CN105907995A - Method for separating and recovering cobalt and manganese in low-cobalt and high-manganese waste by virtue of sulphide salt and oxidizing agent - Google Patents
Method for separating and recovering cobalt and manganese in low-cobalt and high-manganese waste by virtue of sulphide salt and oxidizing agent Download PDFInfo
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- CN105907995A CN105907995A CN201610528150.9A CN201610528150A CN105907995A CN 105907995 A CN105907995 A CN 105907995A CN 201610528150 A CN201610528150 A CN 201610528150A CN 105907995 A CN105907995 A CN 105907995A
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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
- C22B47/00—Obtaining manganese
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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
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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
- C22B47/00—Obtaining manganese
- C22B47/0009—Obtaining manganese from spent catalysts
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a method for separating and recovering cobalt and manganese in a low-cobalt and high-manganese waste by virtue of sulphide salt and oxidizing agent. The method comprises the following step: pretreating the low-cobalt and high-manganese waste; then adding sulphide salt to react with treating liquid; filtering after the reaction is finished so as to obtain a manganese-containing solution and a cobalt sulfide precipitate; performing acid dissolving on cobalt sulfide; then adding the oxidizing agent to a digestion solution to remove manganese residual in the solution so as to obtain a manganese-containing precipitate and a cobalt-containing solution and realize high separation of cobalt from manganese; and finally adding carbonate to a manganese sulfide solution to recover manganese. The method is simple in process, and low in cost; cobalt and manganese can be completely separated, and the recovery rate is high; the recovery rate of cobalt is up to be 95% or above; the recovery rate of manganese is up to be 99% or above; the additional value of a product is high; the method is applicable to mass industrial production.
Description
Technical field
The present invention relates to the separation and recovery method of a kind of cobalt manganese waste material.
Background technology
Cobalt manganese is widely used in industry, manufacturing industry, is production heat-resisting alloy, hard alloy, prevents
Rotten alloy, manufacture manganese alloy, magnetic alloy and the important source material of various cobalt salt；Recent years, China's cobalt
Ore resources lacks serious, and the year consumption figure of cobalt increases year by year, and domestic cobalt promoter manganese can not meet life already
Producing the demand of consumption, most of cobalt manganese raw material depends on import.Therefore the recycling to cobalt manganese seems particularly
Important.
The method reclaiming separation cobalt-manganese catalyst at present has: acid pasting, organic solvent extractionprocess, electrolysis,
Ion exchange etc..It is molten that acid pasting is by three subacids, and compound carries out the mixing of sour molten formation cobalt carbonate manganese
Liquid, is subsequently adding sulphurizing salt and is co-precipitated by cobalt manganese, more first dissolved by cobalt, the solubility product difference of manganese sulfide
Manganese, isolates cobalt sulfide precipitation, then the cobalt sulfide with mixed-acid dissolution indissoluble.This method can be efficient
Separate cobalt, manganese and reclaimed, but three subacids are molten consumes a large amount of acid solution, improves the cost of product,
Environment also can be caused pollution greatly by the discharge of acid solution.Also have method be compound is carried out acid molten,
Separation of cobalt from manganese is come by the mode adding ammonia regulation PH formation cobalt ammonia complex.But it is affected by the limit of condition
System, controlling unit is on the high side, and in actual mechanical process, the response rate is the highest, and cobalt ammonia complex is stable
Property too strong, need hydrazine hydrate reduction could create substantial amounts of cost further with cobalt.
It addition, can efficiently separate out cobalt and manganese with organic solvent extraction, but the demand of organic solvent is relatively
Greatly, the process of organic solvent improves cost undoubtedly, and easily works the mischief environment, forms the step of product
On the high side, it is unfavorable for industrialized production.Electrolysis can reclaim and obtain the electrolytic cobalt that purity is high, but is as electricity
The increase electrolytic efficiency of solution time can reduce, and electrolyte instability is difficult to control and reaches demand of industrial production, also
Consume substantial amounts of electric energy, add cost.Ion exchange can reach purpose that is rich long-pending and that purify simultaneously,
Adsorption rate is fast, but ion exchange resin needs regular regeneration, produces a large amount of alkaline waste water, makes environment
Becoming to pollute, regular root changes ion exchange column and process alkaline waste water can make cost increase.
