CN106350673B - A kind of method for controlling current potential selective precipitation separation cobalt - Google Patents

A kind of method for controlling current potential selective precipitation separation cobalt Download PDF

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CN106350673B
CN106350673B CN201610867704.8A CN201610867704A CN106350673B CN 106350673 B CN106350673 B CN 106350673B CN 201610867704 A CN201610867704 A CN 201610867704A CN 106350673 B CN106350673 B CN 106350673B
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cobalt
solution
copper
liquid
potential
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CN106350673A (en
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刘伟锋
刘亮强
孙百奇
张杜超
杨天足
陈霖
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Central South University
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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
    • 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

A kind of method for controlling current potential selective precipitation separation cobalt, with in copper cobalt manganese slag and copper cobalt manganese solution is to desired pH value, then control simultaneously and vulcanized sodium vulcanization copper removal is added under solution potential and pH value condition, liquid controls addition ethyl xanthate precipitation under solution potential and pH value condition to remove cobalt simultaneously after copper removal, except after cobalt liquid simultaneously control under solution potential and pH value condition add vulcanized sodium vulcanization remove zinc, except after zinc liquid add in soda ash with output manganese carbonate.The essence of the present invention is to realize the fractional precipitation separation of copper in solution, cobalt and zinc using control metal ion in solution mixed potential and pH value simultaneously, especially cobalt content reaches more than 20.0% in cobalt precipitated product, these process tight associations, separate processes can not all reach the Expected Results of valuable metal substep separation.

