CN116177764A - Method and device for in-situ generation of Fe (IV) and use for wastewater treatment - Google Patents
Method and device for in-situ generation of Fe (IV) and use for wastewater treatment Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 68
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 32
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 110
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 238000001556 precipitation Methods 0.000 claims abstract description 33
- 229910052742 iron Inorganic materials 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 69
- 239000002351 wastewater Substances 0.000 claims description 48
- 239000000460 chlorine Substances 0.000 claims description 33
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 27
- 229910052801 chlorine Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 230000002378 acidificating effect Effects 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 19
- 238000007747 plating Methods 0.000 claims description 19
- 238000004062 sedimentation Methods 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
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- 239000010802 sludge Substances 0.000 claims description 3
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
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- 239000002184 metal Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 21
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- 238000006731 degradation reaction Methods 0.000 abstract description 17
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- 239000002957 persistent organic pollutant Substances 0.000 abstract description 6
- 238000005189 flocculation Methods 0.000 abstract description 5
- 230000016615 flocculation Effects 0.000 abstract description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract description 3
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- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 25
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- 230000000052 comparative effect Effects 0.000 description 18
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 4
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- 241000894006 Bacteria Species 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
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- VCUVETGKTILCLC-UHFFFAOYSA-N 5,5-dimethyl-1-pyrroline N-oxide Chemical compound CC1(C)CCC=[N+]1[O-] VCUVETGKTILCLC-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 238000004435 EPR spectroscopy Methods 0.000 description 1
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- 150000001449 anionic compounds Chemical class 0.000 description 1
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- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
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- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
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- C02F1/46104—Devices therefor; Their operating or servicing
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- 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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- 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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- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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Abstract
The invention belongs to the field of environmental electrochemistry, and discloses a method and a device for generating Fe (IV) in situ and being used for wastewater treatment. The Fe electrode, the chlorine-separating electrode and the conductive cathode form a double-anode electrochemical system, and the chlorine-separating electrode utilizes the wide range of acid wastewaterThe ubiquitous chloride ions generate HClO and Fe generated on the Fe electrode 2+ The reaction is carried out, so that Fe (IV) is generated in situ, the high-activity Fe (IV) can oxidize and degrade organic pollutants, the Fe (IV) is reduced and converted into Fe (III) by itself, and then iron flocs are formed to realize flocculation precipitation removal of degradation products. The method is simple, and a double-anode electrochemical system for in-situ Fe (IV) production is constructed on the basis of commercial electrode materials, and has good organic pollutant degradation and removal performances.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a method and a device for generating Fe (IV) in situ and being used for wastewater treatment.
Background
For nearly half a century, the development of industry has been rapid, and a great deal of organic pollutant wastewater is generated, and the pollutants have the characteristics of high toxicity, difficult biodegradation and the like, so that the traditional water treatment technology such as an activated sludge method is difficult to treat efficiently. By means of strongly oxidising free radicals, e.g. ● OH、 ● The advanced oxidation technology for degrading the organic pollutants by Cl is focused, and particularly the electrochemical advanced oxidation technology has wide application prospect in removing the organic pollutants due to the advantages of small compact area of a reactor, easiness in automatic control, modularization production and assembly and the like, and becomes a research hot spot. Wherein the electro-Fenton method can generate Fenton reaction in situ in the electrochemical reactor and indirectly ● OH, realize degrading pollutant, but the cathode is easy to scale and cause electrode deactivation, limit the application of electro-Fenton method in the field of actual wastewater treatment; electrocatalytic oxidation processes degrade organic pollutants by direct anodic oxidation or indirect oxidative degradation of the anodic to strongly oxidizing species, but this process is highly dependent on the efficiency of mass transfer of the pollutants to the anode surface and the number of active sites of the anode, and the anode is also faced with the problem of rapid deactivation of the electrode by deposited polymer. Mixed metal oxide electrodes such as IrO 2 -RuO 2 Ti has lower potential for chlorine and oxygen evolution, when the solution contains Cl - Active chlorine can be generated to degrade organic contaminants.
