CN115232967A - Method for re-leaching nickel hydroxide waste residue with sulfuric acid - Google Patents
Method for re-leaching nickel hydroxide waste residue with sulfuric acid Download PDFInfo
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- CN115232967A CN115232967A CN202210615904.XA CN202210615904A CN115232967A CN 115232967 A CN115232967 A CN 115232967A CN 202210615904 A CN202210615904 A CN 202210615904A CN 115232967 A CN115232967 A CN 115232967A
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- nickel hydroxide
- waste residue
- hydroxide waste
- sulfuric acid
- 30min
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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
- 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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- 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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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for re-leaching nickel hydroxide waste residue sulfuric acid, which comprises the following steps: 1) Pulping the nickel hydroxide waste residue, namely pulping the nickel hydroxide waste residue in a pulping kettle by mixing tap water and the nickel hydroxide waste residue according to the mass ratio of (0.5-1): 1, pulping for 30min after mixing, and keeping the stirring frequency of a motor at 30-35 Hz; 2) Leaching nickel hydroxide waste residues: introducing the slurried nickel hydroxide waste residue into a reaction kettle, adding concentrated sulfuric acid to adjust the pH value of the slurried nickel hydroxide waste residue material to be 0.5-1, reacting for 20-30 min, introducing strong reducing agent gas, wherein the mass ratio of the introduced gas to the nickel hydroxide waste residue is (1-5): 1000, reacting for 30min; 3) And (4) solid-liquid separation. The invention aims to recover nickel and cobalt metals in nickel hydroxide waste residue and overcome the technical problem that the nickel hydroxide waste residue is difficult to leach.
Description
Technical Field
The invention relates to the technical field of nonferrous metal hydrometallurgy, in particular to a method for re-leaching nickel hydroxide waste residue sulfuric acid.
Background
In recent years, with the development of the battery industry, the nickel sulfate industry has developed new opportunities. At present, the production method of nickel sulfate with simple process and low cost is realized by deeply purifying nickel hydroxide leachate and then producing battery-grade nickel sulfate through evaporation and crystallization. After nickel hydroxide is leached, a large amount of waste residues are generated, and the waste residues contain low nickel and cobalt and have high difficulty in recovering nickel-cobalt metals, so that the waste residues are in a blank state for a long time in the process of leaching and recovering nickel-cobalt metals.
Disclosure of Invention
Aiming at the technical problem, the invention provides a method for re-leaching nickel hydroxide waste residue sulfuric acid.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for re-leaching nickel hydroxide waste residue sulfuric acid comprises the following steps:
1) Pulping the nickel hydroxide waste residue, namely pulping the nickel hydroxide waste residue in a pulping kettle by mixing tap water with the nickel hydroxide waste residue according to the mass ratio of (0.5-1): 1, pulping for 30min after mixing, and keeping the stirring frequency of a motor at 30-35 Hz;
2) Leaching nickel hydroxide waste residues: introducing the slurried nickel hydroxide waste residue into a reaction kettle, adding concentrated sulfuric acid to adjust the pH value of the slurried nickel hydroxide waste residue material to be 0.5-1, reacting for 20-30 min, introducing strong reducing agent gas, wherein the mass ratio of the introduced gas to the nickel hydroxide waste residue is (1-5): 1000, reacting for 30min;
3) Solid-liquid separation: after the reaction is finished, standing the materials for more than 30min, then enabling the supernatant to enter a supernatant kettle in a siphoning mode, further carrying out solid-liquid separation, and repeating the steps in the reaction kettle.
In the step 2), concentrated sulfuric acid is added to adjust the pH value of the slurried nickel hydroxide waste residue material to be 0.5-1, and the reaction time is 30min.
Wherein, in the step 2), the strong reducing agent gas is sulfur dioxide gas.
Wherein, in the step 3), the solid-to-liquid ratio in the reaction kettle is required to be kept between 35 and 50 percent when the siphon is opened. .
