CN106350673A - Method for selectively precipitating and separating cobalt in potential-control manner - Google Patents
Method for selectively precipitating and separating cobalt in potential-control manner Download PDFInfo
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- CN106350673A CN106350673A CN201610867704.8A CN201610867704A CN106350673A CN 106350673 A CN106350673 A CN 106350673A CN 201610867704 A CN201610867704 A CN 201610867704A CN 106350673 A CN106350673 A CN 106350673A
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- cobalt
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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
- 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
Abstract
The invention provides a method for selectively precipitating and separating cobalt in a potential-control manner. Copper-cobalt-manganese slag is used for neutralizing a copper-cobalt-manganese solution to a required pH value; then, sodium sulphide is added under the condition of simultaneously controlling the solution potential and the pH value to perform vulcanization copper removal; after the copper removal, sodium ethylxanthate is added under the condition of simultaneously controlling the solution potential and the pH value to perform precipitation cobalt removal; after the cobalt removal, sodium sulphide is added into the solution under the condition of simultaneously controlling the solution potential and the pH value to perform vulcanization zinc removal; after the zinc removal, sodium carbonate is added in the solution for neutralizing and producing manganese carbonate. The method practically realizes the stepped precipitation and separation of the copper, the cobalt and the zinc in the solution through simultaneously controlling the metal ion mixed potential and the pH value in the solution; particularly, the cobalt content in the cobalt precipitate products reaches more than 20.0 percent; the processes are closely associated; the single process cannot reach the expected effect of the stepped separation of valuable metal.
Description
Technical field
The present invention relates to hydrometallurgy process in nonferrous metallurgy field, especially with control current potential selective precipitation separation cobalt
Wet-process metallurgy method.
Background technology
Cobalt is a kind of steel grey and the metal having metallic luster, its excellent physical performance, determines it and closes in hard
The extensive application of gold, heat-resisting alloy, anode material for lithium-ion batteries and pigment industry.And China's cobalt resource is very deficient, for a long time
Rely on import cobalt ore national from the abundant Congo (Congo-Kinshasa) of cobalt resource and Zambia etc., but be as Congo (Congo-Kinshasa) of cobalt ore big export country
The enforcement of government's " limiting cobalt ore outlet, encourage cobalt ore processing " policy, cobalt ore needs to be smelted into copper-cobalt alloy outlet, institute with electric furnace
With copper-cobalt alloy replace cobalt ore become the important cobalt raw material of China market although in copper-cobalt alloy copper and cobalt content all higher, but
It is to bring difficulty to follow-up cobalt extraction process.
Cobalt ore extract cobalt classical technique be: cobalt ore-ore grinding-reducing leaching-remove ferrum-copper removal-removing calcium and magnesium-extracting-back extraction-
Washing-oil removing-concentration-crystallization-packaging-cobaltous sulfate.This technique is applied to commercial production always at present, is changed into when processing raw material
During copper-cobalt alloy, simply dissolution process is different, and the copper-cobalt alloy dissolving method of current document report mainly has control current potential oxygen
Change dissolving, the method such as electrochemical solution, oxidation acid pasting, chlorinating dissolution method, roasting method and mixed acid system dissolve although these
Method enables the selective dissolution of copper-cobalt alloy, but still contains the metals such as copper and manganese in the cobalt-carrying solution of dissolving output,
This just brings adverse effect to follow-up p204 abstraction impurity removal.
Cobalt-carrying solution removes the foreign ions such as de-iron, copper and calcium and magnesium successively through chemical method, then adopts p204 extraction deep again
Degree remove impurity and p507 extraction cobalt, wherein p204 is the commercial designations of diethylhexyl phosphoric acid, and it is a kind of cation extraction of wide spectrum
Take agent, the order of extract and separate metal is in acid medium: fe3+＞ zn2+＞ cu2+＞ mn2+＞ co2+＞ ni2+＞ mg2+＞
ca2+.So, during p204 abstraction impurity removal, fe, zn, cu, mn and part co can be extracted by p204, finally in p204 back extraction
Washing process enters backwash liquor, wherein mainly contains the metals such as copper, cobalt, zinc and manganese, industrial referred to as copper cobalt manganese solution (abbreviation copper
Manganese liquid), this solution is to stack after waste residue generally with alkali precipitation, and rough calculation often produces the product of 1 ton of metallic cobalt amount from remove impurity
Take away cobalt amount in journey and be more than 20kg, also a large amount of metals such as copper, manganese, zinc do not reclaim through effective, and debris dump manufactures into
The loss of valency metal and environmental pollution.
