CN109234525B - low-cost leaching method of heterogenite - Google Patents
low-cost leaching method of heterogenite Download PDFInfo
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- CN109234525B CN109234525B CN201811368282.5A CN201811368282A CN109234525B CN 109234525 B CN109234525 B CN 109234525B CN 201811368282 A CN201811368282 A CN 201811368282A CN 109234525 B CN109234525 B CN 109234525B
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other 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
- 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
- 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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Abstract
the invention discloses a low-cost leaching method of heterogenite, which comprises the following leaching steps: s1, primary leaching and liquid-solid separation; the water cobalt ore which is sieved and absorbs certain moisture by the ceramic filter is slurried and then enters a first-stage leaching process, the leached ore pulp is washed by secondary filter pressing, the filtrate enters a second-stage leaching process, and the filter cake enters a third-stage leaching process; conveying the first-stage leachate to a first-stage copper extraction process for copper extraction; s2, secondary leaching and liquid-solid separation; the three-section concentrated underflow and the primary filtrate of the first-section thickener underflow enter a second-section leaching tank for reduction leaching, the leached ore pulp is subjected to liquid-solid separation by a thickener, the filtrate is subjected to fine filtration and is sent to a second-section copper extraction process, and the underflow enters a slag washing process; returning part of the second-stage raffinate to the second-stage leaching process, and sending the other part of the second-stage raffinate to the third-stage leaching process; and S3, three-stage leaching and liquid-solid separation. The leaching of high-valence cobalt in the heterogenite reduces the addition of an auxiliary reducing agent, relieves the pressure of a subsequent deironing process after reaction, and reduces the oxidation of Fe2+The consumption of the oxidant reduces the post-treatment cost.
Description
Technical Field
The invention relates to the technical field of cobalt hydrometallurgy, in particular to a low-cost leaching method of a cobaltite.
Background
cobalt is an important strategic metal, and elemental cobalt and compounds of cobalt thereof are widely applied, and especially, the demand in the field of lithium batteries is gradually increased.
however, the cobalt resource in China is poor and is mostly associated ore, more than 90% of the cobalt resource depends on African import and comprises hydrocobalt ore, cobalt-nickel sulfide ore, copper-cobalt alloy, crude cobalt hydroxide, cobalt carbonate and the like, wherein the hydrocobalt ore is the main form of the imported cobalt raw material in China. The mineral phase of the water cobalt mineral is complex, the embedding is fine, the cobalt content is generally 1.5-20%, and the water cobalt mineral contains copper, nickel, manganese, zinc, iron, aluminum, calcium, magnesium and the like.
At present, the cobaltous mine in China is mainly subjected to main processes such as reduction acid leaching to obtain a cobalt-rich solution, and then is subjected to purification, impurity removal, extraction, evaporative crystallization, electrolysis and other processes to obtain cobalt salt or metal cobalt. Hydrocobaltite belongs to oxidized ore, wherein cobalt mainly exists in the form of trivalent cobalt and has strong oxidizing property.
The existing process for treating cobaltous ore mainly adopts sodium sulfite and sodium pyrosulfiteSulfur-containing materials such as sulfur dioxide and the like are used as reducing agents. Sulfur dioxide gas is generated in the reaction process. The main problems with the reaction are: firstly, in the extraction process, the working environment of technicians is poor; secondly, the health threat to the technicians is great; thirdly, the cobalt solution after reduction leaching needs to be added with oxidant to oxidize Fe in the iron removal process2+The production cost is high; fourth, the production process is contaminated.
Disclosure of Invention
the invention aims to provide a low-cost leaching method of heterogenite, and aims to solve the technical problems that the extraction process has great threat to the health of technicians, the extraction cost is high, the post-treatment difficulty of the extracted leachate is high, and the pollution in the production process is strong in the process of extracting valuable metals from heterogenite at the present stage.