The invention has the beneficial effects that: the method adopts tap water to pulp the nickel hydroxide waste residue, the pulp is formed into a nickel hydroxide waste residue pulp liquid, and the sulfur dioxide gas is introduced into the pulp liquid after the pulp liquid is leached by concentrated sulfuric acid. The sulfur dioxide and the manganese dioxide in the nickel hydroxide waste residue are subjected to oxidation reduction reaction, so that a small part of nickel-cobalt metal in the manganese dioxide is dissolved, and the purpose of recovering the nickel-cobalt metal in the nickel hydroxide waste residue is achieved. The invention adopts a supernatant siphon mode, which is beneficial to the solid-liquid separation of the leaching solution of the nickel hydroxide waste residue.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Example 1
In a slurrying kettle, 0.6m is added 3 Pulping 1t of nickel hydroxide waste residue by using tap water, conveying the pulped nickel hydroxide waste residue material into a reaction kettle through a chemical pump after 30min, keeping stirring in a rotating state in the reaction kettle, keeping the stirring frequency of a motor at 30Hz, introducing concentrated sulfuric acid to adjust the pH value of the material in the pulping kettle to be 0.5, introducing 1kg of sulfur dioxide gas, reacting for 30min to obtain a nickel hydroxide waste residue solution, stopping stirring, standing the obtained leachate in the reaction kettle for more than 30min, starting siphoning, allowing the leachate after siphoning to enter a supernatant kettle, performing solid-liquid separation, and finally producing the nickel hydroxide waste residue solutionLeaching solution of nickel hydroxide waste residue. The concentration of nickel in the leaching solution is 24.3g/L, and the concentration of cobalt in the leaching solution is 14.47g/L. The leaching rates of nickel and cobalt in the nickel hydroxide waste residue respectively reach 92.86 percent and 89.03 percent,
example 2
In a slurrying kettle, 0.7m is added 3 1t of nickel hydroxide waste residue is pulped by tap water, after 30min, the pulped nickel hydroxide waste residue material is conveyed into a reaction kettle through a chemical pump, the reaction kettle is kept in a stirring state, the stirring frequency of a motor is kept at 35Hz, concentrated sulfuric acid is introduced to adjust the pH value of the material in the pulping kettle to be 0.6, then 2kg of sulfur dioxide gas is introduced, after 30min of reaction, a nickel hydroxide waste residue solution is obtained, the stirring is stopped, the obtained leaching solution is kept static in the reaction kettle for more than 30min, siphoning is started, the leaching solution enters a supernatant kettle after siphoning, solid-liquid separation is carried out, and finally the nickel hydroxide waste residue leaching solution is produced. The concentration of nickel in the leaching solution is 21.25g/L, and the concentration of cobalt in the leaching solution is 7.58g/L. The leaching rates of nickel and cobalt in the nickel hydroxide waste residue respectively reach 94.95 percent and 83.56 percent.
Example 3
In a slurrying kettle, 0.8m is added 3 1t of nickel hydroxide waste residue is pulped by tap water, after 30min, the pulped nickel hydroxide waste residue material is conveyed into a reaction kettle through a chemical pump, the reaction kettle is kept in a stirring state, the stirring frequency of a motor is kept at 32Hz, concentrated sulfuric acid is introduced to adjust the pH value of the material in the pulping kettle to be 0.7, then 3kg of sulfur dioxide gas is introduced, after 30min of reaction, a nickel hydroxide waste residue solution is obtained, the stirring is stopped, the obtained leaching solution is kept static in the reaction kettle for more than 30min, siphoning is started, the leaching solution enters a supernatant kettle after siphoning, solid-liquid separation is carried out, and finally the nickel hydroxide waste residue leaching solution is produced. The concentration of nickel in the leaching solution is 22.26g/L, and the concentration of cobalt in the leaching solution is 9.02g/L. Waste residue of nickel hydroxideThe leaching rates of nickel and cobalt in the nickel and cobalt alloy respectively reach 93.86 percent and 85.92 percent.
