CN111270070A - Washing method and device for P507 cobalt extraction system - Google Patents

Washing method and device for P507 cobalt extraction system Download PDF

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Publication number
CN111270070A
CN111270070A CN201811472008.2A CN201811472008A CN111270070A CN 111270070 A CN111270070 A CN 111270070A CN 201811472008 A CN201811472008 A CN 201811472008A CN 111270070 A CN111270070 A CN 111270070A
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organic phase
washing
value
nickel
acid
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李炳忠
张爱青
伍一根
许东伟
史齐勇
王博
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Gem Jiangsu Cobalt Industry Co Ltd
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Gem Jiangsu Cobalt Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846Phosphoric acid, e.g. (O)P(OH)3
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/02Apparatus therefor
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a washing method for a P507 cobalt extraction system, which is used for separating magnesium and nickel extracted into an organic phase from the organic phase in an extraction process, and specifically comprises the following steps: step 1, adding acid liquor into an organic phase, controlling the pH value of the solution to be 2.0-2.5 to separate nickel from the organic phase, and obtaining a nickel-washed organic phase; step 2, adding acid liquor into the organic phase after nickel washing in the step 1, controlling the pH value of the solution to be 1.5-2.0 to separate magnesium from the organic phase, and finishing washing the organic phase in the extraction process; the invention also discloses a washing device for the P507 cobalt extraction system; according to different extraction rates of cobalt, magnesium and nickel, firstly, sulfuric acid is added into an organic phase, the pH value of the solution is controlled to be 2.0-2.5, so that most of nickel is separated from the organic phase, meanwhile, a part of magnesium is separated, secondly, hydrochloric acid is added, the pH value of the solution is controlled to be 1.5-2.0, and the rest of magnesium and the rest of nickel are separated from the organic phase.

Description

Washing method and device for P507 cobalt extraction system
Technical Field
The invention belongs to the technical field of cobalt extraction, and particularly relates to a washing method and a washing device for a P507 cobalt extraction system.
Background
The cobalt extraction process is a method for adding feed liquid, organic liquid and acid in stages by utilizing an extraction tank, removing impurities by the extraction tank and separating nickel and cobalt by a cobalt-nickel separation tank on the premise of fully stirring; however, during cobalt extraction, a part of the magnesium and nickel in the aqueous phase is extracted into the organic phase, which affects the quality of the organic phase, and thus the magnesium and nickel need to be separated in the washing stage of cobalt extraction.
Disclosure of Invention
The invention aims to provide a washing method for a P507 cobalt extraction system, which is used for washing magnesium and nickel by using acid according to different extraction rates of cobalt, magnesium and nickel.
Another object of the present invention is to provide a scrubbing apparatus for a P507 cobalt extraction system.
The technical scheme adopted by the invention is that,
a washing method for a P507 cobalt extraction system, which is used for separating magnesium and nickel extracted into an organic phase in an extraction process from the organic phase, comprises the following steps:
step 1, adding acid liquor into an organic phase, controlling the pH value of the solution to be 2.0-2.5 to separate nickel from the organic phase, and obtaining a nickel-washed organic phase;
and 2, adding acid liquor into the organic phase after nickel washing in the step 1, controlling the pH value of the solution to be 1.5-2.0 to separate magnesium from the organic phase, and finishing washing the organic phase in the extraction process.
The present invention is also characterized in that,
the acid solution in the step 1 is 1.0-1.2mol/L sulfuric acid.
The pH value of the solution is controlled to be between 2.0 and 2.5 in the step 1 until the concentration ratio of cobalt to nickel is not less than 1000: 1.
the acid solution in the step 2 is 1.5-2.5mol/L hydrochloric acid.
And 2, controlling the pH value of the solution to be 1.5-2.0 until the concentration ratio of cobalt to magnesium is not less than 10000: 1.
and (3) adopting multi-stage countercurrent extraction in the steps 1 and 2, monitoring the pH value on line and realizing automatic acid supplementation through an automatic acid supplementation system.
