CN112708780A - Method for removing aluminum from nickel-cobalt solution - Google Patents
Method for removing aluminum from nickel-cobalt solution Download PDFInfo
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- CN112708780A CN112708780A CN202011449616.9A CN202011449616A CN112708780A CN 112708780 A CN112708780 A CN 112708780A CN 202011449616 A CN202011449616 A CN 202011449616A CN 112708780 A CN112708780 A CN 112708780A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 68
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 65
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 94
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 101
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052759 nickel Inorganic materials 0.000 abstract description 13
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000002184 metal Substances 0.000 abstract description 12
- 229910017052 cobalt Inorganic materials 0.000 abstract description 7
- 239000010941 cobalt Substances 0.000 abstract description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 7
- 238000002386 leaching Methods 0.000 abstract description 7
- 238000000746 purification Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012266 salt solution Substances 0.000 abstract description 2
- 239000002893 slag Substances 0.000 description 16
- 238000001914 filtration Methods 0.000 description 14
- 230000001965 increasing effect Effects 0.000 description 10
- HIMLGVIQSDVUJQ-UHFFFAOYSA-N aluminum vanadium Chemical compound [Al].[V] HIMLGVIQSDVUJQ-UHFFFAOYSA-N 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910020630 Co Ni Inorganic materials 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011152 fibreglass Substances 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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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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- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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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- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
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Abstract
A method for removing aluminum from a nickel-cobalt solution. Relates to the purification of Ni and Co metal salt solution, in particular to a method for removing aluminum by purifying leaching solution in the process of producing nickel and cobalt by a wet method. The method is characterized in that the aluminum removing process sequentially comprises the following steps: (1) the pH value of the liquid control solution before aluminum removal is 2-2.5, and stirring reaction is carried out; (2) controlling the pH value of 0 to be 2.5-3.0 after the reaction, and stirring for reaction; (3) controlling the pH value to be 3.5-3.5 after the reaction, and stirring for reaction; (4) controlling the pH value to be 4.5-4.5 after the reaction, and stirring for reaction; (5) controlling the pH value to be 3.3-3.5 after the reaction, and stirring for reaction; (6) and (4) carrying out liquid-solid separation after the reaction. The method of the invention effectively solves the problem that the solution is extremely difficult to filter, has low reaction temperature and low energy consumption, can realize deep aluminum removal, has wide process adaptability, and can still realize deep aluminum removal when the aluminum content in the solution reaches more than 6 g/L.
Description
Technical Field
A method for removing aluminum from a nickel-cobalt solution. Relates to the purification of Ni and Co metal salt solution, in particular to a method for purifying Ni and Co metal salt leaching solution to remove aluminum in the process of producing nickel and cobalt by a wet method.
Background
In the process of producing nickel and cobalt by a wet method, a leaching method is usually adopted to obtain a Ni and Co metal salt leaching solution. Because the content of Al in the earth crust is third but next to oxygen and silicon, the Al often exists in Co, Ni, and other ores in the form of impurities, the Al enters into the solution along with valuable metals during leaching, when the valuable metal products are recovered from the leaching solution, corresponding purification treatment is required, the content of Al is generally controlled to be 0.1-0.01g/L, and the removal of Al is an important process for producing nickel and cobalt by hydrometallurgy.
At present, the aluminum removal method for Ni and Co metal salt leaching solution is as follows: adding pH regulator into the solution to adjust pH of the solution to 3.5-4.5 to obtain Al (OH)3Then filtered, since Al (OH)3The solution is jelly and is very difficult to filter, the temperature for removing aluminum is generally controlled to be more than 80 ℃ for improving the filtering performance of the solution after aluminum removal, the main reaction time is generally 85 ℃, the reaction temperature is high, the energy consumption is large, deep aluminum removal is difficult to achieve, and the solution after aluminum removal is difficult to filter.
Disclosure of Invention
The invention aims to provide a method for removing aluminum from a nickel-cobalt solution, which can effectively reduce the operation difficulty, reduce the cobalt, nickel and other valuable metals contained in slag, improve the filtering performance of the solution and realize deep purification aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme.
