CN114920344A - Method for treating cadmium wastewater by using electroreduction technology - Google Patents
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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
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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Abstract
The invention provides a method for treating cadmium wastewater by an electroreduction technology in the presence of an anion exchange membrane, which realizes the high-efficiency treatment of the cadmium wastewater by changing the composition of an electrolyte solution on the anode side. Firstly, adopting a bipolar chamber electrolytic cell separated by an anion exchange membrane, treating high-concentration cadmium wastewater by taking a metal electrode plate as a cathode electrode for cathodic electro-reduction, wherein the pH of a solution treated by the anion exchange membrane is not too low; then transferring the low-concentration cadmium wastewater to a bipolar chamber electrolytic cell of which the anode chamber contains a large cation solution with the pH value of more than or equal to 7, and carrying out cathodic electro-reduction treatment by using a metal foam plate to reach the discharge standard; finally, after the low-concentration cadmium wastewater is subjected to repeated electro-reduction for multiple times, the high-concentration cadmium waste liquid obtained by corroding metal cadmium accumulated on the cathode of the foam plate by using an acid solution is subjected to the first-step electro-reduction treatment again. The method provided by the invention efficiently removesCd 2+ The cadmium content is controlled to be 0.05 mg.L ‑1 The method realizes the recycling of the metal cadmium, avoids secondary pollution and simultaneously greatly reduces energy consumption.
Description
Technical Field
The experiment relates to a method for effectively treating low-concentration cadmium wastewater and effectively recovering metal cadmium. More specifically, the invention adopts an electroreduction technology, combines an anion exchange membrane and a large cation to be applied to the electroreduction process, realizes the high-efficiency treatment and cadmium recovery of the cadmium-containing wastewater, and belongs to the cadmium-containing wastewater treatment technology.
Background
Cadmium is a carcinogenic heavy metal, and the harm of cadmium is mainly reflected in that cadmium easily enters a human body through a food chain through water body enrichment, so that kidney damage and chondropathy are caused. In recent years, with the enhancement of environmental improvement in the world, especially in China, cadmium emission is strictly controlled.
The traditional cadmium wastewater mainly comes from electroplating plants, cadmium sulfide production plants, zinc-lead concentrate smelting plants, sponge cadmium production plants, storage battery plants and the like. The common cadmium waste liquid treatment method comprises a chemical precipitation method, a ferrite method, an electric flocculation method, an adsorption method, an ion exchange method and the like. The methods generally have the problems of low cadmium removal rate, high energy consumption and high cost, and often generate solid wastes to cause secondary pollution. In recent years, a cadmium waste liquid treatment technology for directly recovering cadmium metal by adopting an electroreduction technology is gradually developed. However, the electro-reduction technology is still immature, and particularly, the cadmium waste liquid cannot be treated to the discharge standard by adopting the electro-reduction technology alone, and the discharge requirement can be met only by combining other technologies, so that the treatment cost is increased.
In recent years, cadmium telluride thin film photovoltaic cells are gradually used for building photovoltaic power stations in large quantities, and cadmium-containing waste liquid is generated in the production process and the future cell recycling treatment process of the cadmium telluride cells. With the large-scale use of CdTe thin film batteries, it is urgently desired to develop a treatment method for cadmium waste liquid in the production process of cadmium telluride batteries. The electro-reduction treatment technology can directly reduce metal ions in the solution into high-purity metal, and then the metal is recycled to realize resource recycling, so that the cost advantage is obvious. Meanwhile, the cadmium waste liquid in the field of photovoltaic cells has relatively simple composition and extremely low content of organic additives, and is particularly suitable for adopting an electroreduction technology. However, the current electroreduction technology is only suitable for treating high-concentration cadmium wastewater, and the pure electroreduction technology is difficult to treat the low-concentration cadmium-containing waste liquid to the discharge standard. Researches find that the difficulty in treating the low-concentration cadmium waste liquid by the electroreduction method is that the low mass transfer rate of cadmium ions in the solution and the corrosion effect of the weakly acidic solution on cadmium are main limiting factors that the concentration of the cadmium ions cannot be reduced continuously.