The electrochemical oxidation method of active chlorine mediated pollutant conversion solves the problem of low treatment efficiency caused by electrode deactivation or limited electrode active sites, but has lower active chlorine oxidation capability and is opposite to organic mattersMore toxic chlorinated byproducts are easily formed after the reaction. Tetravalent iron [ Fe (IV)]Is an active substance having a molecular structure with O atoms and strong oxidizing property, relative to free radical species (e.g ● OH，·SO 4 2- ) Fe (IV) has more selectivity in oxidation-reduction reaction with other substances; fe (IV) has stronger oxidation activity relative to active chlorine, and Fe (IV) mediated pollutant degradation does not generate chlorinated byproducts; fe (IV) is reduced into Fe (III) after oxidizing pollutant, and can be used as flocculant for adsorption flocculation removal of the substance.
There is therefore a need to design a method and apparatus that can produce Fe (IV) in situ and for wastewater treatment.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the existing electrochemical oxidation techniques, the present invention aims to propose a method for generating Fe (IV) in situ and for wastewater treatment. By constructing a double-anode electrochemical reaction system capable of generating Fe (IV) in situ, oxidant and flocculant are not required to be added exogenously, and self Cl in the solution is fully utilized - Under the conditions of reducing the consumption of chemical agents and efficiently separating precipitated products, the purposes of oxidizing pollutants and removing the pollutants from the water phase are realized.
It is another object of the present invention to provide an apparatus for in situ generation of Fe (IV) and for wastewater treatment.
The aim of the invention is achieved by the following technical scheme:
a method for in situ production of Fe (IV) and for wastewater treatment, the method comprising the steps of:
the chlorine separating electrode and the iron sheet are used as anodes, a conductive cathode is added, a double-anode electrochemical system is formed by the chlorine separating electrode, the iron sheet and the conductive cathode, and the current applied to the electrodes is controlled by a direct current power supply to treat wastewater, namely Fe (IV) can be generated in situ and treated, and the treated wastewater is transferred to a precipitation system for alkaline precipitation.
In the process, chlorine separation reaction occurs on the chlorine separation electrode, and Cl in the solution - Ion conversion to active chlorine; ferrous ions are continuously generated on the ferroelectric electrode. On the one hand, the active chlorine can directly oxidize the wastewaterOrganic contaminants, on the other hand, can react with ferrous ions to form Fe (IV) with strong oxidizing property. Fe (IV) has stronger oxidizing capability and selective oxidizing property, and the Fe (IV) preferentially reacts with organic matters containing electron-rich groups; fe (IV) mediates that the Fe (IV) is converted into Fe (III) after the oxidation of the pollutants is finished, and then iron flocs are formed to realize flocculation separation and removal of the pollutants.
The double-anode electrochemical system specifically comprises: the double-anode electrochemical system controlled by the direct current power supply comprises an Fe electrode, a chlorine-separating electrode and a conductive cathode, and the electrode areas are all 9cm 2 . Wherein, the Fe electrode and the chlorine-separating electrode are used as anodes, the three electrodes are positioned in the middle of the conductive cathode, the Fe electrode and the chlorine-separating electrode are respectively positioned at two sides of the cathode, and the distance between the electrodes is 15mm; the electrode plate is fixed on the electrode rod which can conduct electricity; the direct current power supply selects a constant current mode, and the current applied to the Fe electrode and the chlorine evolution electrode is respectively in the range of 10-100mA and 100-300mA, and the reaction is carried out for 180min.
The electrode rod may be, but is not limited to, a metallic titanium rod.
The chlorine evolving electrode can be, but is not limited to, irO 2 -RuO 2 Ti electrode and IrO 2 -TaO 2 Ti electrode and PbO 2 Ti electrode.
The conductive cathode may be, but is not limited to, stainless steel and Cu/Zn electrodes.
The waste water is preferably acidic nickel plating waste water.