Copper manganese liquid generally adopts neutralisation to process, different with mode according to agents useful for same, generally has in Calx neutralisation, alkali
With method and three kinds of neutralisation of oxidation.Calx neutralisation is directly to neutralize copper cobalt manganese solution Calx, so that heavy metal ion is generated
Hydroxide precipitates, and chloride ion and calcium ion effect generate calcium chloride, reach the purpose of purified solution.The method adopts cost relatively
, as raw material, processing cost is low and process is simple, but haves the shortcomings that maximum is that slag yield is big for low lime cream.Alkali neutralisation
Be that copper cobalt manganese solution Caustic soda or soda are directly neutralized, make heavy metal ion generate hydroxide precipitation, chloride ion and sodium from
Son effect generates sodium chloride, reaches the purpose of purified solution.The advantage of the method is that process is simple and the quantity of slag is less, but adopts
, as raw material, processing cost is high for Caustic soda with high costs or soda, and a large amount of metal ions are mingled with and are difficult to efficient recovery.Oxidation neutralization
Rule is the addition oxidant in solution, so that heavy metal ion is oxidized to high-valence state and precipitate in entrance slag, is simultaneously introduced Caustic soda
, there is oxidation reaction when oxidant is mixed with heavy metal ion-containing waste water in adjustment ph value, so that nickel cobalt etc. is oxidized to high price and hydrolyze
Enter oxidizing slag, supernatant adds pfs(bodied ferric sulfate), on the one hand make itself and nickel generate compound salt precipitation, on the other hand
Its flocculant acts on, and adds sodium hydroxide adjustment solution ph=9.5～10.5 simultaneously, and add a small amount of into groove in mixing channel
Polyacrylamide with accelerate precipitate, now the heavy metal ion in solution precipitates completely.The quantity of slag of the method output is little and golden
Belong to content high, the heavy metals ion qualified discharge after process.But, the method needs using substantial amounts of oxidant, and
Chloride-ion System easily produces chlorine, and operating environment is poor.
About the process of copper cobalt manganese solution, Jinchuan Group Co., Ltd of China has carried out long-term research, and Yang Zhiqiang etc. carries
Go out a kind of method producing selective recovery cobalt copper waste liquid from cobalt copper zinc-manganese, reclaimed using manganese powder or manganese piece selective reduction
The response rate of cobalt and copper, copper and cobalt is more than 95%, and the impurity content of the copper cobalt slag of recovery is less than 3%, the method clean and effective and not
Introduce impurity.Chen Guodong proposes cobalt, copper, zinc, the technique of manganese in a kind of recovery manganese chloride residual liquid, after adjusting chlorine ion concentration
Manganese chloride residual liquid with n235 extract, then the cobalt in substep back extraction organic faciess, copper and zinc, obtain pure cobaltous chloride, chlorination
Copper solution and the precipitate of zinc, with the manganese in p204 purification by liquid extraction raffinate, the manganese salt solution obtaining is through pervaporation, crystallization and dry
Dry, obtain manganese salt product.This technique cobalt, copper, zinc, manganese the response rate more than 90%.What illustrious and influential grade proposes with cooperation precipitation side
Method realizes the Selective Separation of nickel and manganese, adds ammonium salt in solution and adjusts ph value, then passes to co2Gas precipitation output
Manganese carbonate, realizes the Selective Separation of manganese and nickel in solution, and the rate of deposition of manganese is more than 99.8%, and the loss rate of nickel is less than 1.5%.Should
Although method can realize the Selective Separation of manganese and nickel, add a large amount of ammonium salts, change solution system, follow-up to solution
Process brings very big difficulty.
At present, the most common method of industrial application is the alkali neutralisation using sodium carbonate, output substantial amounts of black copper cobalt
Manganese slag, abbreviation copper manganese slag, wherein mainly existed with the carbonate form of the metals such as copper, zinc, ferrum and manganese, because it is difficult by,
Most enterprises can only be stacked at present, not only easily cause secondary pollution, and cause the waste of valuable metal.Research worker is had to carry
Go out to reclaim the valuable metal in copper manganese slag, the method generally adopting is with hydrochloric acid or sulfuric acid dissolution, then adopts iron replacement again
Or neutralization precipitation method recovery section copper is although can be with recovery section valuable metal, but separating effect is still unsatisfactory, face
Face and process same problem with copper cobalt manganese liquid.