Example 4
In a slurrying kettle, 0.9m is added 3 1t of nickel hydroxide waste residue is pulped by tap water, after 30min, the pulped nickel hydroxide waste residue material is conveyed into a reaction kettle through a chemical pump, the reaction kettle is kept in a stirring state, the stirring frequency of a motor is kept at 33Hz, concentrated sulfuric acid is introduced to adjust the pH value of the material in the pulping kettle to be 0.8, then 4kg of sulfur dioxide gas is introduced, after 30min of reaction, a nickel hydroxide waste residue solution is obtained, the stirring is stopped, the obtained leaching solution is kept static in the reaction kettle for more than 30min, siphoning is started, the leaching solution enters a supernatant kettle after siphoning, solid-liquid separation is carried out, and finally the nickel hydroxide waste residue leaching solution is produced. The concentration of nickel in the leaching solution is 13.25g/L, and the concentration of cobalt in the leaching solution is 5.44g/L. The leaching rates of nickel and cobalt in the nickel hydroxide waste residue reach 93.29 percent and 86.91 percent respectively.
Example 5
In a slurrying kettle, 1.0m is added 3 1t of nickel hydroxide waste residue is pulped by tap water, after 30min, the pulped nickel hydroxide waste residue material is conveyed into a reaction kettle through a chemical pump, the reaction kettle is kept in a stirring rotating state, the stirring frequency of a motor is kept at 34Hz, concentrated sulfuric acid is introduced to adjust the pH value of the material in the pulping kettle to be 1, then 5kg of sulfur dioxide gas is introduced, after 30min of reaction, a nickel hydroxide waste residue solution is obtained, the stirring is stopped, the obtained leaching solution is kept still in the reaction kettle for more than 30min, siphoning is started, the leaching solution after siphoning enters a supernatant kettle, solid-liquid separation is carried out, and finally the nickel hydroxide waste residue leaching solution is produced. The concentration of nickel in the leaching solution is 21.04g/L, and the concentration of cobalt in the leaching solution is 15.15g/L. The leaching rates of nickel and cobalt in the nickel hydroxide waste residue are respectively 95.93% and 90.94%.
Example 6
In a slurrying kettle, 0.5m is added 3 1t of nickel hydroxide waste residue is pulped by tap water, after 30min, the pulped nickel hydroxide waste residue material is conveyed into a reaction kettle through a chemical pump, the reaction kettle is kept in a stirring state, the stirring frequency of a motor is kept at 30Hz, concentrated sulfuric acid is introduced to adjust the pH value of the material in the pulping kettle to be 0.5, then 1kg of sulfur dioxide gas is introduced, after 30min of reaction, a nickel hydroxide waste residue solution is obtained, the stirring is stopped, the obtained leaching solution is kept static in the reaction kettle for more than 30min, siphoning is started, the leaching solution enters a supernatant kettle after siphoning, solid-liquid separation is carried out, and finally the nickel hydroxide waste residue leaching solution is produced. The concentration of nickel in the leaching solution is 24.3g/L, and the concentration of cobalt in the leaching solution is 14.47g/L. The leaching rates of nickel and cobalt in the nickel hydroxide waste residue respectively reach 92.86 percent and 89.03 percent.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (4)
1. A method for re-leaching nickel hydroxide waste residue sulfuric acid is characterized by comprising the following steps:
1) Pulping the nickel hydroxide waste residue, namely pulping the nickel hydroxide waste residue in a pulping kettle by mixing tap water and the nickel hydroxide waste residue according to the mass ratio of (0.5-1): 1, pulping for 30min after mixing, and keeping the stirring frequency of a motor at 30-35 Hz;
2) Leaching nickel hydroxide waste residues: introducing the slurried nickel hydroxide waste residue into a reaction kettle, adding concentrated sulfuric acid to adjust the pH value of the slurried nickel hydroxide waste residue material to be 0.5-1, reacting for 20-30 min, introducing strong reducing agent gas, wherein the mass ratio of the introduced gas to the nickel hydroxide waste residue is (1-5): 1000, reacting for 30min;
3) Solid-liquid separation: after the reaction is finished, standing the materials for more than 30min, then enabling the supernatant to enter a supernatant kettle in a siphoning mode, further carrying out solid-liquid separation, and repeating the steps in the reaction kettle.
