CN109234525A - A kind of inexpensive leaching method of heterogenite - Google Patents
A kind of inexpensive leaching method of heterogenite Download PDFInfo
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- CN109234525A CN109234525A CN201811368282.5A CN201811368282A CN109234525A CN 109234525 A CN109234525 A CN 109234525A CN 201811368282 A CN201811368282 A CN 201811368282A CN 109234525 A CN109234525 A CN 109234525A
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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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- 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
- C22B3/20—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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- 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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Abstract
The invention discloses a kind of inexpensive leaching method of heterogenite, leaching step is as follows: S1, one section of leaching and solid-liquor separation；It is sieved after heterogenite slurry after ceramic filter absorbs certain moisture and enters one section of leaching, ore pulp after second level pressure filtration washing, leach into two sections by filtrate after leaching, and filter cake is into three stages acid leach；One section of leachate is delivered to one section of copper extraction process extraction copper；S2, two sections of leachings and solid-liquor separation；Three sections of thickened underflows and one section of thickener underflow first-time filtrate leach ore pulp after concentrator solid-liquor separation, filtrate refined filtration is sent to two sections of copper extraction process, and underflow enters washery slag process into two sections of leaching tanks progress reducing leachings；Two sections of raffinate a part return to two sections of leachings, and a part is sent to three stages acid leach process；S3, three stages acid leach and solid-liquor separation.High price cobalt in heterogenite leaches, and reduces the additive amount of auxiliary material reducing agent, after reaction, alleviates subsequent iron removal step pressure, reduce Oxidation of Fe2+Oxidant consumption, reduce post processing cost.
Description
Technical field
The present invention relates to the technical field of wet metallurgy of cobalt, the inexpensive leaching method of especially a kind of heterogenite.
Background technique
Cobalt is a kind of important strategy metal, and the compound of simple substance cobalt and its cobalt is widely used, and is especially led in lithium battery
The demand in domain is gradually increased.
But China's cobalt resource is poor, mostly associated minerals, and 90% or more cobalt resource relies on African import, including heterogenite, cobalt
Ni sulphide mine, copper-cobalt alloy, crude cobalt hydroxide and cobalt carbonate etc., wherein heterogenite is the main shape of China's import cobalt raw material
Formula.Heterogenite mine is mutually complicated, and embedding cloth is fine, and the range of amount containing cobalt is generally 1.5-20%, at the same cupric, nickel, manganese, zinc, iron, aluminium,
Calcium, magnesium etc..
It obtains currently, domestic heterogenite mainly passes through the prevailing technologies such as reduction acidleach rich in cobalt liquor, then is removed by purification
The processes such as miscellaneous, extraction, evaporative crystallization, electrolysis obtain cobalt salt or metallic cobalt.Heterogenite belongs to oxide ore, and cobalt therein is mainly with three
The form of valence cobalt exists, and shows strong oxidizing property.
Current technology handles heterogenite, mainly using sulfide containing materials conducts such as sodium sulfite, sodium pyrosulfite, sulfur dioxide
Reducing agent.Sulfur dioxide gas is generated in reaction process.Reacting existing main problem is: first, in extraction process, and technology people
The working environment of member is poor；Second, it is big to the health threat of technical staff；Third, the cobalt liquor by reducing leaching are removing iron
Need to add oxidizing Fe in process again2+, production cost is big；4th, production process has pollution.
Summary of the invention
The object of the present invention is to provide a kind of inexpensive leaching method of heterogenite, to solve to mention from heterogenite at this stage
Take it is existing during valuable metal extraction process is big to technical staff's health threat, extraction cost is high, extract leachate after
Manage that difficulty is big, the strong technical problem of production process pollution.
