CN108179272A - Cobalt magnesium separation method in a kind of cobalt nickel wet smelting process - Google Patents
Cobalt magnesium separation method in a kind of cobalt nickel wet smelting process Download PDFInfo
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- CN108179272A CN108179272A CN201810096634.XA CN201810096634A CN108179272A CN 108179272 A CN108179272 A CN 108179272A CN 201810096634 A CN201810096634 A CN 201810096634A CN 108179272 A CN108179272 A CN 108179272A
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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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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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
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
Abstract
The invention discloses cobalt magnesium separation methods in a kind of cobalt nickel wet smelting process, are related to metal purification technique field, this method in cobalt nickel wet smelting process and include：By the magnesium solution containing cobalt in cobalt nickel wet smelting process after abstraction impurity removal, the cobalt metal ion in the magnesium solution containing cobalt described in polyvalent metal absorption resins selective absorption, so as to which cobalt, magnesium metal in solution be detached.It further includes and adsorption saturation polyvalent metal absorption resin de-parsing is obtained into high concentration cobaltatess solution；And the alkali tune containing magnesium solution after adsorption of cobalt is precipitated into filtering, obtain the magnesium hydroxide crystal of high-purity.For cobalt magnesium separation method in existing traditional cobalt nickel wet smelting process, the method of the invention, it is easy to operate easily-controllable, and effectively cobalt, the separation of magnesium metal and cobalt, the high-purity of magnesium metallic element fully recycle in acid dip solution after realization abstraction impurity removal, environment-friendly high-efficiency, process costs are low, and industrial utility value is high.
Description
Technical field
The present invention relates to metal process for separation and purification in a kind of cobalt nickel wet smelting process more particularly to a kind of cobalt nickel wet methods
The separation method of magnesium addition metal and cobalt metal in smelting process.
Background technology
Cobalt nickel wet smelting process is the separating-purifying from cobalt nickel ores or various scrap metals containing retrieving cobalt nickel
The technical process of cobalt, nickel metal usually mainly dissolves three big steps of-abstraction impurity removal-cobalt nickel separation by acidleach and forms.With existing
It is big in acidleach lysate in recycling scrap metal is for cobalt nickel wet smelting process in being widely used for various cobalt magnesium alloys
Contain higher magnesium impurity metal ion more.Also, due in metal extraction dedoping step, extraction curve and the cobalt nickel of magnesium metal
Metal extraction curve is in close proximity, so being generally difficult to by way of abstraction impurity removal, realizes magnesium metal impurities and cobalt nickel metal
Separation.
For in above-mentioned cobalt nickel wet smelting process, the separation problem of magnesium metal impurities mainly uses fluorine in the prior art
Change sodium precipitation magnesium processes, realize the separation to magnesium metal impurities.But due to magnesium fluoride belongs to strong base-weak acid salt in itself, a side
Face needs liquid to have higher pH in magnesium fluoride precipitation process, and a large amount of cobalt or nickel can be caused to generate precipitation and enter in filter residue,
So as to cause cobalt, nickel waste, organic efficiency is low；On the other hand, needing to add in excessive sodium fluoride could completely will be in solution
Magnesium precipitate completely, it will cause in last waste liquid contain a large amount of fluorine ion, be meet the requirement of environmental protection fluorinion in waste water
Discharge standard is less than 5mg/L, then needs to handle waste water again, lead to the increase of process costs.
For this purpose, study a kind of magnesium metal impurities separation method of simple and effective, it has also become existing cobalt nickel wet method smelting process
In technical barrier urgently to be resolved hurrily.
Invention content
The present invention in view of the deficienciess of the prior art, provide cobalt magnesium separation method in a kind of cobalt nickel wet smelting process,
This method simplicity is easily-controllable, environment-friendly high-efficiency, and can be golden to cobalt, magnesium without under influence condition, realizing to discharge of wastewater and smelting continuity
What is belonged to efficiently separates processing.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes：
Cobalt magnesium separation method in a kind of cobalt nickel wet smelting process, by cobalt nickel wet smelting process, after abstraction impurity removal
Magnesium solution containing cobalt, the processing included the following steps：
S1：The cobalt metal ion in the acid dip solution is adsorbed with polyvalent metal absorption resins selective, so as to which magnesium is golden
Belong to ion to stay in the solution.
