CN112777774A - Nickel-containing wastewater treatment device and nickel-containing wastewater treatment method - Google Patents
Nickel-containing wastewater treatment device and nickel-containing wastewater treatment method 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F1/722—Oxidation by peroxides
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/425—Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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Abstract
The application provides a nickel-containing wastewater treatment device and a nickel-containing wastewater treatment method, wherein the nickel-containing wastewater treatment device comprises a collateral breaking pretreatment system which is connected in sequence and is used for carrying out collateral breaking pretreatment on nickel-containing wastewater; the pretreatment system comprises a Fenton oxidation system and an ozone catalytic oxidation system which are sequentially connected; an advanced treatment system comprising an ion exchange resin; and the nickel recovery system comprises a resin desorption system, an extraction system and a distillation system which are arranged in sequence. The nickel-containing wastewater treatment device adopts the pretreatment system and the advanced treatment system for treatment, realizes the dual targets of reaching the standard of wastewater and enriching nickel ions, and does not introduce other pollutants; and then the nickel resource is recovered through a nickel recovery system, and no solid waste is generated in the recovery process.
Description
Technical Field
The application relates to the field of wastewater treatment, in particular to a nickel-containing wastewater treatment device and a nickel-containing wastewater treatment method.
Background
The electroplating is to deposit a required coating on the surface of a product by an electrochemical method, so as to realize the protection and modification of the metal or nonmetal surface, obtain new performance of the product and the like. In recent years, the electroplating industry in China develops rapidly, nickel plating is used as a main mode for metal surface modification, a large amount of nickel-containing wastewater is generated in the process, and according to incomplete statistics, the nickel-containing wastewater is 40 hundred million m per year350% of the discharged electroplating wastewater does not reach the discharge standard, pollutants in the electroplating wastewater are difficult to biodegrade and easy to accumulate in organisms, and the pollutants discharged into the environment can seriously threaten environmental mankind. The common method for treating nickel-containing wastewater is a traditional chemical precipitation method mainly comprising hydroxide and sulfide, which is mainly suitable for treating free nickel, but is difficult to remove complex nickel, and other methods such as electrolysis, ion exchange, adsorption and advanced redox can ensure that the total nickel in effluent reaches the standard, but generally have the disadvantages of high cost, long reaction time, easy secondary pollution and limitation of practical application. With the increasing strictness of wastewater discharge standards, the concentration of Ni2+ remaining in nickel-containing electroplating wastewater after treatment is required to be lower than the emission limit of electroplating pollutant discharge standard (GB21900-2008) of 0.1mg/L, so it is necessary to develop a more stable and effective method for advanced treatment of nickel.
The recovery of nickel resources in electroplating wastewater is mainly realized by changing nickel-containing wastewater into nickel-containing sludge, online recovery or recovery by adopting resin adsorption and other modes, the recovery rate is low, the purity of the recovered nickel salt is poor, the product is difficult to sell, and the technical problem of how to improve the recovery rate and purity of the nickel salt still needs to be solved urgently.
In view of the above, there is a need to provide an improved nickel-containing wastewater treatment apparatus and method for treating nickel-containing wastewater to solve the above-mentioned technical problems.
Disclosure of Invention
An object of the present invention is to provide an apparatus for treating nickel-containing wastewater and a method for treating nickel-containing wastewater, which can solve at least one of the above problems.
In order to achieve the purpose of the application, the following technical scheme is adopted in the application:
nickel-containing wastewater treatment device comprises a plurality of devices which are connected in sequence
The nickel-containing wastewater is subjected to a complex breaking pretreatment;
the pretreatment system comprises a Fenton oxidation system and an ozone catalytic oxidation system which are sequentially connected;
an advanced treatment system comprising an ion exchange resin;
and the nickel recovery system comprises a resin desorption system, an extraction system and a distillation system which are arranged in sequence.
Further, the ion exchange resin is macroporous styrene series chelating type ion exchange resin.