An apparatus for in situ generation of Fe (IV) and for wastewater treatment, the apparatus comprising an electrolysis system, a precipitation system;
the electrolysis system comprises an electrolysis tank, an electrode assembly (Fe electrode, chlorine-separating electrode and conductive cathode), a mechanical stirring paddle, a direct current controller and a wastewater conveying pump; the wastewater is uniformly distributed into the electrolytic tank, fe (IV) is generated in the solution after the direct current power supply controller electrifies the electrode assembly, active species Fe (IV) fully contact and react with organic matters in the wastewater under the operation of the mechanical stirring paddle, and the waste liquid in the electrolytic tank is transported to a precipitation system through the wastewater transport pump after a specific reaction time;
the sedimentation system comprises a sedimentation reaction chamber, wherein a dosing (alkali) port is arranged on the side surface of the sedimentation reaction chamber, high-efficiency separation is realized after the wastewater in the sedimentation reaction chamber is subjected to alkali adding sedimentation, and a sludge discharge port is arranged at the bottom of the sedimentation reaction chamber and used for removing sedimentation flocs after alkali adding sedimentation; the side part of the precipitation reaction chamber is also provided with a water outlet for removing supernatant liquid after adding alkali for precipitation.
The principle of the invention is as follows:
the invention realizes the coupling effect of the electro-oxidation and electro-flocculation process by constructing a double-anode electrochemical reaction system capable of generating Fe (IV) in situ, thereby achieving the purposes of oxidizing pollutants and removing the pollutants from a water phase. The chlorine-separating electrode can utilize Cl widely existing in the acidic nickel plating wastewater by taking the acidic nickel plating wastewater as a treatment object - Ion generation of HClO or ClO - And (3) the active chlorine and ferrous ions are continuously released from the ferroelectric electrode. The active chlorine can directly oxidize metal organic complex and phosphite on one hand, and can react with ferrous ions to generate Fe (IV) on the other hand. Under acidic conditions, the active chlorine overflows out of solution in the form of chlorine gas, and the oxidation-reduction potential of the active chlorine itself is low (HClO/Cl) - 1.49V vs SHE), after constructing the double anode system, the active substance is converted from the initial active chlorine to Fe (IV), thus improving the overall oxidation capacity of the system; the reaction of active chlorine with organic matter produces chlorinated byproducts, which are oxidized by themselves to form higher chlorate, and these products generally exhibit stronger biotoxicity or environmental hazard, and Fe (IV) as an active species avoids the formation of these byproducts, and is a more green and harmless treatment method. For treating acidic nickel plating wastewater, the reaction of a double-anode electrochemical system is more severe due to the cathodic hydrogen evolution reaction, the pH of the solution gradually rises from acidity to neutrality within the reaction time of 180min, a large amount of iron flocs are generated at the moment, and partial free nickel ions and all phosphates can be removed by flocculation precipitation. The subsequent wastewater is transferred to a precipitation system, so that the concentration of nickel ions in the solution can reach the drainage standard.
The reaction formula for in situ generation of active high valence Fe (IV) is as follows:
Fe–2e - →Fe 2+ (1)
2Cl - -2e - +H 2 O→HClO+HCl (2)
Fe 2+ +HClO→Fe(IV)O 2+ +HCl (3)
compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The invention has simple processing system, easy device construction and convenient modularized production.
(2) In the treatment system, the effect of regulating and controlling the reaction can be realized through current regulation without adding chemicals such as oxidant flocculant and the like, the operation is simple and convenient, and the operation of the treatment system are easy and easy to understand, thereby being suitable for popularization.
(3) The iron electrode, the chlorine separation electrode and the conductive cathode in the treatment system are all commercial metal materials, so that the large-scale production is realized, the source is wide, and the price is low.
(4) The treatment system skillfully converts active species from active chlorine to Fe (IV), avoids the generation of chlorinated organic byproducts, reduces the toxicity of treated water, and is an environment-friendly treatment system.
(5) The active species Fe (IV) in the treatment system has strong oxidizing capability and selectivity, and the reaction activity is less influenced by organic matters and inorganic anions in the wastewater.
