CN110759554A - Recycling and zero-discharge treatment method for ammonium adipate wastewater generated in aluminum foil formation - Google Patents
Recycling and zero-discharge treatment method for ammonium adipate wastewater generated in aluminum foil formation Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
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- C02F1/00—Treatment of water, waste water, or sewage
- 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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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F2001/5218—Crystallization
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/346—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from semiconductor processing, e.g. waste water from polishing of wafers
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2301/04—Flow arrangements
- C02F2301/043—Treatment of partial or bypass streams
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- C02F2301/00—General aspects of water treatment
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Abstract
The invention discloses a recycling zero-emission treatment method for ammonium adipate wastewater generated in aluminum foil formation, which comprises the following steps of: adding acid liquor into the ammonium adipate wastewater for acidification treatment, and then performing solid-liquid separation to obtain adipic acid crystals and ammonia-containing wastewater; carrying out ion separation on the ammonia-containing wastewater by using an electric drive membrane method, recovering to obtain acid liquor and ammonia water, and recycling the acid liquor to acidize the adipic acid wastewater; mixing adipic acid crystals with ammonia water for reaction to prepare an ammonium adipate solution; concentrating and refining the ammonium adipate solution by a pressure driving membrane method to obtain a refined ammonium adipate solution, and recycling the refined ammonium adipate solution to an aluminum foil formation step; and (3) concentrating and refining the ammonium adipate solution to obtain waste liquid, and sending the ammonium salt solution obtained by an ion exchange method to an electric drive membrane for recycling. The invention realizes the zero-emission recovery treatment of the ammonium adipate wastewater and is more environment-friendly.
Description
Technical Field
The invention belongs to the technical field of capacitor aluminum foil production, and particularly relates to a technology for recycling ammonium adipate wastewater generated by capacitor aluminum foil formation.
Background
In the aluminum electrolytic capacitor corrosion method, the aluminum foil is etched by hydrochloric acid, and the aluminum foil is corroded and dissolved by the hydrochloric acid to generate a porous corrosion film. After corrosion, the aluminum foil is cleaned by clear water to remove Cl-And aluminum powder on the surface, Al is generated3+The formation process is mainly to form a layer of dense and certain voltage-resistant gamma-Al on the surface of the etched aluminum foil2O3An oxide dielectric layer, typically used as the anode of the capacitor. The chemical solutions mainly used in the chemical conversion process include ammonium adipates, organic acids, boric acids, and nonaqueous chemical solutions. Due to Cl not completely cleaned-And Al3+The chemical solution is accumulated in the chemical solution tank continuously, and the chemical solution is required to be changed into fresh chemical solution after a period of time. In the production process of the aluminum electrolytic capacitor, a large amount of waste liquid is generated by corrosion and formation, and the direct discharge not only pollutes the environment but also wastes resources. In addition, the price of ammonium adipate is very expensive, so that the cost for replacing the electrolyte is very high, the replacement is a heavy burden for the industry of aluminum electrolysis electrode foils, and the economic competitiveness is reduced while the production cost is increased. In addition, the waste liquid not only contains ammonia nitrogen, but also contains organic adipic acid, so that the acidity of the solution is increased, if the waste liquid can be recycled, the production cost is reduced, the environmental pollution is reduced, and the discharge of the waste water is reduced from the source. In the prior art, for example, patents CN103508596A and 200710125602.X disclose a clear wastewater treatment system for ammonium adipate, which only performs acidification, filtration and recovery on adipic acid in the ammonium adipate cleaning wastewater, and still has wastewater discharge and complex process, and cannot achieve low-cost zero discharge.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the existing problems and defects, the invention aims to provide a method for recycling and utilizing the ammonium adipate wastewater generated by aluminum foil formation, which realizes the zero-emission recycling and treatment of the ammonium adipate wastewater and is more environment-friendly.