Summary of the invention
The technical problem to be solved be to provide the separation of a kind of cobalt and manganese very thoroughly, the response rate high,
Reclaim cobalt and the separation and recovery method of manganese in the cobalt manganese waste material that product purity is high, value-added content of product is high.
The technical scheme realizing the object of the invention is:
A kind of sulphurizing salt separates and recovers cobalt and the method for manganese in low cobalt height manganese waste material, comprises the following steps:
1. pretreatment: pending low cobalt height manganese waste material acid is dissolved, controls pH≤3.5 of solution, so
Rear addition excess sulfuric acid ammonium, by solution reacting by heating 0.5～1h in the water-bath that temperature is 70～95 DEG C, sucking filtration,
Adding sodium hydroxide solution again in filtrate, regulate pH to 4～6, sucking filtration after standing, the filtrate obtained is i.e.
Digestion solution, pending；
2. formulating vulcanization saline solution: the concentration of sulphurizing salt solution is 0.1～0.5mol/L；
3. cobalt, manganese separate: add step sulphurizing salt solution 2. in step digestion solution 1. and obtain reactant liquor,
The pH controlling solution is 2-5.5, after reaction terminates, filters, and obtains cobalt sulfide precipitation and manganese containing solution, its
In, sulphurizing salt is 1.1-2:1 with the ratio of the amount of the material of cobalt；
4. manganese is reclaimed: in step manganese containing solution 3., add reducing agent, reducing agent and manganese in manganese containing solution
The ratio of the amount of material is 8.5-15:1, reacts 20～60min, and reaction terminates rear sucking filtration, washing, dried
To the precipitate of manganese, i.e. complete the recovery of manganese；
5. cobalt is purified: cobalt sulfide precipitation acid step 3. obtained is dissolved, and is heated to 80～100 DEG C, control
The pH of solution processed is 2-5, adds oxidant the most again in solution, again obtains precipitating containing manganese, sucking filtration,
The solution obtained comprises only cobalt, cobalt and manganese separated thoroughly and reclaim.
The amount of above-mentioned steps 1. middle ammonium sulfate is 1.1～1.3 times of theoretical amount.
Above-mentioned steps 1. in acid be nitric acid, oxalic acid, acetic acid, phosphoric acid, hydrochloric acid, sulphuric acid or they in
Mixed acid, wherein acetic acid must be used in mixed way with above-mentioned strong acid, and mixed proportion is 1:9～3:7, described acid or
The pH ＜ 1 of person's mixed acid.
The consumption of above-mentioned acid is n (H with the ratio of the amount of the material of cobalt, manganese in cobalt manganese waste material+):[n(Mn)+n
(Co)]=2-6:1.
Above-mentioned steps 2. in sulphurizing salt be one or both in sodium sulfide, sodium bisulfide.
Above-mentioned steps 3. in the reaction condition of reactant liquor be, 20-40 DEG C, mixing speed be 200～500
0.5～2h is reacted under the conditions of r/min.
Above-mentioned steps 4. in reducing agent be the one in sodium carbonate, sodium bicarbonate, ammonium hydrogen carbonate or calcium carbonate
Or several, wherein calcium carbonate and described reducing agent are used in mixed way, and the ratio of calcium carbonate and other reducing agents is
1:9～2:8.
Above-mentioned steps 4. middle reaction temperature condition is 50-80 DEG C.
Above-mentioned steps 5. in acid be the one in nitric acid, oxalic acid, acetic acid, phosphoric acid, hydrochloric acid, sulphuric acid or several
Kind.