Description

A kind of method for controlling current potential selective precipitation separation cobalt
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 has the metal of metallic luster, its excellent physical performance, determines that it is closed in hard The extensive use 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 By the Congo enriched from cobalt resource（Gold）With the national import cobalt ore such as Zambia, but with the Congo of cobalt ore big export country（Gold） The implementation of government " limitation cobalt ore outlet, encourage cobalt ore processing " policy, cobalt ore need to be smelted into copper-cobalt alloy outlet, institute with electric furnace Cobalt ore is replaced to turn into the important cobalt raw material of China market with copper-cobalt alloy, although copper and cobalt content are all higher in copper-cobalt alloy, It is to bring difficulty to follow-up cobalt extraction process.
Cobalt ore extraction cobalt classical technique be：Cobalt ore-ore grinding-reducing leaching-iron removaling-copper removal-removing calcium and magnesium-extracting-back extraction- Washing-oil removing-concentration-crystallization-packaging-cobaltous sulfate.The technique is applied to industrial production always at present, when processing raw material is changed into During copper-cobalt alloy, simply dissolution process is different, and the copper-cobalt alloy dissolving method of document report mainly has control current potential oxygen at present Change the methods of dissolving, electrochemical solution, oxidation acid extracting, chlorinating dissolution method, roasting method and mixed acid system dissolve, although these Method can realize the selective dissolution of copper-cobalt alloy, but dissolve and still contain the metals such as copper and manganese in the cobalt-carrying solution of output, This just brings adverse effect to follow-up P204 abstraction impurity removals.
Cobalt-carrying solution, successively except foreign ions such as de-iron, copper and calcium and magnesiums, is then extracted deeply using P204 again by chemical method Degree removal of impurities and P507 extraction cobalts, wherein P204 is the commercial designations of diethylhexyl phosphoric acid, and it is a kind of cation extraction of wide spectrum Agent is taken, the order of extract and separate metal is in acid medium：Fe3+＞ Zn2+＞ Cu2+＞ Mn2+＞ Co2+＞ Ni2+＞ Mg2+＞ Ca2+.So during P204 abstraction impurity removals, Fe, Zn, Cu, Mn and part Co can be extracted by P204, be finally stripped in P204 Washing process enters backwash liquor, wherein mainly containing the metals such as copper, cobalt, zinc and manganese, is industrially referred to as copper cobalt manganese solution（Abbreviation copper Manganese liquid）, the solution stacks after being generally waste residue with alkali precipitation, is roughly calculated, and often produces the product of 1 ton of metallic cobalt amount from cleaning Cobalt amount is taken away in journey and is more than the metal such as 20kg, also a large amount of copper, manganese, zinc not by effectively reclaiming, debris dump manufactures into The loss and environmental pollution of valency metal.
The processing of copper manganese liquid generally use neutralisation, it is different with mode according to agents useful for same, generally have in lime neutralisation, alkali With method and three kinds of neutralisation of oxidation.Lime neutralisation is directly to neutralize copper cobalt manganese solution with lime, generates heavy metal ion Hydroxide precipitates, chlorion and calcium ion effect generation calcium chloride, reaches the purpose of purified solution.This method using cost compared with Low milk of lime is as raw material, and processing cost is low and process is simple, but the shortcomings that maximum be present is that slag yield is big.Alkali neutralisation Be directly to neutralize copper cobalt manganese solution with caustic soda or soda ash, make heavy metal ion generation hydroxide precipitation, chlorion and sodium from Son effect generation sodium chloride, reach the purpose of purified solution.The advantages of this method is that process is simple and the quantity of slag is smaller, but is used Caustic soda with high costs or soda ash are as raw material, and processing cost is high, and a large amount of metal ions, which are mingled with, to be difficult to effectively reclaim.Oxidation neutralizes Rule is that oxidant is added into solution, heavy metal ion is oxidized to high-valence state and precipitates into slag, while adds caustic soda PH value is adjusted, oxidation reaction occurs when oxidant mixes with heavy metal ion-containing waste water, nickel cobalt etc. is oxidized to high price and hydrolyzes Into oxidizing slag, supernatant adds PFS（Bodied ferric sulfate）, it is generated compound salt with nickel and precipitate, on the other hand Its flocculant is acted on, while sodium hydroxide adjustment pH value of solution=9.5~10.5 are added into mixing channel, and is added on a small quantity into groove Polyacrylamide to accelerate to precipitate, now the heavy metal ion in solution precipitates completely.The quantity of slag of this method output is small and golden It is high to belong to content, the heavy metals ion qualified discharge after processing.But this method needs to use substantial amounts of oxidant, and Chloride-ion System easily produces chlorine, and operating environment is poor.