According to above-mentioned technical proposal, in conventional cobalt nickel hydrometallurgy Call Provision, nickel metal process, through conventional repeatedly extraction
It removes in the solution after wherein most metal impurities, due to the extraction of extracted character and the cobalt of magnesium metal ion, nickel metal
It takes characteristic very close, causes in the solution finally obtained in addition to cobalt, nickel metal, also containing a large amount of magnesium metal ion.For
Magnesium solution containing cobalt after partial extraction removal of impurities, the present invention select polyvalent metal absorption resin by the cobalt in the magnesium solution containing cobalt
Metalloform-selective adsorbs, and magnesium metal ion is stayed in the solution, so as to fulfill the effect detached to cobalt magnesium metal in solution.
Entire technological operation is simple and easy to control, is omitted during the existing magnesium separating treatment to cobalt, the addition and adjusting of various chemical substances
Step, environment-friendly high-efficiency, industrial utility value are high.
Wherein, due to cobalt, nickel metal adsorption characteristic close, to the selective absorption of cobalt while also can be by the nickel in solution
Metal synchronization absorption, so as to which by cobalt nickel absorption polyvalent metal absorption resin, magnesium metal ion be stayed in the solution, realization cobalt,
Nickel and magnesium efficiently separate, and the present invention will be referred to as the selective absorption of cobalt nickel " selective absorption of cobalt ".It is in addition, of the invention
" the polyvalent metal absorption resin " refers to that a kind of selective absorbing chemical valence is divalent and divalent more than metal ion.It is described
" polyvalent metal absorption resin " is higher than its absorption resin to magnesium ion compatibility to the compatibility of cobalt, nickel ion.
Further, cobalt magnesium separation method in a kind of cobalt nickel wet smelting process, further includes：
S2：Into the solution after step 1 adsorption treatment, adjusting pH is 7-9, makes the magnesium Hydrolysis Reactions of Metal-ions in filtrate be
Magnesium hydrate precipitate；
S3：The solution after precipitating will be fully hydrolyzed in step 2, through filter press press filtration, and consolidated after filtering to get magnesium hydroxide
Body filter cake detaches so as to fulfill magnesium metal impurities.
According to above-mentioned preferred embodiment, by the later stage alkali tune to remaining magnesium solution, press filtration, filtration treatment is realized to high-purity
The recycling and utilization of magnesium hydroxide solid are spent, is played to the abundant effective recycling effect of cobalt nickel metals from waste resource.Wherein,
It verifying through inventor's many experiments, when controlling the pH value of solution after selective absorption cobalt in the range of 7-9, sinking to sodium hydroxide
It forms sediment most abundant, and precipitates the obtained purity highest of magnesium hydroxide, up to 97%.The magnesium in pH causes to solution less than 7
Precipitation by metallic ion is insufficient, reduces the rate of recovery of magnesium metal；When pH is higher than 9, then be easy to cause retained in solution it is a small amount of its
His foreign metal hydrolytic precipitation, and then reduce the purity of the magnesium hydroxide of recycling.
Further, the step S1 includes following operation：
S101：It is 2-3 to adjust the pH value of magnesium solution containing cobalt, and controls the magnesium solution containing cobalt in 20-50 DEG C of temperature strip
Under part, with flow velocity 3-6m3/ h adsorbs resin by polyvalent metal, realizes the choosing to cobalt metal ion in the magnesium solution containing cobalt
Selecting property is adsorbed.