Drawings
FIG. 1 is an apparatus for in situ generation of Fe (IV) and for wastewater treatment according to the present invention, wherein a 1-electrolyzer; 2-iron anode; 3-chlorine-separating anode; 4-a conductive cathode; 5-mechanical stirring paddles; 6-a direct current power supply controller; 7-valve; 8-a wastewater delivery pump; 9-a precipitation reaction chamber; 10-a water outlet; 11-a mud discharging port.
FIG. 2 is a graph of EDTA-Ni degradation performance of the method constructed in example 1.
FIG. 3 is a graph of the overall phosphorus removal performance of the process constructed in example 1.
FIG. 4 is a graph showing the effect of removing nickel ions from a solution after electrochemical oxidation and precipitation steps in the method constructed in example 1.
Fig. 5 is an electron paramagnetic resonance spectrum of an active species generated by the method constructed in example 1.
FIG. 6 is a graph of EDTA-Ni degradation performance of the method constructed in example 2.
FIG. 7 is a graph of the overall phosphorus removal performance of the process constructed in example 2.
FIG. 8 is a graph showing the effect of removing nickel ions from a solution after electrochemical oxidation and precipitation steps in the method constructed in example 2.
FIG. 9 is a graph of EDTA-Ni degradation performance of the method constructed in example 3.
FIG. 10 is a graph of the overall phosphorus removal performance of the process constructed in example 3.
FIG. 11 is a graph showing the effect of removing nickel ions from a solution after electrochemical oxidation and precipitation steps in the method constructed in example 3.
FIG. 12 is a graph of the evaluation of biotoxicity of water samples during various treatment periods according to the method constructed in example 1.
FIG. 13 is a graph of EDTA-Ni degradation performance of the method of construction of comparative example 1.
FIG. 14 is a graph of the overall phosphorus removal performance of the method constructed in comparative example 1.
FIG. 15 is a graph showing the effect of removing nickel ions from a solution after electrochemical oxidation and precipitation steps in the method constructed in comparative example 1.
FIG. 16 is a graph of EDTA-Ni degradation performance of the method of construction of comparative example 2.
FIG. 17 is a graph of total phosphorus removal performance of the method constructed in comparative example 2.
FIG. 18 is a graph showing the effect of removing nickel ions from a solution after electrochemical oxidation and precipitation steps in the method constructed in comparative example 2.
FIG. 19 is a graph of the evaluation of biotoxicity of water samples during various treatment periods of the method constructed in comparative example 2.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The reagents used in the examples are commercially available as usual unless otherwise specified.
In the embodiment of the invention, fe (IV) is generated in situ, and the device for treating wastewater is shown in figure 1, the wastewater is uniformly distributed in an electrolytic tank (1), a direct current power supply controller (6) electrifies an electrode assembly (an iron anode (2), a chlorine-separating anode (3) and a conductive cathode (4)) to generate Fe (IV) in solution, under the operation of a mechanical stirring paddle (5), the active species Fe (IV) fully contacts and reacts with organic matters in the wastewater, and after a specific reaction time, waste liquid in the electrolytic tank (1) is transported to a precipitation reaction chamber (9) through a delivery pump (8); the waste liquid in the precipitation reaction chamber (9) is subjected to alkali adding precipitation to realize a solid-liquid separation effect, sediment is discharged from a mud discharge port (11) at the bottom of the precipitation reaction chamber (9), and supernatant is discharged from a side water discharge port (10).