In order to achieve the purpose of the application, the following technical scheme is adopted in the application:
a nickel-containing wastewater treatment method, comprising:
s1, carrying out vein breaking pretreatment, adding alkali liquor to carry out vein breaking pretreatment on the nickel-containing wastewater, and taking supernatant after the vein breaking pretreatment as pretreatment;
s2, pretreating, namely sequentially carrying out pH adjustment, Fenton oxidation and ozone catalytic oxidation treatment on pretreated inlet water;
s3 deep treatment, namely enriching nickel through ion resin;
s4 nickel is recovered, the resin rich in nickel is desorbed to obtain a regenerated liquid containing nickel resin, the regenerated liquid containing nickel resin is extracted, and the extraction liquid is distilled.
Further, step S1 specifically includes adjusting the pH of 30% sodium hydroxide solution to 10-11, which plays a part in breaking the complex.
Further, step S1 includes adding a proper amount of polyacrylamide for flocculation and precipitation after the vein breaking pretreatment, standing, and taking the supernatant as pretreatment inlet water.
Further, step S2 specifically includes:
s21, adjusting the pH value, namely adjusting the parameters of the wastewater to 3.0-4.0 by acid;
s22, Fenton Oxidation, 30% H2O2Is added in an amount of about 1.0ml/L, Fe2+The adding amount of the reaction solution is about 150mg/L, and the reaction is carried out for first preset time;
s23, carrying out ozone catalytic oxidation, and carrying out ozone catalysis on the wastewater subjected to Fenton oxidation, wherein the adding amount of ozone is 300-400 mg/L, and reacting for a second preset time.
Further, wherein the ratio of the first predetermined time to the second predetermined time is 1: 3.
further, in step S3, the pH value is 5-6, and the ion exchange resin is a macroporous styrene series chelating type ion exchange resin.
Further, in step S4, the resin is subjected to a desorption process: desorbing and regenerating the nickel-enriched ion exchange resin by using acid liquor to obtain nickel-containing resin regeneration liquid.
Further, in step S4, the extraction process specifically includes:
firstly, adjusting the pH value of the nickel-containing resin regeneration liquid to about 4.5, and then adding an extracting agent adaptive to an acidic medium for extraction, wherein the volume ratio of the extracting agent to the wastewater is 1: 1, extracting for 2-4min, and standing for layering after extraction;
and then separating nickel ions from the organic phase rich in nickel by using sulfuric acid, namely back extraction, wherein the volume ratio of the organic phase to the sulfuric acid is 1: and 2, standing and layering.
Further, the extractant is a mixture of di- (2-ethylhexyl) -phosphoric acid and kerosene, and the volume ratio of the di- (2-ethylhexyl) -phosphoric acid to the kerosene is 15%.
The beneficial effect of this application is: the nickel-containing wastewater treatment device adopts the pretreatment system and the advanced treatment system for treatment, realizes the dual targets of reaching the standard of wastewater and enriching nickel ions, and does not introduce other pollutants; and then the nickel resource is recovered through a nickel recovery system, and no solid waste is generated in the recovery process.
Drawings
FIG. 1 is a schematic structural view of a nickel-containing wastewater treatment apparatus of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present application will now be described in detail with reference to specific embodiments thereof as illustrated in the accompanying drawings. These embodiments are not intended to limit the present application, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present application.
In the various illustrations of the present application, certain dimensions of structures or portions may be exaggerated relative to other structures or portions for ease of illustration and, thus, are provided to illustrate only the basic structure of the subject matter of the present application.
As shown in fig. 1, a nickel-containing wastewater treatment apparatus according to a preferred embodiment of the present invention includes a complex breaking pretreatment system, a pretreatment system, an advanced treatment system, and a nickel recovery system, which are connected in sequence.
