CN112981114A - Nickel-containing waste battery and nickel-containing waste residue recovery process - Google Patents
Nickel-containing waste battery and nickel-containing waste residue recovery process Download PDFInfo
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- CN112981114A CN112981114A CN202110188703.1A CN202110188703A CN112981114A CN 112981114 A CN112981114 A CN 112981114A CN 202110188703 A CN202110188703 A CN 202110188703A CN 112981114 A CN112981114 A CN 112981114A
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- China
- Prior art keywords
- nickel
- filtrate
- filtering
- carbonate
- containing waste
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
-
- C—CHEMISTRY; METALLURGY
- 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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- 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
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/52—Reclaiming serviceable parts of waste cells or batteries, e.g. recycling
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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
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention discloses a nickel-containing waste battery and nickel-containing waste residue recovery process, which relates to the technical field of nickel-containing solid waste treatment and recovery. The method has the advantages that the nickel is precipitated through the soda ash, the obtained nickel carbonate solid is not nickel sulfate, and the influence of sodium ions on a nickel product is avoided; the invention can further improve the impurity treatment amount and improve the product purity of nickel to more than 99.5 percent by a mode of generating the nickel carbonate for acid dissolution treatment; according to the invention, different products can be obtained as required by preparing nickel carbonate and further processing on the basis of the nickel carbonate.
Description
Technical Field
The invention relates to the technical field of nickel-containing solid waste treatment and recovery, in particular to a nickel-containing waste battery and a nickel-containing waste residue recovery process.
Background
With the increasing seriousness of the environment and resources in China, higher requirements on solid waste treatment in China are put forward, for example, nickel-containing solid waste exists, the nickel-containing solid waste can directly or indirectly harm the health of people, and the waste of resources is caused by burying and discarding, so that great attention is paid to various circles because the treatment of the solid waste which affects the environment and the resources simultaneously.
For nickel-containing solid waste, nickel-containing waste batteries and other nickel-containing waste residues are more frequently found, the difficulty of the current treatment lies in how to remove other metal elements, such as copper, iron, magnesium and the like, and in the patent publication with the patent application number of CN201710579921.1, the background art thereof refers to two other metal treatment methods which are currently used: in order to solve the problem that the two modes of treating precipitated magnesium and extracting and separating nickel by sodium fluoride have good and bad advantages and magnesium ion removal is difficult to reach the target content, the patent application provides a nickel sulfate product with the purity of more than 99.8 percent by treating the nickel in an adsorption-desorption mode by using a chelating resin exchange column. The method has the characteristics of high recovery rate and high product purity, but the price of the chelating resin exchange column is higher, and the treatment scale is difficult to enlarge.
Disclosure of Invention
The invention aims to provide a nickel-containing waste battery and a nickel-containing waste residue recovery process, and aims to solve the technical problems of high treatment cost and difficult treatment scale amplification in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a nickel-containing waste battery and nickel-containing waste residue recovery process comprises two major steps of nickel carbonate preparation and nickel carbonate retreatment;
the preparation of the nickel carbonate comprises the following steps:
removing shells and caps of waste batteries containing nickel and calcium, soaking the waste batteries and the waste residues containing nickel and calcium in sulfuric acid until the solid residue extraction volume is unchanged, filtering and washing to obtain leachate and leaching residues, wherein the leachate is for later use, and the leaching residues are treated in a centralized manner;
oxidizing the leaching solution, adding sodium carbonate after oxidation to adjust the pH value of the system to 4-6, and filtering to obtain filtrate and iron-containing waste residues;
adding sodium thiosulfate into the iron-removed filtrate to generate copper-containing precipitate, and filtering to remove the copper-containing precipitate;
adding sodium fluoride into the decoppered filtrate to generate calcium fluoride and magnesium fluoride precipitates, and filtering to remove the precipitates;
adding soda ash into the obtained calcium and magnesium-removed filtrate for nickel precipitation treatment, washing for a plurality of times to obtain nickel carbonate, and reusing the water phase obtained in the nickel precipitation and washing processes for the impregnation treatment in the step (1);
the nickel carbonate reprocessing comprises the following steps:
dissolving nickel carbonate with dilute acid, and extracting nickel by using a P204 extractant;
dissolving the solid nickel obtained from the extraction phase with dilute acid, adding sodium hydroxide to adjust the pH value to 6-8, filtering to obtain copper-containing precipitate and filtrate, and further purifying the obtained filtrate to obtain a nickel-containing byproduct.
