CN102952954A - Processing method of trivalent cobalt nickel oxide waste material and waste cobalt nickel alloy - Google Patents

Processing method of trivalent cobalt nickel oxide waste material and waste cobalt nickel alloy Download PDF

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CN102952954A
CN102952954A CN2011102467429A CN201110246742A CN102952954A CN 102952954 A CN102952954 A CN 102952954A CN 2011102467429 A CN2011102467429 A CN 2011102467429A CN 201110246742 A CN201110246742 A CN 201110246742A CN 102952954 A CN102952954 A CN 102952954A
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cobalt
nickel
waste
trivalent
cobalt nickel
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CN2011102467429A
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CN102952954B (en
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王勤
陈艳红
张功勋
王超
马琳
闫梨
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深圳市格林美高新技术股份有限公司
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention provides a processing method of trivalent cobalt nickel oxide waste materials and waste cobalt nickel alloy, which comprises the following steps: firstly pulpifing trivalent cobalt nickel oxide waste materials by adding an acid solution with a hydrogen ion concentration of 1-2 mol/l, adding the cobalt nickel alloy waste materials under stirring, wherein the mass ratio of the alloy waste materials to the trivalent cobalt nickel oxide waste materials is 1:0.5-4, reacting at a temperature maintained at 80-99 DEG C, filtering, returning the filter residues to the above mentioned steps for leaching, performing chemical preliminary impurity removal and extraction deep purification impurity removal of the filtrate to obtain a high-concentration, pure cobalt nickel solution. The processing method can greatly reduce consumption of auxiliary materials, improve the leaching rate, shorten the reaction time, reduce the generation of toxic and harmful gas, and has great economic benefits and environment benefits.