The utility model provides a washing device for P507 cobalt extraction system, its includes first scrubbing bath, first automatic acid supplementation subassembly, second scrubbing bath and the automatic acid supplementation subassembly of second, first scrubbing bath and second scrubbing bath pass through the pipe connection, first automatic acid supplementation subassembly is connected with first scrubbing bath and is used for controlling the pH value of first scrubbing bath, the automatic acid supplementation subassembly of second is connected with the second scrubbing bath and is used for controlling the pH value of second scrubbing bath.
The first automatic acid supplementing assembly comprises a sulfuric acid inlet pipe, a first controller and a first pH meter, the first pH meter stretches into the first washing tank to detect the pH value of a solution in the first washing tank in real time and transmits the pH value to the first controller, the first controller compares the pH value with a preset pH threshold value and controls the state of the sulfuric acid inlet pipe according to a comparison result, one end of the sulfuric acid inlet pipe is connected with a sulfuric acid source, and the other end of the sulfuric acid inlet pipe is inserted into the first washing tank.
The second automatic acid supplementing assembly comprises a hydrochloric acid inlet pipe, a second controller and a second pH meter, the second pH meter stretches into the second washing tank to detect the pH value of a solution in the second washing tank in real time and transmits the pH value to the second controller, the second controller compares the pH value with a preset pH threshold value and controls the state of the hydrochloric acid inlet pipe according to a comparison result, one end of the hydrochloric acid inlet pipe is connected with a hydrochloric acid source, and the other end of the hydrochloric acid inlet pipe is inserted into the second washing tank.
The first washing tank and the second washing tank comprise five-stage washing, and each machine washing corresponds to one set of first automatic acid supplementing assembly or second automatic acid supplementing assembly.
The invention has the beneficial effects that according to different extraction rates of cobalt, magnesium and nickel, firstly, sulfuric acid is added into an organic phase, the pH value of the solution is controlled to be between 2.0 and 2.5, so that most of nickel is separated from the organic phase, meanwhile, a part of magnesium is separated, secondly, hydrochloric acid is added, the pH value of the solution is controlled to be between 1.5 and 2.0, and the rest of magnesium and the rest of nickel are separated from the organic phase, so that the method is simple and easy to operate.
Drawings
FIG. 1 is a schematic structural diagram of a washing device for a P507 cobalt extraction system according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a washing method for a P507 cobalt extraction system, which comprises the following steps: firstly, adding 1.0-1.2mol/L sulfuric acid into an organic phase, and controlling the pH value of the solution to be 2.0-2.5 until the concentration ratio of cobalt to nickel is not less than 1000: 1, separating nickel from an organic phase to obtain a nickel-washed organic phase; secondly, adding 1.5-2.5mol/L hydrochloric acid into the organic phase after nickel washing, and controlling the pH value of the solution to be 1.5-2.0 until the concentration ratio of cobalt to magnesium is not less than 10000: 1, separating magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
In addition, in the present embodiment, five stages of countercurrent extraction are adopted in both the nickel washing process in step 1 and the magnesium washing process in step 2, and since each stage of washing can only wash 50-70% of the nickel (magnesium) in the organic phase, after 5 stages of washing, the nickel and magnesium can be basically washed clean.
Under the same hydrogen ion concentration condition, the effect of washing magnesium by using hydrochloric acid is 1.5-2.0 times of that of sulfuric acid, so that the magnesium is easier to wash by using hydrochloric acid; under the same hydrogen ion concentration condition, the effect of washing nickel by using sulfuric acid is 1.5-2.0 times of that of hydrochloric acid, so that the nickel is easier to wash by using hydrochloric acid.
According to the different extraction rates of cobalt, magnesium and nickel, firstly, sulfuric acid is added into an organic phase, the pH value of the solution is controlled to be 2.0-2.5, so that most of nickel is separated from the organic phase, meanwhile, a part of magnesium is separated, secondly, hydrochloric acid is added, the pH value of the solution is controlled to be 1.5-2.0, and the rest of magnesium and the rest of nickel are separated from the organic phase.