A method for removing aluminum from a nickel-cobalt solution is characterized in that the aluminum removing process sequentially comprises the following steps:
(1) the pH value of the liquid control solution before aluminum removal is 2.0-2.5, and stirring reaction is carried out;
(2) controlling the pH value of the reacted liquid in the step (1) to be 2.5-3.0, and stirring for reaction;
(3) controlling the pH value of the reacted liquid in the step (2) to be 3.5-3.5, and stirring for reaction;
(4) controlling the pH value of the reacted liquid in the step (3) to be 4.5-4.5, and stirring for reaction;
(5) controlling the pH value of the reacted liquid in the step (4) to be 3.3-3.5, and stirring for reaction;
(6) and (5) carrying out liquid-solid separation on the reaction product obtained in the step (5).
The method for removing aluminum from the nickel-cobalt solution is characterized in that Na is added in the step (1)2CO3The pH value of the solution is controlled to be 2.0-2.5.
The method for removing aluminum from the nickel-cobalt solution is characterized in that the step (2) is to add Na2CO3The pH value of the solution is controlled to be 2.5-3.0.
The method for removing aluminum from the nickel-cobalt solution is characterized in that the step (3) is to add Na2CO3The pH value of the solution is controlled to be 3.0-3.5.
The method for removing aluminum from the nickel-cobalt solution is characterized in that the step (4) is to add Na2CO3The pH value of the solution is controlled to be 4.0-4.5.
The method for removing aluminum from the nickel-cobalt solution is characterized in that H is added in the step (5)2SO4The pH value of the solution is controlled to be 3.3-3.5.
The method for removing aluminum from the nickel-cobalt solution is characterized in that the reaction temperature is controlled to be 50-60 ℃, and the reaction time is 40 minutes to 2 hours.
The method for removing aluminum from the nickel-cobalt solution is characterized in that the reaction temperature is controlled by heating in a steam introducing mode.
The method for removing aluminum from the nickel-cobalt solution is characterized in that stirring is carried out in the reaction process of aluminum removal, and the stirring speed is 50-350 r/min.
The invention relates to a method for removing aluminum from a nickel-cobalt solution, which is characterized in that the solution in the reaction process of the aluminum removal process is added in a spraying or dispersing mode and falls into the reaction liquid surface in a dropping mode.
The method for removing aluminum from the nickel-cobalt solution is characterized in that the solution obtained after the reaction in the step (5) with the volume ratio of 10% is taken and returned to the step (1) to be used as seed crystal.
The invention relates to a method for removing aluminum from a nickel-cobalt solution, which adopts Na2CO3Adjusting the pH value of the solution, Na2CO3High dissolving speed, weak alkalinity and easily controlled pH value, and simultaneously introduces Na + ions into the reaction solution to improve the content of aluminum vanadium (Na)2(Al6(SO4)4(OH)I2) The yield of the crystal is large, the aluminum vanadium has large molecular weight, the crystal is easy to grow up, the performance is stable, and the crystal is insoluble. Na (Na)2CO3When the additive is added, the additive adopts a dispersing mode in a drop form, prevents the generation of local over-alkali phenomenon and Al (OH)3Formation of Al (OH)3Is a colloidal solid and is extremely difficult to filter.
The process of the present invention, since steps (1) to (3) Al3+High concentration, excessive increase of pH value, generally 0-0.5, and drastic change of local pH value, such as Al (OH)3The production amount is increased, and the difficulty of solution filtration is increased.
The method of the invention, as a further proposal, the reaction temperature of the solution is controlled between 50 ℃ and 60 ℃, and the heating adopts direct steam heating; the steam heating water vapor is changed into water, the volume of the reaction solution is increased, the concentration of main reactants and impurities is reduced, the operation difficulty can be reduced, the cobalt and nickel content of the slag is reduced, and the filtering performance of the solution is improved.
As a further scheme, the volume of the treated liquid in the No. 5 reaction tank is about 10%, the treated liquid is conveyed to the No. 1 reaction tank through a transfer pump and used as a seed crystal, the reaction speed is improved, the grain diameter of filter residue is improved, and the filtering speed of the treated liquid is improved.