Description

The treatment process of a kind of trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy
Technical field
The present patent application relates to a kind of method of processing trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy, belongs to environment protection and resource recycling technical field.
Background technology
The cobalt-nickel oxide that contains trivalent is mainly used in pigment, pottery and ceramic glaze, glass, preparation cobalt nickel salt, oxygenant and catalyzer, battery material etc.Contain cobalt, nickelalloy is mainly used in superalloy, magnetically hard alloy, Wimet, superhard alloy, stainless steel, non-corrosive metal, wear resistant alloy etc.
Contain the cobalt-nickel oxide of trivalent and contain cobalt, the purposes of nickelalloy is all very extensive, and in production and use procedure, can produce waste material and the waste and old cobalt that contains of a large amount of cobalt-nickel oxides that contains trivalent, the alloy of nickel, these contain cobalt, the waste material of nickel can be secondary use, usually the processing that contains the cobalt-nickel oxide waste material of trivalent is that reduction is leached in sour environment, reductive agent mainly is S-WAT, hydrogen peroxide etc., the waste and old cobalt that contains, the alloy of nickel has electrolysis and the molten two kinds of methods of roasting-acid usually, roasting-acid pasting mainly is to leach add oxygenant after the surplus or excess alloy roasting in sour environment, and oxygenant is oxygen normally, sodium chlorate etc.The cobalt-nickel oxide that one ton of usually conduct contains trivalent needs the reductive agent of 1-2 ton, and extraction time is long, and leaching yield is not high; And process the oxygenant that one ton of waste and old alloy that contains cobalt, nickel need to about 0.3-0.5 ton, for the very large alloying pellet of some particles, need repeatedly roasting, and leaching yield is not high yet.
Summary of the invention
The present patent application namely is for the problems referred to above, has proposed the treatment process of a kind of trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy, can greatly reduce supplementary product onsumption, improve leaching yield, Reaction time shorten reduces the generation of toxic and harmful, and huge economic benefit and environmental benefit are arranged.
The mentality of designing of the present patent application is: because the cobalt-nickel oxide of trivalent all has strong oxidizing property, and the alloy that contains cobalt, nickel has reductibility owing to simple substance such as containing the cobalt ferronickel, so they are mixed in sour environment according to a certain percentage leach, do not need to add a large amount of Oxidizing and Reducing Agents, the alloy that contains cobalt, nickel is not needed roasting, avoid again simultaneously the generation of toxic and harmful, improved the cobalt nickel leaching yield of two kinds of waste materials.
Specifically, the treatment process of the present patent application described trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy comprises following step:
The cobalt-nickel oxide waste material that 1) will contain trivalent adds the acid solution pulp that hydrogen ion concentration is 1-2mol/l, and solid-to-liquid ratio is 1:5-20, and temperature of reaction is 80-99 ℃;
2) under agitation add the alloyed scrap that contains cobalt, nickel, mixing speed is 100-800r/min, alloyed scrap and the mass ratio 1:0.5-4 that contains the cobalt-nickel oxide waste material of trivalent, reaction times is 4-10 hour, temperature of reaction maintains 80-99 ℃, need supplemental acid therebetween, keep hydrionic concentration;
3) after the filtration, filter residue returns step 1 and leaches, and filtrate is also contained the impurity of iron, chromium, copper, tungsten, molybdenum, magnesium, aluminium, lithium, manganese except containing the cobalt nickel ion;
4) removal of impurities: the filtrate after the filtration is under temperature 60-99 ℃, adding concentration is the alkaline solution of 6-10mol/l, pull back to about pH=2.0, adding oxygenant oxidation ferrous iron is ferric iron, at 60-99 ℃ of lower stirring reaction 0.5-2 hour, and then readjustment pH=4.0-4.5, at 60-99 ℃ of lower stirring reaction 1-2 hour, in order to remove most iron, aluminium, chromium, while tungsten, molybdenum also can precipitate with the oxygen acid form, filter residue after the filtration is in order to reclaim chromium, tungsten, molybdenum, filtrate is through P204 extraction agent extracting and separating, so that iron, aluminium, chromium, tungsten, molybdenum, copper, manganese and cobalt, nickel, magnesium separates, and then with P507 extraction agent separation of cobalt, nickel and magnesium, and Sync enrichment cobalt and nickel, obtain high density, pure cobalt, nickel solution.
In above-mentioned step 2, the particle diameter that contains the cobalt-nickel oxide waste material of trivalent is 0.1-1.0mm, and the particle diameter that contains the alloyed scrap of cobalt, nickel is 0.1-5.0mm.
In above-mentioned step 3, the filter cloth aperture of filtration is the 1-120 micron.
In above-mentioned step 4, oxygenant is 1:0.5-2 with the ratio of ferrous mole number.
Common oxygenant is the material that electronics is reduced that is easy to get in chemical reaction, comprises typical non-metal simple-substance such as F 2, O 2, Cl 2, Br 2, I 2, S etc.; The high price compound that contains valence variation element is such as KMnO 4, KClO 3, dense H 2SO 4, HNO 3, MnO 2, FeCl 3Deng, and metallic cation is such as Fe 3+, Cu 2+Deng.
The cobalt-nickel oxide waste material of trivalent comprises waste and old cobalt sesquioxide, tricobalt tetroxide, nickel sesquioxide, cobalt acid lithium, lithium nickelate, contains catalyzer of trivalent cobalt nickel etc., and the waste and old alloy that contains cobalt, nickel comprises waste and old cobalt-nickel alloy, cobalt tungsten alloy, cochrome, cobalt-copper alloy, Rhometal, cupronickel etc.
The molecular formula of P204 extraction agent is C16H35O4P, is widely used in the extracting and separating of non-ferrous metal and rare earth, also can be used for the industries such as medicine, printing and dyeing, petrochemical wastewater processing, also can make the starting material of wetting agent and tensio-active agent.
The molecular formula of P507 extraction agent is C 16H 35O 3P is a kind of efficient organophosphorous extractant, is usually used in the separation of nickel-cobalt, copper-zinc, the separating-purifying of the separation of rare earth element and single rare earth metal, rare earth and the aspects such as separating of non-rare earth.
The treatment process of the present patent application described trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy, need not to add a large amount of oxygenants or reductive agent, and extraction time is short, leaching yield is high, and has reduced the discharge of toxic and harmful, the requirement of composite energy-saving environment protection.
Embodiment
