CN110028110A - A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore - Google Patents
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore Download PDFInfo
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- CN110028110A CN110028110A CN201910407906.8A CN201910407906A CN110028110A CN 110028110 A CN110028110 A CN 110028110A CN 201910407906 A CN201910407906 A CN 201910407906A CN 110028110 A CN110028110 A CN 110028110A
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- C01—INORGANIC CHEMISTRY
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- C01G51/00—Compounds of cobalt
- C01G51/06—Carbonates
Abstract
The invention discloses a kind of techniques for preparing basic cobaltous carbonate as raw material using copper cobalt ore, comprising the following steps: one, copper cobalt ore concentrate calcined；Two, the stirring of concentrated sulfuric acid gradient is added after calcining；Three, copper electrodeposition；Four, drift ice is added and carries out oxidation precipitation；Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；Six, suspension obtained in step 5 is aged；Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7；Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains basic cobaltous carbonate product after dry；The present invention carries out obtaining water-soluble cobalt salt by the way of concentrated sulfuric acid gradient stirring and dissolving under the conditions of electrolytic catalysis after roasting direct, and compared to high conversion rate for the mode of sulfating roasting, yield is higher.
Description
Technical field
It is specifically a kind of to prepare alkali formula carbon by raw material of copper cobalt ore the present invention relates to a kind of production method of basic cobaltous carbonate
The technique of sour cobalt.
Background technique
Cobalt, symbol of element Co, silvery white ferromagnetic metal, surface are located at the 4th in silvery white slightly pale pink in periodic table
Period, the VIIIth race, atomic number 27, atomic weight 58.9332, Patterns for Close-Packed Hexagonal Crystal, usual valences are+2 ,+3.Cobalt is that have
The steel grey metal of gloss, it is harder and crisp, there is ferromagnetism, is heated to magnetism at 1150 DEG C and disappears.The chemical valence of cobalt is+divalent
With+trivalent.Discord water effect at normal temperature, it is also very stable in wet air.It is heated to oxygen at 300 DEG C or more in air
Metaplasia burns into Co3O4 in white heat at CoO.Thin metal cobalt powder made of hydrogen reduction method in air can spontaneous combustion generation oxidation
Cobalt.Cobalt is the important source material for producing heat-resisting alloy, hard alloy, anti-corrosion alloy, magnetic alloy and various cobalt salts.
The physics of cobalt, chemical property determine it be production heat-resisting alloy, hard alloy, anti-corrosion alloy, magnetic alloy and
The important source material of various cobalt salts.Cobalt-base alloys or cobalt-containing alloy steel are used as the blade of gas turbine, impeller, conduit, jet and start
Machine, rocket engine, guided missile component and chemical industry equipment in various high load capacities heat-resistant part and atomic energy industry it is important
Metal material.Cobalt can guarantee that hard alloy has certain toughness as the binder in powder metallurgy.Magnetic alloy is modernization
Indispensable material in electronics and mechanotronics, for manufacturing the various elements of sound, light, the equipment such as electrically and magnetically.Cobalt is also forever
The important component of long magnetic alloy.In chemical industry, cobalt is also used to coloured in addition to for high temperature alloy and anti-corrosion alloy
Glass, pigment, enamel and catalyst, desiccant etc..According to Britain " metal Leader ", hard metal department and superalloy are come from
Demand of the aspect to cobalt is more powerful.In addition, cobalt is in battery department consumption figure growth rate highest.Domestic related report says that cobalt exists
The application of battery industry, Diamond Tools Industry and catalyst industry is also by further expansion, thus the demand to metallic cobalt
It is in rising trend.Independent cobalt deposits is generally divided into cobalt arsenides bed, vulcanization cobalt deposits and earthy cobalt mineral deposit three classes.Cobalt removes independent mine
Bed is outer, be largely dispersed in skarn iron deposit, vanadium titano-magnetite, hydrothermal solution polymetallic ore, various types copper mine, deposit cobalt manganese ore,
In the mineral deposits such as copper nickel sulfide mineral, silicic acid nickel minerals, though grade is low, scale is often larger, is the main source for extracting cobalt.It is comprehensive
The evaluation index of mineral deposit association cobalt there is no Uniform provisions, the ore for generally selecting smelting performance good, and grade containing cobalt is greater than 0.01%.Cobalt essence
The grade 0.2% of mine is just valuable, if metalliferous deposit scale is big, ore synthetical recovery is imitated, cobalt how many calculate how much.Cobalt sulphur
According to chemical composition, concentrate is divided into six grades to concentrate, calculates by dry mine grade.
Main cupric and cobalt, copper are insoluble in acid in copper cobalt ore, it is therefore desirable to by carrying out sulphation in fluidized roaster
Roasting, it is desirable that equipment and condition it is higher, and a big chunk cobalt is not converted into cobalt salt, and yield is not high.
