CN104701524A - Method for directly preparing nickel-cobalt-manganese ternary cathode material precursor from nickel electrolyte - Google Patents
Method for directly preparing nickel-cobalt-manganese ternary cathode material precursor from nickel electrolyte Download PDFInfo
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- CN104701524A CN104701524A CN201510093778.6A CN201510093778A CN104701524A CN 104701524 A CN104701524 A CN 104701524A CN 201510093778 A CN201510093778 A CN 201510093778A CN 104701524 A CN104701524 A CN 104701524A
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Abstract
The invention discloses a method for directly preparing a nickel-cobalt-manganese ternary cathode material precursor from nickel electrolyte. The method comprises the following steps: (1) adding MnS into nickel electrolysis cathode liquor after Fe is removed so as to deeply remove Cu, performing solid-separation so as to obtain an acid mixed liquid containing Ni, Co and Mn, and further adding a soluble cobalt salt and manganese salt into the mixed liquid so as to obtain a mixed solution with a certain mole ratio of Ni, Co and Mn; (2) adding a precipitant into the mixed solution, adjusting the pH value of the mixed solution to be within 8-12 by using an alkaline liquid, stirring to react for 0.5-5 hours inside a reactor of 20-90 DEG C, filtering off the precipitate obtained from the reaction, washing with deionized water, and drying, thereby obtaining the nickel-cobalt-manganese ternary cathode material precursor. The method is short in process, simple to operate, low in production cost and easy in industrial application.
Description
Technical field
The invention belongs to the preparing technical field of anode material for lithium-ion batteries, be specifically related to a kind of method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma.
Background technology
Nickel-cobalt-manganternary ternary anode material combines LiCoO
2, LiNiO
2and LiMnO
2the advantage of three kinds of materials, there is obviously cooperative effect: the introducing of Co can suppress cationic mixing, to stabilizing material structure, there is remarkable effect, the interpolation of Ni makes the discharge capacity of material be improved, Mn adds the production cost that not only effectively can reduce material, all have clear improvement to the stability of material and security performance, therefore, nickel-cobalt-manganternary ternary anode material is considered to be in lithium-ion-power cell the material system with outstanding prospect simultaneously.At present, nickel-cobalt-manganternary ternary anode material all adopts chemical pure reagent to prepare, the reagent commonly used is nickel, cobalt, the sulfate of manganese, nitrate or chloride, these slaines are mostly for prepared by raw material with metal or metal oxide, and metal or metal oxide are mostly extract from mineral, therefore, the acquisition of these products all needs the technological process through complexity, especially along with the develop rapidly of lithium ion battery industry, the demand of nickel, cobalt is increasing; And the resource such as nickel, cobalt is day by day deficient, smelting process complexity is loaded down with trivial details simultaneously, and resource utilization is low, and production cost is remained high.So need the preparation method seeking more economy, easy nickel-cobalt-manganternary ternary anode material.
Based on above-mentioned situation, the present invention proposes a kind of new thinking, by metallurgical intersecting with Material Field, directly utilizes nickel electrolyte to prepare the presoma of ternary cathode material of lithium ion battery first.MnS is specifically adopted to be the copper that the decoppering agent degree of depth removes in nickel electrolyte, simultaneously also for nickel-cobalt-manganternary ternary anode material introduces the manganese needed for it; Without the need to carrying out nickel electrolyte oxidation except cobalt in process, being realized the co-precipitation of nickel cobalt manganese by the composition and pH condition adjusting solution, obtaining the presoma of tertiary cathode material.So, not only can simplify the technological process of nickle electrolysis anode solution process in nickel fibers process, reduce the loss of nickel and the generation of metallurgical slag in solution; Simultaneously, nickeliferous, cobalt, manganese solution can prepare ternary material precursor by Direct precipitation, reduce the discharge of the waste water in smelting and material preparation process, waste residue, preparation for ternary material provides the new way of a low cost, short route and environmental protection, not only substantially increase resource utilization, realize mixing together that is metallurgical and Material Field, also there are significant economic benefit and ecological benefits.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma, the component manganese needed for tertiary cathode material is supplemented while nickel electrolyte deep copper removal, by smelting the mixing together with field of material preparation, develop short route, the low cost of a preparation ternary material precursor, the new way of also environmental protection.