Below in conjunction with concrete embodiment; treatment process to described trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy is set forth; purpose is better to understand the described technology contents of the present patent application for the public; rather than to the restriction of described technical scheme; in fact; with the Principles of Chemical Engineering identical or approximate with the present patent application; the improvement that described method steps is carried out; comprise the change that the chemical reagent that is applied to, reaction conditions etc. are made, all within the present patent application technical scheme required for protection.
Embodiment one
Adopt following method that trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy are processed, comprise following step:
1. the nickel sesquioxide waste material is added the sulphuric acid soln pulp that hydrogen ion concentration is 1mol/l, solid-to-liquid ratio is 1:5, and temperature of reaction is 80 ℃;
2. under agitation add the waste and old alloy that contains cobalt, nickel, mixing speed is 100-800r/min, alloyed scrap and the mass ratio 1:0.5 that contains the cobalt-nickel oxide waste material of trivalent, reaction times is 4 hours, and temperature of reaction maintains 80 ℃, needs supplemental acid therebetween, keep hydrionic concentration, wherein, the particle diameter of nickel sesquioxide waste material is 0.1mm, and the particle diameter of the waste and old alloy that contains cobalt, nickel is 0.1mm;
3. after filtering, filter residue returns step 1 and leaches;
4. removal of impurities: the filtrate after the filtration is under temperature 60 C, and adding concentration is the alkaline solution of 6mol/l, pulls back to pH=2.0, adds the oxygenant Oxidation of Fe 2+Be Fe 3+, wherein oxygenant and Fe 2+Mole ratio be 1:0.5,60 ℃ of lower stirring reactions 2 hours, and then readjustment pH=4.0,60 ℃ of lower stirring reactions 2 hours, remove most iron, aluminium, chromium, tungsten, molybdenum also can precipitate with the oxygen acid form simultaneously, filter residue after the filtration is in order to reclaim chromium, tungsten, molybdenum, filtrate is through P204 extraction agent extracting and separating, so that iron, aluminium, chromium, tungsten, molybdenum, copper, manganese separate with cobalt, nickel, magnesium, and then with P507 extraction agent separation of cobalt, nickel and magnesium, and Sync enrichment cobalt and nickel obtain high density, pure cobalt, nickel solution.
Embodiment two
Adopt following method that trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy are processed, comprise following step:
1. the cobalt-nickel oxide waste material that will contain trivalent---cobalt acid lithium, adding hydrogen ion concentration is the sulphuric acid soln pulp of 2mol/l, and solid-to-liquid ratio is 1:20, and temperature of reaction is 99 ℃;
2. under agitation add alloyed scrap---the Rhometal that contains cobalt, nickel, mixing speed is 100-800r/min, alloyed scrap and the mass ratio 1:4 that contains the cobalt-nickel oxide waste material of trivalent, reaction times is 10 hours, and temperature of reaction maintains 99 ℃, needs supplemental acid therebetween, keep hydrionic concentration, wherein, the particle diameter of cobalt acid lithium is 1.0mm, and the particle diameter of Rhometal is 5.0mm;
3. after filtering, filter residue returns step 1 and leaches, and filtrate is also contained the impurity such as iron, chromium, copper, tungsten, molybdenum, magnesium, aluminium, lithium, manganese except containing the cobalt nickel ion;
4. removal of impurities: the filtrate after the filtration is under 99 ℃ of temperature, adding concentration is the alkaline solution of 10mol/l, pull back to about pH=2.0, adding oxygenant oxidation ferrous iron is ferric iron, oxygenant is 1:2 with the ratio of ferrous mole number, 99 ℃ of lower stirring reactions 0.5 hour, and then readjustment pH=4.5,99 ℃ of lower stirring reactions 1 hour, in order to remove most iron, aluminium, chromium, while tungsten, molybdenum also can be with oxygen acid form precipitation, and the filter residue after the filtration is in order to reclaim chromium, tungsten, molybdenum, filtrate is through P204 extraction agent extracting and separating, so that iron, aluminium, chromium, tungsten, molybdenum, copper, manganese and cobalt, nickel, magnesium separates, and then with P507 extraction agent separation of cobalt, nickel and magnesium, and Sync enrichment cobalt and nickel obtain high density, pure cobalt, nickel solution.
Embodiment three
Adopt following method that trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy are processed, comprise following step:
1. the lithium nickelate waste material being added hydrogen ion concentration is the salpeter solution pulp of 1.5mol/l, and solid-to-liquid ratio is 1:10, and temperature of reaction is 90 ℃;
2. under agitation add the cobalt-copper alloy waste material, mixing speed is 100-800r/min, the mass ratio 1:3 of cobalt-copper alloy waste material and lithium nickelate waste material, reaction times is 7 hours, and temperature of reaction maintains 90 ℃, needs supplemental acid therebetween, keep hydrionic concentration, wherein, the particle diameter of lithium nickelate waste material is 0.5mm, and the particle diameter of cobalt-copper alloy waste material is 2.0mm;
3. after filtering, filter residue returns step 1 and leaches, and filtrate is also contained the impurity of iron, chromium, copper, tungsten, molybdenum, magnesium, aluminium, lithium, manganese except containing the cobalt nickel ion;
4. removal of impurities: the filtrate after the filtration is under 90 ℃ of temperature, adding concentration is the alkaline solution of 8mol/l, pull back to about pH=2.0, adding oxygenant oxidation ferrous iron is ferric iron, oxygenant is 1:1 with the ratio of ferrous mole number, 80 ℃ of lower stirring reactions 1 hour, and then readjustment pH=4.2,70 ℃ of lower stirring reactions 1.5 hours, in order to remove most iron, aluminium, chromium, while tungsten, molybdenum also can be with oxygen acid form precipitation, and the filter residue after the filtration is in order to reclaim chromium, tungsten, molybdenum, filtrate is through P204 extraction agent extracting and separating, so that iron, aluminium, chromium, tungsten, molybdenum, copper, manganese and cobalt, nickel, magnesium separates, and then with P507 extraction agent separation of cobalt, nickel and magnesium, and Sync enrichment cobalt and nickel obtain high density, pure cobalt, nickel solution.
Embodiment four
Get the useless cobalt sesquioxide of 100g, adding hydrogen ion concentration is the sulphuric acid soln 1300ml of 2mol/l, stirs and is warmed up to 90 ℃, add useless cobalt-nickel alloy particle 100g(cobalt contents 18.5%, nickel content 6.5% wherein, iron level 23.8%, chromium content 27.3% is between the particle diameter 0.5-3mm), 5 hours reaction times, add midway sulfuric acid with the hydrogen ion concentration of keeping solution at 2mol/l, filter also washing filter residue, obtain filtrate 1500ml, filter residue 8.2g, concrete outcome such as following table:
Generally speaking, the treatment process of the present patent application described trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy, reduced consumption, raising leaching yield, the Reaction time shorten of auxiliary material, reduced the generation of toxic and harmful, huge economic benefit and environmental benefit have been arranged.