Example 1
IrO with chlorine-evolving electrode 2 -RuO 2 Ti (MMO), iron electrode (Fe) as double anode, stainless steel electrode as cathode, electrode area of 9cm 2 The three electrodes are positioned in the middle of the conductive cathode, the Fe electrode and the chlorine separation electrode are respectively positioned at two sides of the cathode, the distance between the electrodes is 15mm, a double-anode electrochemical reaction system for producing Fe (IV) in situ is formed, and EDTA-Ni and phosphate removal experiments are carried out. Preparing water to be treated containing chloride ions by using tap water, wherein the chloride ion content is 2000mg/L, and EDTA-Ni and HPO are added 3 2- EDTA-Ni and HPO as contaminants to be treated 3 2- The concentrations were 0.68mmol/L and 1mmol/L, respectively, as treatment targets, and the volume of wastewater to be treated was 250mL, pH=2.5. The operation was performed for 3 hours in constant current modes of 200mA and 50mA for MMO current and Fe current, respectively, and the test results are shown in FIGS. 2 and 3. The pH of the solution after the reaction was adjusted to 11, and the concentration of nickel ions was measured after filtration using a 0.45 μm filter head, and the experimental results are shown in FIG. 4.
FIG. 2 shows the effect of the double anode electrochemical system used in this example on treating simulated acidic nickel plating wastewater. It can be seen from the figure that the treatment method can realize the decomplexation of EDTA-Ni in a short time.
FIG. 3 shows the removal of phosphate from acidic nickel plating wastewater using the double anode electrochemical system of this example. As can be seen from the figure, the method enables phosphate removal in a short time.
Fig. 4 shows the solubility change of nickel ions in the solution after the treatment of the alkaline precipitation method in this example, and it can be seen from the figure that the concentration of nickel ions in the solution after the electrochemical oxidation and the precipitation step is reduced to the corresponding drainage standard.
To confirm that the process of the present invention does produce Fe (IV), an excess of masking agent was added to the mixture at a concentration of 50mmol/L prior to energizing the DC power supply, then the DC power supply was energized, sampled after 10 minutes and the active species scavenger 5, 5-dimethyl-1-pyrroline-N-oxide (DMPO) was added rapidly, and the final sample had a DMPO concentration of 100mmol/L. The sample was then subjected to electron paramagnetic resonance and the method constructed in example 1 resulted in an electron paramagnetic resonance spectrum of the active species as shown in fig. 5. As can be seen from the figure, the signal intensity is obviously reduced after the active species generated by the double anode electrochemical system are added with Fe (IV) masking agent ethanol (EtOH) and dimethyl sulfoxide (DMSO), but the signal intensity is unchanged after the active species are added with hydroxyl radical masking agent tert-butanol (TBA); description the method constructed in example 1 yields the active species Fe (IV).
Example 2
IrO with chlorine-evolving electrode 2 -RuO 2 Ti (MMO), iron electrode (Fe) as double anode, stainless steel electrode as cathode, electrode area of 9cm 2 The three electrodes are positioned in the middle of the conductive cathode, the Fe electrode and the chlorine separation electrode are respectively positioned at two sides of the cathode, the distance between the electrodes is 15mm, a double-anode electrochemical reaction system for producing Fe (IV) in situ is formed, and EDTA-Ni and phosphate removal experiments are carried out. Preparing water to be treated containing chloride ions by using tap water, wherein the chloride ion content is 2000mg/L, and EDTA-Ni and HPO are added 3 2- EDTA-Ni and HPO as contaminants to be treated 3 2- The concentrations were 0.68mmol/L and 1mmol/L, respectively, and the volumes of wastewater to be treated were 250mL, pH=2.5. The MMO anode current was fixed at 200mA and the different Fe anode currents (10, 30, 50, 70 and 100mA respectively) were run for 3h with experimental results shown in figures 6, 7; the pH of the reacted solution is regulated to 11, and the concentration of nickel ions is measured after the solution is filtered by a 0.45 mu m filter head, so that the reaction is realizedThe test results are shown in FIG. 8.
FIG. 6 shows the effect of the double anode electrochemical system used in this example on treating simulated acidic nickel plating wastewater at different Fe anode currents. From the graph, the degradation effect of EDTA-Ni shows a tendency of increasing and then weakening with the increase of the Fe anode current, and the system shows the best EDTA-Ni degradation performance at the Fe anode current of 50 mA.