In order to achieve the purpose, the invention adopts the following technical scheme: a low-cost leaching method of heterogenite comprises the following specific leaching steps:
S1, primary leaching and liquid-solid separation;
the water cobalt ore which is sieved and absorbs certain moisture by the ceramic filter is slurried and then enters a first-stage leaching process, the leached ore pulp is washed by a second-stage filter pressing process, the filtrate enters a second-stage leaching process, and the filter cake enters a third-stage leaching process;
conveying the first-stage leachate to a first-stage copper extraction process for copper extraction;
S2, secondary leaching and liquid-solid separation;
the three-section concentrated underflow and the primary filtrate of the first-section thickener underflow enter a second-section leaching tank for reduction leaching, the leached ore pulp is subjected to liquid-solid separation by a thickener, the filtrate is subjected to fine filtration and is sent to a second-section copper extraction process, and the underflow enters a slag washing process;
Returning part of the second-stage raffinate to the second-stage leaching process, and sending the other part of the second-stage raffinate to the third-stage leaching process;
S3, three-stage leaching and liquid-solid separation;
the three-stage leaching is to react the first-stage underflow with the second-stage raffinate; (not only is a deironing process, but also is a leaching process) three-stage leaching is carried out, then liquid-solid separation is carried out, the underflow of the thickener enters the second stage leaching, and the overflow fine filtering is carried out to the deironing process.
Further, the cobalt-water mineral aggregate in S1 contains impurity iron element; the molar ratio of cobalt to iron is =10:1 to 1: 2. Further, the granularity of the cobaltous mineral aggregate in S1 is larger than 90% after passing through a 100-mesh sieve, the leaching control pH is 1.5-2.0, the liquid-solid ratio is 3: 1-6: 1, the reaction time is 2-5h, the reaction temperature is 30-60 ℃, and the stirring is carried out at 500-.
Further, ore pulp after the first-stage leaching in the S1 needs to be washed by secondary filter pressing, so that the copper content of the mineral aggregate entering the third-stage leaching is reduced.
Further, the reducing agent used in the reduction leaching in S2 is one or more of sulfur dioxide, sodium metabisulfite and sodium sulfite.
further, the pH value of the reduction leaching reaction in S2 is controlled to be 1.5-2.5, the liquid-solid ratio is 3: 1-5: 1, the reaction time is 2-4h, the reaction temperature is 40-70 ℃, and the stirring is 200-500 r/min.
Further, controlling leaching filtrate Fe in S22+＞8g/L。
Further, the mineral aggregate used for leaching in the S3 is a filter cake obtained by filter pressing and washing the bottom flow of a first-stage thickener; the Cu content of the filter cake is less than 0.4 percent.
Further, the pH value of the leaching solution in the S3 is controlled to be 1.5-2.5, the liquid-solid ratio is 3: 1-6: 1, the reaction time is 2-5h, the reaction temperature is 40-85 ℃, and the stirring is 200-500 r/min.
Further, controlling leaching filtrate Fe in S32+＞0.5g/L。
The invention has the beneficial effects that:
compared with other methods for leaching the heterogenite, the method for leaching the heterogenite mainly utilizes Fe generated in the leaching process of the heterogenite2+The cobalt is used as a reducing agent, high-valence cobalt in the heterogenite is leached, and the addition amount of an auxiliary reducing agent is reduced. Meanwhile, after the reaction is finished, oxidized Fe3+The hydrated FeOOH precipitates in the slag, thereby reducing the pressure of the subsequent iron removal process and reducing the oxidation of Fe2+The consumption of the oxidant reduces the cost of the post-treatment.
2, the low-cost leaching method of the heterogenite provided by the invention has the advantages of simple extraction process and strong operability, and more importantly, provides a better working environment for technical personnel in the extraction process.
3, the low-cost leaching method of the heterogenite provided by the invention reduces the consumption of auxiliary materials such as an oxidant, a reducing agent and the like in the whole leaching process, thereby reducing the environmental pollution caused by the use of the auxiliary materials.
additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The primary objects and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and illustrating the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
As shown in fig. 1, the invention provides a low-cost leaching method of valuable metals of hydrocobaltite, which comprises the following specific leaching steps:
S1, primary leaching and liquid-solid separation;
The water cobalt ore which is sieved and absorbs certain moisture by the ceramic filter is slurried and then enters a first-stage leaching process, the leached ore pulp is washed by a second-stage filter pressing process, the filtrate enters a second-stage leaching process, and the filter cake enters a third-stage leaching process; and conveying the first-stage leachate to a first-stage copper extraction process for copper extraction.
Wherein, the cobaltous mineral aggregate in the S1 contains impurity iron element; the molar ratio of cobalt to iron is =10:1 to 1: 2. Further, the granularity of the cobaltous mineral aggregate in S1 is larger than 90% after passing through a 100-mesh sieve, the leaching control pH is 1.5-2.0, the liquid-solid ratio is 3: 1-6: 1, the reaction time is 2-5h, the reaction temperature is 30-60 ℃, and the stirring is carried out at 500-.
