CN109628738A - A kind of method of the sulfuric acid Selectively leaching of ferronickel concentrate - Google Patents
A kind of method of the sulfuric acid Selectively leaching of ferronickel concentrate Download PDFInfo
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- CN109628738A CN109628738A CN201910139495.9A CN201910139495A CN109628738A CN 109628738 A CN109628738 A CN 109628738A CN 201910139495 A CN201910139495 A CN 201910139495A CN 109628738 A CN109628738 A CN 109628738A
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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
- 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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Abstract
The invention belongs to ferronickel concentrate technical field of wet metallurgy, the method for especially relating to a kind of sulfuric acid Selectively leaching of ferronickel concentrate, including leaching, hydrolyzing except iron, magnetic separation, its leaching process includes that hydrogen peroxide is added to be leached as leaching agent, both the leaching rate of nickel, cobalt had been improved, sulfuric acid acid consumption is reduced, and for sequential hydrolysis except iron creates advantage；Furthermore, hydrolysis of the present invention also using new ferronickel concentrate as leachate removes iron material, react away acid extra in leachate, so that most ferric ion hydrolysis is generated ferric hydroxide precipitate, nickel, cobalt is separated with iron, to realize the Selectively leaching of nickel, cobalt and iron, nickel, cobalt leaching rate are greater than 99%, compared to single vitriol lixiviation, nickel, cobalt leaching rate improve 15% or more, and sulfuric acid acid consumption reduces by 30~50%.
Description
Technical field
The invention belongs to ferronickel concentrate technical field of wet metallurgy, especially relate to a kind of sulfuric acid selection of ferronickel concentrate
Property leach method.
Background technique
The current prevailing technology of laterite pyrometallurgical smelting process is rotary kiln-mineral hot furnace technique (i.e. RKEF technique), is suitble to place
The reason higher ore of grade (generally requires nickel grade to be greater than 1.8%, mass ratio < 12 Fe/Ni).Wet extraction process is mainly suitable for
Low-grade nickel-containing limonite type ore is handled, general nickel content is lower (containing Ni 1% or so), and iron content is higher (generally higher than
40%), content of magnesium is lower (general MgO 5% or so).As high-grade laterite ore resources gradually decrease, low-grade laterite
Exploitation it is more more and more urgent, have both at home and abroad a large amount of nickeliferous 1.0~1.5% laterite have it is to be developed, Low-cost it is red
Native mine extractive technique develops domestic and international low-grade laterite, has preferable economic effect for improving nickel resources recovery utilization rate
Benefit and social benefit.
Compared with traditional pyrometallurgical smelting process, laterite reduction roasting magnetic separation process is with process flow is short, low energy consumption
Advantage, the technique have become the following lateritic nickel ore efficiently, one of the developing direction of low-cost processes, be now subjected to great pass
Note and research.Application number 201610619690.8 discloses a kind of lateritic nickel ore method sodium reduction roasting separation method, especially
For high-speed rail high aluminum low nickel type lateritic nickel ore, nickeliferous 6~10% ferro-nickel product can be obtained, the rate of recovery of nickel is 80% or more；
CN101020957A discloses a kind of method of rotary hearth furnace rapid reduction of carbonaceous lateritic nickel ore pelletizing enriching nickel；CN101413055A
Disclose a kind of technique that ferronickel powder is directly produced by lateritic nickel ore.
The above patent all uses lateritic nickel ore reduction roasting-magnetic separation process, and the ferronickel concentrate which obtains generally contains Ni
4~10%, contain Co 0.1~0.5%, contain Fe 45~80%, contain MgO 1~15%, contains SiO22~25%, contain CaO 0.1
~1%.It is mainly used in stainless steel production, nickel can only be used as low-end product in the process, and cobalt is not as nickel is into
Become rusty steel, causes the waste of cobalt resource.Each metal mainly exists in the form of dilval or simple substance in the ferronickel concentrate, using biography
The sulfuric acid leaching of system, nickel, cobalt leaching rate are low, and sulfuric acid consumption is big, at high cost, and poor selectivity, iron are also leached with nickel, cobalt
It is subsequent also to aoxidize into leachate, it neutralizes except iron is handled.
Therefore, a kind of simple process is researched and developed, efficiently, the leaching method of the strong ferronickel concentrate of selectivity, to reasonable benefit
With resources such as nickel, cobalt, iron in ferronickel concentrate, there is biggish promotion to the popularization and application of the reduction roasting magnetic separation process of laterite
Effect is of great significance to the development and utilization of a large amount of nickeliferous 1.0~1.5% low-grade laterite both at home and abroad.