The method for removing aluminum from the nickel-cobalt solution has the beneficial effects that Na is adopted2CO3Adding Na + ion in the solution as pH regulator, inducing with seed crystal, controlling pH, and making the filter residue mainly contain aluminum vanadium (Na)2(Al6(SO4)4(OH)I2) Large Al-V crystal grain, very low solubility, fast filtering speed of the liquid after removing Al, and no pollution3+Neutralization and hydrolysis to Al (OH)3Colloid and solution are difficult to filter. The reaction temperature is controlled between 50 ℃ and 60 DEG CThe reaction temperature is low, and the energy consumption is low; steam is adopted for heating, and water vapor is condensed into water to enter the solution, so that the volume of the solution is increased, and the operation difficulty can be reduced; the content of liquid aluminum after aluminum removal reaches 0.01g/L, and deep aluminum removal can be realized. The method has wide process adaptability, and can still realize deep aluminum removal when the aluminum content in the solution reaches more than 6 g/L.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention;
FIG. 2 is a process equipment flow diagram of the process of the present invention.
Wherein, 1 is a No. 1 reaction tank; 2 is a liquid spraying pipe before aluminum removal; 3 is Na2CO3A shower pipe; 4 is a 2# reaction tank; 5 is a No. 3 reaction tank; 6 is a No. 4 reaction tank; 7 is a No. 5 reaction tank; 8 is H2SO4A shower pipe; 9 is a middle groove; 10 is a liquid transfer pump; 11 is a filter press; 12 is a steam pipeline; 13 is a flow guiding system.
Detailed Description
A method for removing aluminum from nickel-cobalt solution comprises removing aluminum by five-stage continuous method, adding aluminum-removing precursor solution into No. 1 reaction tank, starting stirring paddle, adding steam, controlling reaction temperature at 50-60 deg.C, and adding Na2CO3Controlling pH value to be 2.0-2.5, adding seed crystal for reaction for about 40 minutes to 2 hours, introducing the reaction solution into a No. 2 reaction tank through a diversion facility, adding steam into the No. 2 reaction tank, keeping the reaction temperature at 50-60 ℃, and adding Na2CO3Controlling the pH value to be 2.5-3.0, introducing the solution into a No. 3 reaction tank through a flow guide device after the reaction time is reached, adding steam into the No. 3 reaction tank to keep the reaction temperature at 50-60 ℃, and adding Na2CO3Controlling the pH value to be 3.0-3.5, introducing the solution into a No. 4 reactor through a flow guide device after the reaction time is reached, and adding steam into a No. 4 reaction tank to keep the reaction temperature at 50-60 ℃; adding Na2CO3Controlling the pH value to be 4.0-4.5, and introducing the solution into a No. 5 reactor through a flow guide device after the reaction time is reached; dilute H is added into the No. 5 reaction tank2SO4Adjusting the pH value back to 3.3-3.5, reacting the solution for 40 minutes to 2 hours, and then entering the next procedure for utilizationThe filter press carries out solid-liquid separation, the separated liquid enters an extraction process, and the aluminum slag enters a washing process.
The method of the invention adopts Na2CO3Controlling the pH of the solution, Na2CO3High solubility, weak alkalinity and easily controlled pH value, and simultaneously introduces Na + ions into the reaction solution to improve the content of aluminum vanadium (Na)2(Al6(SO4)4(OH)I2) Large molecular weight of aluminum and vanadium, easy crystal growth, stable performance and insolubility, and the filtering speed of the aluminum-removed liquid is greatly improved.
The method of the invention, the pre-aluminum removal solution and Na2CO3When the aluminum alloy is added, a dispersion mode is adopted, and the aluminum alloy is in a drop form, so that the local over-alkali phenomenon is prevented from being generated, and the local Al is reduced3+Ion content, prevention of Al (OH)3Formation of Al (OH)3Is colloidal solid, and improves the filtering performance of the liquid after aluminum removal.
Method of the invention, Al in 1-3# reaction tank3+High concentration, excessive increase of pH value, generally 0-0.5, and drastic change of local pH value, such as Al (OH)3The amount of colloidal solids formed is greatly increased, increasing the difficulty of solution filtration.