And ore pulp after the first-stage leaching is washed by secondary filter pressing so as to reduce the copper content of the mineral aggregate entering the third-stage leaching.
S2, secondary leaching and liquid-solid separation;
The three-section concentrated underflow and the primary filtrate of the first-section thickener underflow enter a second-section leaching tank for reduction leaching, the leached ore pulp is subjected to liquid-solid separation by a thickener, the filtrate is subjected to fine filtration and is sent to a second-section copper extraction process, and the underflow enters a slag washing process; one part of the second-stage raffinate is returned to the second-stage leaching, and the other part of the second-stage raffinate is sent to the third-stage leaching process.
Wherein, the reducing agent used in the reduction leaching in the S2 is one or more of sulfur dioxide, sodium metabisulfite and sodium sulfite. The pH value of the reduction leaching reaction is controlled to be 1.5-2.5, the liquid-solid ratio is 3: 1-5: 1, the reaction time is 2-4h, the reaction temperature is 40-70 ℃, and the stirring is 200-. Controlled leaching of filtrate Fe2+＞8g/L。
S3, three-stage leaching and liquid-solid separation;
Three stage leaching is carried out by reacting first stage underflow with second stage raffinate.
the main characteristics are that: by Fe in two-stage raffinate2+reducing high-valence cobalt in the first-stage dense underflow slag by using a reducing agent, and reducing the high-valence cobalt in the slag into Co2+into solution. Essentially redox metathesis of oxides and salts,
The reaction principle is as follows:
Co2O3 + 2FeSO4 +H2O == 2CoSO4 + 2FeOOH
From the above equation, it can be seen that: the first-stage dense underflow slag and the second-stage raffinate are adopted for reaction, so that neither acid nor alkali is consumed. The method is not only an iron removal process, but also a leaching process, and can reduce the consumption of auxiliary materials such as acid, alkali, oxidant and the like.
And (4) carrying out liquid-solid separation after the third-stage leaching, feeding underflow of a thickener into the second-stage leaching, and carrying out overflow fine filtration to a deironing process.
The main chemical reaction equations generated in the process of the invention are as follows:
first-stage leaching: MeO + H2SO4＝MeSO4＋H2O (Me: Cu, Co, Ni, Fe, etc.)
Secondary leaching: fe3++e=Fe2+
Three-stage leaching: co2O3 + 2FeSO4 +H2O == 2CoSO4 + 2FeOOH
Wherein, the mineral aggregate used for leaching in the S3 is a filter cake obtained by filter pressing and washing the bottom flow of a first-stage thickener; the Cu content of the filter cake is less than 0.4 percent. The pH value of the leaching solution in S3 is controlled to be 1.5-2.5, the liquid-solid ratio is 3: 1-6: 1, the reaction time is 2-5h, the reaction temperature is 40-85 ℃, and the stirring is 200-. Controlling leaching filtrate Fe in S32+＞0.5g/L。
Examples 1 and 2
Table 1 shows the composition details of the hydrocobaltite in examples 1 and 2
Table 2 examples 1, 2 the respective reaction stages
according to the process indexes of the table 2, the three-stage leachate obtained after the system is stabilized in the example 1 has lower contents of Co28g/L, Cu0.2g/L, Ni0.3g/L and Fe0.6g/L, impurities of Cu, Fe and the like, and is suitable for subsequent iron and cobalt removal and extraction processes.
The three-stage leachate obtained after the system is stabilized in the embodiment 2 has lower contents of Co22g/L, Cu0.2g/L, Ni0.4g/L, Fe0.7g/L, impurities of Cu, Fe and the like, and is suitable for subsequent iron and cobalt removal and extraction processes.
TABLE 3 valuable Metal Leaching Rate details of examples 1 and 2
From the above table 2 and table 3, it can be seen that the leaching method provided by the invention has the advantages of high leaching efficiency, good effect and short time.
In conclusion, the low-cost leaching method for the heterogenite provided by the invention overcomes the defects of the cobalt extraction process at the present stage, and provides a new method for extracting valuable metals from the heterogenite, which is simple to operate, low in cost, strong in practicability and environment-friendly. The method provides a good working environment for technicians, ensures the high-efficiency extraction of the metal, has good market value and can realize large-scale production.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that may be made by those skilled in the art within the technical scope of the present invention will be covered by the scope of the present invention.