With the development of membrane technology and related engineering sciences, various water permeable membranes are gradually used in Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF), Reverse Osmosis (RO), Forward Osmosis (FO), Membrane Distillation (MD), etc., and successfully applied to drinking water softening, sea water softening, etcThe field of water desalination and wastewater recovery. Solute permeable membranes rely on the affinity of chemicals for membranes to separate chemicals, have selective permeability to chemicals, and allow or block the movement of certain chemicals for resource recovery. The combination of membrane selectivity with the electrical driving power of electrochemical technology provides the possibility of water treatment, for example electrodialysis technology can achieve a minimization of the volume of salt solution by concentration. Our earlier studies found that anion exchange membranes were introduced into electroreduction technology, although Cd in high concentration cadmium waste streams could be reduced 2+ The concentration is reduced to 1.06 mg.L -1 The removal rate reaches 99.99 percent, but still cannot reach the emission standard, and the energy consumption is obviously increased at the later stage of treatment. Therefore, a method is needed to thoroughly solve the problems of low ion mass transfer rate and weak acid corrosion in the later stage of cadmium wastewater treatment, so that the discharge requirement can be met by directly adopting an electroreduction technology.
Disclosure of Invention
The purpose of the invention is as follows: in the process of removing cadmium by electroreduction, H generated by oxygen evolution reaction at the anode side + Can diffuse to the cathode side under the action of concentration difference and electric field, not only aggravates the hydrogen evolution effect and energy consumption when the cadmium is electrically reduced, but also corrodes the metal cadmium and weakens the cadmium removal effect. The introduction of an Anion Exchange Membrane (AEM) allows the diffusion of cathode side anions towards the anode while suppressing H produced by the anodic oxygen evolution reaction + Diffusing to the cathode to prevent the pH of the cathode solution from excessively decreasing, but due to H + Small radius and still have part H + The cadmium ions are diffused to the cathode side solution, show weak acidity and have certain corrosion effect on metal cadmium, so that the cadmium ions are partially remained and cannot reach the cadmium discharge standard. Therefore, the corrosion of the electro-reduction metal cadmium by the weak acidity of the cathode chamber solution is a main reason that the electro-reduction cannot reach the discharge standard. Therefore, the invention transfers the low-concentration cadmium ion solution to an electrolytic bath with anode solution containing large cations and pH more than or equal to 7 for continuous treatment in the later period to prevent H + And the metal cadmium is diffused to the cathode, so that the corrosion of acid to the electro-reduction metal cadmium is completely inhibited, and the discharge standard of the cadmium is reached.
The invention provides a method for removing cadmium by electroreduction, which comprises the following steps.
(1) A bipolar chamber circulating electrolytic tank which is divided into a cathode chamber and an anode chamber by an AEM membrane is adopted, cadmium-containing wastewater is introduced into the cathode chamber and flows circularly, and sulfuric acid solution with proper concentration is filled into the anode chamber. The cathode is a metal plate or a cadmium-coated metal plate, and the anode is a metal titanium plate coated with a Mixed Metal Oxide (MMO) oxygen generation catalyst. The electric reduction is carried out under the constant voltage (or constant current) and the circulation flow of the cathode solution, the metal cadmium electroplated from the cathode plate can be cleaned and taken out at any time, the cathode plate can be recycled, and the electric reduction is continued until the concentration of the cadmium in the cathode chamber solution is reduced to 10 mg.L -1 The following.
(2) And transferring the treated cadmium waste liquid into an electrolytic cell with another AEM membrane to divide into two electrode chambers, wherein the anode chamber contains a large cation solution with a certain concentration, the pH value of the solution is more than or equal to 7, the anode electrode plate is an MMO plate, and the cathode is a porous copper foam plate or a porous carbon foam plate. Performing electric reduction under constant voltage (or constant current) and cathode circulation flow until the concentration of the cadmium waste liquid is reduced to 0.05 mg.L -1 The emission standard is met below.