The exploitation of these methods, it is possible to achieve the recovery of valuable metal in copper cobalt manganese solution, but all there are some and restrict it
The problems such as defect of commercial Application, such as processing cost height, technological process length and wastewater treatment difficulty, so have in copper cobalt manganese solution
The recovery that efficiently separates of valency metal remains this area problem in the urgent need to address.A kind of (control current potential sulfuration point such as Liu Weifeng
The method of valuable metal in exsolution liquid, application number: 201610030160.x, the applying date: 2016-01-18) propose using control electricity
Position sulfuration separates the valuable metal in copper cobalt manganese solution, removes copper and produces initially with control current potential sulfuration method from copper cobalt manganese solution
Go out copper sulfide concentrate, secondly adopt control current potential sulfuration method liquid after copper removal and cobalt and zinc are all precipitated with sulphided form,
Precipitate output manganous carbonate slag with neutralisation more afterwards, although the method achieves efficiently separating of copper and cobalt zinc in copper cobalt manganese solution,
But cobalt and zinc are precipitated with sulphided form in liquid after copper removal simultaneously, extract to later separation and bring very big difficulty.
Content of the invention
In order to overcome the shortcomings of copper cobalt manganese solution conventional process, the present invention provides one kind by controlling current potential precipitate and separate cobalt,
And the Wet-process metallurgy method that the cobalt response rate is high, environmental pollution is little and processing cost is low.
Reaching above-mentioned purpose the technical solution used in the present invention is: with copper cobalt manganese slag and copper cobalt manganese solution is to requiring
Ph value, adds sodium sulfide sulfuration copper removal simultaneously, continues after solution potential is stablized under the conditions of then controlling solution potential and ph value
Stirring is filtered after a period of time, and copper sulfide concentrate is as the raw material reclaiming copper；After copper removal, liquid controls solution potential and ph value simultaneously
Under the conditions of add ethyl xanthate precipitation remove cobalt, after solution potential stablize continue stirring a period of time after filter, cobalt precipitate work
Raw material for Call Provision；Except adding sodium sulfide sulfuration to remove zinc under the conditions of liquid controls solution potential and ph value after cobalt simultaneously, work as solution
Filter after continuing stirring a period of time after current potential is stable, zinc sulfide concentrates as the raw material reclaiming zinc, except after zinc liquid add pure
With output manganous carbonate slag in alkali.The essence of the present invention is to be realized using control metal ion in solution mixed potential simultaneously and ph value
In solution, the fractional precipitation of copper, cobalt and zinc separates, these process tight association, and separate processes all can not reach valuable metal substep
Detached Expected Results.
Specific technical process and parameter are as follows:
1 control current potential sulfuration copper removal
With in copper cobalt manganese slag and copper cobalt manganese solution is to certain ph value, then controlling potential and ph value selectivity vulcanize and remove simultaneously
Copper；With in copper cobalt manganese slag and copper cobalt manganese solution control terminal ph=0.1～0.5 of mixed solution, then keeping solution temperature 30
～50 DEG C and mixing speed 100～200r/min, it is subsequently adding the sodium sulfide solution that concentration is 234～390g/l, is simultaneously introduced
The ph value that technical-grade hydrochloric acid adjusts solution remains at 0.5～2.0, when metal ion in solution mixed potential is with respect to calomel
Electrode is 80～120mv and stablizes 15～30min, realizes solid-liquid separation using filter press mode, obtain after continuing stirring 60min
The liquid to after copper removal.The main chemical reactions that control current potential vulcanizes the generation of copper removal process are as follows:
2hcl+meco3=mecl2+co2↑+h2O (1)
cucl2+na2S=cus ↓+2nacl (2)
2 control current potential precipitate cobalt
After copper removal, liquid controls solution potential and ph value simultaneously and adds sodium ethyl xanthate precipitation to remove cobalt；After copper removal liquid temperature 30～
Under the conditions of 50 DEG C and mixing speed 100～200r/min, it is subsequently adding the sodium ethyl xanthate solution that concentration is 10～50g/l, with
When add technical-grade hydrochloric acid adjust solution ph value remain at 2.1～4.0, when metal ion in solution mixed potential with respect to
For -80mv～-40mv and stablize 31～60min in calomel electrode, realized using filter press mode solid after continuing stirring 30min
Liquid separates, and obtains except liquid after cobalt.The main chemical reactions that control current potential precipitate cobalt process occurs are as follows:
cocl2+2c2h5ocssna=co(c2h5ocss)2↓+2nacl (3)
3 control current potential sulfurations remove zinc
Except liquid controls solution potential and the sulfuration of ph value selectivity to remove cobalt after cobalt simultaneously；Except after cobalt liquid in 30～70 DEG C of temperature and stirring
Under the conditions of speed 100～200r/min, it is subsequently adding the sodium sulfide solution that concentration is 39～156g/l, is simultaneously introduced technical grade salt
Acid adjustment solution ph value remain at 4.1～6.0, when metal ion in solution mixed potential with respect to calomel electrode for-
240～-210mv and stablize 15～30min, realizes solid-liquid separation using filter press mode after continuing stirring 60～90min, obtains
To liquid after zinc.The main chemical reactions that control current potential sulfuration occurs except cobalt process are as follows:
zncl2+na2S=zns ↓+2nacl (4)
Described sodium sulfide, hydrochloric acid and sodium ethyl xanthate are technical grade reagent, and wherein sodium sulfide weight/mass percentage composition is not less than
60.0%, not less than 31.0% and sodium ethyl xanthate weight/mass percentage composition is not less than 82.0% to hydrochloric acid weight/mass percentage composition.