The term "sequentially connected" as used herein means that the two adjacent systems are connected directly by a pipeline, so that the wastewater flows to the next treatment system automatically, or indirectly, i.e. there is no pipeline between the two systems, and the wastewater is transferred from the previous treatment system to the next treatment system by manual intervention.
The nickel-containing wastewater sequentially passes through the complex breaking pretreatment system, the advanced treatment system and the nickel recovery system, so that the dual targets of reaching the standard of wastewater treatment and nickel ion enrichment are realized.
The system for the pretreatment of the broken collaterals carries out the treatment of broken collaterals by adding the alkali liquor into the wastewater, reduces the dosage of chemical reagents in a subsequent pretreatment system and improves the treatment effect of the subsequent procedures.
The pretreatment system comprises a Fenton treatment system and an ozone catalytic oxidation system; the Fenton treatment system can decompose part of organic pollutants in the wastewater, and can achieve the effects of oxidizing and breaking the complex so as to convert the metal nickel in the complex state into the free state; but also can oxidize organic matters and the like in the wastewater. The ozone catalytic oxidation system can further oxidize organic matters, reduce COD (chemical oxygen demand) of the wastewater and remove part of metal ions such as iron and the like.
The advanced treatment system comprises ion exchange resins for adsorbing and enriching nickel, and preferably comprises two or more stages of ion exchange resins in series. The ion exchange resin is preferably a macroporous cation exchange resin having the most excellent effect of adsorbing and removing nickel ions in wastewater, for example, a macroporous styrene series chelate ion exchange resin.
The nickel recovery system comprises a resin desorption system, an extraction system and a distillation system which are arranged in sequence. The extraction system is used for extracting nickel and extracting and separating other impurity metals, and the application preferably selects a multistage extraction system with two or more stages, so that the extraction rate is high. The distillation system is a reduced pressure distillation system.
The nickel-containing wastewater treatment method comprises the following steps:
s1, carrying out the breaking pretreatment, adding alkali liquor to carry out the breaking pretreatment on the nickel-containing wastewater, and taking the supernatant after the breaking pretreatment as the pretreatment. In general, the nickel-containing electroplating wastewater is acidic, and is subjected to pH adjustment by a complex breaking pretreatment system, for example, the pH is adjusted to 10-10.5 by using 30% sodium hydroxide solution, so as to perform a partial complex breaking function.
Further, after the vein breaking pretreatment, adding a proper amount of Polyacrylamide (PAM) for flocculation and precipitation, standing, taking supernatant, and taking the supernatant as pretreatment inlet water.
S2, pretreating, namely sequentially carrying out pH adjustment, Fenton oxidation and ozone catalytic oxidation treatment on pretreated inlet water.
Step S2 specifically includes: s21pH, adjusting the parameters of the wastewater to a pH value of 3.0-4.0 by acid; adjusting the pH value of the wastewater to about 3.0 by sulfuric acid for example; s22 Fenton Oxidation, 30% H2O2Is added in an amount of about 1.0ml/L, Fe2+The adding amount of the reaction solution is about 150mg/L, and the reaction is carried out for first preset time; s23 ozone catalytic oxidation, directly carrying out ozone catalysis on the wastewater after Fenton oxidation, wherein the adding amount of ozone is 300-400 mg/L, and reacting for the second preset time. Wherein the ratio of the first predetermined time to the second predetermined time is 1: 3, the removal rate of the nickel concentration in the effluent of the pretreatment system can reach 60-70%.
S3 deep treatment, namely, the nickel-containing wastewater after pretreatment is subjected to deep treatment by ion resin enrichment, namely, a resin ion exchange mode is adopted to realize the dual purposes of reaching the standard of the wastewater and enriching nickel ions, and other pollutants are not introduced as much as possible.
Preferably, two or more stages of resin adsorption columns connected in series are adopted for adsorption, so that the adsorption effect is improved.