(3) After the electro-reduction is repeatedly carried out for a plurality of times to treat the low-concentration cadmium wastewater, a certain amount of metal cadmium is accumulated on the foam cathode and needs to be cleaned in time, otherwise, the porous structure of the foam cathode is blocked, and the effective area is reduced. Because the pressure of a peristaltic pump adopted by the cathode solution in a circulating manner is certain, when the water yield is reduced by 40 percent, namely the foam cathode holes are blocked by 40 percent, the efficiency is continuously reduced, the anode acid solution recovered in the process of treating the high-concentration cadmium wastewater is adopted for corrosion, and the high-concentration cadmium waste liquid obtained again after corrosion is subjected to the first electro-reduction treatment again.
The invention adopts a bipolar chamber electrolytic tank, introduces an AEM membrane to separate a cathode chamber and an anode chamber, allows anions to diffuse from the cathode to the anode, and simultaneously prevents H generated by oxygen evolution reaction + Diffusion towards the cathode to avoid the pH value of the solution at the cathode side being too low, because the too low pH value can aggravate the hydrogen evolution reaction and energy consumption on the one hand and can generate a large amount of bubbles due to hydrogen evolution to block Cd 2+ Contacting with an electrode to inhibit cadmium removal effect; on the other hand, too low pH will corrode the metallic cadmium formed by the electroreduction, further reducing the cadmium removal effect. In order to maintain a certain degree of electrical conductivity,cdso to be treated at cathode 4 Or CdCl 2 The pH of the solution may be in the range of 2 to 5.
The invention fully utilizes the selective permeability of the AEM film and utilizes the selective permeability to SO 4 2- Or Cl - And its permeability to H + The barrier property of a certain degree maintains the electrical neutrality of the system, and ensures the smooth proceeding of the electrical reduction of cadmium.
The method is characterized in that a large cation electrolyte is introduced into the anode side solution at the later stage of treatment, the pH value of the solution is maintained to be more than or equal to 7, and H with small radius is blocked + The corrosion of metal cadmium caused by the reduction of the pH value of the solution is prevented by the AEM membrane entering the cathode chamber. Meanwhile, ions of the added large cations cannot pass through the AEM membrane, so that anions on the cathode side can be more favorably transferred to the anode under the action of an electric field, and the purification of the wastewater is favorably realized.
The invention has the beneficial effect.
(1) The method is simple and practical, the pure electric reduction technology can reach the national emission standard, and the recycling of the metal cadmium is realized. Because the solution at the anode side does not need to be replaced frequently, the treatment of a large amount of cathode wastewater can be met by adopting a small amount of the anode solution, the operation is simple and effective, and compared with the treatment by other membrane technologies, the method greatly reduces the energy consumption.
(2) Chemical medicines such as flocculating agent and the like do not need to be additionally added in the treatment process, the treatment cost is reduced, and the treated water solution almost reaches the standard of pure water and can be recycled.
(3) The selected large cation electrolyte is degradable organic salt, can be concentrated and reused, and can prevent secondary pollution while reducing the treatment cost.
(4) The method conforms to the strategy of sustainable development and improves the recovery rate of cadmium. After the high-concentration cadmium-containing wastewater is treated, the metal cadmium deposited on the cathode is obtained by mechanical separation and can be directly recycled; after the low-concentration cadmium-containing wastewater is treated, the metal cadmium accumulated on the cathode is subjected to acid corrosion to obtain high-concentration cadmium waste liquid, and the high-concentration cadmium waste liquid is subjected to electrical reduction treatment again to obtain the metal cadmium.
Drawings
FIG. 1 is a flow chart of the present invention, and FIG. 2 is a schematic diagram of the present invention.