To achieve the above object, the present invention adopts the following technical scheme: a kind of inexpensive leaching method of heterogenite, specifically
Leaching step is as follows:
S1, one section of leaching and solid-liquor separation；
It is sieved after the heterogenite slurry after ceramic filter absorbs certain moisture into one section of leaching, ore pulp is through two after leaching
After grade pressure filtration washing, wherein filtrate is leached into two sections, and filter cake is into three stages acid leach；
One section of leachate is delivered to one section of copper extraction process extraction copper；
S2, two sections of leachings and solid-liquor separation；
Three sections of thickened underflows and one section of thickener underflow first-time filtrate leach ore pulp through dense into two sections of leaching tanks progress reducing leachings
After close machine solid-liquor separation, filtrate refined filtration is sent to two sections of copper extraction process, and underflow enters washery slag process；
Two sections of raffinate a part return to two sections of leachings, and a part is sent to three stages acid leach process；
S3, three stages acid leach and solid-liquor separation；
Three stages acid leach is with one section of underflow and two sections of raffinate reactions；(being both an iron removal and a leaching process)
Solid-liquor separation is carried out after three stages acid leach, thickener underflow enters two sections and leaches, to iron removal step after overflow refined filtration.
Further, contain impurity ferro element in S1 in heterogenite material；The molar ratio of cobalt and iron is=10:1~1:2.Into one
It walks, the granularity of heterogenite material is sieved with 100 mesh sieve greater than 90% in S1, leaches control pH1.5-2.0, and liquid-solid ratio is 3:1~6:1, reaction
Time 2-5h, stirs 200-500r/min by 30-60 DEG C of reaction temperature.
Further, ore pulp need to be contained through second level pressure filtration washing with being lowered into the mineral aggregate of three stages acid leach after one section of leaching in S1
Amount of copper.
Further, the reducing agent that reducing leaching uses in S2 is one of sulfur dioxide, sodium pyrosulfite, sodium sulfite
Or it is several.
Further, in 1.5-2.5, liquid-solid ratio is 3:1~5:1, reaction time for the pH value in reaction control of reducing leaching in S2
2-4h, stirs 200-500r/min by 40-70 DEG C of reaction temperature.
Further, filtrate Fe is leached in control in S22+> 8g/L.
Further, it is filter cake of one section of thickener underflow after pressure filtration washing that the mineral aggregate used is leached in S3；The filter cake
Its contained Cu < 0.4%.
Further, control pH1.5-2.5 is leached in S3, liquid-solid ratio is 3:1~6:1, reaction time 2-5h, reaction temperature
40-85 DEG C, stir 200-500r/min.
Further, filtrate Fe is leached in control in S32+> 0.5g/L.
The beneficial effects of the present invention are embodied in:
1, a kind of inexpensive leaching method of heterogenite provided by the invention provides compared with the method that other heterogenites leach
Leaching method mainly utilize the Fe generated in heterogenite itself leaching process2+For reducing agent, the high price cobalt in heterogenite is soaked
Out, reduce the additive amount of auxiliary material reducing agent.Meanwhile after the reaction was completed, the Fe after oxidation3+It is precipitated in the form of being hydrated FeOOH
In slag, subsequent iron removal step pressure is alleviated, Oxidation of Fe is reduced2+Oxidant consumption, reduce the cost of post-processing.
2, a kind of inexpensive leaching method of heterogenite provided by the invention, extraction process is simple, strong operability more
It is important that providing preferable working environment to technical staff in extraction process.
3, a kind of inexpensive leaching method of heterogenite provided by the invention is aoxidized due to reducing in entire leaching process
The supplementary product onsumptions such as agent and reducing agent, to reduce auxiliary material use process bring environmental pollution.
Other features and advantages of the present invention will be illustrated in the following description, and partly becomes from specification
It is clear that understand through the implementation of the invention.The main object of the present invention and further advantage can be by specifications, power
Specifically noted scheme is achieved and obtained in sharp claim.
Detailed description of the invention
The present invention will be further described in detail with reference to the accompanying drawing.
Fig. 1 is present invention process flow diagram.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is only exemplary,
It is only capable of for explanation and illustration technical solution of the present invention, and the limitation to technical solution of the present invention cannot be construed to.
As shown in Figure 1, specific leaching step is such as the present invention provides the inexpensive leaching method of the valuable metal of heterogenite
Under:
S1, one section of leaching and solid-liquor separation；
It is sieved after the heterogenite slurry after ceramic filter absorbs certain moisture into one section of leaching, ore pulp is through two after leaching
After grade pressure filtration washing, wherein filtrate is leached into two sections, and filter cake is into three stages acid leach；One section of leachate is delivered to one section of copper extraction work
Sequence extracts copper.