Choosing of the resin to the cobalt metal in magnesium solution containing cobalt after abstraction impurity removal is adsorbed to advanced optimize the polyvalent metal
Adsorption effect is selected, this preferred embodiment to the acid dip solution pH (2-3), temperature (20-50 DEG C) and passes through multivalence gold
Solution flow rate (3-6m when belonging to absorption resin3/ h) carry out further specific limit.Wherein,
Control to the pH=2-3 of magnesium solution containing cobalt, is directly related to the adsorption effect to cobalt metal in solution, through hair
Person of good sense's many experiments are found, only by acid solution pH controls in the range of 2-3, effect is adsorbed to the cobalt metal selective in solution
Fruit is best；If pH is excessively high, the cobalt in solution is caused to hydrolyze, cobalt is adsorbed insufficient；If pH is too low, the multivalence after adsorption of cobalt
Metal-resin parses in acid solution, and it is insufficient to also result in cobalt absorption.
Control to the flow velocity of magnesium solution containing cobalt determines in actual industrial production application according to different operating modes.Knot
It closes to described 20-25 DEG C of condition of temperature, controls the acid dip solution with 3-6m3The flow velocity of/h adsorbs resin by polyvalent metal
When, it is more preferable to the cobalt metal adsorption effect in solution under the premise of entire process efficiency is ensured.
Further, the step S1 further includes following operating procedure：
S102：After cobalt tenor in polyvalent metal absorption resin water outlet is more than 0.01g/L, acid concentration is used
Desorbed solution for 4-9% parses polyvalent metal and adsorbs resin, and the volume ratio that the desorbed solution and polyvalent metal adsorb resin is 2-
4:1。
Wherein, it to the preferred control of the desorbed solution acid concentration 5-8%, is directly related to and polyvalent metal is adsorbed in resin
The parsing effect of adsorption of cobalt.If acid concentration is excessively high, not only acid solution is caused to waste, be also easy to cause equipment etching problem；If acid is dense
Spend it is low, then can not by polyvalent metal adsorb resin in cobalt fully parse, cause aunt's metal recovery rate reduction.With reference to described
Acid solution acid concentration (4-9%, preferably 3-8%) and the desorbed solution and polyvalent metal absorption resin volume ratio (2-4:1, preferably
It is 3:1) it limits, further the dosage relation between the desorbed solution and polyvalent metal absorption resin limits, so that it is guaranteed that right
Cobaltatess solution after parsing is returned to extraction and used, so as to fulfill to cobalt metal ion in solution by the parsing effect of cobalt metal
Purification recycling.
Further, the polyvalent metal absorption resin is the Special Resin of model CH -90.
The CH-90 Special Resins are as a kind of currently preferred polyvalent metal absorption resin, to cobalt metal ion
Affinity is high, thereby further ensures that the selective absorption effect of cobalt metal in the magnesium solution containing cobalt.
Further, the desorbed solution is sulfuric acid.
Further, according to cobalt magnesium separation method, 1m in a kind of cobalt nickel wet smelting process of the present invention3The multivalence gold
The weight for belonging to the absorption adsorbable cobalt of resin is 150-180kg.
Further, the step S2 selects one or more of sodium hydroxide, potassium hydroxide to adjust pH.
Further, it is 90-97% through filtering gained magnesium hydroxide solid purity in the step S3.
Further, the optimization technique side as cobalt magnesium separation method in a kind of cobalt nickel wet smelting process of the present invention
Case specifically includes：By in cobalt nickel wet smelting process, the magnesium solution containing cobalt after abstraction impurity removal is included the following steps
Processing：
S1：It is 2-3 to adjust the pH value of magnesium solution containing cobalt, and controls the magnesium solution containing cobalt in 20-50 DEG C of temperature condition
Under, with flow velocity 3-6m3/ h, by Special Resin CH -90, the selective absorption cobalts of Special Resin CH -90, and magnesium is stayed in
In solution；
After the cobalt in Special Resin water outlet is more than 0.01g/L, using the sulfuric acid that acid concentration is 5-8% as parsing
Resin is analysed in lyolysis, and the sulfuric acid and resin volume ratio are 3:1, until the cobalt content in desorbed solution reaches in the magnesium solution containing cobalt
Cobalt content until；Wherein, the desorbed solution can Reusability；
S2：It will adjust pH to 7~9 through step 1 treated solution using sodium hydroxide solution, make the magnesium water in liquid
It solves as magnesium hydrate precipitate；
S3：The solution that will be fully hydrolyzed in step 2 after precipitation, through filter press press filtration, and after filtering to get purity for 90~
97% magnesium hydroxide solid filter cake detaches so as to fulfill magnesium metal impurities；Gained filtrate meets environmental emission standard, Ke Yizhi
Run in and put.