Summary of the invention
In view of the problems of the existing technology the present invention, provides a kind of method of the sulfuric acid Selectively leaching of ferronickel concentrate,
This method is directed to lateritic nickel ore reduction roasting magnetic separation process ferronickel concentrate obtained, by adding leaching agent, is using it
When sulfuric acid makees leaching agent, under the conditions of atmospheric low-temperature realize efficiently, Rapid Leaching, be added in leachate new ferronickel concentrate into
Row hydrolysis removes iron, carries out magnetic separation after reaction, realizes efficiently separating for nickel, cobalt and iron.
In view of the above-mentioned problems, the present invention provides a kind of sulfuric acid Selectively leaching method of ferronickel concentrate, which is characterized in that should
Method includes:
(1) leaching process: leaching agent, ferronickel concentrate are uniformly mixed by 2:1~15:1 in mass ratio, preferably 3:1~8:1,
It is then slowly added into leaching agent, at 50~90 DEG C, preferably 60~80 DEG C, is leached 0.5~6 hour, preferably 1~3 hour；It leaches
Slurry is separated by solid-liquid separation, and leached mud and leachate, leached mud direct emission are obtained；(2) hydrolysis removes iron and magnetic separation process: solid by liquid
New ferronickel concentrate is added in leachate, and is slowly added to leaching agent by mass ratio 2:1~10:1, preferably 3:1~8:1,50
At~90 DEG C, preferably 60~80 DEG C, leach 0.5~6 hour, preferably 1~3 hour, control endpoint pH was 1.5~3, reaction knot
Magnetic separation is carried out after beam, magnetic concentrate, which returns, leaches process, and magnetic tailing is separated by filtration, and obtained slag is ferric hydroxide precipitate
Slag, solution are nickeliferous, cobalt leachate.
Wherein, it is preferred that step (1):
The leaching agent is sulfuric acid solution.
It is furthermore preferred that the sulfuric acid solution concentrated sulfuric acid and water 1:1~1:14 in mass ratio, preferably 1:2~1:7 preparation
It forms.
The leaching agent is hydrogenperoxide steam generator.
It is furthermore preferred that the mass concentration of the hydrogenperoxide steam generator is 10%~25%, preferably 15%~20%.
It is furthermore preferred that the mass ratio of the ferronickel concentrate and leaching agent is 2:1~5:1.
Wherein, step (1) leached mud main component is silica, direct emission.
Preferably, step (2):
The leaching agent is hydrogenperoxide steam generator.
It is furthermore preferred that the mass concentration of the hydrogenperoxide steam generator is 10%~25%, preferably 15%~20%.
It is furthermore preferred that the mass ratio of the leaching agent and the ferronickel concentrate being newly added is 1:5~1:10.
Preferably, the magnetic field strength of the magnetic separation is 500~2000Gs, preferably 800~1500Gs.
Wherein, new ferronickel concentrate and leaching agent solution is added in step (2), and the purpose of leaching is to react away extra acid,
Most ferric ion hydrolysis is set to generate precipitating.
Preferably, ferronickel concentrate of the present invention is the concentrate after the enrichment of laterite reduction roasting magnetic separation, wherein containing Ni 4
~10%, contain Co 0.1~0.5%, contain Fe 45~80%, contain MgO 1~15%, contains SiO22~25%, contain Al2O31~
3%, contain CaO 0.1~1%.It is furthermore preferred that the granularity of the ferronickel concentrate be content accounting less than 0.074mm be 80~
95%.