Wherein, contain impurity ferro element in S1 in heterogenite material；The molar ratio of cobalt and iron is=10:1~1:2.Further,
The granularity of heterogenite material is sieved with 100 mesh sieve greater than 90% in S1, leaches control pH1.5-2.0, and liquid-solid ratio is 3:1~6:1, when reaction
Between 2-5h, 30-60 DEG C of reaction temperature, stir 200-500r/min.
Ore pulp need to be through second level pressure filtration washing, to be lowered into the mineral aggregate copper content of three stages acid leach after one section of leaching.
S2, two sections of leachings and solid-liquor separation；
Three sections of thickened underflows and one section of thickener underflow first-time filtrate leach ore pulp through dense into two sections of leaching tanks progress reducing leachings
After close machine solid-liquor separation, filtrate refined filtration is sent to two sections of copper extraction process, and underflow enters washery slag process；Two sections of raffinate a part are returned
Two sections of leachings are returned, a part is sent to three stages acid leach process.
Wherein, the reducing agent that reducing leaching uses in S2 be one of sulfur dioxide, sodium pyrosulfite, sodium sulfite or
Person is several.In 1.5-2.5, liquid-solid ratio is 3:1~5:1, reaction time 2-4h, reaction temperature for the pH value in reaction control of reducing leaching
40-70 DEG C, stir 200-500r/min.Filtrate Fe is leached in control2+> 8g/L.
S3, three stages acid leach and solid-liquor separation；
Three stages acid leach is with one section of underflow and two sections of raffinate reactions.
It is mainly characterized by: with Fe in two sections of raffinates2+The high price cobalt in one section of thickened underflow slag is restored for reducing agent, in slag
High price cobalt is reduced to Co2+And enter solution.The substantially redox metathesis reaction of oxide and salt,
Its reaction principle are as follows:
Co2O3 + 2FeSO4 +H2O == 2CoSO4 + 2FeOOH
From the above reaction equation it can be seen that neither consumption is sour using one section of thickened underflow slag and two sections of raffinate reactions, also do not consume
Alkali.It is both an iron removal and a leaching process, the consumption of the auxiliary materials such as acid, alkali, oxidant can be reduced.
Solid-liquor separation is carried out after three stages acid leach, thickener underflow enters two sections and leaches, to iron removal step after overflow refined filtration.
The main chemical reactions equation occurred during present invention process are as follows:
One section of leaching: MeO+H2SO4=MeSO4+ H2O(Me:Cu, Co, Ni, Fe etc.)
Two sections of leachings: Fe3++e=Fe2+
Three stages acid leach: Co2O3 + 2FeSO4 +H2O == 2CoSO4 + 2FeOOH
Wherein, it is filter cake of one section of thickener underflow after pressure filtration washing that the mineral aggregate used is leached in S3；The filter cake is contained by it
Cu < 0.4%.In S3 leach control pH1.5-2.5, liquid-solid ratio be 3:1~6:1, reaction time 2-5h, 40-85 DEG C of reaction temperature,
Stir 200-500r/min.Filtrate Fe is leached in control in S32+> 0.5g/L.
Embodiment 1 and embodiment 2
Table 1 is embodiment 1, the ingredient detail of 2 heterogenites
2 embodiment 1 of table, 2 each conversion zones
Mineral aggregate presses the technic index of upper table 2, gained three stages acid leach liquid Co28g/L, Cu0.2g/L after system is stablized in embodiment 1,
Ni0.3g/L, Fe0.6g/L, impurity Cu, Fe equal size is lower, is suitble to subsequent except iron and cobalt extraction process.
Gained three stages acid leach liquid Co22g/L, Cu0.2g/L, Ni0.4g/L, Fe0.7g/L after system is stablized in embodiment 2,
Impurity Cu, Fe equal size is lower, is suitble to subsequent except iron and cobalt extraction process.
The valuable metal leaching rate detail of 3 Examples 1 and 2 of table
By upper table 2, table 3 it can be seen that leaching method provided by the invention, leaching efficiency is high, and effect is good, and the time is short.