Claims (6)

1. the treatment process of a trivalent cobalt-nickel oxide waste material and waste and old cobalt, nickelalloy is characterized in that, described method comprises following step:
The cobalt-nickel oxide waste material that 1) will contain trivalent adds the aqueous solution pulp that hydrogen ion concentration is 1-2mol/l, and solid-to-liquid ratio is 1:5-20, and temperature of reaction is 80-99 ℃;
2) under agitation add the alloyed scrap that contains cobalt, nickel, mixing speed is 100-800r/min, alloyed scrap and the mass ratio 1:0.5-4 that contains the cobalt-nickel oxide waste material of trivalent, reaction times is 4-10 hour, temperature of reaction maintains 80-99 ℃, need supplemental acid therebetween, keep hydrionic concentration;
3) after the filtration, filter residue returns step 1 and leaches, and filtrate is also contained the impurity of iron, chromium, copper, tungsten, molybdenum, magnesium, aluminium, lithium, manganese except containing the cobalt nickel ion;
4) removal of impurities: the filtrate after the filtration is under temperature 60-99 ℃, adding concentration is the alkaline solution of 6-10mol/l, pull back to about pH=2.0, adding oxygenant oxidation ferrous iron is ferric iron, at 60-99 ℃ of lower stirring reaction 0.5-2 hour, and then readjustment pH=4.0-4.5, at 60-99 ℃ of lower stirring reaction 1-2 hour, in order to remove most iron, aluminium, chromium, while tungsten, molybdenum also can precipitate with the oxygen acid form, filter residue after the filtration is in order to reclaim chromium, tungsten, molybdenum, filtrate is through P204 extraction agent extracting and separating, so that iron, aluminium, chromium, tungsten, molybdenum, copper, manganese and cobalt, nickel, magnesium separates, and then with P507 extraction agent separation of cobalt, nickel and magnesium, and Sync enrichment cobalt and nickel, obtain high density, pure cobalt, nickel solution.
2. treatment process according to claim 1 is characterized in that: in above-mentioned step 2) in, the particle diameter that contains the cobalt-nickel oxide waste material of trivalent is 0.1-1.0mm, the particle diameter that contains the alloyed scrap of cobalt, nickel is 0.1-5.0mm.
3. treatment process according to claim 1, it is characterized in that: in above-mentioned step 3), the filter cloth aperture of filtration is the 1-120 micron.
4. treatment process according to claim 1, it is characterized in that: in above-mentioned step 4), oxygenant is 1:0.5-2 with the ratio of ferrous mole number.
5. treatment process according to claim 1, it is characterized in that: in above-mentioned step 4), described oxygenant comprises F 2, O 2, Cl 2, Br 2, I 2, S, KMnO 4, KClO 3, dense H 2SO 4, dense HNO 3, MnO 2, FeCl 3, Fe 3+Or Cu 2+
6. treatment process according to claim 1, it is characterized in that: the cobalt-nickel oxide waste material of described trivalent comprises waste and old cobalt sesquioxide, tricobalt tetroxide, nickel sesquioxide, cobalt acid lithium, lithium nickelate or contains the catalyzer of trivalent cobalt nickel that the described waste and old alloy that contains cobalt, nickel comprises waste and old cobalt-nickel alloy, cobalt tungsten alloy, cochrome, cobalt-copper alloy, Rhometal or cupronickel.
CN201110246742.9A 2011-08-26 2011-08-26 Processing method of trivalent cobalt nickel oxide waste material and waste cobalt nickel alloy CN102952954B (en)

