CN109609785A - The method of cobalt is separated from cobalt, manganese carbonate mixture - Google Patents
The method of cobalt is separated from cobalt, manganese carbonate mixture Download PDFInfo
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- CN109609785A CN109609785A CN201811565084.8A CN201811565084A CN109609785A CN 109609785 A CN109609785 A CN 109609785A CN 201811565084 A CN201811565084 A CN 201811565084A CN 109609785 A CN109609785 A CN 109609785A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- 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
- C22B23/0469—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods by chemical substitution, e.g. by cementation
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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
- C22B7/007—Wet processes by acid leaching
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The method that the invention discloses a kind of to separate cobalt from cobalt, manganese carbonate mixture.Method includes the following steps: S1, cobalt, manganese carbonate mixture are dissolved, obtain sour solution using inorganic acid；Alkali is added into sour solution in S2, adjusts solution ph to 7.3~7.5, sedimentation filtration, filter residue is Co (OH)2；Manganese powder is added in filtered filtrate into S2 in S3, displaces the Co in filtrate.It applies the technical scheme of the present invention, adjusts pH value first with inorganic acid solution slag (also known as, cobalt, manganese carbonate mixture), then with alkali, the Co (OH) in precipitating2It is obtained through filtering, the remaining cobalt in filtrate carries out displacement reaction with manganese powder, and the overall recovery of Co is made to reach 99%.The process flow is short, simple and easy, at low cost, high income, is suitble to large-scale production and application, and environmental protection and economy.
Description
Technical field
The present invention relates to metal purification technical fields, separate from cobalt, manganese carbonate mixture in particular to one kind
The method of cobalt.
Background technique
Cobalt is a kind of considerable national defense construction strategic materials, be widely used in space flight, aviation, electronics, battery,
The high-tech areas such as magnetic metal material.Content of the cobalt in the earth's crust is only 0.0012%, is belonged to than sparser metal, and
In nature, cobalt is coexisted with metallic elements such as manganese, nickel mostly.Since chemical property is similar, pole is brought to separating-purifying
The earth is difficult.
Existing cobalt, manganese isolation technics mainly have following three kinds: 1) hydroxide precipitation method: the separation of cobalt from manganese in hydrometallurgy
Crude separation is usually carried out using carbonate precipitation method, then carries out extracting and refining.This method higher cost, complex process, and
The final rate of recovery of cobalt only has 92%~94% or so, and a large amount of cobalt resources are wasted.2) manganese oxidation-precipitation method: is made by oxidant
With MnO2Form precipitating, so that it be separated with cobalt；Usually with ozone, chloric acid, SO2/O2Mixture is that oxidant carries out instead
It answers, but due to Co3+Become Co2+Normal potential be 1.8V, and Mn4+Become Mn2+Normal potential be 1.23V, the electricity of the two
Potential difference is larger, only controls oxidizer and pH value appropriate, can just make Mn2+Preferential Co2+Oxidation generates MnO2Precipitating.
3) solvent extraction: since above-mentioned two classes method separating effect is poor, also there is the technology for recycling extractant to be refined,
But higher cost has implemented certain difficulty.
Wherein, hydroxide precipitation method is mainly that the difference for the hydroxide solubility product that cobalt and manganese is utilized carries out selecting to sink
It forms sediment, Mn (OH)2: 19 × 10-13；Co(OH)2:1.6×10-15Cobalt is precipitated prior to manganese salt.It is single but since the two solubility product is close
One can not be thoroughly by separation of cobalt from manganese using hydroxide, Co (OH) that precipitation reaction obtains2In often contain more manganese.And it is sharp
With joint ammonia process, manganese is precipitated in the form of manganese carbonate, and cobalt then stays in the solution due to forming ammino-complex, though this method can carry out depth
Degree separation, but complex process, higher cost are unfavorable for production application.
To sum up, in prior art technology, energy consumption is high, yield is low for the purification of cobalt, and there is also environmental issues for some, greatly
Making full use of for resource is affected, causes much to waste.
Summary of the invention
The present invention is intended to provide a kind of method that cobalt is separated from cobalt, manganese carbonate mixture, to solve in the prior art
The technical problem that the separating energy consumption of cobalt is big, yield is low.
To achieve the goals above, according to an aspect of the invention, there is provided one kind is from cobalt, manganese carbonate mixture
The method for separating cobalt.Method includes the following steps: S1, cobalt, manganese carbonate mixture are dissolved, it is molten to obtain acid using inorganic acid
Solution；Alkali is added into sour solution by S2, and adjustment solution ph to 7.3~7.6, filtering, filter residue is Co (OH)2；S3, to
Manganese powder is added in filtered filtrate in S2, displaces the Co in filtrate.