FIG. 7 shows the removal of phosphate from acidic nickel plating wastewater at different Fe anode currents using the double anode electrochemical system used in this example. As can be seen from the graph, the phosphate removing effect gradually increases with the increase of the Fe anode current, and a positive correlation is exhibited between the two.
Fig. 8 shows the solubility change of nickel ions in the solution after the treatment by the alkali precipitation method in this example, and it can be seen from the graph that the concentration of nickel ions in the solution has the best effect in a set of experiments with a Fe current of 50mA, and the EDTA-Ni degradation rate under this condition is the fastest, which proves that the removal of nickel ions is based on EDTA-Ni degradation.
Example 3
IrO with chlorine-evolving electrode 2 -RuO 2 Ti (MMO), iron electrode (Fe) as double anode, stainless steel electrode as cathode, electrode area of 9cm 2 The three electrodes are positioned in the middle of the conductive cathode, the Fe electrode and the chlorine separation electrode are respectively positioned at two sides of the cathode, the distance between the electrodes is 15mm, a double-anode electrochemical reaction system for producing Fe (IV) in situ is formed, and EDTA-Ni and phosphate removal experiments are carried out. Preparing water to be treated containing chloride ions by using tap water, wherein the chloride ion content is 2000mg/L, and EDTA-Ni and HPO are added 3 2- EDTA-Ni and HPO as contaminants to be treated 3 2- The concentrations are 0.68mmol/L and 1mmol/L respectively, the volume of the wastewater to be treated is 250mL, the pH=2.5, the Fe anode current is fixed at 50mA, and different MMO anode currents (100, 150, 200, 250 and 300mA respectively) are operated for 3 hours, and the experimental results are shown in figures 9 and 10; the pH of the solution after the reaction was adjusted to 11, and the concentration of nickel ions was measured after filtration using a 0.45 μm filter head, and the experimental results are shown in FIG. 11.
FIG. 9 shows the effect of the double anode electrochemical system used in this example on treating simulated acidic nickel plating wastewater at different MMO anode currents. It can be seen from the graph that the degradation effect of EDTA-Ni increases with the increase of MMO anode current; wherein the degradation effect of EDTA-Ni is obviously enhanced in the process of increasing the MMO anode current from 100mA to 200mA, and the degradation effect of EDTA-Ni is slightly improved in the process of increasing the MMO anode current from 200mA to 300 mA.
FIG. 10 shows the removal of phosphate from acidic nickel plating wastewater at different MMO anode currents using the double anode electrochemical system used in this example. From the graph, the removal rule of phosphate is similar to the degradation rule of EDTA-Ni, and increases with the increase of MMO anode current.
Fig. 11 shows the solubility change of nickel ions in the solution after the treatment by the alkali precipitation method in this example, and it can be seen from the graph that the concentration of nickel ions in the solution has the best removal effect in a set of experiments with an MMO current of 200 mA.
Example 4
And (3) performing toxicity evaluation experiments on water samples in different treatment time periods in the embodiment 1, taking 0.5ml of the water sample to be tested into a reaction container, and adding excessive EDTA (ethylene diamine tetraacetic acid) serving as a heavy metal toxicity masking agent to prepare the mixed solution to be tested. After adjusting the pH of the mixture to 6.5, the acute toxicity of the mixture was measured by the method of GB/T15441-1995. The experimental results are shown in FIG. 12.
FIG. 12 shows the acute toxicity of the acidic nickel plating wastewater of example 1 after various treatment times. As can be seen from the graph, the inhibition rate of the by-products in the water sample treated by the method to the luminescence of the luminescent bacteria is lower, which indicates that the acute toxicity of the by-products in the water sample treated by the method is lower.
