graphene, graphite, platinum and gold; the anode electrode 14 and the cathode electrode 24 are respectively and electrically connected with the positive electrode and the negative electrode of the adjustable direct current power supply 4; a first bottom inert electrode 18 and a second bottom inert electrode 28 are respectively arranged at the positions of the side walls of the anode reaction kettle 1 and the cathode reaction kettle 2 close to the bottoms, and the bottom inert electrodes are insulated from the reaction kettles and are inserted into the reaction kettles in a sealed manner; the inert electrode material comprises graphite, activated carbon fiber, platinum and gold. The first bottom inert electrode 18 and the second bottom inert electrode 28 are electrically connected by a lead, and a high-precision variable resistor 3 is connected in series between the leads for maintaining an activation current when the activated medicament is used, wherein the minimum step value of the high-precision variable resistor 3 is less than or equal to 0.1 omega. A process based on an electrokinetic persulfate activation technology comprises the following steps:
(1) respectively adding sodium persulfate solution with the concentration of 20% into the anode reaction kettle 1 and the cathode reaction kettle 2, enabling the solution to respectively submerge the anode electrode 14 and the cathode electrode 24, and starting a stirrer to start stirring;
(2) adjusting the pH value of the solution in the anode reaction kettle 1 to 5 by using 10% HCl, and adjusting the pH value of the solution in the cathode reaction kettle 2 to 9 by using 20% NaOH;
(3) adjusting the resistance value of the high-precision variable resistor 3, switching on the adjustable direct-current power supply 4 and slowly boosting; if the concentration of liquid ions in the initial reaction kettle is low and the resistance of the liquid is high, the voltage of the adjustable direct current power supply 4 needs to be increased and the resistance value of the high-precision variable resistor 3 needs to be reduced; during the reaction, the anode 14 undergoes an oxidation reaction, and the transition metal of the anode 14 is oxidized into transition metal ions, which coat the surface of the anode 14, so that the anode 14 needs to be moved downward continuously to stabilize the transition metal of the anode 14 in the liquid.
(4) HCl or NaOH is dripped to keep the pH value in the reaction kettle unchanged and stirred for 10min, so that the sodium persulfate solution with acidic activation and alkaline activation is obtained.
The anode reactor 1 is provided with a first stirrer 11, a first acidic chemical control valve 12, a first basic chemical control valve 13, a vertically movable positive electrode 14 made of preferably pure iron, a first pH sensor 15, a first chemical discharge control valve 16, a first chemical detection sampling port 17, a first bottom inert electrode 18, a first chemical injection control valve 19, and a first chemical inlet 20.
As shown by the reaction formulas (1) and (2) at the anode side, it is seen from the reaction results that a catalyst having a strong oxidizing effect is obtained
Fe-2e-→Fe2+ (1)
The cathode reaction vessel 2 is provided with a second stirrer 21, a second acidic chemical control valve 22, a second alkaline chemical control valve 23, an inert cathode electrode 24 preferably made of activated carbon fiber, a second pH sensor 25, a second chemical discharge control valve 26, a second chemical detection sampling port 27, a second bottom inert electrode 28, a second chemical injection control valve 29, and a second chemical inlet 30.
As shown in the reaction formula (3) at the cathode terminal, a catalyst having strong oxidation is obtainedEffect of
Example 1 step 1, soil in a site contaminated by site of a certain steel mill was taken, and the type and concentration of the contaminants are shown in table 1 as sample 01. Accurately weighing 3 parts of soil sample, wherein each part is 300g, and the serial numbers are respectively 01, 1A and 1B, wherein 01 is a blank sample.
After the steps 5 and 8h, samples 11A and 11B are respectively taken for inspection, and the experimental data are shown in Table 1.
TABLE 1 Experimental data (mg/kg)
From the data in Table 1, it is seen that sodium persulfate upon electrokinetic activation has very good oxidizing properties.