Utilize nickel electrolyte directly to prepare a method for nickel-cobalt-manganternary ternary anode material presoma, comprise the steps:
(1) MnS is joined in the nickle electrolysis anode solution after except Fe and carry out the degree of depth except Cu, obtain the acid mixed solution containing Ni, Co, Mn after Separation of Solid and Liquid, then according to proportioning needed for nickel-cobalt-manganternary ternary anode material, the water-soluble salt of Co and the water-soluble salt of Mn are added in acid mixed solution;
(2) precipitation reagent and alkali lye are joined in the acidic mixed solution of step (1) gained, and the pH value by regulating alkali lye addition to control acid mixed solution, to react gained sedimentation and filtration, after washing, drying can obtain nickel-cobalt-manganternary ternary anode material presoma.
Except the content≤0.004g/L of Fe in the nickle electrolysis anode solution after Fe in said method.
In said method, the degree of depth is except the content≤0.003g/L of Cu in the solution after Cu.
The water-soluble salt of the Co described in said method is the mixing of one or more in cobaltous sulfate, cobalt chloride, cobalt nitrate, cobalt acetate.
The water-soluble salt of the Mn described in said method is the mixing of one or more in manganese sulfate, manganese chloride, manganese nitrate, manganese acetate.
Needed for above-mentioned nickel-cobalt-manganternary ternary anode material, proportioning is as follows: Ni:Co:Mn mol ratio is 1:1:1 or 5:2:3 or 6:2:2 or 8:1:1.
Precipitation reagent described in said method is the mixing of one or more in ammonium carbonate, carbonic hydroammonium, ammoniacal liquor.
The pH of mixed liquor regulates and controls in 8 ~ 12 scopes by said method alkali lye, stirring reaction 0.5 ~ 5h under the condition of 20 ~ 90 DEG C.
Alkali lye described in said method is the mixing of one or more in NaOH, KOH, sodium carbonate.
To react gained sedimentation and filtration in step (2) in said method, after spending deionized water, drying can obtain nickel-cobalt-manganternary ternary anode material presoma.
Advantage applies of the present invention following several in:
1, take nickel electrolyte as raw material, directly utilize Co, Ni wherein, cost comparatively adopts chemical pure reagent to reduce about 1/3;
2, adopt MnS to carry out deep copper removal to nickel electrolyte, synchronously achieve the removal of impurity copper and the adjustment of component, introduce the manganese needed for nickel-cobalt-manganternary ternary anode material;
3, simplify the flow process of nickle electrolysis anode solution process in nickel fibers process, be conducive to reducing production cost;
As: in nickel fibers process, due to the Co containing 0.1-0.3g/L in nickel electrolyte, in order to not affect the quality of electric nickel, in industrial nickel electrolyte, the content of Co must control at below 0.01g/L, the method that usual employing oxidation removes cobalt removes, the method that current industrial more employing chlorine oxidation removes cobalt purifies nickel electrolyte, and the cobalt slag that removes of gained reclaims for preparing cobalt product again.This process need uses hazardous gas---chlorine, there is potential safety hazard in production process, and the generation simultaneously removing cobalt slag also can cause the precipitation of part of nickel, causes the loss of nickel in electrolyte.The inventive method is then without the need to removing cobalt separately;
4, decrease the discharge of waste water and waste residue in smelting and material preparation process, there are significant ecological benefits.
Accompanying drawing explanation
Fig. 1 process chart of the present invention.
Embodiment
In order to explain the present invention in more detail, enumerating following examples and being described, but the present invention is not limited to these embodiments.
Embodiment 1
1gMnS solid is joined in the 50mL nickel electrolyte after yellow modumite method deironing (Fe content=3mg/L), make the concentration of the Cu in solution be reduced to 2.5mg/L, in filtrate, after Separation of Solid and Liquid, add the MnSO of 1mol/L
4the CoCl of solution and 1mol/L
2solution, adjusts to 1:1:1 by the mol ratio of the Ni:Co:Mn in solution; The NaOH solution of the sal volatile of 20mL 0.5mol/L and 1mol/L is joined in the mixed solution containing Ni, Co, Mn simultaneously, by the pH=11 regulating the addition of NaOH solution to control mixed solution, 30min is reacted in the stirred reactor of 50 DEG C, after solid-liquor separation, precipitate with deionized water is washed, dry at 80 DEG C and namely obtain nickel-cobalt-manganternary ternary anode material presoma.