Specifically, the ion exchange resin is preferably a macroporous cation exchange resin having the most excellent effect of adsorbing and removing nickel ions in wastewater, for example, a macroporous styrene series chelate ion exchange resin. The optimal treatment parameters are that the pH value range is 5-6, the removal rate of nickel is continuously improved along with the increase of the addition amount of resin, and finally the removal rate of nickel reaches about 90%.
S4 nickel is recovered, the resin rich in nickel is desorbed to obtain a regenerated liquid containing nickel resin, the regenerated liquid containing nickel resin is extracted, and the extraction liquid is distilled.
Specifically, the resin is desorbed as follows: the nickel-containing resin regeneration liquid is obtained by desorbing and regenerating the nickel-enriched ion exchange resin by using acid liquor, the concentration of nickel ions of the nickel-containing resin regeneration liquid reaches more than dozens of g/L, and the nickel-containing resin regeneration liquid has a recovery value. For example, sulfuric acid solution with mass fraction of 3% is used for regenerating and desorbing the ion exchange resin which is adsorbed and saturated and is rich in nickel, and the concentration of nickel ions in the obtained nickel resin regeneration solution reaches 20 g/L.
The extraction process specifically comprises the following steps: firstly, adjusting the pH value of the nickel-containing resin regeneration liquid to about 4.5, and then adding an extracting agent adaptive to an acidic medium for extraction, wherein the volume ratio of the extracting agent to the wastewater is 1: 1, extracting for 2-4min, and standing for layering after extraction. The extractant is a mixture of di- (2-ethylhexyl) -phosphoric acid (P204) and kerosene, the volume ratio of the P204 to the kerosene is 15%, and the nickel extraction rate reaches more than 90%, for example, about 95% by 3-stage extraction at room temperature.
And then separating nickel ions from the organic phase rich in nickel by using sulfuric acid, namely back extraction, wherein the volume ratio of the organic phase to the sulfuric acid is 1: and 2, standing and layering. The extraction separation is to remove other impurity ions in the nickel-containing resin regeneration liquid, such as a small amount of metal impurities such as iron, zinc and the like, and obtain a nickel-containing solution with higher purity.
The distillation process is as follows: and (3) recovering the nickel salt by crystallization in a reduced pressure distillation mode to realize the recovery of industrial-grade nickel salt resources, evaporating and concentrating the mixed solution to 3 times in the extracted nickel salt purified solution under a proper negative pressure, and then cooling and crystallizing to obtain the nickel salt with certain purity. In the invention, the nickel salt product of the heavy metal nickel ion conversion crystallization treated by the waste water is recycled, thereby avoiding resource waste, reducing the discharge of dangerous waste and having good environmental benefit and economic benefit.
In conclusion, the pretreatment system and the advanced treatment system are adopted for treatment, so that the dual targets of reaching the standard of the wastewater and enriching the nickel ions are realized, and other pollutants are not introduced; and then the nickel resource is recovered through a nickel recovery system, and no solid waste is generated in the recovery process.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above list of details is only for the concrete description of the feasible embodiments of the present application, they are not intended to limit the scope of the present application, and all equivalent embodiments or modifications that do not depart from the technical spirit of the present application are intended to be included within the scope of the present application.
Claims (11)
1. A nickel-containing wastewater treatment device is characterized by comprising a plurality of devices which are connected in sequence
The nickel-containing wastewater is subjected to a complex breaking pretreatment;
the pretreatment system comprises a Fenton oxidation system and an ozone catalytic oxidation system which are sequentially connected;
an advanced treatment system comprising an ion exchange resin;
and the nickel recovery system comprises a resin desorption system, an extraction system and a distillation system which are arranged in sequence.
2. The nickel-containing wastewater treatment plant according to claim 1, characterized in that: the ion exchange resin is macroporous styrene series chelating type ion exchange resin.