Example 1
The embodiment 1 of the invention provides a washing method for a P507 cobalt extraction system, which comprises the following steps: firstly, adding 1.0mol/L sulfuric acid into an organic phase, and controlling the pH value of the solution to be 2.0 to separate nickel from the organic phase to obtain a nickel-washed organic phase; secondly, adding 1.5mol/L hydrochloric acid into the organic phase after nickel washing, controlling the pH value of the solution to be 1.5 to separate magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
After detection, after washing by the method of the embodiment, the ratio of cobalt to nickel and the ratio of cobalt to magnesium in the final organic phase are all more than 10000; wherein the cobalt content is 12.31g/L, the nickel content is 0.00095g/L, and the magnesium content is 0.00085 g/L.
Example 2
The embodiment 2 of the invention provides a washing method for a P507 cobalt extraction system, which comprises the following steps: firstly, adding 1.2mol/L sulfuric acid into an organic phase, and controlling the pH value of the solution to be 2.5 to separate nickel from the organic phase to obtain a nickel-washed organic phase; secondly, adding 2.5mol/L hydrochloric acid into the organic phase after nickel washing, controlling the pH value of the solution to be 2.0 to separate magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
After detection, after washing by the method of the embodiment, the ratio of cobalt to nickel and the ratio of cobalt to magnesium in the final organic phase are all more than 10000; wherein, the cobalt content is 11.31g/L, the nickel content is 0.00083g/L, and the magnesium content is 0.00072 g/L.
Example 3
The embodiment 3 of the invention provides a washing method for a P507 cobalt extraction system, which comprises the following steps: firstly, adding 1.1mol/L sulfuric acid into an organic phase, and controlling the pH value of the solution to be 2.2 to separate nickel from the organic phase to obtain a nickel-washed organic phase; secondly, adding 2mol/L hydrochloric acid into the organic phase after nickel washing, controlling the pH value of the solution to be 1.8 to separate magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
After detection, after washing by the method of the embodiment, the ratio of cobalt to nickel and the ratio of cobalt to magnesium in the final organic phase are all more than 10000; wherein, the content of cobalt is 13.11g/L, the content of nickel is 0.0011g/L, and the content of magnesium is 0.00098 g/L.
Example 4
The embodiment 4 of the invention provides a washing method for a P507 cobalt extraction system, which comprises the following steps: firstly, adding 1.15mol/L sulfuric acid into an organic phase, and controlling the pH value of the solution to be 2.4 to separate nickel from the organic phase to obtain a nickel-washed organic phase; secondly, adding 2.2mol/L hydrochloric acid into the organic phase after nickel washing, controlling the pH value of the solution to be 1.8 to separate magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
After detection, after washing by the method of the embodiment, the ratio of cobalt to nickel and the ratio of cobalt to magnesium in the final organic phase are all more than 10000; wherein, the cobalt content is 12.68g/L, the nickel content is 0.00087g/L, and the magnesium content is 0.00078 g/L.
Example 5
The embodiment 5 of the invention provides a washing method for a P507 cobalt extraction system, which comprises the following steps: firstly, adding 1.05mol/L sulfuric acid into an organic phase, and controlling the pH value of the solution to be 2.3 to separate nickel from the organic phase to obtain a nickel-washed organic phase; secondly, adding 1.9mol/L hydrochloric acid into the organic phase after nickel washing, controlling the pH value of the solution to be 1.6 to separate magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
After detection, after washing by the method of the embodiment, the ratio of cobalt to nickel and the ratio of cobalt to magnesium in the final organic phase are all more than 10000; wherein the cobalt content is 14.11g/L, the nickel content is 0.00075g/L, and the magnesium content is 0.00088 g/L.
Example 6
Embodiment 6 of the present invention provides a washing method for a P507 cobalt extraction system, which specifically comprises: firstly, adding 1.13mol/L sulfuric acid into an organic phase, controlling the pH value of the solution to be 2.1 to separate nickel from the organic phase, and obtaining a nickel-washed organic phase; secondly, adding 1.2mol/L hydrochloric acid into the organic phase after nickel washing, controlling the pH value of the solution to be 1.85 to separate magnesium from the organic phase, and finishing the washing of the organic phase in the extraction process; in the washing process, the pH meter detects the pH value of the solution on line in real time, and automatic acid supplementation is realized through an automatic acid supplementation system.