Further, in S1, the pH of obtained sour solution is 1.5~2.5.
Further, in S1, cobalt, manganese carbonate mixture are dissolved using inorganic acid under the conditions of 20~60 DEG C of temperature,
Preferably 35~45 DEG C.
Further, in S3, the molar ratio that cobalt content in the amount and solution of manganese powder is added into filtrate is 1.5~3:1, excellent
It is selected as 2~2.5:1.
Further, in S3, filtrate is warming up to 60~90 DEG C, manganese powder is then added.
Further, the content of cobalt is 2~4g/L in filtrate.
Further, in the filtrate after manganese powder is replaced Co content≤0.2g/L.
Further, inorganic acid is sulfuric acid.
Further, alkali is sodium hydroxide, potassium hydroxide or sodium carbonate solid or aqueous solution.
Further, alkali is sodium hydroxide solution.
It applies the technical scheme of the present invention, first with inorganic acid solution slag (also known as, cobalt, manganese carbonate mixture), then
PH value is adjusted with alkali, the Co (OH) in precipitating2It is obtained through filtering, the remaining cobalt in filtrate carries out displacement reaction with manganese powder, makes Co
Overall recovery reach 99%.The process flow is short, simple and easy, at low cost, high income, is suitble to large-scale production and application, and
Environmental protection and economy.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
For in the prior art, the technical problem that the separating energy consumption of cobalt is big, yield is low, the present inventor is proposed down
Column technical solution.
A kind of typical embodiment according to the present invention provides a kind of side that cobalt is separated from cobalt, manganese carbonate mixture
Method.Method includes the following steps: S1, cobalt, manganese carbonate mixture are dissolved, obtain sour solution using inorganic acid；S2, to
Alkali is added in sour solution, adjustment solution ph to 7.3~7.6, filtering, filter residue is Co (OH)2；S3, after being filtered into S2
Filtrate in manganese powder is added, displace the Co in filtrate.
It applies the technical scheme of the present invention, first with inorganic acid solution slag (also known as, cobalt, manganese carbonate mixture), then
PH value is adjusted with alkali, the Co (OH) in precipitating2It is obtained through filtering, the remaining cobalt in filtrate carries out displacement reaction with manganese powder, makes Co
Overall recovery reach 99%.The process flow is short, simple and easy, at low cost, high income, is suitble to large-scale production and application, and
Environmental protection and economy.
Wherein, alkali can be sodium hydroxide, potassium hydroxide or sodium carbonate solid or aqueous solution, from industrial effect and
Cost consideration is preferably sodium hydroxide.PH value regulation is carried out using sodium hydroxide, provides advantage for accurate heavy cobalt, strictly
The pH value of solution is controlled in appropriate range (pH value 7.3~7.6), can obtain containing the lower cobalt hydroxide of manganese and higher cobalt
Yield.
Preferably, in S1, the pH of obtained sour solution is 1.5~2.5, under this acidity condition, can either guarantee cobalt
Abundant dissolution, and will not make the presence of excessive superfluous acid in system.
Preferably, in S1, at 20~60 DEG C, use inorganic acid by cobalt, manganese carbonate under the conditions of preferably 35~45 DEG C of temperature
Mixture dissolution, can be such that cobalt dissolves faster, and excessive side reaction will not occur, and can take into account in this temperature condition
The reasonability of production efficiency and energy consumption.
Mn/Co ratio determines the replacement rate that manganese powder quantity and cobalt is added, it is preferred that in S3, manganese powder is added into filtrate
Amount and the molar ratio of cobalt content in solution are 1.5~3:1, and preferably 2~2.5:1 accomplishes on the basis of making full use of raw material
Cobalt is sufficiently displaced from.
Manganese powder displacement when temperature determine replacement rate, it is preferred that in S3, filtrate is warming up to 60~90 DEG C, then plus
Enter manganese powder, under the conditions of this temperature, can be realized the high efficiency displacement of cobalt.
A kind of typical embodiment according to the present invention, the content of cobalt is 2~4g/L in filtrate；After manganese powder is replaced
Content≤0.2g/L of Co in filtrate.
Theoretically, the present invention in inorganic acid can with sulfuric acid, hydrochloric acid or nitric acid etc., but from industrial cost, operation
Convenience and the corrosivity etc. of equipment is comprehensively considered, inorganic acid preferably sulfuric acid.
