CN109468472A - A method of separating cobalt from the material containing cobalt and nickel - Google Patents
A method of separating cobalt from the material containing cobalt and nickel Download PDFInfo
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- CN109468472A CN109468472A CN201811549620.5A CN201811549620A CN109468472A CN 109468472 A CN109468472 A CN 109468472A CN 201811549620 A CN201811549620 A CN 201811549620A CN 109468472 A CN109468472 A CN 109468472A
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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
- C22B23/0476—Separation of nickel from cobalt
- C22B23/0492—Separation of nickel from cobalt in ammoniacal type solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/34—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing sulfur, e.g. sulfonium
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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
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Abstract
The invention belongs to material recovery field, a method of separating cobalt from the material containing cobalt and nickel.(1) alkali soaks: hydrogen peroxide and dilute sulfuric acid mixed liquor will be added in the material powder containing cobalt and nickel, after being sufficiently mixed, adds (NH4)2SO4With concentrated ammonia liquor mixed liquor, sufficiently after reaction, extraction stoste is obtained；(2) it extracts: sulphur cyanogen type Arquad is added into extraction stoste and carries out cobalt extraction, obtains the extraction phase containing cobalt；(3) it is stripped: dilute hydrochloric acid being added in extraction phase containing cobalt and is stripped to obtain cobalt chloride；Wherein sulphur cyanogen type Arquad is R3CH3NSCN, wherein R is the group of C8~C12.Selectivity height is leached using alkali, only copper, cobalt, nickel can enter solution with ammonium ion formation complex compound with ammonium root complex form, and other metals do not enter, and can save complicated removal step.The application technique carries out under room temperature, normal pressure, and temperature and pressure is not the restrictive condition of extraction.
Description
Technical field
The invention belongs to material recovery fields, and in particular to a method of cobalt is separated from the material containing cobalt and nickel.
Background technique
China's cobalt resource extremely lacks, and cobalt and nickel are often association and symbiosis in mineral products, leads to cobalt, nickel separative efficiency
It is not high.Also contain each metalloid in used Li ion cell, wherein content is high in cobalt lithium metal battery electrode material, and some is even super
30% is crossed, cobalt content is 850 times or more of association cobalt ore content.Since lithium ion battery learies increase year by year, at present to useless
The heavy metal recovery of old lithium ion battery obtains extensive concern.Cobalt is expensive, and cobalt is being cured not only in national defense and military fields
Play a significant role in the products such as medicine, industry, therefore secondary resource valuable when cobalt in used Li ion cell, recycle useless lithium from
Cobalt has very high economic benefit and environmental benefit in sub- battery.
Since cobalt and nickel chemical property are close, when leading to Call Provision, there is the interference of nickel and make the rate of recovery of cobalt low and return
Receive the problems such as purity is not high.In used Li ion cell recycling smithcraft, is pre-processed, finally obtained containing cobalt by Ore Leaching etc.
Solution, wherein more containing the foreign metals such as nickel and a small amount of iron, magnesium, manganese, calcium, to reduce the cobalt rate of recovery and purity.This
Outside, the problem of cobalt and nickel separation difficulty can be met in hydrometallurgy cobalt ore；In industries such as electrodeposit, petrochemical industry, Precise Alloys
The electroplate liquid containing cobalt, nickel can be generated, when recycling cobalt therein, also faces the problem of cobalt, nickel separation hardly possible.
To improve the cobalt rate of recovery and recycling purity, needing a kind of pair, cobalt metal selective is strong, recovery efficiency is high, reaction rate
Fastly, simple process, input cost low method and technique, while recovery process condition carries out under room temperature, normal pressure.Call Provision
Technology has Ore Leaching, electrolysis, extraction etc., and wherein extraction has the characteristics that selectivity is high, at low cost, is hydrometallurgical mature work
Skill, a wide range of industrial applications.The extractant of Call Provision mostly uses phosphoric acid kind of extractants at present, as Cyanex272,
D2EHPA, P204, P507 etc., these extractants or expensive, such as Cyanex272, usually import extractant or
Extract cobalt selectivity it is not high, cause Call Provision purity not high, still containing 10% or so nickel, or need two kinds or two kinds with
Upper extractant coextraction increases process complexity.Ammonium salt kind of extractants selectivity in terms of cobalt extraction is high, cheap, but has
The interference of the foreign metals such as iron, manganese, nickel, magnesium causes recycling purity and the rate of recovery to reduce, and therefore, ammonium salt kind of extractants is useless
Seldom, relevant report yet there are no for the cobalt extraction aspect application of lithium battery.