In the method, the reaction solution is heated by steam; the steam heating water vapor is changed into water, the volume of the reaction solution is increased, the concentration of main reactants and impurities is reduced, the operation difficulty can be reduced, the slag content of valuable metals such as cobalt and nickel is reduced, and meanwhile, the filtering performance of the solution is improved.
According to the method, the treated liquid in the 5# reaction tank, the volume of which is about 10%, is conveyed to the 1# reactor through the transfer pump and used as the seed crystal, so that the reaction speed is increased, the grain diameter of the filter residue is increased, and the filtering speed of the treated liquid is increased.
Example 1
The equipment used is shown in fig. 2.
(1) Adding the solution before aluminum removal into the solution 1, wherein the element content (g/L) in the solution is as follows:
1 volume 25m3The solution is added in a spraying mode through a liquid adding device 2, and the volume adding amount is 12m3When the solution is submerged by the paddle, starting the stirring paddle, rotating the stirring paddle at the speed of 300r/min, adopting a propelling paddle, adding steam by 12, heating by adopting direct steam, controlling the reaction temperature of the solution at 50 ℃, and adding Na by 32CO3The pH was controlled between 2.0 and 2.5, the 1-solution fill time was 1 hour and 40 minutes, and the 1-fill was followed by 13-entry to 4. 1 during the first reaction, adding 100Kg of aluminum-vanadium seed crystal, and during the continuous reaction, adding 7 volumes of the treated solution of 2m3/h.
(2)4 volume 25m3The solution is reacted at 50 ℃ and Na is added through 32CO3Controlling the pH value between 2.5 and 3.0, the rotating speed of a stirring paddle to be 300r/min and the volume flow to be 14m3Reaction time was about 1 hour and 30 minutes, and the reaction was complete with continuous feed through 13 to 5.
(3)5 volume 25m3The solution is reacted at 50 ℃ and Na is added through 32CO3Controlling the pH value between 3.0 and 3.5, the rotating speed of a stirring paddle to be 300r/min and the volume flow to be 14m3Reaction time was about 1 hour and 30 minutes, and the reaction was complete, passing through 13, and continuously entering 6.
(4)6 volume 25m3The solution is reacted at 50 ℃ and Na is added through 32CO3Controlling the pH value to be 4.0, the rotating speed of a stirring paddle to be 300r/min and the volume flow to be 14m3Reaction time was about 1 hour and 30 minutes, and the reaction was complete, passing through 13, and continuously entering 7.
(5)7 volume 25m3The solution is reacted at 50 ℃ and H is added through 82SO4Controlling the pH value between 3.3 and 3.5, the rotating speed of a stirring paddle to be 300r/min and the volume flow to be 14m3Reaction time 1 hour 30 minutes, end of reaction, 13, 9(9 volumes 30 m)3The material is as follows: glass fiber reinforced plastic) is conveyed from 10 to 11 and 1, the liquid after aluminum removal is subjected to filter pressing to separate out liquid after filter pressing and aluminum slag, the liquid after filter pressing enters the next working procedure for extraction, and the aluminum slag enters the washing working procedure.
(7) Solution treatment results:
| element(s) | Co | Ni | Cu | Fe | Al |
| Content g/L | 58.30 | 3.02 | 2.40 | 0.0021 | 0.012 |
The slag containing valuable metals
| Element(s) | Co | Ni | Cu | Fe | Al |
| Content% | 0.21 | 0.05 | 0.12 | 11.25 | 36.58 |
The total aluminum content of the liquid after aluminum removal is 0.012g/L and less than 0.05g/L, the Co content of the slag is 0.21 percent and less than 0.5 percent, the filtering speed is greatly improved, and the production requirement is met.
Example 2
The equipment used is shown in fig. 2.