The present invention is applied to copper cobalt manganese solution and the copper cobalt manganese slag of cobalt smelting system abstraction impurity removal process, copper cobalt manganese solution master
Composition range is wanted to be (g/l): cu10-80, co0.5-5.0, zn1.0-10.0, ca1.0-10.0, mn50-150, cl120-240
And h10-50.Copper cobalt manganese slag main component scope is (%): cu1.0-30.0, zn1.0-15.0, co0.1-10.0 and mn5.0-
25.0.
The present invention is compared with traditional copper cobalt manganese solution and copper cobalt manganese Slag treatment method, has the advantage that the 1, present invention adopts
Control the substep that metal ion in solution mixed potential and ph value mode achieve copper, cobalt and zinc in copper cobalt manganese solution to divide simultaneously
From；2nd, efficiently separating of cobalt and zinc in liquid after copper removal is achieved using control current potential sulfide precipitation technology, in cobalt precipitated product, cobalt contains
Amount reaches more than 20.0%；3rd, the present invention has that technical process is simple, technical specification is stable, labor intensity is little and low production cost
The advantages of.
Brief description
Fig. 1: present invention process schematic flow sheet.
Specific embodiment
Embodiment 1:
The copper cobalt manganese solution of cobalt smelting system abstraction impurity removal process and copper cobalt manganese slag, copper cobalt manganese solution main component scope is (g/
L): cu15.4, co2.2, zn9.8, ca6.24, mn105.2, cl180 and h4.5, copper cobalt manganese slag main component scope is (%):
Cu17.5, zn4.3, co0.8 and mn22.8.Sodium sulfide, hydrochloric acid and sodium ethyl xanthate are technical grade reagent, sodium sulfide quality hundred
Content is divided to be not less than 60.0%, hydrochloric acid weight/mass percentage composition is not less than 31.0% and is not less than with sodium ethyl xanthate weight/mass percentage composition
82.0%.
First with copper cobalt manganese slag and copper cobalt manganese solution control the terminal ph=0.4 of mixed solution, then keeping solution temperature
45 DEG C of degree and mixing speed 120r/min, are subsequently adding the sodium sulfide solution that concentration is 234g/l, are simultaneously introduced technical-grade hydrochloric acid
The ph value of adjustment solution remains at 1.5, when metal ion in solution mixed potential with respect to calomel electrode for 90mv and surely
Determine 20min, after continuing stirring 60min, solid-liquid separation is realized using filter press mode, in liquid after copper removal, copper concentration is reduced to
0.02g/l, copper content 52.3% in copper sulfide concentrate.
After copper removal, liquid, under the conditions of temperature 45 C and mixing speed 120r/min, is subsequently adding the ethyl that concentration is 30g/l
Sodium xanthate solution, the ph value being simultaneously introduced technical-grade hydrochloric acid adjustment solution remains at 3.0, when metal ion in solution mixing
Current potential is -60mv and stable 35min with respect to calomel electrode, realizes solid-liquid using filter press mode after continuing stirring 30min
Separate, except in liquid after cobalt, cobalt concentration is reduced to 0.03g/l, in cobalt precipitate, cobalt content is 23.5%.
Except liquid, under the conditions of temperature 50 C and mixing speed 120r/min, is subsequently adding the sulfuration that concentration is 78g/l after cobalt
Sodium solution, the ph value being simultaneously introduced technical-grade hydrochloric acid adjustment solution remains at 5.0, when metal ion in solution mixed potential
It is -220mv and stable 30min with respect to calomel electrode, after continuing stirring 60min, solid-liquid is realized using filter press mode and divide
From except in liquid after zinc, zinc concentration is reduced to 0.02g/l, Zinc Content in Zinc Sulphide Concentrate content is 48.5%.