Claims (7)
1. A low-cost leaching method of heterogenite is characterized in that: the specific leaching steps are as follows:
S1, primary leaching and liquid-solid separation;
the water cobalt ore which is sieved and absorbs certain moisture by the ceramic filter is slurried and then enters a first-stage leaching process, the leached ore pulp is washed by a second-stage filter pressing process, the filtrate enters a second-stage leaching process, and the filter cake enters a third-stage leaching process;
Conveying the first-stage leachate to a first-stage copper extraction process for copper extraction;
S2, secondary leaching and liquid-solid separation;
the three-section concentrated underflow and the primary filtrate of the first-section thickener underflow enter a second-section leaching tank for reduction leaching, the leached ore pulp is subjected to liquid-solid separation by a thickener, the filtrate is subjected to fine filtration and is sent to a second-section copper extraction process, and the underflow enters a slag washing process;
Wherein, the reducing agent used in the reduction leaching in the S2 is one or more of sulfur dioxide, sodium metabisulfite and sodium sulfite; controlling the reaction pH value of reduction leaching to be 1.5-2.5, controlling the liquid-solid ratio to be 3: 1-5: 1, controlling the reaction time to be 2-4h, controlling the reaction temperature to be 40-70 ℃, and stirring for 200-; controlled leaching of filtrate Fe2+＞8g/L；
Returning part of the second-stage raffinate to the second-stage leaching process, and sending the other part of the second-stage raffinate to the third-stage leaching process;
S3, three-stage leaching and liquid-solid separation;
The three-stage leaching is to react the first-stage underflow with the second-stage raffinate;
And (4) carrying out liquid-solid separation after the third-stage leaching, feeding underflow of a thickener into the second-stage leaching, and carrying out overflow fine filtration to a deironing process.
2. The low-cost leaching method of the cobaltite according to claim 1, wherein the cobaltite material in S1 contains impurity iron element; the molar ratio of cobalt to iron is =10:1 to 1: 2.
3. The low-cost leaching method of the cobaltite as claimed in claim 1, wherein the granularity of the cobaltite material in S1 is larger than 90% through a 100-mesh sieve, the leaching control pH is 1.5-2.0, the liquid-solid ratio is 3: 1-6: 1, the reaction time is 2-5h, the reaction temperature is 30-60 ℃, and the stirring is 200-500 r/min.
4. the method for leaching the heterogenite as claimed in claim 1, wherein the ore pulp after the first-stage leaching in the S1 is washed by two-stage pressure filtration so as to reduce the copper content of the ore material entering the third-stage leaching.
5. The low-cost leaching method of the heterogenite as claimed in claim 1, wherein the mineral aggregate used in the leaching in the S3 is a filter cake obtained by filter pressing and washing of a bottom flow of a first-stage thickener; the Cu content of the filter cake is less than 0.4 percent.
6. The low-cost leaching method of the heterogenite as claimed in claim 1, wherein the pH value of the leaching in the S3 is controlled to be 1.5-2.5, the liquid-solid ratio is 3: 1-6: 1, the reaction time is 2-5h, the reaction temperature is 40-85 ℃, and the stirring is 200-.
7. The method for low-cost leaching of hydrocobaltite according to claim 1, wherein the control of the leaching filtrate Fe in S32+＞0.5g/L。
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| CN111534686A (en) * | 2020-05-27 | 2020-08-14 | 浙江工贸职业技术学院 | Iron removal equipment and iron removal method for nickel cobalt raffinate |
| CN112359225A (en) * | 2020-11-12 | 2021-02-12 | 格林美（江苏）钴业股份有限公司 | Selective leaching process of rough cobalt hydroxide ore |
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| CA2767034A1 (en) * | 2009-08-07 | 2011-02-10 | Metaleach Limited | Method for leaching cobalt from oxidised cobalt ores |
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Application publication date: 20190118 Assignee: INSTITUTE OF NEW MATERIALS & INDUSTRIAL TECHNOLOGY, WENZHOU University Assignor: Wenzhou University Contract record no.: X2020330000099 Denomination of invention: A low cost leaching method for cobalt ore Granted publication date: 20191217 License type: Common License Record date: 20201115 |
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