Preferably, the dilute acid used in the step a is dilute sulfuric acid, the filtrate obtained in the step b is added with soda to adjust the pH value of the system to 4-6, then the filtrate and the iron-containing waste residue are obtained by filtering, the obtained filtrate is continuously added with soda to adjust the pH value of the system until no precipitate is generated, nickel protoxide is obtained by filtering, drying and calcining, and washing and packaging are carried out, thus obtaining a nickel protoxide product; and b, adding sulfuric acid into the copper-containing precipitate to evaporate and crystallize to obtain a copper sulfate byproduct.
Preferably, the dilute acid used in the step a is dilute hydrochloric acid, and the filtrate obtained in the step b is evaporated and crystallized to obtain the nickel chloride product.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, solid slag containing nickel and calcium is introduced, calcium impurities are introduced, and in the magnesium removal process, the obtained precipitate is easier to filter and remove than pure magnesium impurities due to the introduction of calcium, and meanwhile, the removal rate of magnesium is greatly improved;
the method has the advantages that the nickel is precipitated through the soda ash, the obtained nickel carbonate solid is not nickel sulfate, and the influence of sodium ions on a nickel product is avoided;
the invention can further improve the impurity treatment amount and improve the product purity of nickel to more than 99.5 percent by a mode of generating the nickel carbonate for acid dissolution treatment;
according to the invention, different products can be obtained as required by preparing nickel carbonate and further processing on the basis of the nickel carbonate.
Drawings
FIG. 1 is a flow chart of nickel carbonate production.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention is further described below with reference to various embodiments, and the implementation manner of the present invention includes but is not limited to the following embodiments.
Example 1
As shown in fig. 1, the process for preparing nickel carbonate according to the present invention comprises the following steps:
removing shells and caps of waste batteries containing nickel and calcium, soaking the waste batteries and the waste residues containing nickel and calcium in sulfuric acid until the solid residue extraction volume is unchanged, filtering and washing to obtain leachate and leaching residues, wherein the leachate is for later use, and the leaching residues are treated in a centralized manner;
oxidizing the leaching solution, adding sodium carbonate after oxidation to adjust the pH value of the system to 4-6, and filtering to obtain filtrate and iron-containing waste residues;
adding sodium thiosulfate into the iron-removed filtrate to generate copper-containing precipitate, and filtering to remove the copper-containing precipitate;
adding sodium fluoride into the decoppered filtrate to generate calcium fluoride and magnesium fluoride precipitates, and filtering to remove the precipitates, wherein the precipitates are easy to filter, and the filtering time is 2 min;
adding soda ash into the obtained calcium and magnesium-removed filtrate for nickel precipitation treatment, washing for a plurality of times to obtain nickel carbonate, and reusing the water phase obtained in the nickel precipitation and washing processes for the impregnation treatment in the step (1).
Dissolving nickel carbonate in dilute sulfuric acid to obtain solution with magnesium content of 0.01%, and extracting nickel with P204 extractant; dissolving solid nickel obtained from the extraction phase by using dilute sulfuric acid, adding sodium hydroxide to adjust the pH value to 6-8, filtering to obtain copper-containing precipitate and filtrate, adding soda to the filtrate to adjust the pH value of a system to 4-6, filtering to obtain filtrate and iron-containing waste residues, continuously adding soda to the filtrate to adjust the pH value of the system until the precipitate is not generated, filtering, drying and calcining to obtain nickel protoxide, washing and packaging to obtain a nickel protoxide product with the purity of 99.9%; adding sulfuric acid into the copper-containing precipitate, evaporating and crystallizing to obtain a copper sulfate byproduct with the purity of 98%.
Example 2
Dissolving nickel carbonate in dilute hydrochloric acid in the nickel carbonate obtained in the example 1, wherein the magnesium content in the solution is 0.01%, and extracting nickel by using a P204 extractant after dissolving; dissolving solid nickel obtained from the extraction phase by using dilute hydrochloric acid, adding sodium hydroxide to adjust the pH value to 6-8, filtering to obtain copper-containing precipitate and filtrate, and evaporating and crystallizing the obtained filtrate to obtain a nickel chloride product with the purity of 99.2%; adding sulfuric acid into the copper-containing precipitate, and evaporating and crystallizing to obtain a copper sulfate byproduct with the purity of 95%.