(1) Adding the solution before aluminum removal into the solution 1, wherein the element content (g/L) in the solution is as follows:
1 volume 25m3The solution is added in a spraying mode through a liquid adding device 2, and the volume adding amount is 15m3When the solution is over the blades, starting the stirring paddle, rotating the stirring paddle at the speed of 50r/min, adopting a propelling blade, adding steam through 12, heating by adopting direct steam, controlling the reaction temperature of the solution at 60 ℃, and adding Na through 32CO3The pH was controlled between 2.0 and 2.5, the 1-fill time was 40 minutes, and the 1-fill was followed by 13-into 4. 1 during the first reaction, aluminum vanadium seed crystal is added with the addition amount of about 100Kg, and in the continuous reaction process, 7 treated liquid with the volume amount of 3m is added3/h.
(2)4 volume 25m3The solution is reacted at 60 ℃ and Na is added through 32CO3Controlling the pH value between 2.5 and 3.0, the rotating speed of a stirring paddle to be 50r/min and the volume flow to be 17.5m3Reaction time of about 40 minutes, reactionEnding with a continuous entry through 13 to 5.
(3)5 volume 25m3The solution is reacted at 60 ℃ and Na is added through 32CO3Controlling the pH value between 3.0 and 3.5, the rotating speed of a stirring paddle to be 50r/min and the volume flow to be 17.5m3Reaction time was about 40 minutes, reaction was complete, via 13, and continuous feed 6 was obtained.
(4)6 volume 25m3The solution is reacted at 60 ℃ and Na is added through 32CO3Controlling the pH value between 4.0 and 4.5, the rotating speed of a stirring paddle to be 50r/min and the volume flow to be 17.5m3Reaction time was about 40 minutes, reaction was complete, via 13, and continuous feed 7 was obtained.
(5)7 volume 25m3The solution is reacted at 60 ℃ and H is added through 82SO4Controlling the pH value between 3.3 and 3.5, the rotating speed of a stirring paddle to be 50r/min and the volume flow to be 17.5m3Reaction time was about 40 minutes, reaction was complete, 13, into 9(9 volumes 30 m)3The material is as follows: glass fiber reinforced plastic) is conveyed from 10 to 11 and 1, the liquid after aluminum removal is subjected to filter pressing to separate out liquid after filter pressing and aluminum slag, the liquid after filter pressing enters the next working procedure for extraction, and the aluminum slag enters the washing working procedure.
(7) Solution treatment results:
| element(s) | Co | Ni | Cu | Fe | Al |
| Content g/L | 58.30 | 3.02 | 2.40 | 0.0021 | 0.012 |
The slag containing valuable metals
| Element(s) | Co | Ni | Cu | Fe | Al |
| Content% | 0.21 | 0.05 | 0.12 | 11.25 | 36.58 |
The total aluminum content of the aluminum-removed liquid is 0.011g/L and less than 0.05g/L, the Co content of the slag is 0.22 percent and less than 0.5 percent, the filtering speed is greatly improved, and the production requirement is met.
Example 3
(1) Adding the solution before aluminum removal into the solution 1, wherein the element content (g/L) in the solution is as follows:
1 volume 25m3The solution is added in a spraying mode through a liquid adding device 2, and the volume adding amount is 13m3When the solution is submerged by the paddle, starting the stirring paddle, rotating the stirring paddle at the speed of 100r/min, adopting a propelling paddle, adding steam through 12, heating by adopting direct steam, controlling the reaction temperature of the solution to be 55 ℃, and adding Na through 32CO3The pH was controlled between 2.0 and 2.5, the 1-solution fill time was 1 hour and 40 minutes, and the 1-fill was followed by 13-entry to 4. 1 during the first reaction, aluminum vanadium seed crystal is added with the addition amount of about 100Kg, and in the continuous reaction process, 7 treated liquid with the volume amount of 2.5m is added3/h.
(2)4 volume 25m3The solution is reacted at 55 ℃ and Na is added through 32CO3Controlling the pH value between 2.5 and 3.0, the rotating speed of a stirring paddle to be 100r/min and the volume flow to be 16m3Reaction time was about 1 hour and 30 minutes, and the reaction was complete with continuous feed through 13 to 5.
(3)5 volume 25m3The solution is reacted at 55 ℃ and Na is added through 32CO3Controlling the pH value between 3.0 and 3.5, the rotating speed of a stirring paddle to be 100r/min and the volume flow to be 16m3Reaction time was about 1 hour and 30 minutes, and the reaction was complete, passing through 13, and continuously entering 6.