Summary of the invention
The purpose of the present invention is to provide one kind not to need sulfating roasting, improves preparing by raw material of copper cobalt ore for yield
The technique of basic cobaltous carbonate, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.5~2.0, be then added drift ice into
Row oxidation precipitation, drift ice is 38~50g/L containing alkali, is 50~60g/L containing chlorine, stops when drift ice to most 2.5~2.8 PH are added
Only, filtrate is obtained by filters pressing, the impurity elements such as zinc, iron, lead is precipitated；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
As a further solution of the present invention: the mass ratio 2.5:1 of filtrate and sodium carbonate in the step 5.
As a further solution of the present invention: sodium carbonate liquor is first added in reaction kettle in the step 5, then to general
Filtrate obtained in a dropping step four in reaction kettle, rate of addition 1.17m3/h are added dropwise with controlling terminal Ph=7.6~8.0
Process is stirred continuously, and 80 DEG C of reaction temperature, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
As a further solution of the present invention: the technique of basic cobaltous carbonate, including following step are prepared using copper cobalt ore as raw material
It is rapid:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.6, and drift ice is then added and is aoxidized
Precipitating, drift ice is 42g/L containing alkali, is 52g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
As a further solution of the present invention: the technique of basic cobaltous carbonate, including following step are prepared using copper cobalt ore as raw material
It is rapid:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.7, and drift ice is then added and is aoxidized
Precipitating, drift ice is 43g/L containing alkali, is 52g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
As a further solution of the present invention: the technique of basic cobaltous carbonate, including following step are prepared using copper cobalt ore as raw material
It is rapid:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.9, and drift ice is then added and is aoxidized
Precipitating, drift ice is 50g/L containing alkali, is 55g/L containing chlorine, stops when drift ice to most 2.7 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
As a further solution of the present invention: the technique of basic cobaltous carbonate, including following step are prepared using copper cobalt ore as raw material
It is rapid:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 2.0, and drift ice is then added and is aoxidized
Precipitating, drift ice is 42g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
As a further solution of the present invention: the technique of basic cobaltous carbonate, including following step are prepared using copper cobalt ore as raw material
It is rapid:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.8, and drift ice is then added and is aoxidized
Precipitating, drift ice is 45g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Compared with prior art, the beneficial effects of the present invention are: the present invention using electrolytic catalysis after roasting direct under the conditions of
The mode for carrying out concentrated sulfuric acid gradient stirring and dissolving obtains water-soluble cobalt salt, compared to high conversion rate for the mode of sulfating roasting,
Yield is higher；
The purity is high of basic cobaltous carbonate made from processing technology of the invention.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment one
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；It can make in miberal powder
Copper, cobalt large ratio be converted into sulfate.
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；Copper is separated using electrolytic deposition.
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.5, and drift ice is then added and is aoxidized
Precipitating, drift ice is 38g/L containing alkali, is 50g/L containing chlorine, stops when drift ice to most 2.5 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.Repeatedly reaction and filters pressing improve cobalt carbonate yield.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
Embodiment two
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.6, and drift ice is then added and is aoxidized
Precipitating, drift ice is 42g/L containing alkali, is 52g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
| Chemical component w/% | National standard HG/T4519-2013 | The present embodiment product |
| Co | ≥45 | 46 |
| Ni | ≤0.02 | 0.01 |
| Cu | ≤0.001 | 0.0008 |
| Fe | ≤0.005 | 0.003 |
| Na | ≤0.02 | 0.02 |
| Pb | ≤0.005 | 0.005 |
| Zn | ≤0.001 | 0.001 |
| Ca | ≤0.01 | 0.008 |
| Sulfate | ≤0.05 | 0.04 |
| Chloride | ≤0.05 | 0.05 |
| Hydrochloric acid insoluble substance | ≤0.02 | 0.02 |
Embodiment three
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.7, and drift ice is then added and is aoxidized
Precipitating, drift ice is 43g/L containing alkali, is 52g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
Example IV
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.9, and drift ice is then added and is aoxidized
Precipitating, drift ice is 50g/L containing alkali, is 55g/L containing chlorine, stops when drift ice to most 2.7 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
| Chemical component w/% | National standard HG/T4519-2013 | The present embodiment product |
| Co | ≥45 | 46 |
| Ni | ≤0.02 | 0.01 |
| Cu | ≤0.001 | 0.0006 |
| Fe | ≤0.005 | 0.004 |
| Na | ≤0.02 | 0.01 |
| Pb | ≤0.005 | 0.004 |
| Zn | ≤0.001 | 0.001 |
| Ca | ≤0.01 | 0.007 |
| Sulfate | ≤0.05 | 0.03 |
| Chloride | ≤0.05 | 0.04 |
| Hydrochloric acid insoluble substance | ≤0.02 | 0.01 |