Processing about copper cobalt manganese solution, Jinchuan Group Co., Ltd of China have carried out long-term research, and Yang Zhiqiang etc. carries A kind of method that selective recovery cobalt copper in waste liquid is produced from cobalt copper zinc-manganese is gone out, has been reclaimed using manganese powder or the selective reduction of manganese piece The rate of recovery 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%, this 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 raffinate, after adjustment chlorine ion concentration Manganese chloride raffinate extracted with N235, then substep back extraction organic phase in cobalt, copper and zinc, obtain pure cobalt chloride, chlorination The sediment of copper solution and zinc, with the manganese in P204 purification by liquid extraction raffinates, obtained manganese salt solution is through pervaporation, crystallization and does It is dry, obtain manganese salt product.The technique cobalt, copper, zinc, the rate of recovery of manganese are more than 90%.What illustrious and influential grade proposition cooperation precipitation side Method realizes the Selective Separation of nickel and manganese, i.e., ammonium salt is added into solution and adjusts pH value, then passes to CO2Gas precipitation output Manganese carbonate, the Selective Separation of manganese and nickel in solution is realized, the rate of deposition of manganese is more than 99.8%, and the loss late of nickel is less than 1.5%.Should Although method can realize the Selective Separation of manganese and nickel, a large amount of ammonium salts are added, change solution system, it is follow-up to solution Processing brings very big difficulty.
At present, it is to use the alkali neutralisation of sodium carbonate, the substantial amounts of black copper cobalt of output industrially to apply most common method Manganese slag, abbreviation copper manganese slag, wherein mainly exist with the carbonate form of the metals such as copper, zinc, iron 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.There is researcher to carry Go out to reclaim the valuable metal in copper manganese slag, the method for generally use is to use hydrochloric acid or sulfuric acid dissolution, then uses iron replacement again Or neutralization precipitation method recovery section copper, although can be with recovery section valuable metal, separating effect be still unsatisfactory, face Face and handle the problem of same 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 restrict it in the presence of some The defects of commercial Application, such as the problems such as processing cost height, technological process length and wastewater treatment difficulty, so having in copper cobalt manganese solution The recovery that efficiently separates of valency metal is still the problem of this area is in the urgent need to address.Liu Weifeng etc.（One kind control current potential vulcanization point The method of valuable metal, application number in exsolution liquid:201610030160.X the applying date: 2016-01-18）It is proposed using control electricity Valuable metal in position vulcanization separation copper cobalt manganese solution, is removed copper and is produced from copper cobalt manganese solution using control current potential vulcanization method first Go out copper sulfide concentrate, secondly use control current potential vulcanization method all to precipitate cobalt and zinc with sulphided form in liquid after copper removal, most Precipitating output manganous carbonate slag with neutralisation again afterwards, although this method realizes efficiently separating for copper and cobalt zinc in copper cobalt manganese solution, But cobalt and zinc are precipitated with sulphided form in liquid after copper removal simultaneously, very big difficulty is brought to later separation extraction.
The 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 precipitation separation cobalt, And the cobalt rate of recovery is high, the small Wet-process metallurgy method low with processing cost of environmental pollution.
It is to reach above-mentioned purpose the technical solution adopted by the present invention：With in copper cobalt manganese slag and copper cobalt manganese solution is to requiring PH value, then control simultaneously and vulcanized sodium vulcanization copper removal is added under solution potential and pH value condition, continue after solution potential is stable Filtered after stirring a period of time, raw material of the copper sulfide concentrate as recovery copper；Liquid controls solution potential and pH value simultaneously after copper removal Under the conditions of add ethyl xanthate precipitation and remove cobalt, filtered after continuing to stir a period of time after solution potential is stable, cobalt sediment work For the raw material of Call Provision；Except liquid controls addition vulcanized sodium vulcanization under solution potential and pH value condition to remove zinc after cobalt simultaneously, work as solution Continue to filter after stirring a period of time after current potential is stable, zinc sulfide concentrates as the raw material for reclaiming zinc, except after zinc liquid add it is pure In alkali and output manganous carbonate slag.The present invention essence be using and meanwhile control metal ion in solution mixed potential and pH value realization The fractional precipitation separation of copper, cobalt and zinc, these process tight associations, separate processes can not all reach valuable metal substep in solution The Expected Results of separation.
Specific technical process and parameter are as follows：
1 control current potential vulcanization copper removal
With, with copper cobalt manganese solution to certain pH value, then controlling potential and pH value selectively vulcanize simultaneously in copper cobalt manganese slag Copper removal；With in copper cobalt manganese slag and copper cobalt manganese solution and terminal pH=0.1~0.5 of mixed solution is controlled, solution temperature is then kept 30~50 DEG C and 100~200r/min of mixing speed, the sodium sulfide solution that concentration is 234~390g/L is then added, is added simultaneously The pH value for entering technical-grade hydrochloric acid adjustment solution remains at 0.5~2.0, when metal ion in solution mixed potential is relative to sweet Mercury electrode is 80~120mV and to stablize 15~30min, continues to stir and realizes separation of solid and liquid using plate compression mode after 60min, Obtain liquid after copper removal.It is as follows to control the main chemical reactions that current potential vulcanization copper removal process occurs：