After detection, after washing by the method of the embodiment, the ratio of cobalt to nickel and the ratio of cobalt to magnesium in the final organic phase are all more than 10000; wherein, the content of cobalt is 12.97g/L, the content of nickel is 0.00079g/L, and the content of magnesium is 0.00095 g/L.
The embodiment of the invention also provides a washing device for a P507 cobalt extraction system, which comprises a first washing tank 1, a first automatic acid supplementing assembly 2, a second washing tank 3 and a second automatic acid supplementing assembly 4, wherein the first washing tank 1 and the second washing tank 3 are connected through a pipeline, the first automatic acid supplementing assembly 2 is connected with the first washing tank 1 and used for controlling the pH value of the first washing tank 1, and the second automatic acid supplementing assembly 4 is connected with the second washing tank 3 and used for controlling the pH value of the second washing tank 3, as shown in fig. 1.
The first automatic acid supplementing assembly 2 comprises a sulfuric acid inlet pipe 21, a first controller 22 and a first pH meter 23, the first pH meter 23 extends into the first washing tank 1 to detect the pH value of the solution in the first washing tank 1 in real time and transmit the pH value to the first controller 22, the first controller 22 compares the pH value with a preset pH threshold value and controls the state of the sulfuric acid inlet pipe 21 according to the comparison result, one end of the sulfuric acid inlet pipe 21 is connected with a sulfuric acid source, and the other end of the sulfuric acid inlet pipe 21 is inserted into the first washing tank 1.
The second automatic acid-supplementing assembly 4 includes a hydrochloric acid inlet pipe 41, a second controller 42 and a second pH meter 43, the second pH meter 43 extends into the second washing tank 3 to detect the pH value of the solution in the second washing tank 3 in real time and transmit the pH value to the second controller 42, the second controller 42 compares the pH value with a preset pH threshold value and controls the state of the hydrochloric acid inlet pipe 41 according to the comparison result, one end of the hydrochloric acid inlet pipe 41 is connected with a hydrochloric acid source, and the other end of the hydrochloric acid inlet pipe 41 is inserted into the second washing tank 3.
The first washing tank 1 and the second washing tank 3 both comprise five-stage washing, and each machine washing corresponds to one set of the first automatic acid supplementing assembly 2 or the second automatic acid supplementing assembly 4.
The using method of the embodiment comprises the following steps: firstly, adding an organic phase in the P507 cobalt extraction process into a first washing tank 1, secondly, adding sulfuric acid into the organic phase, adding the sulfuric acid into the first washing tank 1 through a first automatic acid supplementing assembly 2, controlling the pH value of the solution to be 2.0-2.5 to separate most of nickel from the organic phase, simultaneously separating a part of magnesium, secondly, discharging the solution into a second washing tank 3 through a pipeline, adding hydrochloric acid into the solution through a second automatic acid supplementing assembly 4, and controlling the pH value of the solution to be 1.5-2.0 to separate the rest of magnesium and the rest of nickel from the organic phase.
The embodiment realizes that nickel and magnesium in an organic phase are separated in the washing process through the mutual matching of the first washing tank, the first automatic acid supplementing assembly, the second washing tank and the second automatic acid supplementing assembly, and the quality of the organic phase is improved.
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 can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. A washing method for a P507 cobalt extraction system is characterized in that the method is used for separating magnesium and nickel extracted into an organic phase in an extraction process from the organic phase, and specifically comprises the following steps:
step 1, adding acid liquor into an organic phase, controlling the pH value of the solution to be 2.0-2.5 to separate nickel from the organic phase, and obtaining a nickel-washed organic phase;
and 2, adding acid liquor into the nickel-washed organic phase liquid obtained in the step 1, controlling the pH value of the solution to be 1.5-2.0 to separate magnesium from the organic phase, and finishing washing the organic phase in the extraction process.
2. The washing method for the P507 cobalt extraction system as claimed in claim 1, wherein the acid solution in the step 1 is 1.0-1.2mol/L sulfuric acid.
3. The washing method for the P507 cobalt extraction system as claimed in claim 2, wherein the pH value of the solution is controlled in the step 1 to be between 2.0 and 2.5 until the concentration ratio of cobalt to nickel is not less than 1000: 1.
