CN114573051A - Method for resource utilization of nickel-containing waste liquid - Google Patents
Method for resource utilization of nickel-containing waste liquid Download PDFInfo
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- CN114573051A CN114573051A CN202210276574.6A CN202210276574A CN114573051A CN 114573051 A CN114573051 A CN 114573051A CN 202210276574 A CN202210276574 A CN 202210276574A CN 114573051 A CN114573051 A CN 114573051A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for resource utilization of nickel-containing waste liquid, which comprises the following steps: and (2) exchanging the filtrate obtained after the solid-liquid separation of the nickel-containing waste liquid by using an ion exchange column, eluting by using a sulfuric acid solution to obtain a nickel sulfate solution, uniformly mixing the nickel sulfate solution and an ammonium sulfate solution in proportion, standing for crystallization to obtain a nickel ammonium sulfate crystal, and recycling the crystallization mother liquor through the ion exchange column. The invention adopts a two-stage nickel recovery processing method, firstly, the pressure-filtered nickel-containing waste liquid/water is subjected to ion exchange enrichment and elution to obtain a nickel sulfate solution, nickel ammonium sulfate crystals are obtained through the same ion effect, then, the crystallization mother liquor is subjected to repeated ion exchange enrichment, so that nickel resources are effectively recovered, and the nickel removal rate in the waste liquid/water reaches more than 99%; the produced ammonium nickel sulfate crystal can be used as a raw material of electroplating-grade nickel sulfate.
Description
Technical Field
The invention relates to a method for recycling nickel-containing waste liquid, belonging to the technical field of nickel-containing waste liquid treatment.
Background
With the wide application of metal materials, the need for metal surface treatment is also increasing. Nickel is widely used in electroplating production due to its excellent wear resistance, corrosion resistance and weldability, and the processing amount of nickel is second to that of zinc plating, which is the second place in the whole electroplating industry. The nickel-containing waste liquid/water mainly comes from plating bath waste liquid and plated part rinsing water in the nickel plating production process, the waste plating liquid amount is small, but the nickel ion concentration content is very high, and the plated part rinsing water amount is large, but the nickel ion concentration content is low.
If the nickel-containing waste liquid/water is discharged without any treatment, not only can the environment and the human health be harmed, but also the waste of precious metal resources can be caused. Therefore, the nickel-containing waste liquid/water is effectively and normatively treated, and the method has very important significance for reducing environmental pollution.
The method for treating nickel-containing electroplating wastewater can be divided into three main categories according to different principles: chemical, physicochemical, and biological processes. The chemical method for treating the nickel-containing electroplating wastewater mainly comprises a traditional chemical precipitation method, a novel process ferrite method and a heavy metal chelation precipitation method; the physical and chemical method for treating nickel-containing electroplating wastewater mainly comprises an adsorption technology, an ion exchange technology, a membrane separation technology, an ion flotation technology and the like, which are water treatment technologies developed based on resource recovery; the biological adsorption method is to utilize the strains for adsorbing nickel ions, but the adsorption quantity is generally low.
In the prior patent CN104528997B, 6-8% NaCl eluent is adopted to elute saturated ion exchange resin to obtain a nickel ion concentrated solution, the nickel ion concentrated solution, industrial and agricultural byproducts and a microbial agent are uniformly mixed according to a certain weight, and the mixture is fermented and dried to prepare the organic nickel feed additive. In the actual use process, the proportion of the nickel ion concentrated solution is only 0.5-0.8 per mill, the usage amount is not large, and the treatment of the nickel-containing waste liquid is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recycling nickel-containing waste liquid, which adopts a physical-chemical method and a chemical method in combination and utilizes the principle of the same ion effect to convert nickel resources in the nickel-containing waste liquid into a nickel ammonium sulfate product.
The purpose of the invention is realized by the following technical scheme:
a method for resource utilization of nickel-containing waste liquid is characterized by comprising the following steps:
and (2) exchanging the filtrate obtained after the solid-liquid separation of the nickel-containing waste liquid by using an ion exchange column, eluting by using a sulfuric acid solution to obtain a nickel sulfate solution, uniformly mixing the nickel sulfate solution and an ammonium sulfate solution in proportion, standing for crystallization to obtain a nickel ammonium sulfate crystal, and recycling the crystallization mother liquor through the ion exchange column.
In the invention, sulfuric acid or ammonia water is added before solid-liquid separation of the nickel-containing waste liquid to adjust the pH value of the nickel-containing waste liquid to 6.0-6.5. The nickel-containing waste liquid can be subjected to solid-liquid separation by using a filter press.
In the present invention, the ion exchange resin is any one of a D113 macroporous cation exchange resin, a KP752 macroporous cation exchange resin, a D751 macroporous chelate ion exchange resin, an IRC-718 chelate ion exchange resin and a CH-90Na chelate cation exchange resin.
When the filtrate passes through the ion exchange column, the weight ratio of the nickel content of the filtrate to the ion exchange resin is 1: 20-25 at a flow rate of 3-5 BV/h, and controlling the content of nickel in the liquid after nickel removal to be less than 1 mg/L.