The technical scheme is as follows: in order to realize the purpose, the invention adopts the following technical scheme: a recycling zero-emission treatment method for ammonium adipate wastewater generated in aluminum foil formation comprises the following steps:
(1) adding acid liquor into the ammonium adipate wastewater for acidification treatment, and then performing solid-liquid separation to obtain adipic acid crystals and ammonia-containing wastewater;
(2) performing ion separation on the ammonia-containing wastewater obtained in the step (1) by using an electric drive membrane method, recovering to obtain acid liquor and ammonia water, and recycling the acid liquor to acidize the adipic acid wastewater;
(3) mixing adipic acid crystals obtained in the step (1) and ammonia water obtained in the step (2) for reaction to prepare an ammonium adipate solution;
(4) concentrating and refining the ammonium adipate solution obtained in the step (3) by a pressure driving membrane method to obtain a refined ammonium adipate solution, and recycling the refined ammonium adipate solution to aluminum foil formation;
(5) and (4) concentrating and refining the ammonium adipate solution in the step (4) to obtain waste liquid, and sending the ammonium salt solution obtained by an ion exchange method to the electrically driven membrane in the step (3) for recycling.
Preferably, the electrically driven membrane process is electrodialysis or bipolar membrane electrodialysis.
Preferably, the pressure-driven membrane process is one of nanofiltration, reverse osmosis or diffusion osmosis.
Preferably, before the ammonium adipate wastewater in the step (1) is subjected to acidification treatment, ammonia water is added to adjust the pH value to be within the range of 6.5-8.5, the temperature is reduced to 10-15 ℃, and then the ammonium adipate wastewater is filtered by a PP cotton filter with the filtering diameter of 1-5 microns.
Preferably, adipic acid seed crystals are added in the solid-liquid separation of the adipic acid crystals in the step (1).
Preferably, nitric acid, hydrochloric acid or sulfuric acid is used as the acid solution in the step (1).
Preferably, the waste liquid generated by the ion exchange method in the step (5) is recycled as cleaning water to the aluminum foil corrosion line.
Has the advantages that: compared with the prior art, the method has the advantages that acid liquor and ammonia water are recovered from the acidified ammonium adipate waste liquid through electrodialysis, ammonium salt in the waste liquid after ammonium adipate refining is recovered through a pressure permeable membrane, and the ammonia water, the acid liquor, the ammonium salt and the ammonium adipate obtained through concentration and purification are recycled, so that the recycling zero-emission treatment of the ammonium adipate waste water is realized.
Drawings
FIG. 1 is a schematic flow diagram of the process for recycling zero-emission treatment of ammonium adipate wastewater from aluminum foil formation according to the present invention.
Detailed Description
The present invention is further illustrated by the following figures and specific examples, which are to be understood as illustrative only and not as limiting the scope of the invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification.
As shown in figure 1, the method for recycling and utilizing the ammonium adipate wastewater generated in the aluminum foil formation comprises the steps of ammonia filtration, ammonium adipate acidification treatment, membrane treatment of waste liquid after acidification, ammonium adipate purification treatment and ion exchange treatment of generated waste liquid. Adding ammonia water into the ammonium adipate acidized waste liquid, adjusting the pH value to be 6.5-8.0, stirring to enable alumina to precipitate, filtering by a 2-micron PP cotton core to reduce the concentration of aluminum ions in the waste liquid, acidizing by using recovered HCl, obtaining adipic acid crystals and the waste liquid after acidizing, reusing hydrochloric acid generated by the waste liquid after bipolar membrane electrodialysis treatment to an acidizing unit, preparing ammonium adipate from the generated ammonia water and the adipic acid, purifying the obtained ammonium adipate by using a diffusion dialysis method, removing the generated waste liquid by using an ion exchange method to enable the waste liquid to serve as standard-reaching cleaning water, and enabling ammonium salts generated by the ion exchange method to enter the bipolar membrane electrodialysis for treatment. In the invention, adipic acid and ammonia water are mixed and reacted to obtain crude ammonium adipate, and the crude ammonium adipate is purified by a pressure driving membrane so as to remove Cl possibly remained-Or removing impurity ions such as sulfate ions, which form a filmLoud, especially Cl-The influence of (c). The following is described in detail by way of specific examples:
example 1
The process is used for treating the formed line ammonium adipate waste liquid of certain aluminum foil company, and the concentration of the ammonium adipate is about 0.5mol-1Firstly, adding ammonia water to adjust the pH value to be 6.5-8.0, stirring to enable alumina to precipitate, filtering by a 2-micron PP cotton core to reduce the concentration of aluminum ions in the waste liquid, and then adding 1mol.L of ammonium adipate to the waste liquid-1While stirring, a small amount of adipic acid crystals was added as seed crystals. Then separating out adipic acid by filtration, and treating the generated waste liquid by bipolar membrane electrodialysis to obtain HC with concentration of 0.45mol.L-1In addition, the obtained ammonia water reacts with adipic acid to prepare ammonium adipate, the obtained ammonium adipate is dissolved and then is purified by a diffusion dialysis method, and the flow intensity is 10L/(h m)2) Initially, ammonium adipate solution contained Cl-100mg/L of treated ammonium adipate solution containing Cl-The obtained ammonium adipate solution with the concentration of 30mg/L can be directly utilized to a production line, in addition, the solution of the waste liquid generated in the process after being treated by the ion exchange resin can be reused to wash water of a corrosion line, the waste liquid generated by the regeneration of the ion exchange resin is subjected to electrodialysis again, and the obtained hydrochloric acid concentration is 0.2mol-1And the solution obtained by treating the waste liquid generated by the ion exchange method can be reused as washing water. The treatment process can ensure that the ammonium adipate waste liquid treatment process can reach the standard of zero emission.