Beneficial effects of the present invention are further illustrated below in conjunction with embodiment, the step of being not described in the present invention
Or substance can be realized or be commercially available by ordinary skill in the art means.
Comparative example 1,
With in sodium hydroxide and heavy cobalt
Raw material: cobalt, manganese carbonate mixture main component: Mn:24.84%.Co:13.20%, moisture content of the raw material:
20.0% raw material: 125g, 100g containing siccative.Add water to size mixing to 400ml, sulfuric acid 42ml is added and sufficiently dissolves, endpoint pH control
2.5, sodium hydroxide solution is added and adjusts pH value, the cobalt terminal pH that sinks is 7.41.Filtration washing must sink liquid and cobalt slag after cobalt.After heavy cobalt
Liquid 600ml, 3.39g/L containing cobalt.Cobalt slag 25.18g, cobalt slag contain Co 43.8%, Mn 8.76%.
The rate of deposition of cobalt are as follows: 84.59%.
Comparative example 2,
Heavy cobalt is replaced with manganese powder
Test stoste is the cobalt-carrying solution 500ml, 4.40g/L containing Co prepared.5.13g manganese powder is claimed to be added to cobalt-carrying solution
In, it is stirred to react 1h at 60 DEG C, the 500ml that filters to get filtrate (including a small amount of wash water).Manganese powder use level coefficient is 2.50 (mol/
Mol), filtrate 0.2g/L containing Co.
The rate of deposition of cobalt are as follows: 95.45%.
Two above test has respectively represented precipitating when sodium hydroxide neutralization precipitation method and the exclusive use of manganese powder displacement method
Effect.The former rate of deposition is low, and medicament is cheap, and the latter's rate of deposition is high, but manganese powder price is higher.Two methods are combined, hydrogen is first used
Sodium oxide molybdena uses manganese powder afterwards, then the higher rate of recovery not only may be implemented, but also medicament expense can be greatly lowered.Two kinds of slags merge
The as product of this technique, the technique realize the enrichment of cobalt, and have got rid of most of manganese.
Embodiment 1
In one section of sodium hydroxide and heavy cobalt
Claim wet feed 125g, adds water slurry to 400ml, add sulfuric acid 42ml, be equivalent to pure H2SO474.09g is abundant at 40 DEG C
1h is dissolved, terminal PH is 2.5.Thereafter with residual acid and heavy cobalt in adding sodium hydroxide solution, altogether plus NaOH 16.3g, terminal PH are
7.34.It is filtered after reaction 2h, obtains filtrate 650ml, cobalt slag 28.35g.Filtrate 2.92g/L containing Co, cobalt slag contain Co 41.82%, Mn
10.38%, Co/Mn=4.03 (g/g) in slag.
The rate of deposition of cobalt are as follows: 85.62%.
Two sections of manganese powders replace heavy cobalt
Liquid 600ml after heavy cobalt, manganese addition powder 2.86g are taken, manganese powder use level coefficient is 1.75 (mol/mol).It is stirred at 80 DEG C
1h filtering is reacted, filtrate 640ml, replacement slag 3.55g are obtained.Filtrate 0.43g/L containing Co, replacement slag contain Co 39.26%, Mn
32.02%, Co/Mn=1.23 (g/g) in slag.
The replacement rate of cobalt are as follows: 84.29%.
Total rate of deposition of two sections of cobalts is 97.74%, the Co/Mn=in rich cobalt material (two kinds of precipitation mixtures, the same below)
3.20 (g/g), the removal efficiency of manganese are as follows: 85.06%.
Embodiment 2
In one section of sodium hydroxide and heavy cobalt
Claim wet feed 125g, adds water slurry to 500ml, add sulfuric acid 45ml, be equivalent to H2SO479.38g.It is stirred at 60 DEG C
0.5h is dissolved, terminal PH is 1.93.With residual acid and heavy cobalt in adding sodium hydroxide solution, altogether plus NaOH 22.21g, terminal PH are
7.49.It is filtered after reaction 1h, obtains filtrate 714ml, cobalt slag 29.11g.Filtrate 2.45g/L containing Co, cobalt slag contain Co39.20%,
Mn9.26%, Co/Mn=4.07 (g/g) in slag.