4. a washing method for a P507 cobalt extraction system as claimed in claim 3, wherein the acid solution in the step 2 is 1.5-2.5mol/L hydrochloric acid.
5. The washing method for the P507 cobalt extraction system as claimed in claim 4, wherein the step 2 is to control the pH value of the solution to be between 1.5 and 2.0 until the concentration ratio of cobalt to magnesium is not less than 10000: 1.
6. the washing method for the P507 cobalt extraction system as claimed in any one of claims 1 to 5, wherein the steps 1 and 2 adopt multi-stage countercurrent extraction, and pH value is monitored on line and automatic acid supplementation is realized through an automatic acid supplementation system.
7. The utility model provides a washing device for P507 cobalt extraction system, its characterized in that, its includes first scrubbing bath (1), first automatic acid supplementation subassembly (2), second scrubbing bath (3) and second automatic acid supplementation subassembly (4), first scrubbing bath (1) and second scrubbing bath (3) pass through the pipe connection, first automatic acid supplementation subassembly (2) are connected with first scrubbing bath (1) and are used for controlling the pH value of first scrubbing bath (1), second automatic acid supplementation subassembly (4) are connected with second scrubbing bath (3) and are used for controlling the pH value of second scrubbing bath (3).
8. The washing device for the P507 cobalt extraction system as claimed in claim 7, wherein the first automatic acid supplementing assembly (2) comprises a sulfuric acid inlet pipe (21), a first controller (22) and a first pH meter (23), the first pH meter (23) extends into the first washing tank (1) to detect the pH value of the solution in the first washing tank (1) in real time and transmit the pH value to the first controller (22), the first controller (22) compares the pH value with a preset pH threshold value and controls the state of the sulfuric acid inlet pipe (21) according to the comparison result, one end of the sulfuric acid inlet pipe (21) is connected with a sulfuric acid source, and the other end of the sulfuric acid inlet pipe (21) is inserted into the first washing tank (1).
9. The washing device for the P507 cobalt extraction system as claimed in claim 8, wherein the second automatic acid supplementing assembly (4) comprises a hydrochloric acid inlet pipe (41), a second controller (42) and a second pH meter (43), the second pH meter (43) extends into the second washing tank (3) to detect the pH value of the solution in the second washing tank (3) in real time and transmit the pH value to the second controller (42), the second controller (42) compares the pH value with a preset pH threshold value and controls the state of the hydrochloric acid inlet pipe (41) according to the comparison result, one end of the hydrochloric acid inlet pipe (41) is connected with a hydrochloric acid source, and the other end of the hydrochloric acid inlet pipe (41) is inserted into the second washing tank (3).
10. The washing device for the P507 cobalt extraction system is characterized in that the first washing tank (1) and the second washing tank (3) comprise five-stage washing, and each machine washing corresponds to one set of the first automatic acid supplementing assembly (2) or the second automatic acid supplementing assembly (4).
CN201811472008.2A 2018-12-04 2018-12-04 Washing method and device for P507 cobalt extraction system Pending CN111270070A (en)

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CN114990355A (en) * 2022-05-30 2022-09-02 金川集团镍盐有限公司 Method for producing cobalt solution by removing magnesium from high-magnesium low-cobalt solution
CN115259247A (en) * 2022-08-11 2022-11-01 重庆吉恩冶炼有限公司 Cobalt-magnesium separation method based on nickel sulfate production

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CN108441633A (en) * 2018-05-21 2018-08-24 兰州金川新材料科技股份有限公司 A kind of production method of electronic-grade sulfuric acid cobalt liquor
CN209652387U (en) * 2018-12-04 2019-11-19 格林美(江苏)钴业股份有限公司 A kind of wash mill for P507 cobalt extracting system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114990355A (en) * 2022-05-30 2022-09-02 金川集团镍盐有限公司 Method for producing cobalt solution by removing magnesium from high-magnesium low-cobalt solution
CN115259247A (en) * 2022-08-11 2022-11-01 重庆吉恩冶炼有限公司 Cobalt-magnesium separation method based on nickel sulfate production

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Application publication date: 20200612