(4)6 volume 25m3The solution is reacted at 55 ℃ and Na is added through 32CO3Controlling the pH value between 4.0 and 4.5, the rotating speed of a stirring paddle to be 100r/min and the volume flow to be 16m3Reaction time was about 1 hour and 30 minutes, and the reaction was complete, passing through 13, and continuously entering 7.
(5)7 volume 25m3The solution reaction temperature is 55 ℃, H is added through 82SO4Controlling the pH value between 3.3 and 3.5, the rotating speed of a stirring paddle to be 100r/min and the volume flow to be 16m3Reaction time 1 hour 30 minutes, end of reaction, 13, 9(9 volumes 30 m)3The material is as follows: glass fiber reinforced plasticAnd) then conveying the aluminum-removed liquid from the tank 10 to the tank 11 and the tank 1, performing filter pressing on the aluminum-removed liquid to separate out filter-pressed liquid and aluminum slag, extracting the filter-pressed liquid in the next process, and washing the aluminum slag.
(7) Solution treatment results:
the slag containing valuable metals
| Element(s) | Co | Ni | Cu | Fe | Al |
| Content% | 0.22 | 0.04 | 0.11 | 11.24 | 36.56 |
The total aluminum content of the liquid after aluminum removal is 0.012g/L and less than 0.05g/L, the Co content of the slag is 0.21 percent and less than 0.5 percent, the filtering speed is greatly improved, and the production requirement is met.
Claims (11)
1. A method for removing aluminum from a nickel-cobalt solution is characterized in that the aluminum removing process sequentially comprises the following steps:
(1) the pH value of the liquid control solution before aluminum removal is 2-2.5, and stirring reaction is carried out;
(2) controlling the pH0 value of the reacted liquid in the step (1) to be 2.5-3.0, and stirring for reaction;
(3) controlling the pH value of the reacted liquid in the step (2) to be 3.5-3.5, and stirring for reaction;
(4) controlling the pH value of the reacted liquid in the step (3) to be 4.5-4.5, and stirring for reaction;
(5) controlling the pH value of the reacted liquid in the step (4) to be 3.3-3.5, and stirring for reaction;
(6) and (5) carrying out liquid-solid separation on the reaction product obtained in the step (5).
2. The method of claim 1 wherein said step (1) is conducted by adding Na2CO3The pH value of the solution is controlled to be 2.0-2.5.
3. The method of claim 1 wherein said step (2) is conducted by adding Na2CO3The pH value of the solution is controlled to be 2.5-3.0.
4. The method of claim 1 wherein said step (3) is conducted by adding Na2CO3The pH value of the solution is controlled to be 3.0-3.5.
5. The method of claim 1 wherein said step (4) is conducted by adding Na2CO3The pH value of the solution is controlled to be 4.0-4.5.
6. A nickel cobalt as claimed in claim 1The method for removing aluminum from solution is characterized in that the step (5) is to add H2SO4The pH value of the solution is controlled to be 3.3-3.5.
7. The method of claim 1 wherein the reaction temperature is controlled to be 50-60 ℃ and the reaction time is 40 minutes to 2 hours.
8. The method of claim 1 wherein the reaction temperature is controlled by heating with steam.
9. The method of claim 1 wherein the reaction process is stirred at a speed of 50 to 350 r/min.
10. The method of claim 1 wherein the solution is added in a spray or dispersion form to drop into the reaction liquid surface in the form of drops.
11. The method for removing aluminum from nickel cobalt solution according to claim 1, characterized in that 10% by volume of the solution after the step (5) reaction is taken and returned to the step (1) to be used as seed crystal.
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Effective date of registration: 20240208 Address after: 737100 No. 2 Lanzhou Road, Beijing Road Street, Jinchuan District, Jinchang City, Gansu Province Patentee after: Jinchuan Group Nickel Cobalt Co.,Ltd. Country or region after: China Patentee after: LANZHOU JINCHUAN ADVANGCED MATERIALS TECHNOLOGY Co.,Ltd. Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China Patentee before: LANZHOU JINCHUAN ADVANGCED MATERIALS TECHNOLOGY Co.,Ltd. |