Compared with prior art, beneficial effects of the present invention：
1st, for cobalt magnesium separation method in existing traditional cobalt nickel wet smelting process, the method for the invention, behaviour
Make simple and easy to control, and effectively realize after abstraction impurity removal cobalt, the separation of magnesium metal and cobalt, the height of magnesium metallic element in magnesium solution containing cobalt
Purity fully recycles, and environment-friendly high-efficiency, process costs are low, and industrial utility value is high.
2nd, cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to the present invention, inhales with reference to polyvalent metal
In the processing step of attached resins selective adsorption of cobalt metal, to technological parameters controls such as the pH of magnesium solution containing cobalt, flow velocity, temperature
System effectively improves the polyvalent metal and adsorbs resin to the adsorbance of cobalt metal, 1m3The polyvalent metal absorption resin is adsorbable
The weight of cobalt is 150-180kg.
3rd, in addition, cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to the present invention, separates and recovers
To magnesium hydroxide solid purity be up to 90-97%, can be used directly as magnesium salts resource utilization；Separate and recover obtained cobalt
Acid salt solution can be used for producing cobaltatess crystal or producing LITHIUM BATTERY ternary precursor, further improve cobalt, magnesium metal recovery
Utility value is realized and the high value of cobalt magnesium metal in the scrap metal of nickel containing cobalt is recycled.
4th, for cobalt magnesium method in existing cobalt nickel wet smelting process, in cobalt magnesium separation method of the present invention,
The environmentally harmful chemical substance such as heavy metal, fluorine is not contained in filtrate after being detached to cobalt magnesium, without being carried out to the filtrate
Reprocessing, you can recipe step is further omitted in direct emission or recycling, reduces process costs.
Specific embodiment
With reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
Range for the above-mentioned theme of the present invention is only limitted to following embodiment, all to belong to this based on the technology that the content of present invention is realized
The range of invention.
Embodiment 1
The present embodiment provides cobalt magnesium metal separation method, concrete operations in a kind of cobalt nickel wet smelting process to be：
The magnesium solution containing cobalt after abstraction impurity removal in cobalt nickel wet smelting process is taken, after testing, in the magnesium solution containing cobalt
Cobalt content is：14.6g/L, content of magnesium 3.4g/L.The pH of magnesium solution containing cobalt is adjusted to 2.1 again, and is 27 DEG C in temperature
Under, the magnesium solution containing cobalt is controlled with 6m3/ h flow velocitys cross Special Resin CH -90.Treat that the resin columns of Special Resin CH -90 go out
After cobalt tenor reaches 0.01g/L in oral fluid, using 5% sulfuric acid solution as desorbed solution rinse resin column, desorbed solution with
15m3The flow velocity of/h rinses resin 1 hour, and it is 3 to control the desorbed solution and Special Resin volume ratio:1, after iterative parsing, obtain
Cobalt content in desorbed solution is 14.5g/L, returns again to extraction workshop section after removal of impurities, extracting sulfuric acid cobalt crystal or LITHIUM BATTERY ternary
Presoma.
Again by the solution after selective absorption cobalt metal, after being 7.4 with sodium hydroxide tune pH, it is to be precipitated fully after, press filtration
Filtering carries out separation of solid and liquid, and content of magnesium is in gained filtrate：0.07g/L, cobalt content are：0.0002g/L；Gained filter cake is hydrogen
Magnesia crystal, after testing, gained magnesium hydroxide crystal purity are 90%.