Example 3
On the basis of the embodiment 1, the waste residue containing nickel and calcium is not added, the precipitate generated in the step (4) is difficult to filter, the filtering time is as long as 30min, and the precipitate has high viscosity; finally, dissolving nickel carbonate by using dilute sulfuric acid, wherein the magnesium content in the solution is 0.05%, and extracting nickel by using a P204 extracting agent after dissolving; dissolving solid nickel obtained from the extraction phase by using dilute sulfuric acid, adding sodium hydroxide to adjust the pH value to 6-8, filtering to obtain copper-containing precipitate and filtrate, adding soda to the filtrate to adjust the pH value of a system to 4-6, filtering to obtain filtrate and iron-containing waste residues, continuously adding soda to the filtrate to adjust the pH value of the system until the precipitate is not generated, filtering, drying and calcining to obtain nickel protoxide, washing and packaging to obtain a nickel protoxide product with the purity of 99.3%; adding sulfuric acid into the copper-containing precipitate, evaporating and crystallizing to obtain a copper sulfate byproduct with the purity of 98%.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (3)
1. A nickel-containing waste battery and nickel-containing waste residue recovery process is characterized by comprising two steps of preparing nickel carbonate and retreating the nickel carbonate;
the preparation of the nickel carbonate comprises the following steps:
removing shells and caps of waste batteries containing nickel and calcium, soaking the waste batteries and the waste residues containing nickel and calcium in sulfuric acid until the solid residue extraction volume is unchanged, filtering and washing to obtain leachate and leaching residues, wherein the leachate is for later use, and the leaching residues are treated in a centralized manner;
oxidizing the leaching solution, adding sodium carbonate after oxidation to adjust the pH value of the system to 4-6, and filtering to obtain filtrate and iron-containing waste residues;
adding sodium thiosulfate into the iron-removed filtrate to generate copper-containing precipitate, and filtering to remove the copper-containing precipitate;
adding sodium fluoride into the decoppered filtrate to generate calcium fluoride and magnesium fluoride precipitates, and filtering to remove the precipitates;
adding soda ash into the obtained calcium and magnesium-removed filtrate for nickel precipitation treatment, washing for a plurality of times to obtain nickel carbonate, and reusing the water phase obtained in the nickel precipitation and washing processes for the impregnation treatment in the step (1);
the nickel carbonate reprocessing comprises the following steps:
dissolving nickel carbonate with dilute acid, and extracting nickel by using a P204 extractant;
dissolving the solid nickel obtained from the extraction phase with dilute acid, adding sodium hydroxide to adjust the pH value to 6-8, filtering to obtain copper-containing precipitate and filtrate, and further purifying the obtained filtrate to obtain a nickel-containing byproduct.
2. The nickel-containing waste battery and nickel-containing waste residue recovery process of claim 1, wherein the dilute acid used in the step a is dilute sulfuric acid, the filtrate obtained in the step b is added with soda to adjust the pH value of the system to 4-6, then the filtrate and the iron-containing waste residue are obtained by filtering, the filtrate is continuously added with soda to adjust the pH value of the system until no precipitation is generated, nickel protoxide is obtained by filtering, drying and calcining, and the nickel protoxide product is obtained by washing and packaging; and b, adding sulfuric acid into the copper-containing precipitate to evaporate and crystallize to obtain a copper sulfate byproduct.
3. The process of claim 1, wherein the dilute acid used in step a is dilute hydrochloric acid, and the filtrate obtained in step b is evaporated and crystallized to obtain nickel chloride product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110188703.1A CN112981114A (en) | 2021-02-18 | 2021-02-18 | Nickel-containing waste battery and nickel-containing waste residue recovery process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110188703.1A CN112981114A (en) | 2021-02-18 | 2021-02-18 | Nickel-containing waste battery and nickel-containing waste residue recovery process |
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| CN112981114A true CN112981114A (en) | 2021-06-18 |
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| CN202110188703.1A Pending CN112981114A (en) | 2021-02-18 | 2021-02-18 | Nickel-containing waste battery and nickel-containing waste residue recovery process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112744852A (en) * | 2021-02-18 | 2021-05-04 | 甘肃万众环保科技有限公司 | Waste carbon silica brick recovery process |
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2021
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Application publication date: 20210618 |