Summary of the invention
The present invention in order to solve the problems, such as that the cobalt rate of recovery is low in the presence of the prior art, purity is not high, provide it is a kind of from
The method of cobalt is separated in material containing cobalt and nickel.
In order to solve the above technical problems, technical solution used by the application is, it is a kind of to divide from the material containing cobalt and nickel
Method from cobalt, includes the following steps:
(1) alkali soaks:
Hydrogen peroxide and dilute sulfuric acid mixed liquor will be added in material containing cobalt and nickel, after being sufficiently mixed, adds (NH4)2SO4
With concentrated ammonia liquor mixed liquor, sufficiently after reaction, extraction stoste is obtained；
(2) it extracts:
Sulphur cyanogen type Arquad is added into extraction stoste and carries out cobalt extraction, obtains extraction phase containing cobalt；
(3) it is stripped:
Dilute hydrochloric acid is added in extraction phase containing cobalt to be stripped to obtain cobalt chloride；
Wherein sulphur cyanogen type Arquad is R3CH3NSCN, wherein R is the group of C8~C12.
Specifically, the material containing cobalt and nickel is the cathode electrode material or cathode and anode of used Li ion cell
Mixed electrode material.
Further, the alkali is carried out after the electrode material being crushed again and soaks step；(NH is added in step (1)4)2SO4
It after sufficiently reacting with concentrated ammonia liquor mixed liquor, carries out extraction Copper treatment: obtaining including separation removal solid powder containing cobalt, copper, nickel
After solution, containing cobalt, copper, nickel solution in copper extractant extracting copper is added, obtain the solution containing cobalt and nickel, i.e. extraction original
Liquid.Extraction Copper treatment is enough effectively to avoid influence of the copper to extraction, and copper extractant can be used any in N902 and AD100.
Further, hydrogen peroxide concentration is 2~5M in hydrogen peroxide described in step (1) and dilute sulfuric acid mixed solution, described
Dilute sulfuric acid concentration is 0.1~1M；The volume ratio of the hydrogen peroxide and dilute sulfuric acid is 1:1~1:4；The electrode material and hydrogen peroxide
Mixed liquor solid-liquid mass ratio with dilute sulfuric acid is 1:3~1:10.H is added2O2It is that the trivalent cobalt in material is reduced to divalent cobalt,
H2O2As reducing agent.
Preferably, (the NH4)2SO4With (NH in concentrated ammonia liquor mixed liquor4)2SO4Concentration is 1~6M and concentrated ammonia liquor concentration
For 5~9M, (NH4)2SO4It is 1:1~5:1, the concentrated ammonia liquor and electrode material powder liquid stereoplasm with concentrated ammonia liquor mass ratio
Amount is than being 3:1~10:1.
Preferably, by the sulphur cyanogen type Arquad and diluent sulfonated kerosene and modifying agent isopropanol when extracting
Mixing, wherein being calculated as 10~30% diluent sulfonated kerosenes, 5~25% modifying agent isopropanols and 45~65% by volume fraction
R3CH3NSCN extractant, when extraction sulphur cyanogen type Arquad concentration in organic phase be 0.8~1.6mol/L, compare
O/A is 1~3, and the extraction initial pH of stoste is 5~8；The extraction is under room temperature, normal pressure with the three-level counter-current extraction residence time
30~50min is then allowed to stand layering, is stripped.
Further, the concentration of the dilute hydrochloric acid is 0.02~0.1M, compared to A/O is 1~3 when back extraction, the residence time
For 20-40min.
Further, the R3CH3NSCN is by R3CH3NCl and the 1.6M KSCN solution newly configured are sufficiently mixed shape
At it is 1 that wherein water phase, which compares A/O ratio with oil,.
The utility model has the advantages that H2O2As reducing agent, trivalent cobalt effectively can be reduced to divalent cobalt, the cobalt in material is as oxygen
Agent.Alkali leaching uses (NH4)2SO4High with concentrated ammonia liquor selectivity, cobalt, copper, nickel in material can form complex compound with ammonium ion
Enter solution with ammonium root complex form, and other metals do not enter, so that cobalt, copper, nickel metal are immersed in solution, and its
His metal stays in electrode material powder, and [Co (the NH of ammonium complex compound containing cobalt is obtained after extracting copper3)6]SO4With nickel ammonium complex compound [Ni
(NH3)6]SO4Solution.Complicated removal step can be saved.