Above-mentioned steps 5. in oxidant be ozone, potassium permanganate, sodium hypochlorite, Ammonium persulfate., persulfuric acid
One or more in sodium, potassium peroxydisulfate, potassium chlorate, sodium chlorate, chlorine.
There is advantages that
(1) separation and recovery method of the present invention is suitable for all cobalt manganese waste materials, and particularly cobalt manganese ratio is 1:1's～4
Low cobalt height manganese waste material, such as petroleum industry produce the useless cobalt-manganese catalyst that PTA produces.
(2) present invention process is simple, and while being substantially reduced cost recovery, the response rate of cobalt and manganese is the highest,
The response rate of cobalt can be up to more than 95%, and the response rate of manganese can reach more than 99%.
(3) the present invention is directed to raw material and underestimate the characteristic of Gao Meng, first cobalt is removed with the form of cobalt sulfide rather than
First go demanganization or co-precipitation, farthest ensure that the response rate of cobalt, it is to avoid first sink manganese time cobalt
It is co-precipitated or carries secretly and cause the loss of cobalt, not only ensureing the response rate of cobalt but also improve the purity of manganese carbonate.
If first sinking manganese, a part of cobalt will be caused to get off along with one piece of co-precipitation of manganese or be entrained,
The amount of the cobalt in solution will reduce, then the response rate of cobalt will reduce, and the market price of cobalt is higher than manganese,
So the response rate improving cobalt has the biggest economic benefit.
(4) present invention carries out secondary purification to cobalt sulfide, the segregation ratio of cobalt and manganese is brought up to 10000 times with
On, both improve the response rate of cobalt, in turn ensure that the purity of cobalt reached 99%,.
Detailed description of the invention
Presently in connection with embodiment, the present invention is further detailed explanation.
In heretofore described low cobalt height manganese waste material, cobalt content is less than equal to Fe content, in low cobalt height manganese waste material
Cobalt, the mass ratio of manganese are 1:1～1:4.
(embodiment 1)
Cobalt manganese waste material handled by embodiment is the useless cobalt-manganese catalyst produced during PTA produces, wherein the containing of cobalt
Amount is 10.25wt%, and the content of manganese is 19.23wt%.
Embodiment 1
A kind of sulphurizing salt-oxidant separates and recovers cobalt and the method for manganese in low cobalt height manganese waste material, including following step
Rapid:
(1) pretreatment: take 10g cobalt manganese waste material, adds 10% in the reaction vessel filling cobalt manganese waste material
Salpeter solution 220mL, clear up after completely until cobalt manganese waste material, the pH value measuring the molten rear liquid of acid is 0.7,
Ammonium sulfate is added in solution, heating in water bath 30min, sucking filtration in the water-bath of 90 DEG C, go to deacidify molten after
Organic substance in material and iron ion.
The sodium hydroxide solution of 5mol/L is added so that it is pH value increases to 4.5 in filtrate；Stand 30min
Rear sucking filtration, the filtrate obtained i.e. digestion solution is pending.Recording cobalt content in digestion solution is 29.55g/L, and manganese contains
Amount is 67.66g/L.If having possibly together with iron ion in the molten rear material of acid, iron ion generates hydrogen-oxygen in this step
Change ferrum precipitation, remove from digestion solution after sucking filtration.
(2) join sulphurizing salt solution: be dissolved in water by sodium sulfide, obtain the sulfuration that concentration is 0.3mol/L
Sodium solution is stand-by.
(3) cobalt, manganese separate: the digestion solution 50mL obtained after taking step (1) sucking filtration, are slowly added to step
(2) the sodium sulfide solution 110.8mL prepared, addition after cure sodium is 1.3:1 with the ratio of the amount of the material of manganese,
Add acetic acid controlling the pH value of reactant liquor is 4.8, by reactant liquor temperature be 25 DEG C, mixing speed be 300
React 1h under conditions of r/min, after question response terminates, filter, respectively obtain cobalt sulfide precipitation and manganese containing solution,
Cobalt sulfide washing of precipitate weighs after drying and obtains 5.7892g, and in low cobalt height manganese waste material, the response rate of cobalt is 96.2%,
The purity reclaiming the cobalt sulfide obtained is 98.8%.