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Cited By (7)

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CN103849775A (en) * 2014-03-25 2014-06-11 西北有色金属研究院 Method for recycling nickel and cobalt from high temperature alloyed scrap
CN105568001A (en) * 2016-02-03 2016-05-11 广东佳纳能源科技有限公司 Combined high-pressure acid leaching method for cobalt alloy and oxide cobalt minerals
CN105568000A (en) * 2016-02-03 2016-05-11 广东佳纳能源科技有限公司 Combined high-pressure acid leaching method for cobalt containing sulfide and heterogenite
US9648870B2 (en) 2014-12-26 2017-05-16 Industrial Technology Research Institute Antimicrobial composite material and method for fabricating the same
CN106834742A (en) * 2017-02-22 2017-06-13 桂林理工大学 It is a kind of to clean the method for extracting nickel cobalt
CN108408745A (en) * 2018-04-02 2018-08-17 方嘉城 A kind of method that waste lithium cell prepares battery-level lithium carbonate
CN109943733A (en) * 2019-03-12 2019-06-28 衢州华友钴新材料有限公司 A kind of crude cobalt/nickel salt raw material efficiently separates cobalt/nickel magnesium manganese method

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CN101575676A (en) * 2009-06-18 2009-11-11 中南大学 Method for removing iron and enriching nickel cobalt through precipitation of laterite type nickel ores
CN102061390A (en) * 2010-12-03 2011-05-18 安化金源新材料有限责任公司 Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste
CN102101701A (en) * 2010-12-31 2011-06-22 湖南邦普循环科技有限公司 Method for recovering cobalt and lithium from waste lithium cobaltite and preparing lithium cobaltite

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Publication number Priority date Publication date Assignee Title
CN101575676A (en) * 2009-06-18 2009-11-11 中南大学 Method for removing iron and enriching nickel cobalt through precipitation of laterite type nickel ores
CN102061390A (en) * 2010-12-03 2011-05-18 安化金源新材料有限责任公司 Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste
CN102101701A (en) * 2010-12-31 2011-06-22 湖南邦普循环科技有限公司 Method for recovering cobalt and lithium from waste lithium cobaltite and preparing lithium cobaltite

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849775A (en) * 2014-03-25 2014-06-11 西北有色金属研究院 Method for recycling nickel and cobalt from high temperature alloyed scrap
CN103849775B (en) * 2014-03-25 2016-01-13 西北有色金属研究院 A kind of method reclaiming nickel and cobalt from high-temperature alloy waste material
US9648870B2 (en) 2014-12-26 2017-05-16 Industrial Technology Research Institute Antimicrobial composite material and method for fabricating the same
CN105568001A (en) * 2016-02-03 2016-05-11 广东佳纳能源科技有限公司 Combined high-pressure acid leaching method for cobalt alloy and oxide cobalt minerals
CN105568000A (en) * 2016-02-03 2016-05-11 广东佳纳能源科技有限公司 Combined high-pressure acid leaching method for cobalt containing sulfide and heterogenite
CN106834742A (en) * 2017-02-22 2017-06-13 桂林理工大学 It is a kind of to clean the method for extracting nickel cobalt
CN108408745A (en) * 2018-04-02 2018-08-17 方嘉城 A kind of method that waste lithium cell prepares battery-level lithium carbonate
CN109943733A (en) * 2019-03-12 2019-06-28 衢州华友钴新材料有限公司 A kind of crude cobalt/nickel salt raw material efficiently separates cobalt/nickel magnesium manganese method
WO2020181745A1 (en) * 2019-03-12 2020-09-17 衢州华友钴新材料有限公司 Method for efficiently separating cobalt/nickel magnesium manganese from crude cobalt/nickel salt raw material

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