It is stripped with dilute hydrochloric acid, back extraction is more preferable compared to pure water back extraction effect.
The application technique carries out under room temperature, normal pressure, and temperature and pressure is not the restrictive condition of extraction.
Detailed description of the invention
Fig. 1 is 1 process flow chart of embodiment；
Fig. 2 is 1 three-level counter-current extraction process flow chart of embodiment；
Specific embodiment
Technical solution of the invention is further illustrated combined with specific embodiments below, these embodiments should not be understood as
It is the limitation to technical solution.
Embodiment 1
Step as shown in Figure 1 are as follows:
(1) alkali soaks: after useless ion battery electric discharge, decladding, dismantling, natural air drying smashes cathode electrode material to 200
Mesh.Add H2O2(4M)+H2SO4(0.1M) mixed solution (hydrogen peroxide is 1:3 with dilute sulfuric acid volume ratio), the electrode material
It is 1:3 with the mixed liquor solid-liquid mass ratio of hydrogen peroxide and dilute sulfuric acid, wherein will be reduced to divalent cobalt by trivalent cobalt, sufficiently after reaction,
Add (NH4)2SO4(1M) and concentrated ammonia liquor (5M) (wherein (NH4)2SO4With concentrated ammonia liquor mass ratio be 5:1, concentrated ammonia liquor with
It is 3:1 that electrode material powder liquid, which consolidates mass ratio), sufficiently after reaction, then obtain through filtering removal solid powder containing cobalt, copper, nickel
Solution, then containing cobalt, copper, nickel solution in copper extractant N902 extracting copper is added, obtain the solution containing cobalt and nickel, i.e., extraction is former
Liquid:
(2) it extracts: sulphur cyanogen type Arquad is added into extraction stoste and carries out three-level counter-current extraction (as shown in Figure 2),
Obtain extraction phase containing cobalt；
Wherein sulphur cyanogen type Arquad is R3CH3NSCN, R is C8 alkyl in the present embodiment, by the sulphur cyanogen when extraction
Type Arquad is mixed with diluent sulfonated kerosene and modifying agent isopropanol, wherein being calculated as 10% diluent by volume fraction
Sulfonated kerosene, 25% modifying agent isopropanol and 65%R3CH3NSCN extractant, sulphur cyanogen type Arquad is organic when extraction
Concentration is 1mol/L in phase, is 1 compared to O/A, and the initial stoste pH that extracts is 8, and extraction is to be extracted under room temperature, normal pressure with three stage countercurrents
It takes, residence time 30min is then allowed to stand layering.
(3) it is stripped: dilute hydrochloric acid being added in extraction phase containing cobalt and is stripped to obtain cobalt chloride, wherein the concentration of dilute hydrochloric acid is
0.02M, A/O is 1 when back extraction, residence time 25min.
Wherein extractant is R3CH3The preparation method of NSCN is, by R3CH3NCl is filled with the 1.6M KSCN solution newly configured
Divide and be mixed to form, it is 1 that wherein water phase, which compares A/O ratio with oil,.
Through detecting, the extraction yield 98.2% of cobalt, the back extraction ratio of cobalt is 99.95%.Finally obtain the cobalt chloride rate of recovery
98.2%, purity 97.7%.
Embodiment 2
(1) alkali soaks: after useless ion battery electric discharge, decladding, dismantling, natural air drying, by anode and cathode electrode material one
It smashes with mixing to 200 mesh.Add H2O2(2M)+H2SO4(0.6M) mixed solution (hydrogen peroxide is 1 with dilute sulfuric acid volume ratio:
1), the mixed liquor solid-liquid mass ratio of the electrode material and hydrogen peroxide and dilute sulfuric acid is 1:6, wherein will be reduced to divalent by trivalent cobalt
Cobalt adds (NH sufficiently after reaction4)2SO4(3M) and concentrated ammonia liquor (7M) (wherein (NH4)2SO4With concentrated ammonia liquor mass ratio
For 2:1, concentrated ammonia liquor and electrode material powder liquid consolidate mass ratio as 7:1), sufficiently after reaction, then remove solid powder through filtering
Obtain containing cobalt, copper, nickel solution, then containing cobalt, copper, nickel solution in copper extractant N902 extracting copper is added, obtain containing cobalt and
The solution of nickel, i.e. extraction stoste.