2HCl+MeCO3=MeCl2+CO2↑+H2O （1）
CuCl2+Na2S=CuS↓+2NaCl （2）
2 control current potential precipitate cobalts
Liquid, which controls solution potential and pH value simultaneously and adds sodium ethyl xanthate precipitation, after copper removal removes cobalt；Liquid is in temperature after copper removal Under the conditions of 30~50 DEG C and 100~200r/min of mixing speed, it is molten then to add the sodium ethyl xanthate that concentration is 10~50g/L Liquid, while the pH value for adding technical-grade hydrochloric acid adjustment solution remains at 2.1~4.0, when metal ion in solution mixes electricity Position is -80mV~-40mV relative to calomel electrode and stablizes 31~60min, continues to use plate compression mode after stirring 30min Separation of solid and liquid is realized, is obtained except liquid after cobalt.It is as follows to control the main chemical reactions that current potential precipitate cobalt process occurs：
CoCl2+2C2H5OCSSNa=Co(C2H5OCSS)2↓+2NaCl （3）
3 control current potential vulcanizations remove zinc
Except liquid controls the selectively vulcanization of solution potential and pH value to remove cobalt after cobalt simultaneously；Except after cobalt liquid in 30~70 DEG C of temperature and Under the conditions of 100~200r/min of mixing speed, then add concentration and be 39~156g/L sodium sulfide solution, while add industry The pH value of grade hydrochloric acid adjustment solution remains at 4.1~6.0, when metal ion in solution mixed potential is relative to calomel electrode For -240~-210mV and stablize 15~30min, continue to realize solid-liquid point using plate compression mode after 60~90min of stirring From, obtain remove zinc after liquid.Current potential vulcanization is controlled except the main chemical reactions that cobalt process occurs are as follows：
ZnCl2+Na2S=ZnS↓+2NaCl （4）
The vulcanized sodium, hydrochloric acid and sodium ethyl xanthate are technical grade reagent, and wherein vulcanized sodium weight/mass percentage composition is not small In 60.0%, hydrochloric acid weight/mass percentage composition is not less than 31.0% and sodium ethyl xanthate weight/mass percentage composition is not less than 82.0%.
The present invention is applied to the copper cobalt manganese solution and copper cobalt manganese slag of cobalt smelting system abstraction impurity removal process, copper cobalt manganese solution master The 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 has the advantage that compared with traditional copper cobalt manganese solution and copper cobalt manganese Slag treatment method：1st, the present invention uses Metal ion in solution mixed potential and pH value mode is controlled to realize the substep point of copper, cobalt and zinc in copper cobalt manganese solution simultaneously From；2nd, efficiently separating for cobalt and zinc in liquid is realized after copper removal using control current potential sulfide precipitation technology, cobalt contains in cobalt precipitated product Amount reaches more than 20.0%；3rd, the present invention has simple technical process, technical indicator stabilization, labor intensity small low with production cost The advantages that.
Brief description of the drawings
Fig. 1：Present invention process schematic flow sheet.
Embodiment
Embodiment 1：
The copper cobalt manganese solution and copper cobalt manganese slag of cobalt smelting system abstraction impurity removal process, copper cobalt manganese solution main component scope are （g/L）：Cu15.4, Co2.2, Zn9.8, Ca6.24, Mn105.2, Cl180 and H4.5, copper cobalt manganese slag main component scope are （%）：Cu17.5, Zn4.3, Co0.8 and Mn22.8.Vulcanized sodium, hydrochloric acid and sodium ethyl xanthate are technical grade reagent, vulcanized sodium matter Measure percentage composition and be not less than 60.0%, hydrochloric acid weight/mass percentage composition is not less than 31.0% and sodium ethyl xanthate weight/mass percentage composition is not small In 82.0%.
First with copper cobalt manganese slag and copper cobalt manganese solution and terminal pH=0.4 of mixed solution is controlled, solution temperature is then kept 45 DEG C of degree and mixing speed 120r/min, then add concentration and be 234g/L sodium sulfide solution, while add technical-grade hydrochloric acid The pH value of adjustment solution remains at 1.5, when metal ion in solution mixed potential relative to calomel electrode is 90mV and steady Determine 20min, continue to stir and separation of solid and liquid is realized using plate compression mode after 60min, copper concentration is reduced in liquid after copper removal 0.02g/L, copper content 52.3% in copper sulfide concentrate.
After copper removal then liquid adds the ethyl that concentration is 30g/L under the conditions of temperature 45 C and mixing speed 120r/min Sodium xanthate solution, while the pH value for adding technical-grade hydrochloric acid adjustment solution remains at 3.0, when metal ion in solution mixes Current potential relative to calomel electrode is -60mV and stable 35min, continues to stir and realizes solid-liquid using plate compression mode after 30min Separation, except cobalt concentration is reduced to 0.03g/L in liquid after cobalt, cobalt content is 23.5% in cobalt sediment.
Except liquid under the conditions of temperature 50 C and mixing speed 120r/min, then adds the vulcanization that concentration is 78g/L after cobalt Sodium solution, while the pH value for adding technical-grade hydrochloric acid adjustment solution remains at 5.0, when metal ion in solution mixed potential Relative to calomel electrode it is -220mV and stable 30min, continues to stir and realize that solid-liquid divides using plate compression mode after 60min From except zinc concentration is reduced to 0.02g/L in liquid after zinc, Zinc Content in Zinc Sulphide Concentrate content is 48.5%.