The concentration of the sulfuric acid solution for elution is 10-15%.
In the invention, the molar ratio of nickel to ammonium of the nickel sulfate solution to the ammonium sulfate solution is 1: 2.5-3.0 mixing; adjusting the pH value of the mixed solution of nickel sulfate and ammonium sulfate to 1.0-2.0 by using sulfuric acid, stirring to room temperature, and standing for crystallization; standing for crystallization for at least 24 hours.
Compared with the prior art, the invention has the following advantages:
the invention adopts a two-stage nickel recovery processing method, firstly, the pressure-filtered nickel-containing waste liquid/water is subjected to ion exchange enrichment and elution to obtain a nickel sulfate solution, nickel ammonium sulfate crystals are obtained through the same ion effect, then, the crystallization mother liquor is subjected to repeated ion exchange enrichment, so that nickel resources are effectively recovered, and the nickel removal rate in the waste liquid/water reaches more than 99%; the produced ammonium nickel sulfate crystal can be used as a raw material of electroplating-grade nickel sulfate.
Drawings
FIG. 1 is a diagram of the product of ammonium nickel sulfate crystals according to the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following specific examples:
a method for resource utilization of nickel-containing waste liquid comprises the following steps:
a. adding sulfuric acid or ammonia water to adjust the pH value of the nickel-containing waste liquid to 6.0-6.5, and then carrying out solid-liquid separation treatment to obtain filtrate and sludge;
b. and (3) passing the filtrate through ion exchange resin, wherein the weight ratio of the nickel content of the filtrate to the ion exchange resin is 1: 20-25 at a flow rate of 3-5 BV/h, and controlling the content of nickel in the liquid after nickel removal to be less than 1 mg/L.
c. After the ion exchange resin is completely adsorbed, eluting the ion exchange resin by using a 10-15% sulfuric acid solution to obtain a nickel sulfate solution, wherein the nickel content is 40-60 g/L;
d. mixing a nickel sulfate solution and an ammonium sulfate solution according to the molar ratio of nickel to ammonium of 1: 2.5-3.0, injecting into a crystallization tank, uniformly mixing, adjusting the pH value to 1.0-2.0 by using sulfuric acid, continuously stirring until the system is cooled to room temperature, discharging the mixed solution into the crystallization tank, and standing for at least 24 hours;
e. carrying out centrifugal separation on the materials in the crystallization tank to obtain nickel ammonium sulfate crystals; and (4) collecting the centrifugal clear liquid and repeating the steps a and b to realize the full recycling of the nickel.
In the crystallization process, the longer the standing time is, the better the crystallization process is, the coarser the nickel ammonium sulfate particles are, and the crystallization of the nickel ammonium sulfate is a general green crystalline solid.
Example 1
A method for resource utilization of nickel-containing waste liquid comprises the following steps:
a. adding ammonia water into acidic nickel-containing waste liquid (the pH value is 2.5, and the content of nickel is 9.8 g/L) to adjust the pH value to 6.0, and performing solid-liquid separation treatment in a plate-and-frame filter press to obtain filtrate and sludge, wherein the nickel content of the filtrate is 9.5 g/L;
b. and (3) passing the filtrate through ion exchange resin, wherein the weight ratio of the nickel content of the filtrate to the ion exchange resin is 1: 20. the flow rate is 3-5 BV/h, and the nickel content in the clear liquid after nickel removal is less than 1 mg/L;
c. after the ion exchange resin is completely adsorbed, eluting the ion exchange resin by using a 12% sulfuric acid solution to obtain a nickel sulfate solution, wherein the nickel content is 40-60 g/L;
d. mixing a nickel sulfate solution and an ammonium sulfate solution according to the molar ratio of nickel to ammonium of 1: 2.8, injecting the mixture into a crystallization tank, uniformly mixing, adjusting the pH value to 1.0-2.0 by using sulfuric acid, continuously stirring until the system is cooled to room temperature, discharging the mixed solution into the crystallization tank, and standing for 24 hours;
e. carrying out centrifugal separation on the materials in the crystallization tank to obtain nickel ammonium sulfate crystals; and (4) collecting the centrifugal clear liquid and repeating the steps a and b to realize the full recycling of the nickel.