(2) it extracts: sulphur cyanogen type Arquad is added into extraction stoste and carries out three-level counter-current extraction, obtain extracting containing cobalt
Phase；
Wherein sulphur cyanogen type Arquad is R3CH3NSCN, R is C10 alkyl in the present embodiment, by the sulphur when extraction
Cyanogen type Arquad is mixed with diluent sulfonated kerosene and modifying agent isopropanol, wherein being calculated as 30% dilution by volume fraction
Agent sulfonated kerosene and 25% modifying agent isopropanol, 45%R3CH3NSCN extractant, sulphur cyanogen type Arquad is having when extraction
Concentration is 0.8mol/L in machine phase, is 2 compared to O/A, and the initial stoste pH that extracts is 7, and extraction is under room temperature, normal pressure with three stage countercurrents
Extraction, residence time 40min are then allowed to stand layering.
(3) it is stripped: dilute hydrochloric acid being added in extraction phase containing cobalt and is stripped to obtain cobalt chloride, wherein the concentration of dilute hydrochloric acid is
0.06M compared to A/O is 2 when back extraction, residence time 30min.
Through detecting, the extraction yield 97.9% of cobalt, the back extraction ratio of cobalt is 99.95%.Finally obtain the cobalt chloride rate of recovery
97.9%, purity 97.2%.
Embodiment 3
(1) alkali soaks: after useless ion battery electric discharge, decladding, dismantling, natural air drying, by anode and cathode electrode material one
It smashes with mixing to 200 mesh.Add H2O2(5M)+H2SO4(1M) mixed solution (hydrogen peroxide is 1:4 with dilute sulfuric acid volume ratio),
The mixed liquor solid-liquid mass ratio of the electrode material and hydrogen peroxide and dilute sulfuric acid is 1:10, wherein will be reduced to divalent by trivalent cobalt
Cobalt adds (NH sufficiently after reaction4)2SO4(6M) and concentrated ammonia liquor (9M) (wherein (NH4)2SO4With concentrated ammonia liquor mass ratio
For 1:1, concentrated ammonia liquor and electrode material powder liquid consolidate mass ratio as 10:1), sufficiently after reaction, then remove solid powder through filtering
Obtain containing cobalt, copper, nickel solution, then containing cobalt, copper, nickel solution in copper extractant N902 extracting copper is added, obtain containing cobalt and
The solution of nickel, i.e. extraction stoste；
(2) it extracts: sulphur cyanogen type Arquad is added into extraction stoste and mutually carries out three-level counter-current extraction, obtain extracting containing cobalt
Take phase；
Wherein sulphur cyanogen type Arquad is R3CH3NSCN, R is C12 alkyl in the present embodiment, by the sulphur when extraction
Cyanogen type Arquad is mixed with diluent sulfonated kerosene and modifying agent isopropanol, wherein being calculated as 30% dilution by volume fraction
Agent sulfonated kerosene, 5% modifying agent isopropanol and 65%R3CH3NSCN extractant, sulphur cyanogen type Arquad is organic when extraction
Concentration is 1.6mol/L in phase, is 3 compared to O/A, and extracting initial pH in stoste is 5, and extraction is under room temperature, normal pressure with three stage countercurrents
Extraction, residence time 50min are then allowed to stand layering.
(3) it is stripped: dilute hydrochloric acid being added in extraction phase containing cobalt and is stripped to obtain cobalt chloride, wherein the concentration of dilute hydrochloric acid is
0.1M compared to A/O is 3 when back extraction, residence time 20min.
Through detecting, the extraction yield 98.8% of cobalt, the back extraction ratio of cobalt is 99.92%.Finally obtain the cobalt chloride rate of recovery
98.8%, purity 97.0%.
Comparative example
Stripping agent dilute hydrochloric acid in embodiment 1 is replaced with into pure water, the other the same as in Example 1.
Stripping agent is done with pure water, calculates the back extraction ratio of cobalt, obtained data such as the following table 1.
Table 1
From table 1 it follows that the stratification time is 0.58h when being 1 compared to A/O, the back extraction ratio of cobalt is
96.34%, back extraction ratio when less than in the application using dilute hydrochloric acid as stripping agent.