Claims (2)
1. a kind of method of control current potential selective precipitation separation cobalt is it is characterised in that comprise the following steps:
(1) control current potential sulfuration copper removal
With in copper cobalt manganese slag and copper cobalt manganese solution control terminal ph=0.1～0.5 of mixed solution, then keeping solution temperature
30～50 DEG C and mixing speed 100～200r/min, are subsequently adding the sodium sulfide solution that concentration is 234～390g/l, simultaneously plus
The ph value entering technical-grade hydrochloric acid adjustment solution remains at 0.5～2.0, when metal ion in solution mixed potential is with respect to sweet
Mercury electrode is 80～120mv and stablizes 15～30min, realizes solid-liquid separation using filter press mode after continuing stirring 60min,
Obtain liquid after copper removal；
(2) control current potential precipitate cobalt
After copper removal, liquid is under the conditions of 30～50 DEG C of temperature and mixing speed 100～200r/min, be subsequently adding concentration be 10～
The sodium ethyl xanthate solution of 50g/l, the ph value being simultaneously introduced technical-grade hydrochloric acid adjustment solution remains at 2.1～4.0, when molten
In liquid, metal ion mixed potential is -80mv～-40mv with respect to calomel electrode and stablizes 31～60min, continues stirring 30min
Afterwards solid-liquid separation is realized using filter press mode, obtain except liquid after cobalt；
(3) sulfuration of control current potential removes zinc
Except after cobalt liquid under the conditions of 30～70 DEG C and mixing speed 100～200r/min of temperature, be subsequently adding concentration be 39～
The sodium sulfide solution of 156g/l, the ph value being simultaneously introduced technical-grade hydrochloric acid adjustment solution remains at 4.1～6.0, works as solution
Middle metal ion mixed potential is -240～-210mv and stablize 15～30min with respect to calomel electrode, continue stirring 60～
After 90min, solid-liquid separation is realized using filter press mode, obtain except liquid after zinc.
2. as claimed in claim 1 a kind of method of control current potential selective precipitation separation cobalt it is characterised in that described ethyl
Sodium xanthate weight/mass percentage composition is not less than 82.0%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107058745A (en) * | 2017-04-21 | 2017-08-18 | 青海快驴电动汽车科技有限公司 | A kind of method that valuable metal is extracted in cobalt metallurgical waste |
| CN109266837A (en) * | 2018-10-09 | 2019-01-25 | 中色华鑫湿法冶炼有限公司 | A method of recycling copper, cobalt from wet type copper smelting waste liquid containing cobalt |
| CN112266096A (en) * | 2020-09-30 | 2021-01-26 | 中南大学 | Method for separating sulfide heavy metal precipitate by adopting multiple parallel field flows |
| CN112575200A (en) * | 2020-12-08 | 2021-03-30 | 衢州华友钴新材料有限公司 | Method for replacing and separating copper, zinc and manganese in inverse copper-manganese solution by using sulfide precipitation controlled electric position |
| CN113957249A (en) * | 2021-01-18 | 2022-01-21 | 郑州大学 | Method for separating zinc and cobalt ions in solution |
| CN114466941A (en) * | 2019-10-18 | 2022-05-10 | 杰富意钢铁株式会社 | Method and apparatus for recovering manganese from waste dry battery |
| CN114555839A (en) * | 2019-10-18 | 2022-05-27 | 杰富意钢铁株式会社 | Method and apparatus for recovering manganese from waste dry battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107058745A (en) * | 2017-04-21 | 2017-08-18 | 青海快驴电动汽车科技有限公司 | A kind of method that valuable metal is extracted in cobalt metallurgical waste |
| CN109266837A (en) * | 2018-10-09 | 2019-01-25 | 中色华鑫湿法冶炼有限公司 | A method of recycling copper, cobalt from wet type copper smelting waste liquid containing cobalt |
| CN114466941A (en) * | 2019-10-18 | 2022-05-10 | 杰富意钢铁株式会社 | Method and apparatus for recovering manganese from waste dry battery |
| CN114555839A (en) * | 2019-10-18 | 2022-05-27 | 杰富意钢铁株式会社 | Method and apparatus for recovering manganese from waste dry battery |
| CN112266096A (en) * | 2020-09-30 | 2021-01-26 | 中南大学 | Method for separating sulfide heavy metal precipitate by adopting multiple parallel field flows |
| CN112575200A (en) * | 2020-12-08 | 2021-03-30 | 衢州华友钴新材料有限公司 | Method for replacing and separating copper, zinc and manganese in inverse copper-manganese solution by using sulfide precipitation controlled electric position |
| CN113957249A (en) * | 2021-01-18 | 2022-01-21 | 郑州大学 | Method for separating zinc and cobalt ions in solution |
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