Embodiment 2
The magnesium solution containing cobalt after abstraction impurity removal in cobalt nickel wet smelting process is taken, after testing, in the magnesium solution containing cobalt
Cobalt content is：18.2g/L, content of magnesium 5.3g/L.The pH of magnesium solution containing cobalt is adjusted to 2.4 again, and at 32 DEG C of temperature,
The control magnesium solution containing cobalt is with 4m3/ h flow velocitys cross Special Resin CH -90.It treats in the Special Resin column outlet liquid, cobalt content
After reaching 0.008g/L, using 7% sulfuric acid solution as desorbed solution, and control desorbed solution with 15m3The flow velocity of/h rinses resin
1 hour, after being parsed in solution cobalt content be 16.2g/L, return again to extraction workshop section after removal of impurities, extracting sulfuric acid cobalt crystal or
Person's LITHIUM BATTERY ternary precursor.
Again by the solution after selective absorption cobalt metal, after being 8.4 with potassium hydroxide tune pH, it is to be precipitated fully after, press filtration
Filtering carries out separation of solid and liquid, and content of magnesium is in gained filtrate：0.05g/L, cobalt content are：0.0003g/L；Gained filter cake is hydrogen
Magnesia crystal, after testing, gained magnesium hydroxide crystal purity are 94%.
Embodiment 3
The magnesium solution containing cobalt after abstraction impurity removal in cobalt nickel wet smelting process is taken, after testing, in the magnesium solution containing cobalt
Cobalt content is：26.7g/L, content of magnesium 7.6g/L.The pH of magnesium solution containing cobalt is adjusted to 2.7 again.In 38 DEG C of temperature, control
The magnesium solution containing cobalt is with 3m3/ h flow velocitys cross Special Resin CH -90.It treats to reach 0.007g/ in the Special Resin column outlet liquid
After L, the hydrochloric acid solution using 8% rinses resin column as desorbed solution, and desorbed solution is with 15m3The flow velocity of/h rinses resin 1 hour,
Cobalt content is 21.8g/L in solution after being parsed, and returns again to extraction workshop section after removal of impurities, extracting sulfuric acid cobalt crystal or battery
Grade ternary precursor.
Again by the solution after selective absorption cobalt metal, after being 8.8 with potassium hydroxide tune pH, make the abundant water of the magnesium in solution
After solving and precipitating, press filtration filtering carries out separation of solid and liquid and obtains filtrate and filter cake.After testing, content of magnesium is remained in gained filtrate is
0.09g/L, cobalt content are：The rate of recovery of 0.0004g/L, corresponding cobalt metal and magnesium metal is up to more than 99.8%.Gained filter cake
As magnesium hydroxide crystal, and the magnesium hydroxide crystal purity is 95%.
Embodiment 4
The magnesium solution containing cobalt after abstraction impurity removal in cobalt nickel wet smelting process is taken, after testing, in the magnesium solution containing cobalt
Cobalt content is：10g/L, content of magnesium are：2g/L.The pH of magnesium solution containing cobalt is adjusted to 2 again, controlled at 20~50 DEG C,
Make the magnesium solution containing cobalt with 5m3/ h flow velocitys cross Special Resin CH -90.Treat the cobalt in the columns of Special Resin CH -90 water outlet
After content is less than 0.01g/L, sulfuric acid or hydrochloric acid using acidity 3% parse Special Resin as desorbed solution, control the parsing
Liquid and Special Resin volume ratio are 4:1, after iterative parsing, the cobalt content in gained desorbed solution reaches 15g/L, returns again to extraction work
Section produces cobaltatess crystal or LITHIUM BATTERY ternary precursor after removal of impurities.
Again by the solution after selective absorption cobalt, it is 9 with sodium hydroxide solution tune pH, the magnesium in solution is made to be fully hydrolyzed simultaneously
After precipitation, press filtration filtering carries out separation of solid and liquid and obtains filtrate and filter cake.After testing, remained in gained filtrate content of magnesium for 0.1~
0.5g/L, cobalt content are 0.0001~0.0005g/L, reach and are sufficiently separated recovering effect.Gained filter cake is magnesium hydroxide crystalline substance
Body, and the magnesium hydroxide crystal purity is 96%.