Comparative example 1
Takes an iron electrode (Fe) as an anode, a stainless steel electrode as a cathode, and the electrode areas are all 9cm 2 The distance between the electrodes is 15mm, a single anode electrochemical system is formed, and EDTA-Ni and phosphate removal experiments are carried out. Preparing water to be treated containing chloride ions by using tap water, wherein the chloride ion content is 2000mg/L, and EDTA-Ni and HPO are added 3 2- EDTA-Ni and HPO as contaminants to be treated 3 2- The concentrations are respectively0.68mmol/L and 1mmol/L, the volume of wastewater to be treated was 250mL, pH=2.5. The test results are shown in fig. 13 and 14, and the test is performed for 3 hours in a constant current mode in which the Fe current is 50 mA. The pH of the solution after the reaction was adjusted to 11, and the concentration of nickel ions was measured after filtration using a 0.45 μm filter head, and the experimental results are shown in FIG. 15.
FIG. 13 shows the effect of treating a simulated acidic nickel plating wastewater using a single anode electrochemical system employed in this comparative example. As can be seen from the figure, the system exhibited poor EDTA-Ni degradation performance.
FIG. 14 shows the removal of phosphate from acidic nickel plating wastewater using the single anode electrochemical system of this comparative example. As can be seen from the figure, the system exhibited poor phosphate removal performance.
Fig. 15 shows the solubility change of nickel ions in the solution after the treatment by the alkali-adjusting precipitation method in this comparative example, and it can be seen from the figure that the concentration change of nickel ions before and after the treatment is not large. The treatment method constructed by the invention has better removal performance for nickel ions and phosphate in the acidic nickel plating wastewater.
Comparative example 2
IrO with chlorine-evolving electrode 2 -RuO 2 Ti (MMO) as anode, stainless steel electrode as cathode, electrode area of 9cm 2 The distance between the electrodes is 15mm to form a single anode electrochemical system, and EDTA-Ni and phosphate removal experiments are carried out. Preparing water to be treated containing chloride ions by using tap water, wherein the chloride ion content is 2000mg/L, and EDTA-Ni and HPO are added 3 2- EDTA-Ni and HPO as contaminants to be treated 3 2- The concentrations were 0.68mmol/L and 1mmol/L, respectively, and the volumes of wastewater to be treated were 250mL, pH=2.5. The test results are shown in FIGS. 16 and 17, and the test is performed for 3 hours in a constant current mode with an MMO current of 200 mA. The pH of the solution after the reaction was adjusted to 11, and the concentration of nickel ions was measured after filtration using a 0.45 μm filter head, and the experimental results are shown in FIG. 18.
FIG. 16 shows the effect of treating a simulated acidic nickel plating wastewater using a single anode electrochemical system employed in this comparative example. As can be seen from the figure, the system exhibited poor EDTA-Ni degradation performance.
FIG. 17 is a view showing the removal of phosphate from acidic nickel plating wastewater using the single anode electrochemical system of the present comparative example. As can be seen from the figure, the system exhibited poor phosphate removal performance.
Fig. 18 shows the solubility change of nickel ions in the solution after the treatment by the alkali-adjusting precipitation method in this comparative example, and it can be seen from the figure that the concentration change of nickel ions before and after the treatment is not large. The treatment method constructed by the invention has better removal performance for nickel ions and phosphate in the acidic nickel plating wastewater.
Comparative example 3
And (3) performing toxicity evaluation experiments on water samples in different time periods in the comparative example 2, taking 0.5ml of the water sample to be tested into a reaction container, and adding excessive EDTA (ethylene diamine tetraacetic acid) serving as a heavy metal toxicity masking agent to prepare the mixed solution to be tested. After adjusting the pH of the mixture to 6.5, the acute toxicity of the mixture was measured by the method of GB/T15441-1995. The experimental results are shown in FIG. 19.
FIG. 19 shows acute toxicity of the acidic nickel plating wastewater of comparative example 2 after various treatment times. According to the graph, the method has the advantages that the inhibition rate of the by-products in the water sample treated by the method to the luminescence of the luminescent bacteria is high, and the acute toxicity of the by-products in the water sample treated by the method is high, so that the method constructed by the method is an environment-friendly treatment mode.
The embodiments described above are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the embodiments described above, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the present invention should be made in the equivalent manner, and are included in the scope of the present invention.