(4) manganese is reclaimed: be placed in water-bath by the manganese containing solution that step (3) is filtrated to get and be heated to 80 DEG C.
In the manganese containing solution of 80 DEG C, add sodium carbonate 6.6407g, maintain water-bath 80 DEG C reaction 30min, obtain carbon
Acid manganese precipitation.
(5) purification of cobalt: precipitation step (3) being filtrated to get is dissolved with the nitric acid of 10%, is heated to
90 DEG C, the pH=2 after control acid is molten, in solution, add 1g Ammonium persulfate., react 0.5h, again obtain
Precipitation containing manganese, sucking filtration, in the solution obtained, the ratio of cobalt manganese reaches 15000:1, and the response rate of cobalt reaches 96%,
The separation of cobalt and manganese is the most thorough.
Embodiment 2-8 is substantially the same manner as Example 1, difference such as table 1.
Table 1
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, related work
Personnel can carry out various change and amendment completely in the range of without departing from this invention technological thought.
The content that the technical scope of this invention is not limited in description, it is necessary to according to right
Determine its technical scope.
Claims (10)
1. one kind separates and recovers cobalt and the method for manganese in low cobalt height manganese waste material with sulphurizing salt, it is characterised in that bag
Include following steps:
1. pretreatment: pending low cobalt height manganese waste material acid is dissolved, controls pH≤3.5 of solution, so
Rear addition excess sulfuric acid ammonium, by solution reacting by heating 0.5～1h in the water-bath that temperature is 70～95 DEG C, sucking filtration,
Adding sodium hydroxide solution again in filtrate, regulate pH to 4～6, sucking filtration after standing, the filtrate obtained is i.e.
Digestion solution, pending；
2. formulating vulcanization saline solution: the concentration of sulphurizing salt solution is 0.1～0.5mol/L；
3. cobalt, manganese separate: add step sulphurizing salt solution 2. in step digestion solution 1. and obtain reactant liquor,
The pH controlling solution is 2-5.5, after reaction terminates, filters, and obtains cobalt sulfide precipitation and manganese containing solution, its
In, sulphurizing salt is 1.1-2:1 with the ratio of the amount of the material of cobalt；
4. manganese is reclaimed: in step manganese containing solution 3., add reducing agent, reducing agent and manganese in manganese containing solution
The ratio of the amount of material is 8.5-15:1, reacts 20～60min, and reaction terminates rear sucking filtration, washing, dried
To the precipitate of manganese, i.e. complete the recovery of manganese；
5. cobalt is purified: cobalt sulfide precipitation acid step 3. obtained is dissolved, and is heated to 80～100 DEG C, control
The pH of solution processed is 2-5, adds oxidant the most again in solution, again obtains precipitating containing manganese, sucking filtration,
The solution obtained comprises only cobalt, cobalt and manganese separated thoroughly and reclaim.
2. separate and recover cobalt and the side of manganese in low cobalt height manganese waste material according to a kind of sulphurizing salt described in claim 1
Method, it is characterised in that: the amount of described step 1. middle ammonium sulfate is 1.1～1.3 times of theoretical amount.
A kind of sulphurizing salt the most according to claim 1 separates and recovers cobalt and manganese in low cobalt height manganese waste material
Method, it is characterised in that: described step 1. in acid be nitric acid, oxalic acid, acetic acid, phosphoric acid, hydrochloric acid, sulfur
Acid or the mixed acid in them, wherein acetic acid must be used in mixed way with above-mentioned strong acid, and mixed proportion is 1:
9～3:7, the pH ＜ 1 of described acid or mixed acid.
A kind of sulphurizing salt the most according to claim 2 separates and recovers cobalt and manganese in low cobalt height manganese waste material
Method, it is characterised in that: the consumption of described acid is n with the ratio of the amount of the material of cobalt, manganese in cobalt manganese waste material
(H+): [n (Mn)+n (Co)]=2-6:1.