The rate of deposition of cobalt are as follows: 86.75%
Two sections of manganese powders replace heavy cobalt
Liquid 600ml after heavy cobalt, manganese addition powder 3.43g are taken, manganese powder use level coefficient is 2.50 (mol/mol).It is stirred at 60 DEG C
2h is reacted, filter to get filtrate 700ml, replacement slag 6.32g.Filtrate 0.24g/L containing Co, replacement slag contain Co18.91%,
Mn40.80%, Co/Mn=0.46 (g/g) in slag.
The replacement rate of cobalt are as follows: 88.57%
Total rate of deposition of two sections of cobalts is 98.49%, the Co/Mn=2.19 (g/g) in rich cobalt material, the removal efficiency of manganese are as follows:
80.07%.
Embodiment 3
The heavy cobalt of one section of sodium hydroxide
Claim wet feed 125g, adds water slurry to 400ml, add sulfuric acid 45ml, be equivalent to pure H2SO479.38g dissolves at 60 DEG C
1h, terminal PH are 2.0.Thereafter adding sodium hydroxide solution sinks cobalt, altogether plus NaOH 24.5g, terminal PH7.60.It is filtered after reaction 2h.
Filtrate 600ml, cobalt slag 30.3g, filtrate contain Co1.95g/L, cobalt slag contains Co39.40%, Mn10.20%, Co/Mn=in slag
3.86(g/g)。
The rate of deposition of cobalt are as follows: 91.14%
Liquid 550ml after heavy cobalt, manganese addition powder 2.5g are taken, manganese powder use level coefficient is 2.50 (mol/mol).It is stirred at 80 DEG C anti-
1h is answered, filtrate 590ml is obtained, replacement slag 4.61g. filtrate contains Co0.18g/L.Replacement slag contains Co21.01%Mn38.60%, in slag
Co/Mn=0.54 (g/g).
Cobalt replacement rate are as follows: 90.10%
Total rate of deposition of two sections of cobalts are as follows: 99.12%.Co/Mn=2.58 (g/g) in rich cobalt material.
The removal efficiency of manganese are as follows: 81.75%.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
1) solvent extraction, simple process and low cost are replaced with manganese powder；
2) in manganese powder addition system, other property substances will not be introduced, are clean system, no environmental issue；
3) rate of recovery of Co is increased to 99% by 95% or so of conventional method, and economic benefit is obvious；
4) all operations step can carry out in same equipment, without extra equipment investment is increased, compared with traditional handicraft advantage
Obviously.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method for separating cobalt from cobalt, manganese carbonate mixture, which comprises the following steps:
Cobalt, manganese carbonate mixture are dissolved using inorganic acid, obtain sour solution by S1；
Alkali is added into the sour solution in S2, and adjustment solution ph to 7.3~7.6, filtering, filter residue is Co (OH)2；
Manganese powder is added in filtered filtrate in S3, Xiang Suoshu S2, displaces the Co in the filtrate.
2. the method according to claim 1, wherein the pH of the obtained sour solution is 1.5 in the S1
~2.5.
3. the method according to claim 1, wherein using nothing under the conditions of 20~60 DEG C of temperature in the S1
Machine acid dissolves cobalt, manganese carbonate mixture, and preferably 35~45 DEG C.
4. the method according to claim 1, wherein in the S3, be added in Xiang Suoshu filtrate the amount of manganese powder with
The molar ratio of cobalt content is 1.5~3:1, preferably 2~2.5:1 in solution.
5. according to the method described in claim 3, it is characterized in that, the filtrate is warming up to 60~90 DEG C, so in the S3
After manganese powder is added.
6. the method according to claim 1, wherein the content of cobalt is 2~4g/L in the filtrate.
7. the method according to claim 1, wherein in filtrate after manganese powder is replaced Co content≤
0.2g/L。
8. the method according to claim 1, wherein the inorganic acid is sulfuric acid.
9. the method according to claim 1, wherein the alkali is that sodium hydroxide, potassium hydroxide or sodium carbonate are solid
Body or aqueous solution.
10. according to the method described in claim 9, it is characterized in that, the alkali is sodium hydroxide solution.
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| CN201811565084.8A CN109609785B (en) | 2018-12-20 | 2018-12-20 | Method for separating cobalt from cobalt and manganese carbonate mixture |
| PCT/CN2019/096005 WO2020125000A1 (en) | 2018-12-20 | 2019-07-15 | Method for separating cobalt from cobalt and manganese carbonate mixture |
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| WO2020125000A1 (en) * | 2018-12-20 | 2020-06-25 | 中国恩菲工程技术有限公司 | Method for separating cobalt from cobalt and manganese carbonate mixture |
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