Embodiment five
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 2.0, and drift ice is then added and is aoxidized
Precipitating, drift ice is 42g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
Embodiment six
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.8, and drift ice is then added and is aoxidized
Precipitating, drift ice is 45g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.6 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
| Chemical component w/% | National standard HG/T4519-2013 | The present embodiment product |
| Co | ≥45 | 47 |
| Ni | ≤0.02 | 0.02 |
| Cu | ≤0.001 | 0.001 |
| Fe | ≤0.005 | 0.005 |
| Na | ≤0.02 | 0.01 |
| Pb | ≤0.005 | 0.003 |
| Zn | ≤0.001 | 0.001 |
| Ca | ≤0.01 | 0.006 |
| Sulfate | ≤0.05 | 0.03 |
| Chloride | ≤0.05 | 0.04 |
| Hydrochloric acid insoluble substance | ≤0.02 | 0.02 |
Embodiment seven
A kind of technique that basic cobaltous carbonate is prepared as raw material using copper cobalt ore, comprising the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient, gradient is added
The program of stirring includes stirring at low speed to stir 8-10min, moderate-speed mixer 1200-1400r/ for the revolving speed of 800-900r/min
The revolving speed of min stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode
Electrode leads to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out to the mine liquid in step 2
Copper electrodeposition obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, removes the nonmetallic inclusions such as deliming, removal of impurities
Filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 2.0, and drift ice is then added and is aoxidized
Precipitating, drift ice is 50g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.8 PH are added, filtered by filters pressing
The impurity elements such as zinc, iron, lead are precipitated in liquid；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirring 1 is small
When, obtain slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and is obtained after dry
To basic cobaltous carbonate product.
Preferably, in step 5 filtrate and sodium carbonate mass ratio 2.5:1.
Preferably, sodium carbonate liquor is first added in reaction kettle in step 5, then to will be in reaction kettle in a dropping step four
Obtained filtrate, rate of addition 1.17m3/h, to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, reaction temperature
80 DEG C of degree, and the sodium ascorbate of 5-10g/KgCo is added into reaction kettle to prevent block.
| Chemical component w/% | National standard HG/T4519-2013 | The present embodiment product |
| Co | ≥45 | 46 |
| Ni | ≤0.02 | 0.01 |
| Cu | ≤0.001 | 0.001 |
| Fe | ≤0.005 | 0.002 |
| Na | ≤0.02 | 0.01 |
| Pb | ≤0.005 | 0.003 |
| Zn | ≤0.001 | 0.001 |
| Ca | ≤0.01 | 0.005 |
| Sulfate | ≤0.05 | 0.03 |
| Chloride | ≤0.05 | 0.03 |
| Hydrochloric acid insoluble substance | ≤0.02 | 0.01 |
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (8)
1. a kind of technique for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which comprises the following steps:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient is added, gradient stirring
Program include stirring at low speed to stir 8-10min for the revolving speed of 800-900r/min, moderate-speed mixer is 1200-1400r/min
Revolving speed stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode electrode,
Lead to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out copper electricity to the mine liquid in step 2
Solution deposition, obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, and removal of impurities filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.5~2.0, and drift ice is then added and carries out oxygen
Change precipitating, drift ice is 38~50g/L containing alkali, it is 50~60g/L containing chlorine, stops when drift ice to most 2.5~2.8 PH are added,
Filtrate is obtained by filters pressing；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirs 1 hour, obtains
To slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains alkali after dry
Formula cobalt carbonate product.
2. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that the step
The mass ratio 2.5:1 of filtrate and sodium carbonate in rapid five.
3. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that the step
Sodium carbonate liquor is first added in reaction kettle in rapid five, and then to by filtrate obtained in a dropping step four in reaction kettle, speed is added dropwise
Degree is 1.17m3/h, and to control terminal Ph=7.6~8.0, dropwise addition process is stirred continuously, 80 DEG C of reaction temperature, and to reaction kettle
The sodium ascorbate of 5-10g/KgCo of middle addition is to prevent block.
4. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that including with
Lower step:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient is added, gradient stirring
Program include stirring at low speed to stir 8-10min for the revolving speed of 800-900r/min, moderate-speed mixer is 1200-1400r/min
Revolving speed stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode electrode,
Lead to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out copper electricity to the mine liquid in step 2
Solution deposition, obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, and removal of impurities filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.6, and then it is heavy to carry out oxidation for addition drift ice
It forms sediment, drift ice is 42g/L containing alkali, is 52g/L containing chlorine, stops when drift ice to most 2.6 PH are added, obtain filtrate by filters pressing；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirs 1 hour, obtains
To slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains alkali after dry
Formula cobalt carbonate product.
5. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that including with
Lower step:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient is added, gradient stirring
Program include stirring at low speed to stir 8-10min for the revolving speed of 800-900r/min, moderate-speed mixer is 1200-1400r/min
Revolving speed stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode electrode,
Lead to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out copper electricity to the mine liquid in step 2
Solution deposition, obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, and removal of impurities filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.7, and then it is heavy to carry out oxidation for addition drift ice
It forms sediment, drift ice is 43g/L containing alkali, is 52g/L containing chlorine, stops when drift ice to most 2.6 PH are added, obtain filtrate by filters pressing；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirs 1 hour, obtains
To slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains alkali after dry
Formula cobalt carbonate product.
6. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that including with
Lower step:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient is added, gradient stirring
Program include stirring at low speed to stir 8-10min for the revolving speed of 800-900r/min, moderate-speed mixer is 1200-1400r/min
Revolving speed stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode electrode,
Lead to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out copper electricity to the mine liquid in step 2
Solution deposition, obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, and removal of impurities filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.9, and then it is heavy to carry out oxidation for addition drift ice
It forms sediment, drift ice is 50g/L containing alkali, is 55g/L containing chlorine, stops when drift ice to most 2.7 PH are added, obtain filtrate by filters pressing；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirs 1 hour, obtains
To slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains alkali after dry
Formula cobalt carbonate product.
7. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that including with
Lower step:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient is added, gradient stirring
Program include stirring at low speed to stir 8-10min for the revolving speed of 800-900r/min, moderate-speed mixer is 1200-1400r/min
Revolving speed stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode electrode,
Lead to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out copper electricity to the mine liquid in step 2
Solution deposition, obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, and removal of impurities filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 2.0, and then it is heavy to carry out oxidation for addition drift ice
It forms sediment, drift ice is 42g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.6 PH are added, obtain filtrate by filters pressing；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirs 1 hour, obtains
To slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains alkali after dry
Formula cobalt carbonate product.
8. the technique according to claim 1 for preparing basic cobaltous carbonate as raw material using copper cobalt ore, which is characterized in that including with
Lower step:
One, copper cobalt ore concentrate is calcined；
Two, calcined copper cobalt ore concentrate is milled to 2400 mesh, is placed in agitator and the stirring of concentrated sulfuric acid gradient is added, gradient stirring
Program include stirring at low speed to stir 8-10min for the revolving speed of 800-900r/min, moderate-speed mixer is 1200-1400r/min
Revolving speed stirs 15-18min, and the revolving speed that high-speed stirred is 2000-2400r/min stirs 10-15min；Using fine copper as anode electrode,
Lead to electrocatalytic reaction by cathode electrode of the carbon-point of graphene modified, stands 80min；Obtain mine liquid；
Three, blister copper is made to slab in advance as anode, fine copper, which is laminated, makees cathode, carries out copper electricity to the mine liquid in step 2
Solution deposition, obtains cathode copper, is then filtered, washed mine liquid with plate and frame filter press, and removal of impurities filtrate enters next program；
Four, removal of impurities filtrate obtained in step 3 is added dilute sulfuric acid and adjusts pH value to 1.8, and then it is heavy to carry out oxidation for addition drift ice
It forms sediment, drift ice is 45g/L containing alkali, is 60g/L containing chlorine, stops when drift ice to most 2.6 PH are added, obtain filtrate by filters pressing；
Five, filtrate obtained in step 4 is added in reaction kettle with sodium carbonate liquor and reacts to obtain suspension；
Six, suspension obtained in step 5 is aged, when ageing needs to stir, temperature-resistant；
Seven, after to the filter press filters pressing of suspension obtained in step 6, obtained filter cake is washed with deionized；
Eight, sodium carbonate liquor is added after sizing mixing in filter cake deionized water obtained in step 7, is warming up to 80 DEG C, stirs 1 hour, obtains
To slurries；
Nine, after the filter press filters pressing of slurries obtained in step 8, obtained filter cake is washed with deionized, and obtains alkali after dry
Formula cobalt carbonate product.
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| CN112846209A (en) * | 2019-11-28 | 2021-05-28 | 荆门市格林美新材料有限公司 | Preparation method of rod-shaped cobalt powder |
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|---|---|---|---|---|
| CN112846209A (en) * | 2019-11-28 | 2021-05-28 | 荆门市格林美新材料有限公司 | Preparation method of rod-shaped cobalt powder |
| CN112846209B (en) * | 2019-11-28 | 2023-06-09 | 荆门市格林美新材料有限公司 | Preparation method of rod-shaped cobalt powder |
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