Embodiment 5
The magnesium solution containing cobalt after abstraction impurity removal in cobalt nickel wet smelting process is taken, after testing, in the magnesium solution containing cobalt
Cobalt content is：30g/L, content of magnesium are：10g/L.The pH of magnesium solution containing cobalt is adjusted to 3 again, controlled at 20~50 DEG C,
Make the magnesium solution containing cobalt with 5-6m3/ h flow velocitys cross Special Resin CH -90.It treats in the columns of Special Resin CH -90 water outlet
After cobalt content is less than 0.01g/L, sulfuric acid or hydrochloric acid using acidity 9% parse Special Resin as desorbed solution, control the solution
It is 2 to analyse liquid and Special Resin volume ratio:1, after iterative parsing, the cobalt content obtained in desorbed solution reaches 30g/L, returns again to extraction
Workshop section produces cobaltatess crystal or LITHIUM BATTERY ternary precursor after removal of impurities.
Again by the solution after selective absorption cobalt, it is 8 with sodium hydroxide solution tune pH, the magnesium in solution is made to be fully hydrolyzed simultaneously
After precipitation, press filtration filtering carries out separation of solid and liquid and obtains filtrate and filter cake.After testing, remained in gained filtrate content of magnesium for 0.1~
0.5g/L, cobalt content are 0.0001~0.0005g/L, reach and are sufficiently separated recovering effect.Gained filter cake is magnesium hydroxide crystalline substance
Body, and the magnesium hydroxide crystal purity is 97%.
Comparative example 1
It is to verify in resins selective is adsorbed with polyvalent metal and absorbs cobalt metal step, the acid dip solution pH=2-3
The influence to cobalt adsorption effect is controlled, inventor sets following contrast experiment's example relative to embodiment 1：
Comparative example 101
The comparative example is set relative to embodiment 1, and compared with Example 1, difference lies in take cobalt nickel wet smelting process
The pH value of solution is adjusted to 0.1 by the middle magnesium solution containing cobalt after abstraction impurity removal, remaining step of preparation process and parameter all same.
After testing, in the desorbed solution obtained after final iterative parsing, cobalt tenor is significantly reduced as 9.56g/L.
Comparative example 102
The comparative example is set relative to embodiment 1, and compared with Example 1, difference lies in take cobalt nickel wet smelting process
Acid dip solution pH is adjusted to 5 by the middle magnesium solution containing cobalt after abstraction impurity removal, remaining step of preparation process and parameter are homogeneous
Together.
After testing, in the desorbed solution obtained after final iterative parsing, cobalt tenor is significantly reduced as 10.2g/L.
Comparative example 2
To verify that the parsing liquid acidity (4-9%) adsorbs polyvalent metal the parsing influential effect of adsorption of cobalt in resin,
Applicant sets following contrast experiment's example relative to embodiment 1：
Comparative example 201
The comparative example is set relative to embodiment 1, and compared with Example 1, difference lies in by the parsing in embodiment 1
Liquid is transformed to acidity as 10% sulfuric acid, remaining step of preparation process and parameter all same.
After testing, in the desorbed solution obtained after final iterative parsing, cobalt tenor is significantly reduced as 11.2g/L.
Comparative example 202
The comparative example is set relative to embodiment 1, and compared with Example 1, difference lies in by the parsing in embodiment 1
Liquid is transformed to acidity as 2% sulfuric acid, remaining step of preparation process and parameter all same.
After testing, in the desorbed solution obtained after final iterative parsing, cobalt tenor is significantly reduced as 8.9g/L.
Claims (10)
1. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process, which is characterized in that by cobalt nickel wet smelting process, through extraction
Remove it is miscellaneous after magnesium solution containing cobalt, the processing included the following steps：
S1：Cobalt ions in the magnesium solution containing cobalt described in polyvalent metal absorption resins selective absorption, so as to which magnesium ion be stayed in
In solution.
2. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 1, which is characterized in that also wrap
It includes：
S2：Solution after step 1 adsorption treatment is adjusted into pH=7-9, the magnesium ion in filtrate is made to be converted into magnesium hydroxide and is sunk
It forms sediment；
S3：By the solution after being precipitated in step 2, with filter press press filtration, magnesium hydroxide solid filter cake is obtained, so as to fulfill magnesium elements point
From.
3. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 1, which is characterized in that the step
Rapid S1 includes following operation：
S101：The pH=2-3 of magnesium solution containing cobalt is adjusted, and controls the magnesium solution containing cobalt under 20-50 DEG C of temperature condition, with
3-6m3/ h flow velocitys adsorb resin by polyvalent metal, realize the selective absorption to cobalt metal ion in the sour magnesium liquid containing cobalt.
4. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 1 or 3, which is characterized in that institute
It states step S1 and further includes following operating procedure：
S102：The use of acid concentration is 4-9% after cobalt content in polyvalent metal absorption resin water outlet is more than 0.01g/L
Desorbed solution parsing polyvalent metal absorption resin, the desorbed solution and polyvalent metal absorption resin volume ratio be 2-4:1.
5. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 4, which is characterized in that described more
Valency metal adsorption resin is the Special Resin of model CH -90.
6. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 4, which is characterized in that the solution
Analysis liquid is sulfuric acid.
7. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process stated according to claim 4, which is characterized in that 1m3It is described more
The weight of the adsorbable cobalt of valency metal adsorption resin is 150-180kg.
8. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 2, which is characterized in that step S2
One or more of sodium hydroxide, potassium hydroxide is selected to adjust pH.
9. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 2, which is characterized in that described in warp
Filtering gained magnesium hydroxide solid purity is 90-97% in step S3.
10. cobalt magnesium separation method in a kind of cobalt nickel wet smelting process according to claim 2, which is characterized in that by cobalt
In nickel wet smelting process, the magnesium solution containing cobalt after abstraction impurity removal, the processing included the following steps：
S1：It is 2-3, and control the solution under 20-50 DEG C of temperature condition to adjust the pH value of magnesium solution containing cobalt, with flow velocity 3-
6m3/ h, by Special Resin CH -90, the selective absorption cobalts of Special Resin CH -90, and magnesium is stayed in the solution；
After the cobalt in Special Resin water outlet is more than 0.01g/L, using the sulfuric acid that acid concentration is 5-8% as parsing lyolysis
Resin is analysed, the sulfuric acid and resin volume ratio are 3:1, until the cobalt that the cobalt content in desorbed solution reaches in the acid dip solution contains
Until amount；Wherein, the desorbed solution can Reusability；
S2：It will adjust pH to 7~9 through step 1 treated solution using sodium hydroxide solution, be hydrolyzed to the magnesium in solution
Magnesium hydrate precipitate；
S3：The solution that will be fully hydrolyzed in step 2 after precipitating is 90~97% to get purity through filter press press filtration, and after filtering
Magnesium hydroxide solid filter cake, so as to fulfill magnesium metal impurities detach；Gained filtrate meets environmental emission standard, can directly arrange
It puts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810096634.XA CN108179272A (en) | 2018-01-31 | 2018-01-31 | Cobalt magnesium separation method in a kind of cobalt nickel wet smelting process |
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| CN109081475A (en) * | 2018-09-30 | 2018-12-25 | 荆门市格林美新材料有限公司 | A kind of comprehensive resource processing unit for the raffinate that cobalt nickel leaching process generates |
| CN109797294A (en) * | 2019-02-02 | 2019-05-24 | 广东芳源环保股份有限公司 | The method of nickel, cobalt is recycled in a kind of magnesium water |
| CN115161495A (en) * | 2022-08-18 | 2022-10-11 | 上海锦源晟新能源材料有限公司 | Method for separating and enriching cobalt from high-impurity cobalt sulfate solution |
| CN115341104A (en) * | 2022-08-19 | 2022-11-15 | 上海锦源晟新能源材料有限公司 | Method for reducing new water consumption in application process of ion exchange resin |
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| CN115341104B (en) * | 2022-08-19 | 2024-05-03 | 上海锦源晟新能源材料有限公司 | Method for reducing new water consumption in application process of ion exchange resin |
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