In conclusion a kind of inexpensive leaching method of heterogenite provided by the invention, the cobalt overcome at this stage is extracted
The deficiency of technique provides and extracts the new of valuable metal in easy to operate, inexpensive, practical, environmental-friendly heterogenite
Method.The high efficiency extraction that ensure that metal while providing good working environment to technical staff, the market price having had
Value is, it can be achieved that large-scale production.
The foregoing is merely the preferable specific embodiments of the present invention, but scope of protection of the present invention is not limited thereto,
The change or replacement that anyone skilled in the art is expected in the technical scope disclosed by the present invention should all be contained
Lid is within protection scope of the present invention.
Claims (10)
1. a kind of inexpensive leaching method of heterogenite, it is characterised in that: specific leaching step is as follows:
S1, one section of leaching and solid-liquor separation；
It is sieved after the heterogenite slurry after ceramic filter absorbs certain moisture into one section of leaching, ore pulp is through two after leaching
After grade pressure filtration washing, wherein filtrate is leached into two sections, and filter cake is into three stages acid leach；
One section of leachate is delivered to one section of copper extraction process extraction copper；
S2, two sections of leachings and solid-liquor separation；
Three sections of thickened underflows and one section of thickener underflow first-time filtrate leach ore pulp through dense into two sections of leaching tanks progress reducing leachings
After close machine solid-liquor separation, filtrate refined filtration is sent to two sections of copper extraction process, and underflow enters washery slag process；
Two sections of raffinate a part return to two sections of leachings, and a part is sent to three stages acid leach process；
S3, three stages acid leach and solid-liquor separation；
Three stages acid leach is with one section of underflow and two sections of raffinate reactions；
Solid-liquor separation is carried out after three stages acid leach, thickener underflow enters two sections and leaches, to iron removal step after overflow refined filtration.
2. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that containing miscellaneous in heterogenite material in S1
Matter ferro element；The molar ratio of cobalt and iron is=10:1~1:2.
3. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that the granularity mistake of heterogenite material in S1
100 meshes are greater than 90%, leach control pH1.5-2.0, and liquid-solid ratio is 3:1~6:1, reaction time 2-5h, reaction temperature 30-60
DEG C, stir 200-500r/min.
4. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that ore pulp needs after one section of leaching in S1
Through second level pressure filtration washing, to be lowered into the mineral aggregate copper content of three stages acid leach.
5. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that reducing leaching used in S2 goes back
Former agent is one of sulfur dioxide, sodium pyrosulfite, sodium sulfite or several.
6. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that the reaction pH of reducing leaching in S2
In 1.5-2.5, liquid-solid ratio is 3:1~5:1, reaction time 2-4h for value control, 40-70 DEG C of reaction temperature, stirs 200-500r/
min。
7. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that filtrate Fe is leached in control in S22+
> 8g/L.
8. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that leaching the mineral aggregate used in S3 is
Filter cake of one section of thickener underflow after pressure filtration washing；Its contained Cu < 0.4% of the filter cake.
9. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that leach control pH1.5- in S3
2.5, liquid-solid ratio is 3:1~6:1, reaction time 2-5h, 40-85 DEG C of reaction temperature, stirs 200-500r/min.
10. the inexpensive leaching method of heterogenite as described in claim 1, which is characterized in that filtrate Fe is leached in control in S32+
> 0.5g/L.
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Cited By (5)
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|---|---|---|---|---|
| CN110699557A (en) * | 2019-10-23 | 2020-01-17 | 金川集团股份有限公司 | Low-cost treatment device and method for nickel hydroxide cobalt slag |
| 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 |
| CN114318002A (en) * | 2021-12-31 | 2022-04-12 | 中国瑞林工程技术股份有限公司 | Pre-acidification displacement dewatering system before leaching |
| CN115652105A (en) * | 2022-11-18 | 2023-01-31 | 金川集团股份有限公司 | Sectional leaching process for cobalt raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114318002A (en) * | 2021-12-31 | 2022-04-12 | 中国瑞林工程技术股份有限公司 | Pre-acidification displacement dewatering system before leaching |
| CN115652105A (en) * | 2022-11-18 | 2023-01-31 | 金川集团股份有限公司 | Sectional leaching process for cobalt raw material |
| CN115652105B (en) * | 2022-11-18 | 2023-12-19 | 金川集团股份有限公司 | Sectional leaching process for cobalt raw material |
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