A kind of sulphurizing salt the most according to claim 1 separates and recovers cobalt and manganese in low cobalt height manganese waste material
Method, it is characterised in that: described step 2. in sulphurizing salt be the one in sodium sulfide, sodium bisulfide or two
Kind.
A kind of sulphurizing salt separates and recovers cobalt and the side of manganese in low cobalt height manganese waste material
Method, it is characterised in that: the reaction condition of described step 3. middle reactant liquor is, 20-40 DEG C, mixing speed
It it is reaction 0.5～2h under the conditions of 200～500r/min.
A kind of sulphurizing salt separates and recovers cobalt and the side of manganese in low cobalt height manganese waste material
Method, it is characterised in that: described step 4. in reducing agent be sodium carbonate, sodium bicarbonate, ammonium hydrogen carbonate or carbon
One or more in acid calcium, wherein calcium carbonate and described reducing agent are used in mixed way, and calcium carbonate is with other also
The ratio of former dose is 1:9～2:8.
A kind of sulphurizing salt separates and recovers cobalt and the side of manganese in low cobalt height manganese waste material
Method, it is characterised in that: described step 4. middle reaction temperature condition is 50-80 DEG C.
A kind of sulphurizing salt separates and recovers cobalt and the side of manganese in low cobalt height manganese waste material
Method, it is characterised in that: described step 5. in acid be nitric acid, oxalic acid, acetic acid, phosphoric acid, hydrochloric acid, sulphuric acid
In one or more.
A kind of sulphurizing salt separates and recovers cobalt and manganese in low cobalt height manganese waste material
Method, it is characterised in that: described step 5. in oxidant be ozone, potassium permanganate, sodium hypochlorite, mistake
One or more in ammonium sulfate, sodium peroxydisulfate, potassium peroxydisulfate, potassium chlorate, sodium chlorate, chlorine.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904402A (en) * | 2017-10-18 | 2018-04-13 | 江苏理工学院 | A kind of method of cobalt and manganese in separation cobalt manganese waste material |
| CN108736090A (en) * | 2018-05-30 | 2018-11-02 | 安徽南都华铂新材料科技有限公司 | A kind of recoverying and utilizing method of iron manganese phosphate anode material of lithium battery |
| CN108928847A (en) * | 2017-05-27 | 2018-12-04 | 江苏凯力克钴业股份有限公司 | A kind of copper sulfide purifying technique and device |
| CN109609785A (en) * | 2018-12-20 | 2019-04-12 | 中国恩菲工程技术有限公司 | The method of cobalt is separated from cobalt, manganese carbonate mixture |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108928847A (en) * | 2017-05-27 | 2018-12-04 | 江苏凯力克钴业股份有限公司 | A kind of copper sulfide purifying technique and device |
| CN108928847B (en) * | 2017-05-27 | 2023-05-12 | 格林美（江苏）钴业股份有限公司 | Copper sulfide purification process and device |
| CN107904402A (en) * | 2017-10-18 | 2018-04-13 | 江苏理工学院 | A kind of method of cobalt and manganese in separation cobalt manganese waste material |
| CN107904402B (en) * | 2017-10-18 | 2019-11-22 | 江苏理工学院 | A method of cobalt and manganese in separation cobalt manganese waste material |
| CN108736090A (en) * | 2018-05-30 | 2018-11-02 | 安徽南都华铂新材料科技有限公司 | A kind of recoverying and utilizing method of iron manganese phosphate anode material of lithium battery |
| CN108736090B (en) * | 2018-05-30 | 2020-04-21 | 安徽南都华铂新材料科技有限公司 | Recycling method of lithium iron manganese phosphate battery positive electrode material |
| CN109609785A (en) * | 2018-12-20 | 2019-04-12 | 中国恩菲工程技术有限公司 | The method of cobalt is separated from cobalt, manganese carbonate mixture |
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Application publication date: 20160831 |