Example 2
Step 1, taking polluted underground water of a site polluted by a coal gas plant, wherein the types and concentrations of pollutants are shown as 02 samples in a table 2. Accurately measuring 5 water samples, each sample is 200ml, and the serial numbers are 02, 22A, 22B, 33A and 33B respectively, wherein 02 is a blank sample.
After the steps 5 and 150min, samples 22A and 22B are respectively taken for inspection, and the experimental data are shown in Table 2.
TABLE 2 Experimental data (μ g/L)
After completing the example 2, the power was cut off for 5min, and 50ml of activated Na was taken from the anode beaker2S2O8Adding 33A into the solution, stirring, standing, and collecting 50ml of activated Na from cathode beaker2S2O8The solution was added to 33B and stirred well and allowed to stand. Bubble generation was also seen in the sample at this time, but no example 2 was found to be vigorousIndicating the presence of, in the medicament over time
Some of which may be lost, the experimental data are shown in table 2.
Claims (9)
1. An apparatus based on electric persulfate activation technology is characterized by comprising an anode reaction kettle, a cathode reaction kettle adjustable direct current power supply and a high-precision variable resistor;
the anode reaction kettle is provided with an anode electrode which can move up and down; a cathode electrode is arranged on the cathode reaction kettle; the anode electrode and the cathode electrode are respectively and electrically connected with the positive electrode and the negative electrode of the adjustable direct current power supply; the bottom inert electrodes are respectively arranged at the positions of the side walls of the anode reaction kettle and the cathode reaction kettle close to the bottom, the two bottom inert electrodes are electrically connected with each other by a lead, and a high-precision variable resistor is connected in series between the leads.
2. The equipment based on the electro-kinetic activated persulfate technology as claimed in claim 1, wherein the anode electrode material is a transition metal comprising iron, copper, zinc, manganese, silver, cobalt.
3. The electro-dynamically activated persulfate technology based equipment as claimed in claim 1, wherein the cathode electrode material comprises activated carbon fiber, graphene, graphite, platinum, gold.
4. The equipment based on the electro-kinetic activated persulfate technology as claimed in claim 1, wherein the bottom inert electrode is insulated from the reaction vessel and is inserted into the reaction vessel in a sealed manner; the inert electrode material comprises graphite, activated carbon fiber, platinum and gold.
5. An apparatus as claimed in claim 1, wherein the minimum step value of the high precision variable resistor is less than or equal to 0.1 Ω.
6. The apparatus of claim 1, wherein the adjustable dc power supply is an adjustable phase-shifted full-bridge dc power supply.
7. A process based on an electric persulfate activation technology is characterized by comprising the following steps:
(1) adding persulfate solution with the concentration of 20% into the anode reaction kettle and the cathode reaction kettle respectively, so that the anode electrode and the cathode electrode are immersed in the solution respectively, and starting a stirrer to start stirring;
(2) adjusting the pH value of the solution in the anode reaction kettle to 5 by using 10% HCl, and adjusting the pH value of the solution in the cathode reaction kettle to 9 by using 20% NaOH;
(3) adjusting the resistance value of the high-precision variable resistor, switching on the adjustable direct-current power supply and slowly boosting the voltage; if the concentration of liquid ions in the initial reaction kettle is low and the resistance of the liquid is high, the voltage of the adjustable direct current power supply needs to be increased and the resistance value of the high-precision variable resistor needs to be reduced;
(4) HCl or NaOH is dripped to keep the pH value in the reaction kettle unchanged and stirred for 10min, and then acidic activated and alkaline activated persulfate solutions are obtained.
8. A process according to claim 7, wherein the anodic electrode undergoes an oxidation reaction during the reaction, and the transition metal of the anodic electrode is oxidized into transition metal ions, thereby requiring the anodic electrode to be moved downwards continuously to stabilize the transition metal of the anodic electrode in the liquid.
9. A process based on electrokinetically activated persulfate technology as in claim 7, wherein the persulfate solution comprises sodium persulfate solution.
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