The invention has the following advantages:
(1) addition of leaching agent solution of the present invention has the effect of being significantly improved to the leaching of ferronickel concentrate, of the invention
Leaching agent has following features: 1) during sulfuric acid leaching, oxygen is the key factor for influencing nickel cobalt leaching velocity, hydrogen peroxide
Addition may insure that oxygen is fast and is evenly dispersed in ore pulp, guarantees the dissolved oxygen amount of ore pulp, so as to shorten extraction time, improves
Leaching effect；2) during traditional sulfuric acid leaching, the iron in leachate is ferrous ion, and subsequent iron removal also needs to be added
Oxidant is further by Fe2+It is oxidized to Fe3+, oxidants hydrogen peroxide that the present invention needs subsequent iron removal is creative
It is applied to the sulfuric acid leaching process of ferronickel concentrate, i.e., without increasing cost, and improves the leaching effect of nickel, cobalt；3) of the invention
Leaching agent cleaning, the environmental protection used, harmful components will not be left in leachate, are conducive to subsequent impurity removal process；
(2) hydrolysis of the present invention using new ferronickel concentrate as leachate removes iron material, and it is extra in leachate to react away
Acid, so that the hydrolysis of most ferric ion is generated ferric hydroxide precipitate, realize the Selectively leaching of nickel, cobalt and iron, nickel,
Cobalt enters solution, and iron becomes ferric hydroxide precipitate slag, so that nickel, cobalt be separated with iron；
(3) leaching rate of nickel, cobalt greatly improved in the method for the present invention, and nickel, cobalt leaching rate are greater than 99%, compared to single sulphur
Acidleach, nickel, cobalt leaching rate improve 15% or more, and sulfuric acid acid consumption reduces by 30~50%.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the process flow diagram of the embodiment of the present invention.
Specific embodiment
The present invention will be further described with reference to the examples below.Described embodiment and its result are merely to illustrate
The present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
(1) chemical component of ferronickel concentrate is as shown in table 1.
1 ferronickel concentrate chemical component (%) of table
| Element | Ni | Fe | Co | CaO | Al2O3 | SiO2 | MgO |
| Content | 6.24 | 65.40 | 0.34 | 0.27 | 1.27 | 12.20 | 8.36 |
(2) the 80mL concentrated sulfuric acid is measured, water is added, consolidating mass ratio by liquid is that 3:1 is added in 50g ferronickel concentrate, leaches temperature
Degree is 85 DEG C, and extraction time is 5 hours, after leaching, is separated by solid-liquid separation, and solution is nickeliferous, cobalt leachate, in assay solution
The content of nickel, cobalt, and the leaching rate of nickel, cobalt is calculated, wherein nickel leaching rate is 78.45%, and cobalt leaching rate is 76.39%, sulfuric acid
Dosage is 46.24t/tNi.
Embodiment 2
(1) chemical component of ferronickel concentrate is as shown in table 2.
2 ferronickel concentrate chemical component (%) of table
| Element | Ni | Fe | Co | CaO | Al2O3 | SiO2 | MgO |
| Content | 6.24 | 65.40 | 0.34 | 0.27 | 1.27 | 12.20 | 8.36 |
(2) the 50mL concentrated sulfuric acid is measured, water is added, consolidating mass ratio by liquid is that 3:1 is added in 50g ferronickel concentrate, is being stirred
Under the conditions of be slowly added to 80mL concentration be 15% hydrogenperoxide steam generator, extraction temperature be 60 DEG C, extraction time be 2 hours, leaching
It after out, is separated by solid-liquid separation, the direct outlet of leached mud, leachate continues hydrolysis except iron；New ferronickel essence is added into leachate
Mine 25g is slowly added to the hydrogenperoxide steam generator that 25mL concentration is 15%, and extraction temperature is 60 DEG C, and endpoint pH 2.0 leaches
Time is 3 hours；Then magnetic separation, magnetic concentrate return to leaching process, and magnetic tailing is separated by solid-liquid separation, and obtain ferric hydroxide precipitate
Slag, solution are nickeliferous, cobalt leachate, the content of nickel, cobalt in assay solution, and calculate the leaching rate of nickel, cobalt, and wherein nickel leaches
Rate is 99.37%, and cobalt leaching rate is 99.18%, sulfuric acid dosage 28.90t/tNi.
Embodiment 3
(1) chemical component of ferronickel concentrate is as shown in table 3.
3 ferronickel concentrate chemical component (%) of table
| Element | Ni | Fe | Co | CaO | Al2O3 | SiO2 | MgO |
| Content | 5.05 | 52.78 | 0.25 | 0.38 | 2.07 | 20.50 | 13.47 |
(2) the 45mL concentrated sulfuric acid is measured, water is added, consolidating mass ratio by liquid is that 4:1 is added in 50g ferronickel concentrate, is being stirred
Under the conditions of be slowly added to 100mL concentration be 10% hydrogenperoxide steam generator, extraction temperature be 85 DEG C, extraction time be 1 hour, leaching
It after out, is separated by solid-liquid separation, the direct outlet of leached mud, leachate continues hydrolysis except iron；New ferronickel essence is added into leachate
Mine 15g is slowly added to the hydrogenperoxide steam generator that 20mL concentration is 10%, and extraction temperature is 85 DEG C, and endpoint pH 1.5 leaches
Time is 4 hours；Then magnetic separation, magnetic concentrate return to leaching process, and magnetic tailing is separated by solid-liquid separation, and obtain ferric hydroxide precipitate
Slag, solution are nickeliferous, cobalt leachate, the content of nickel, cobalt in assay solution, and calculate the leaching rate of nickel, cobalt, and wherein nickel leaches
Rate is 99.24%, and cobalt leaching rate is 99.11%, sulfuric acid dosage 32.14t/tNi.