Claims (10)
1. A method for in situ production of Fe (IV) for wastewater treatment, comprising the steps of:
the chlorine separating electrode and the iron sheet are used as anodes and added with conductive cathodes to form a double-anode electrochemical system, and the current applied to the electrodes is controlled by a direct current power supply to treat wastewater, namely Fe (IV) can be generated in situ and the wastewater is treated.
2. The method of in situ generation of Fe (IV) for wastewater treatment according to claim 1, wherein: the treated wastewater is transferred to a precipitation system for alkaline precipitation.
3. The method of in situ generation of Fe (IV) and use in wastewater treatment according to claim 1 or 2, characterized in that:
the double-anode electrochemical system specifically comprises: the double-anode electrochemical system controlled by the direct current power supply comprises an Fe electrode, a chlorine-separating electrode and a conductive cathode, wherein the Fe electrode and the chlorine-separating electrode are used as anodes, the conductive cathode is positioned in the middle, the Fe electrode and the chlorine-separating electrode are respectively positioned at two sides of the cathode, and the distance between the electrodes is 15mm.
4. A method of producing Fe (IV) in situ for use in wastewater treatment according to claim 3, wherein:
the electrode plate is fixed on the electrode rod which can conduct electricity; the electrode rod is a metal titanium rod.
5. The method of in situ generation of Fe (IV) and use in wastewater treatment according to claim 1 or 2, characterized in that:
the direct current power supply selects a constant current mode, and the current applied to the Fe electrode and the chlorine evolution electrode is respectively in the range of 10-100mA and 100-300 mA.
6. The method of in situ generation of Fe (IV) and use in wastewater treatment according to claim 1 or 2, characterized in that:
the treatment time was 180min.
7. The method of in situ generation of Fe (IV) and use in wastewater treatment according to claim 1 or 2, characterized in that:
the chlorine-separating electrode is IrO 2 -RuO 2 Ti electrode and IrO 2 -TaO 2 Ti electrode and PbO 2 One of the Ti electrodes.
8. The method of in situ generation of Fe (IV) and use in wastewater treatment according to claim 1 or 2, characterized in that:
the conductive electrode is one of a stainless steel and a Cu/Zn electrode.
9. The method of in situ generation of Fe (IV) and use in wastewater treatment according to claim 1 or 2, characterized in that:
the waste water is acidic nickel plating waste water.
10. An apparatus for in situ generation of Fe (IV) for wastewater treatment, characterized in that the apparatus comprises an electrolysis system, a precipitation system;
the electrolysis system comprises an electrolysis tank, an electrode assembly, a mechanical stirring paddle, a direct current controller and a wastewater conveying pump; the wastewater is uniformly distributed into the electrolytic tank, fe (IV) is generated in the solution after the direct current power supply controller electrifies the electrode assembly, active species Fe (IV) fully contact and react with organic matters in the wastewater under the operation of the mechanical stirring paddle, and the waste liquid in the electrolytic tank is transported to a precipitation system through the wastewater transport pump after a specific reaction time; wherein the electrode assembly comprises an Fe electrode, a chlorine evolution electrode and a conductive cathode;
the sedimentation system comprises a sedimentation reaction chamber, a dosing port is arranged on the side face of the sedimentation reaction chamber, high-efficiency separation is realized after alkaline precipitation of wastewater in the sedimentation reaction chamber, and a sludge discharge port is arranged at the bottom of the sedimentation reaction chamber and used for removing precipitated flocs after alkaline precipitation; the side part of the precipitation reaction chamber is also provided with a water outlet for removing supernatant liquid after adding alkali for precipitation.
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| 李勇东等: "PbO2/Fe双阳极耦合促进焦化废水除碳脱氮", 《环境化学》, vol. 39, no. 6, 30 June 2020 (2020-06-30), pages 1650 - 1659 * |
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| CN117417032A (en) * | 2023-10-11 | 2024-01-19 | 华南理工大学 | Preparation and application of high-selectivity chlorine-separating anode |
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