Example 2
The process is used for treating the formed line ammonium adipate waste liquid of certain aluminum foil company, and the concentration of the ammonium adipate is about 0.4mol-1Firstly, adding ammonia water to adjust the pH value to be 6.5-8.0, stirring to enable alumina to precipitate, filtering by a 2-micron PP cotton core to reduce the concentration of aluminum ions in the waste liquid, and then firstly adding 0.5mol.L into the ammonium adipate waste liquid-1While stirring, a small amount of adipic acid crystals was added. The adipic acid is then separated off by filtrationThe generated waste liquid is treated by bipolar membrane electrodialysis, and the HC concentration obtained by the bipolar membrane electrodialysis treatment is 0.35mol.L-1In addition, the obtained ammonia water reacts with adipic acid to prepare ammonium adipate, the obtained ammonium adipate is dissolved and then is purified by a diffusion dialysis method, and the flow intensity is 10L/(h m)2) Initially, ammonium adipate solution contained Cl-200mg/L of treated ammonium adipate solution containing Cl-The obtained ammonium adipate solution with the concentration of 0.2 mol/L can be directly utilized to a production line, in addition, the solution of the waste liquid generated in the process after being treated by the ion exchange resin can be reused to wash water of a corrosion line, and the waste liquid generated in the regeneration of the ion exchange resin is subjected to the bipolar membrane electrodialysis again to obtain the hydrochloric acid with the concentration of 0.2 mol/L-1And the solution obtained by treating the waste liquid generated by the ion exchange method can be reused as washing water. The treatment process can ensure that the ammonium adipate waste liquid treatment process can reach the standard of zero emission.
Embodiment 3
The process is used for treating the formed line ammonium adipate waste liquid of certain aluminum foil company, and the concentration of the ammonium adipate is about 0.65mol-1Firstly, adding ammonia water to adjust the pH value to be 6.5-8.0, stirring to enable alumina to precipitate, filtering by a 2-micron PP cotton core to reduce the concentration of aluminum ions in the waste liquid, and then adding 1mol.L of ammonium adipate to the waste liquid-1While stirring, a small amount of adipic acid crystals was added. Then separating out adipic acid by filtration, and treating the generated waste liquid by bipolar membrane electrodialysis to obtain HC with concentration of 0.5mol.L-1In addition, the obtained ammonia water reacts with adipic acid to prepare ammonium adipate, the obtained ammonium adipate is dissolved and then is purified by a diffusion dialysis method, and the flow intensity is 10L/(h m)2) Initially, ammonium adipate solution contained Cl-500mg/L, Cl in the treated ammonium adipate solution-40 mg/L. The obtained ammonium adipate solution can be directly utilized to a production line, and in addition, the solution obtained by treating waste liquid generated in the process by using ion exchange resin can be reused to wash water of a corrosion line and the ion exchange resinThe waste liquid generated by regeneration is treated by bipolar membrane electrodialysis again, and the concentration of the obtained hydrochloric acid is 0.3mol-1And the solution obtained by treating the waste liquid generated by the ion exchange method can be reused as washing water. The treatment process can ensure that the ammonium adipate waste liquid treatment process can reach the standard of zero emission.