Embodiment 4
(1) chemical component of ferronickel concentrate is as shown in table 4.
4 ferronickel concentrate chemical component (%) of table
| Element | Ni | Fe | Co | CaO | Al2O3 | SiO2 | MgO |
| Content | 7.61 | 72.93 | 0.45 | 0.18 | 0.42 | 5.15 | 3.41 |
(2) the 70mL concentrated sulfuric acid is measured, water is added, consolidating mass ratio by liquid is that 8:1 is added in 50g ferronickel concentrate, is being stirred
Under the conditions of be slowly added to 60mL concentration be 25% hydrogenperoxide steam generator, extraction temperature be 70 DEG C, extraction time be 2 hours, leaching
It after out, is separated by solid-liquid separation, the direct outlet of leached mud, leachate continues hydrolysis except iron；New ferronickel essence is added into leachate
Mine 15g is slowly added to the hydrogenperoxide steam generator that 10mL concentration is 25%, and extraction temperature is 70 DEG C, and endpoint pH 1.5 leaches
Time is 2 hours, and then magnetic separation, magnetic concentrate returns to leaching process, and magnetic tailing is separated by solid-liquid separation, and obtains ferric hydroxide precipitate
Slag, solution are nickeliferous, cobalt leachate, the content of nickel, cobalt in assay solution, and calculate the leaching rate of nickel, cobalt, and wherein nickel leaches
Rate is 99.76%, and cobalt leaching rate is 99.32%, sulfuric acid dosage 33.17t/tNi.
Embodiment 5
(1) chemical component of ferronickel concentrate is as shown in table 5.
5 ferronickel concentrate chemical component (%) of table
| Element | Ni | Fe | Co | CaO | Al2O3 | SiO2 | MgO |
| Content | 4.18 | 46.23 | 0.16 | 0.68 | 2.67 | 23.85 | 14.74 |
(2) the 35mL concentrated sulfuric acid is measured, water is added, consolidating mass ratio by liquid is that 5:1 is added in 50g ferronickel concentrate, is being stirred
Under the conditions of be slowly added to 55mL concentration be 20% hydrogenperoxide steam generator, extraction temperature be 80 DEG C, extraction time be 4 hours, leaching
It after out, is separated by solid-liquid separation, the direct outlet of leached mud, leachate continues hydrolysis except iron；New ferronickel essence is added into leachate
Mine 20g is slowly added to the hydrogenperoxide steam generator that 10mL concentration is 20%, and extraction temperature is 80 DEG C, and endpoint pH 2.5 leaches
Time is 4 hours, and then magnetic separation, magnetic concentrate returns to leaching process, and magnetic tailing is separated by solid-liquid separation, and obtains ferric hydroxide precipitate
Slag, solution are nickeliferous, cobalt leachate, the content of nickel, cobalt in assay solution, and calculate the leaching rate of nickel, cobalt, and wherein nickel leaches
Rate is 99.28%, and cobalt leaching rate is 99.09%, sulfuric acid dosage 30.20t/tNi.
Above content is only to examples of the invention and explanation, affiliated those skilled in the art are to being retouched
Various modifications may be made or supplement for the specific embodiment stated, and without departing from design of the invention or surmounts the claims and is defined
Range, be within the scope of protection of the invention.
Claims (10)
1. a kind of method of the sulfuric acid Selectively leaching of ferronickel concentrate, which is characterized in that this method comprises:
(1) leaching process: leaching agent, ferronickel concentrate are uniformly mixed by 2:1~15:1 in mass ratio, preferably 3:1~8:1, then
It is slowly added to leaching agent, at 50~90 DEG C, preferably 60~80 DEG C, is leached 0.5~6 hour, preferably 1~3 hour；Leach slurry
It is separated by solid-liquid separation, obtains leached mud and leachate, leached mud direct emission；(2) hydrolysis removes iron and magnetic separation process: pressing liquid stereoplasm amount
Than 2:1~10:1, preferably 3:1~8:1, new ferronickel concentrate is added in leachate, and be slowly added to leaching agent, 50~90
At DEG C, preferably 60~80 DEG C, leach 0.5~6 hour, preferably 1~3 hour, control endpoint pH was 1.5~3, after reaction
Magnetic separation is carried out, magnetic concentrate, which returns, leaches process, and magnetic tailing is separated by filtration, and obtained slag is ferric hydroxide precipitate slag, molten
Liquid is nickeliferous, cobalt leachate.