The cadmium content testing method comprises the following steps: flame atomic absorption method, apparatus: shimadzu AA-7000F/G atomic absorption spectrophotometer.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in further detail with reference to specific examples. It is to be understood that the embodiments described are only some embodiments of the invention, and not all embodiments. In addition, the present invention relates to a two-step process treatment of higher and lower concentration cadmium solutions, and although the examples are based on the treatment of low concentration cadmium solutions, it is clear that after the treatment of the first step of the high concentration solution, the direct treatment of the low concentration solution with the second step according to the present invention is still applicable. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Although the invention describes the heavy metal ion removal process by taking cadmium wastewater as an example, the electro-reduction principle and the process provided by the invention still have guiding significance for the field of wastewater treatment of other heavy metal ions such as Pb, Hg and the like.
Preparation of the experiment: accurately preparing 5-10 mg.L -1 Cd (2) 2+ Solution of H 2 SO 4 Adjusting the pH = 2-5 to obtain a solution to be treated; accurately preparing 0.01-0.5 mol.L -1 As the solution on the anode side, there may be provided some organic bases or organic salts containing no metal ions, such as tetramethyl ammonium hydroxide, tetramethyl ammonium sulfate, tetramethyl ammonium chloride, or pyridine hydrochloride, etc.; the experiment was carried out in a two-compartment cell with an MMO plate as the anode and a cathode which may be a metal or graphite plate, more preferably a conductive porous foam plate.
Example 1.
Separating the two chambers with AEM membrane, and collecting 10 mg.L -1 Cd (2) 2+ 100mL of solution to be treated, the pH value of the solution to be treated is adjusted to be 2.0, the solution is placed on the cathode side, 0.1M tetramethylammonium chloride solution is placed on the anode side, the electric reduction is carried out by using 0.02A constant current, the time is 200min, the energy consumption is 2.3Wh, and the final cadmium contentIs 0.05 mg.L -1 。
Example 2.
Take 1 mg.L -1 Cd (2) 2+ The solution to be treated is 100mL, the pH is adjusted to 5, the solution is placed on the cathode side, 0.01M tetramethyl ammonium sulfate solution is placed on the anode side, then the electroreduction is carried out at the constant voltage of 40V, the time is taken for 150min, the energy consumption is 1.5Wh, and the final cadmium content is 0.03 mg.L -1 。
Example 3.
Take 5 mg.L -1 Cd (2) 2+ 100mL of solution to be treated, the pH value of the solution to be treated is adjusted to be 3.0, the solution is placed on the cathode side, 0.05M pyridine hydrochloride solution is placed on the anode side, then the solution is subjected to electric reduction at constant current of 0.04A, the time consumption is 200min, the energy consumption is 2.5Wh, and the final cadmium content is 0.05 mg.L -1 。
Example 4.
Take 5 mg. L -1 Cd (2) 2+ 100mL of solution to be treated, the pH value of the solution to be treated is adjusted to be 2.4, the solution is placed on the cathode side, 0.2M tetramethylammonium chloride solution is placed on the anode side, then the solution is subjected to electric reduction at a constant current of 0.02A, the time is 200min, the energy consumption is 1.9Wh, and the final cadmium content is 0.09 mg.L -1 。
Compared with the above examples, the method has remarkable effect in treating the low-concentration cadmium wastewater, so that the cadmium content meets the discharge standard, and the energy consumption is low.
Claims (17)
1. A method for treating cadmium wastewater by utilizing an electroreduction technology comprises the following steps:
(1) adopting a bipolar chamber electrolytic cell separated by an anion exchange membrane to carry out electro-reduction treatment on the high-concentration cadmium wastewater;
(2) adopting a bipolar chamber electrolytic cell separated by an anion exchange membrane, adding a solution of large cations into an anode chamber, and performing electro-reduction treatment on the low-concentration cadmium wastewater;
(3) after the low-concentration cadmium wastewater is treated by repeated electro-reduction, the high-concentration cadmium waste liquid obtained by corroding metal cadmium accumulated on the cathode by an acid solution is subjected to the first-step electro-reduction treatment again.