Claims (2)

  1. A kind of 1. method for controlling current potential selective precipitation separation cobalt, it is characterised in that comprise the following steps：
    （1）Control current potential vulcanization copper removal
    With in copper cobalt manganese slag and copper cobalt manganese solution and terminal pH=0.1~0.5 of mixed solution is controlled, solution temperature is then kept 30~50 DEG C and 100~200r/min of mixing speed, the sodium sulfide solution that concentration is 234~390g/L is then added, is added simultaneously The pH value for entering technical-grade hydrochloric acid adjustment solution remains at 0.5~2.0, when metal ion in solution mixed potential is relative to sweet Mercury electrode is 80~120mV and to stablize 15~30min, continues to stir and realizes separation of solid and liquid using plate compression mode after 60min, Obtain liquid after copper removal；
    （2）Control current potential precipitate cobalt
    Liquid is under the conditions of 30~50 DEG C of temperature and 100~200r/min of mixing speed after copper removal, then add concentration be 10~ 50g/L sodium ethyl xanthate solution, while the pH value for adding technical-grade hydrochloric acid adjustment solution remains at 2.1~4.0, when molten Metal ion mixed potential is -80mV~-40mV relative to calomel electrode and stablizes 31~60min in liquid, continues to stir 30min Separation of solid and liquid is realized using plate compression mode afterwards, obtained except liquid after cobalt；
    （3）Control current potential vulcanization removes zinc
    Except after cobalt liquid under the conditions of 30~70 DEG C of temperature and 100~200r/min of mixing speed, then add concentration be 39~ 156g/L sodium sulfide solution, while the pH value for adding technical-grade hydrochloric acid adjustment solution remains at 4.1~6.0, works as solution Middle metal ion mixed potential is -240~-210mV and to stablize 15~30min relative to calomel electrode, continue stirring 60~ Separation of solid and liquid is realized using plate compression mode after 90min, obtained except liquid after zinc.
  2. A kind of 2. method for controlling current potential selective precipitation separation cobalt as claimed in claim 1, it is characterised in that described ethyl Sodium xanthate weight/mass percentage composition is not less than 82.0%.
CN201610867704.8A 2016-09-30 2016-09-30 A kind of method for controlling current potential selective precipitation separation cobalt Expired - Fee Related CN106350673B (en)

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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
JP7036229B2 (en) * 2019-10-18 2022-03-15 Ｊｆｅスチール株式会社 Manganese recovery method and recovery equipment from waste batteries
JP7004091B2 (en) * 2019-10-18 2022-02-04 Ｊｆｅスチール株式会社 Manganese recovery method and recovery equipment from waste batteries
CN112266096B (en) * 2020-09-30 2021-09-21 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
CN113957249B (en) * 2021-01-18 2023-07-25 郑州大学 Method for separating zinc and cobalt ions in solution

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