2. the method according to claim 1, wherein leaching agent described in step (1) is sulfuric acid solution.
3. according to the method described in claim 2, it is characterized in that, the sulfuric acid solution concentrated sulfuric acid and water in mass ratio 1:
1~1:14, preferably 1:2~1:7 are formulated.
4. the method according to claim 1, wherein leaching agent described in step (1), (2) is that hydrogen peroxide is molten
Liquid.
5. according to the method described in claim 4, it is characterized in that, the mass concentration of the hydrogenperoxide steam generator be 10%~
25%, preferably 15%~20%.
6. the method according to claim 1, wherein the quality of ferronickel concentrate and leaching agent described in step (1)
Than for 2:1~5:1.
7. the method according to claim 1, wherein leaching agent described in step (2) and the ferronickel essence being newly added
The mass ratio of mine is 1:5~1:10.
8. the method according to claim 1, wherein the magnetic field strength of magnetic separation described in step (2) be 500~
2000Gs, preferably 800~1500Gs.
9. the method according to claim 1, wherein the ferronickel concentrate is that laterite reduction roasting magnetic separation is rich
Concentrate after collection contains Co 0.1~0.5% wherein containing Ni 4~10%, contains Fe 45~80%, contains MgO 1~15%, contains
SiO22~25%, contain Al2O31~3%, contain CaO 0.1~1%.
10. according to the method described in claim 9, it is characterized in that, the granularity of the ferronickel concentrate is less than 0.074mm's
Content accounting is 80~95%.
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Cited By (5)
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| CN112646976A (en) * | 2020-12-17 | 2021-04-13 | 矿冶科技集团有限公司 | Method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore and application |
| CN113355511A (en) * | 2021-06-01 | 2021-09-07 | 四川省有色矿冶科技有限公司 | Method for selectively reducing vanadium and titanium content in vanadium-titanium magnetite concentrate through ammonium-ammonia oxidation leaching system |
| WO2022140863A1 (en) * | 2021-01-04 | 2022-07-07 | Hatch Ltd. | Ferronickel alloy direct refining processes and processes for producing nickel sulfate or other nickel products |
| CN115652106A (en) * | 2022-12-22 | 2023-01-31 | 金川镍钴研究设计院有限责任公司 | Method for selectively leaching nickel from ferronickel |
| WO2024055510A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Method for preparing lithium iron phosphate from nickel-rion alloy and use thereof |
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| CN112646976A (en) * | 2020-12-17 | 2021-04-13 | 矿冶科技集团有限公司 | Method for synergistically leaching nickel, cobalt and manganese by utilizing waste lithium ion battery black powder and nickel cobalt sulfide ore and application |
| WO2022140863A1 (en) * | 2021-01-04 | 2022-07-07 | Hatch Ltd. | Ferronickel alloy direct refining processes and processes for producing nickel sulfate or other nickel products |
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| CN113355511A (en) * | 2021-06-01 | 2021-09-07 | 四川省有色矿冶科技有限公司 | Method for selectively reducing vanadium and titanium content in vanadium-titanium magnetite concentrate through ammonium-ammonia oxidation leaching system |
| CN113355511B (en) * | 2021-06-01 | 2022-04-05 | 四川省有色矿冶科技有限公司 | Method for selectively reducing vanadium and titanium content in vanadium-titanium magnetite concentrate through ammonium-ammonia oxidation leaching system |
| WO2024055510A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Method for preparing lithium iron phosphate from nickel-rion alloy and use thereof |
| CN115652106A (en) * | 2022-12-22 | 2023-01-31 | 金川镍钴研究设计院有限责任公司 | Method for selectively leaching nickel from ferronickel |
| CN115652106B (en) * | 2022-12-22 | 2024-03-05 | 金川镍钴研究设计院有限责任公司 | Method for selectively leaching nickel from ferronickel |
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Application publication date: 20190416 |