2. Electroreduction plant according to claim 1The method for treating the cadmium wastewater, wherein the cadmium content of the high-concentration cadmium wastewater in the step (1) is generally more than 10 mg.L -1 The upper limit is not particularly limited.
3. The method for treating cadmium wastewater by electroreduction as claimed in claim 1, wherein the anion exchange membrane of the separation electrolyzer is Cl-tolerant - Or SO 4 2- Passing through an anion exchange membrane.
4. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the hydrochloric acid or sulfuric acid solution with the same anion concentration as that in the cadmium wastewater is used in the anode chamber of the bipolar chamber electrolytic cell in step (1) and can be recovered after being used for a plurality of times.
5. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the electroreduction in the high concentration cadmium wastewater in step (1) can be performed in constant current or constant voltage mode, and the applied current or voltage is such that the current does not exceed the maximum ion current allowed to pass through the anion exchange membrane.
6. The method for treating cadmium wastewater by electroreduction as claimed in claim 1, wherein the cathode used in the step (1) is copper plate or other metal plate with low potential for producing cadmium and easy removal of metal cadmium.
7. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the treatment of the high concentration cadmium wastewater of step (1) further comprises a mechanical separation process of a large amount of metallic cadmium on a flat cathode.
8. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the final concentration of the treated high concentration cadmium wastewater of step (1) is less than 10 mg-L -1 。
9. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein in the treatment of the low concentration cadmium wastewater of step (2), the large cation electrolyte is an organic base or an organic salt free of metal ions, and is composed of organic cations and anions, such as; tetramethylammonium hydroxide, tetramethylammonium sulfate, tetramethylammonium chloride, pyridine hydrochloride, or the like.
10. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the concentration of the low concentration cadmium solution in the cathode chamber in the step (2) is less than 10 mg-L -1 The pH value is 2-5.
11. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the anode used in step (2) is a titanium plate or a titanium mesh coated with MMO, and the cathode is a metal or graphite plate or a porous foam plate, preferably a porous foam plate.
12. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the low concentration cadmium wastewater is treated in the step (2), and the electroreduction can be performed in a constant current or constant voltage mode.
13. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the acid used for accumulating the corrosion of metallic cadmium in step (3) is derived from the anode solution recovered in step (1).
14. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein in step (3), when the water yield is reduced by 40% under constant pressure, the foam cathode is subjected to acid corrosion to clean the accumulated cadmium metal.
15. The macrocation electrolyte in the anode chamber according to claim 9, wherein the concentration of the initial solution of macrocations is 0.01 to 0.5 mol-L -1 The pH value of the solution is more than or equal to 7.
16. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein said plate or foam electrode can be reused without affecting the performance.
17. The method for treating cadmium wastewater by electroreduction according to claim 1, wherein the treatment is performed at room temperature.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102912380A (en) * | 2012-10-12 | 2013-02-06 | 彩虹集团公司 | Low-temperature electro-deposition method for cadmium by ionic liquid |
| CN109252190A (en) * | 2018-11-07 | 2019-01-22 | 广州市吉池环保科技有限公司 | A method of it recycling 99.98% copper powder from etching solution and prepares 99.999% tough cathode |
| CN109534455A (en) * | 2018-11-09 | 2019-03-29 | 西安交通大学 | A kind of electrochemical method of low-consumption high-efficiency processing heavy metal wastewater thereby |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102912380A (en) * | 2012-10-12 | 2013-02-06 | 彩虹集团公司 | Low-temperature electro-deposition method for cadmium by ionic liquid |
| CN109252190A (en) * | 2018-11-07 | 2019-01-22 | 广州市吉池环保科技有限公司 | A method of it recycling 99.98% copper powder from etching solution and prepares 99.999% tough cathode |
| CN109534455A (en) * | 2018-11-09 | 2019-03-29 | 西安交通大学 | A kind of electrochemical method of low-consumption high-efficiency processing heavy metal wastewater thereby |
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