Example 2
A method for resource utilization of nickel-containing waste liquid comprises the following steps:
a. adding ammonia water into a weakly acidic nickel-containing waste liquid (the pH value is 5.8, the content of nickel is 9 g/L) to adjust the pH value to 6.3, and performing solid-liquid separation treatment in a plate-and-frame filter press to obtain a filtrate and sludge, wherein the nickel content of the filtrate is 8.6 g/L;
b. and (3) passing the filtrate through ion exchange resin, wherein the weight ratio of the nickel content of the filtrate to the ion exchange resin is 1: 22. the flow rate is 3-5 BV/h, and the nickel content in the clear liquid after nickel removal is less than 1 mg/L;
c. after the ion exchange resin is completely adsorbed, eluting the ion exchange resin by using a 10% sulfuric acid solution to obtain a nickel sulfate solution, wherein the nickel content is 40-60 g/L;
d. mixing a nickel sulfate solution and an ammonium sulfate solution according to the molar ratio of nickel to ammonium of 1: 3.0, injecting the mixture into a crystallization tank, uniformly mixing, adjusting the pH value to 1.0-2.0 by using sulfuric acid, continuously stirring until the system is cooled to room temperature, discharging the mixed solution into the crystallization tank, and standing for 30 hours;
e. carrying out centrifugal separation on the materials in the crystallization tank to obtain nickel ammonium sulfate crystals; and (4) collecting the centrifugal clear liquid and repeating the steps a and b to realize the full recycling of the nickel.
Example 3
The method for resource utilization of the nickel-containing waste liquid comprises the following steps:
a. adding sulfuric acid into weakly alkaline nickel-containing waste liquid (the pH value is 8.5, the content of nickel is 9.0 g/L) to adjust the pH value to 6.5, and performing solid-liquid separation treatment in a plate-and-frame filter press to obtain filtrate and sludge, wherein the nickel content of the filtrate is 8.5 g/L;
b. and (3) passing the filtrate through ion exchange resin, wherein the weight ratio of the nickel content of the filtrate to the ion exchange resin is 1: 25. the flow rate is 3-5 BV/h, and the nickel content in the clear liquid after nickel removal is less than 1 mg/L;
c. after the ion exchange resin is completely adsorbed, eluting the ion exchange resin by using a 15% sulfuric acid solution to obtain a nickel sulfate solution, wherein the nickel content is 40-60 g/L;
d. mixing a nickel sulfate solution and an ammonium sulfate solution according to the molar ratio of nickel to ammonium of 1: 2.5, injecting the mixture into a crystallization tank, uniformly mixing, adjusting the pH value to 1.0-2.0 by using sulfuric acid, continuously stirring until the system is cooled to room temperature, discharging the mixed solution into the crystallization tank, and standing for 36 hours;
e. carrying out centrifugal separation on the materials in the crystallization tank to obtain nickel ammonium sulfate crystals; and (4) collecting the centrifugal clear liquid and repeating the steps a and b to realize the full recycling of the nickel.
The purity of the nickel ammonium sulfate crystal obtained by the invention is not less than 98% (calculated by nickel ammonium sulfate hexahydrate) and the granularity is not less than 40 meshes by using the process disclosed by the invention as shown in figure 1.
Claims (8)
1. A method for resource utilization of nickel-containing waste liquid is characterized by comprising the following steps:
and (2) exchanging the filtrate obtained after the solid-liquid separation of the nickel-containing waste liquid by using an ion exchange column, eluting by using a sulfuric acid solution to obtain a nickel sulfate solution, uniformly mixing the nickel sulfate solution and an ammonium sulfate solution in proportion, standing for crystallization to obtain a nickel ammonium sulfate crystal, and recycling the crystallization mother liquor through the ion exchange column.
2. The method for recycling nickel-containing waste liquid according to claim 1, characterized in that sulfuric acid or ammonia water is added to adjust the pH value of the nickel-containing waste liquid to 6.0-6.5 before the solid-liquid separation of the nickel-containing waste liquid.
3. The method according to claim 1, wherein the ion exchange resin is any one of a D113 macroporous cation exchange resin, a KP752 macroporous cation exchange resin, a D751 macroporous chelating ion exchange resin, an IRC-718 chelating ion exchange resin, and a CH-90Na chelating cation exchange resin.
4. The method for resource utilization of the nickel-containing waste liquid according to claim 1, wherein when the filtrate passes through the ion exchange column, the weight ratio of the nickel content of the filtrate to the weight of the ion exchange resin is 1: 20-25 at a flow rate of 3-5 BV/h, and controlling the content of nickel in the liquid after nickel removal to be less than 1 mg/L.
5. The method for resource utilization of nickel-containing waste liquid according to claim 1, wherein the concentration of the sulfuric acid solution is 10-15%.
6. The method for recycling nickel-containing waste liquid according to claim 1, wherein the molar ratio of nickel sulfate solution to ammonium sulfate solution is 1: 2.5 to 3.0.
7. The method for resource utilization of nickel-containing waste liquid according to claim 1, wherein the pH value of the mixed solution of nickel sulfate and ammonium sulfate is adjusted to 1.0-2.0 by using sulfuric acid, the mixed solution is stirred to room temperature and is kept stand for crystallization.
8. The method for recycling nickel-containing waste liquid according to claim 1, wherein the standing crystallization time is at least 24 hours.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115747521A (en) * | 2022-12-29 | 2023-03-07 | 江苏电科环保有限公司 | Method for recovering and preparing lithium carbonate from waste lithium ion battery positive electrode material |
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Publication number | Priority date | Publication date | Assignee | Title |
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