3. A nickel-containing wastewater treatment method, comprising:
s1, carrying out vein breaking pretreatment, adding alkali liquor to carry out vein breaking pretreatment on the nickel-containing wastewater, and taking supernatant after the vein breaking pretreatment as pretreatment;
s2, pretreating, namely sequentially carrying out pH adjustment, Fenton oxidation and ozone catalytic oxidation treatment on pretreated inlet water;
s3 deep treatment, namely enriching nickel through ion resin;
s4 nickel is recovered, the resin rich in nickel is desorbed to obtain a regenerated liquid containing nickel resin, the regenerated liquid containing nickel resin is extracted, and the extraction liquid is distilled.
4. The nickel-containing wastewater treatment method according to claim 3, characterized in that: step S1 specifically includes adjusting the pH to 10-11 with 30% sodium hydroxide solution to partially break the collaterals.
5. The nickel-containing wastewater treatment method according to claim 4, characterized in that: and step S1, adding a proper amount of polyacrylamide for flocculation and precipitation after the vein breaking pretreatment, standing, and taking the supernatant as pretreatment inlet water.
6. The nickel-containing wastewater treatment method according to claim 3, characterized in that: step S2 specifically includes:
s21, adjusting the pH value, namely adjusting the parameters of the wastewater to 3.0-4.0 by acid;
s22, Fenton Oxidation, 30% H2O2Is added in an amount of about 1.0ml/L, Fe2+The adding amount of the reaction solution is about 150mg/L, and the reaction is carried out for first preset time;
s23, carrying out ozone catalytic oxidation, and carrying out ozone catalysis on the wastewater subjected to Fenton oxidation, wherein the adding amount of ozone is 300-400 mg/L, and reacting for a second preset time.
7. The nickel-containing wastewater treatment method according to claim 6, characterized in that: wherein the ratio of the first predetermined time to the second predetermined time is 1: 3.
8. the nickel-containing wastewater treatment method according to claim 3, characterized in that: in step S3, the pH value is 5-6, and the ion exchange resin is macroporous styrene series chelating type ion exchange resin.
9. The nickel-containing wastewater treatment method according to claim 3, characterized in that: in step S4, the resin desorption process includes: desorbing and regenerating the nickel-enriched ion exchange resin by using acid liquor to obtain nickel-containing resin regeneration liquid.
10. The nickel-containing wastewater treatment method according to claim 3, characterized in that: in step S4, the extraction process specifically includes:
firstly, adjusting the pH value of the nickel-containing resin regeneration liquid to about 4.5, and then adding an extracting agent adaptive to an acidic medium for extraction, wherein the volume ratio of the extracting agent to the wastewater is 1: 1, extracting for 2-4min, and standing for layering after extraction;
and then separating nickel ions from the organic phase rich in nickel by using sulfuric acid, namely back extraction, wherein the volume ratio of the organic phase to the sulfuric acid is 1: and 2, standing and layering.
11. The nickel-containing wastewater treatment method according to claim 10, characterized in that: the extractant is a mixture of di- (2-ethylhexyl) -phosphoric acid and kerosene, and the volume ratio of the di- (2-ethylhexyl) -phosphoric acid to the kerosene is 15%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115057558A (en) * | 2022-08-19 | 2022-09-16 | 北京高能时代环境技术股份有限公司 | Method and system for recovering nickel and phosphorus from chemical nickel plating wastewater |
| CN115069237A (en) * | 2022-05-06 | 2022-09-20 | 云南驰宏锌锗股份有限公司 | Ozone catalyst, preparation method thereof and treatment method of high-salt low-COD wastewater |
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2019
- 2019-11-08 CN CN201911087108.8A patent/CN112777774A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115069237A (en) * | 2022-05-06 | 2022-09-20 | 云南驰宏锌锗股份有限公司 | Ozone catalyst, preparation method thereof and treatment method of high-salt low-COD wastewater |
| CN115057558A (en) * | 2022-08-19 | 2022-09-16 | 北京高能时代环境技术股份有限公司 | Method and system for recovering nickel and phosphorus from chemical nickel plating wastewater |
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