Claims (8)
1. a kind of method for separating cobalt from the material containing cobalt and nickel, which comprises the steps of:
(1) alkali soaks:
Hydrogen peroxide and dilute sulfuric acid mixed liquor will be added in material containing cobalt and nickel, after being sufficiently mixed, adds (NH4)2SO4With it is dense
Ammonia water mixture sufficiently after reaction, obtains extraction stoste；
(2) it extracts:
Sulphur cyanogen type Arquad is added into extraction stoste and carries out cobalt extraction, obtains extraction phase containing cobalt；
(3) it is stripped:
Dilute hydrochloric acid is added in extraction phase containing cobalt to be stripped to obtain cobalt chloride；
Wherein sulphur cyanogen type Arquad is R3CH3NSCN, wherein R is the group of C8~C12.
2. the method according to claim 1 for separating cobalt from the material containing cobalt and nickel, which is characterized in that described contains cobalt
Material with nickel is the cathode electrode material of used Li ion cell or the mixed electrode material of cathode and anode.
3. the method according to claim 2 for separating cobalt from the material containing cobalt and nickel, which is characterized in that by the electrode
The alkali leaching step is carried out after material disintegrating again；
(NH is added in step (1)4)2SO4After sufficiently reacting with concentrated ammonia liquor mixed liquor, carry out extraction Copper treatment: obtain containing cobalt, copper,
After the solution of nickel, containing cobalt, copper, nickel solution in be added copper extractant extracting copper, obtain the solution containing cobalt and nickel, i.e., the described extraction
Stoste.
4. the method according to claim 3 for separating cobalt from the material containing cobalt and nickel, which is characterized in that in step (1)
Hydrogen peroxide concentration is 2~5M in the hydrogen peroxide and dilute sulfuric acid mixed solution, and the dilute sulfuric acid concentration is 0.1~1M；It is described double
The volume ratio of oxygen water and dilute sulfuric acid is 1:1~1:4；The mixed liquor solid-liquid mass ratio of the electrode material and hydrogen peroxide and dilute sulfuric acid
For 1:3~1:10.
5. the method according to claim 3 for separating cobalt from the material containing cobalt and nickel, which is characterized in that (the NH4)2SO4With (NH in concentrated ammonia liquor mixed liquor4)2SO4Concentration is 1~6M and concentrated ammonia liquor concentration is 5~9M, (the NH4)2SO4With it is dense
Ammonium hydroxide mass ratio is 1:1~5:1, and it is 3:1~10:1 that the concentrated ammonia liquor and electrode material powder liquid, which consolidate mass ratio,.
6. the method according to claim 3 for separating cobalt from the material containing cobalt and nickel, which is characterized in that by institute when extraction
Sulphur cyanogen type Arquad is stated to mix with diluent sulfonated kerosene and modifying agent isopropanol, wherein 10 are calculated as by volume fraction~
30% diluent sulfonated kerosene, 5~25% modifying agent isopropanols and 45~65%R3CH3NSCN extractant, when extraction the sulphur cyanogen
Type Arquad concentration in organic phase is 0.8~1.6mol/L, is 1~3 compared to O/A, and the extraction initial pH of stoste is 5~8；
The extraction is to be then allowed to stand layering with three-level counter-current extraction 30~50min of residence time under room temperature, normal pressure, is carried out anti-
Extraction.
7. the method according to claim 3 for separating cobalt from the material containing cobalt and nickel, it is characterised in that: dilute salt
The concentration of acid is 0.02~0.1M, compared to A/O is 1~3 when back extraction, residence time 20-40min.
8. the method according to claim 1 for separating cobalt from the material containing cobalt and nickel, which is characterized in that described
R3CH3NSCN is by R3CH3NCl is thoroughly mixed to form with the 1.6M KSCN solution newly configured, and wherein water phase compares A/O ratio with oil
It is 1.
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| CN113026056A (en) * | 2021-03-08 | 2021-06-25 | 成都盛威兴科新材料研究院合伙企业(有限合伙) | Method for producing electrolytic cobalt by adopting secondary electrolysis of cobalt intermediate product |
| JP7442891B1 (en) | 2023-05-15 | 2024-03-05 | メック株式会社 | How to dispose of lithium-ion battery waste |
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| JP7442891B1 (en) | 2023-05-15 | 2024-03-05 | メック株式会社 | How to dispose of lithium-ion battery waste |
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