2. The method for releaching the nickel hydroxide waste residue with sulfuric acid as claimed in claim 1, wherein in the step 2), concentrated sulfuric acid is added to adjust the pH value of the slurried nickel hydroxide waste residue material to 0.5-1, and the reaction time is 30min.
3. The method for releaching the nickel hydroxide waste sulfuric acid as recited in claim 1, wherein in the step 2), the strong reducing agent gas is sulfur dioxide gas.
4. The method for resubmerging nickel hydroxide waste sulfuric acid as claimed in claim 1, wherein in the step 3), the solid-to-liquid ratio in the reaction kettle is maintained at 35-50% when siphon is opened.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210615904.XA CN115232967A (en) | 2022-06-01 | 2022-06-01 | Method for re-leaching nickel hydroxide waste residue with sulfuric acid |
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| CN202210615904.XA CN115232967A (en) | 2022-06-01 | 2022-06-01 | Method for re-leaching nickel hydroxide waste residue with sulfuric acid |
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| CN115232967A true CN115232967A (en) | 2022-10-25 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000203848A (en) * | 1999-01-08 | 2000-07-25 | Sumitomo Metal Mining Co Ltd | Production of low-chlorine nickel cobalt sulfate solution |
| CN106566933A (en) * | 2016-11-01 | 2017-04-19 | 金川集团股份有限公司 | Method for reducing content of cobalt in mixed slag generated in nickel sulfate production |
| CN110423898A (en) * | 2019-08-27 | 2019-11-08 | 中国恩菲工程技术有限公司 | Desilication method in lateritic nickel ore leaching process |
| CN111910075A (en) * | 2020-08-12 | 2020-11-10 | 矿冶科技集团有限公司 | Method for leaching nickel and cobalt from rough nickel and cobalt hydroxide in two stages |
| CN112159897A (en) * | 2020-09-09 | 2021-01-01 | 广东邦普循环科技有限公司 | Method for purifying nickel-cobalt-manganese leaching solution |
| CN112553478A (en) * | 2020-12-02 | 2021-03-26 | 金川集团镍盐有限公司 | Method for quickly leaching nickel hydroxide cobalt sulfuric acid system |
-
2022
- 2022-06-01 CN CN202210615904.XA patent/CN115232967A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000203848A (en) * | 1999-01-08 | 2000-07-25 | Sumitomo Metal Mining Co Ltd | Production of low-chlorine nickel cobalt sulfate solution |
| CN106566933A (en) * | 2016-11-01 | 2017-04-19 | 金川集团股份有限公司 | Method for reducing content of cobalt in mixed slag generated in nickel sulfate production |
| CN110423898A (en) * | 2019-08-27 | 2019-11-08 | 中国恩菲工程技术有限公司 | Desilication method in lateritic nickel ore leaching process |
| CN111910075A (en) * | 2020-08-12 | 2020-11-10 | 矿冶科技集团有限公司 | Method for leaching nickel and cobalt from rough nickel and cobalt hydroxide in two stages |
| CN112159897A (en) * | 2020-09-09 | 2021-01-01 | 广东邦普循环科技有限公司 | Method for purifying nickel-cobalt-manganese leaching solution |
| CN112553478A (en) * | 2020-12-02 | 2021-03-26 | 金川集团镍盐有限公司 | Method for quickly leaching nickel hydroxide cobalt sulfuric acid system |
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Application publication date: 20221025 |