Claims (7)
1. A recycling zero-emission treatment method for ammonium adipate wastewater generated in aluminum foil formation is characterized by comprising the following steps:
(1) adding acid liquor into the ammonium adipate wastewater for acidification treatment, and then performing solid-liquid separation to obtain adipic acid crystals and ammonia-containing wastewater;
(2) performing ion separation on the ammonia-containing wastewater obtained in the step (1) by using an electric drive membrane method, recovering to obtain acid liquor and ammonia water, and recycling the acid liquor to acidize the adipic acid wastewater;
(3) mixing adipic acid crystals obtained in the step (1) and ammonia water obtained in the step (2) for reaction to prepare an ammonium adipate solution;
(4) concentrating and refining the ammonium adipate solution obtained in the step (3) by a pressure driving membrane method to obtain a refined ammonium adipate solution, and recycling the refined ammonium adipate solution to aluminum foil formation;
(5) and (4) concentrating and refining the ammonium adipate solution in the step (4) to obtain waste liquid, and sending the ammonium salt solution obtained by an ion exchange method to the electrically driven membrane in the step (3) for recycling.
2. The method for recycling and utilizing ammonium adipate wastewater generated in aluminum foil formation according to claim 1, which is characterized by comprising the following steps of: the electrically driven membrane process is electrodialysis or bipolar membrane electrodialysis.
3. The method for recycling and utilizing ammonium adipate wastewater generated in aluminum foil formation according to claim 1, which is characterized by comprising the following steps of: the pressure-driven membrane method is one of nanofiltration, reverse osmosis or diffusion osmosis.
4. The method for recycling and utilizing ammonium adipate wastewater generated in aluminum foil formation according to claim 1, which is characterized by comprising the following steps of: adding ammonia water to adjust the pH value to be 6.5-8.5 before acidizing the ammonium adipate wastewater in the step (1), cooling to 10-15 ℃, and then filtering by a PP cotton filter with the filtering diameter of 1-5 microns.
5. The method for recycling and utilizing ammonium adipate wastewater generated in aluminum foil formation according to claim 1, which is characterized by comprising the following steps of: and (2) adding adipic acid seed crystals during solid-liquid separation of the adipic acid crystals in the step (1).
6. The method for recycling and utilizing ammonium adipate wastewater generated in aluminum foil formation according to claim 1, which is characterized by comprising the following steps of: the acid solution in the step (1) is nitric acid, hydrochloric acid or sulfuric acid.
7. The method for recycling and utilizing ammonium adipate wastewater generated in aluminum foil formation according to claim 1, which is characterized by comprising the following steps of: and (5) recycling the waste liquid generated by the ion exchange method in the step (5) as cleaning water to the aluminum foil corrosion line.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408717A (en) * | 2020-11-27 | 2021-02-26 | 苏州聚微环保科技有限公司 | Novel resource utilization process of boric acid waste liquid |
| CN113274882A (en) * | 2021-06-09 | 2021-08-20 | 温州大学新材料与产业技术研究院 | Ammonium adipate waste liquid recovery method and device based on high-temperature bipolar membrane electrodialysis |
| CN114011243A (en) * | 2021-10-19 | 2022-02-08 | 温州大学新材料与产业技术研究院 | Purification device and method for capacitance-level high-purity ammonium salt |
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2019
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408717A (en) * | 2020-11-27 | 2021-02-26 | 苏州聚微环保科技有限公司 | Novel resource utilization process of boric acid waste liquid |
| CN112408717B (en) * | 2020-11-27 | 2022-11-08 | 苏州聚微环保科技有限公司 | Novel resource utilization process of boric acid waste liquid |
| CN113274882A (en) * | 2021-06-09 | 2021-08-20 | 温州大学新材料与产业技术研究院 | Ammonium adipate waste liquid recovery method and device based on high-temperature bipolar membrane electrodialysis |
| CN113274882B (en) * | 2021-06-09 | 2022-05-17 | 温州大学新材料与产业技术研究院 | Ammonium adipate waste liquid recovery method and device based on high-temperature bipolar membrane electrodialysis |
| CN114011243A (en) * | 2021-10-19 | 2022-02-08 | 温州大学新材料与产业技术研究院 | Purification device and method for capacitance-level high-purity ammonium salt |
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Application publication date: 20200207 |