Embodiment 2
2gMnS solid is joined in the 50mL nickel electrolyte after yellow modumite method deironing (Fe content=3.5mg/L), make the concentration of the Cu in solution be reduced to 2mg/L, in solution, add the Mn (NO of 1mol/L
3)
2the CoSO of solution and 1mol/L
4solution, adjusts to 5:2:3 by the mol ratio of the Ni:Co:Mn in solution; The KOH solution of the ammonium bicarbonate soln of 20mL 0.5mol/L and 1mol/L is joined in the mixed solution containing Ni, Co, Mn simultaneously, the addition of KOH solution is regulated to control the pH=12 of mixed solution, 5h is reacted in the stirred reactor of 25 DEG C, after solid-liquor separation, precipitate with deionized water is washed, dry at 100 DEG C and namely obtain nickel-cobalt-manganternary ternary anode material presoma.
Embodiment 3
5gMnS solid is joined in the 150mL nickel electrolyte after yellow modumite method deironing (Fe content=4mg/L), make the concentration of the Cu in solution be reduced to 3mg/L, in solution, add the MnSO of 1mol/L
4the CoSO of solution and 1mol/L
4solution, adjusts to 6:2:2 by the mol ratio of the Ni:Co:Mn in solution; The NaOH solution of the ammonium bicarbonate soln of 30mL 2mol/L and 2mol/L is joined in the mixed solution containing Ni, Co, Mn simultaneously, the addition of NaOH solution is regulated to control the pH=8 of mixed solution, 2h is reacted in the stirred reactor of 90 DEG C, after solid-liquor separation, precipitate with deionized water is washed, dry at 90 DEG C and namely obtain nickel-cobalt-manganternary ternary anode material presoma.
Embodiment 4
5gMnS solid is joined in the 250mL nickel electrolyte after yellow modumite method deironing (Fe content=2mg/L), make the concentration of the Cu in solution be reduced to 3mg/L, in solution, add the MnSO of 0.5mol/L
4the CoSO of solution and 0.5mol/L
4solution, adjusts to 8:1:1 by the mol ratio of the Ni:Co:Mn in solution; By the ammoniacal liquor of 50mL 20% and the Na of 2mol/L
2cO
3solution joins in the mixed solution containing Ni, Co, Mn simultaneously, regulates Na
2cO
3solution addition controls the pH=9 of mixed solution, in the stirred reactor of 70 DEG C, react 1h, precipitate with deionized water is washed, dry and namely obtain nickel-cobalt-manganternary ternary anode material presoma at 90 DEG C after solid-liquor separation.
Embodiment 5
5gMnS solid is joined in the 200mL nickel electrolyte after yellow modumite method deironing (Fe content=3mg/L), make the concentration of the Cu in solution be reduced to 3mg/L, in solution, add the MnSO of 2mol/L
4the CoSO of solution and 2mol/L
4solution, adjusts to 8:1:1 by the mol ratio of the Ni:Co:Mn in solution; The NaOH solution of the ammoniacal liquor of 50mL 20% and 4mol/L is joined in the mixed solution containing Ni, Co, Mn simultaneously, NaOH solution addition is regulated to control the pH=12 of mixed solution, 1.5h is reacted in the stirred reactor of 50 DEG C, after solid-liquor separation, precipitate with deionized water is washed, dry at 90 DEG C and namely obtain nickel-cobalt-manganternary ternary anode material presoma.
Claims (10)
1. utilize nickel electrolyte directly to prepare a method for nickel-cobalt-manganternary ternary anode material presoma, it is characterized in that, comprise the steps:
(1) MnS is joined in the nickle electrolysis anode solution after except Fe and carry out the degree of depth except Cu, obtain the acid mixed solution containing Ni, Co, Mn after Separation of Solid and Liquid, then according to proportioning needed for nickel-cobalt-manganternary ternary anode material, the water-soluble salt of Co and the water-soluble salt of Mn are added in acid mixed solution;
(2) precipitation reagent and alkali lye are joined in the acidic mixed solution of step (1) gained, and the pH value by regulating alkali lye addition to control acid mixed solution, to react gained sedimentation and filtration, after washing, drying can obtain nickel-cobalt-manganternary ternary anode material presoma.
2. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, is characterized in that, except the content≤0.004g/L of Fe in the nickle electrolysis anode solution after Fe.
3. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, is characterized in that, the degree of depth is except the content≤0.003g/L of Cu in the solution after Cu.
4. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, is characterized in that, the water-soluble salt of described Co is the mixing of one or more in cobaltous sulfate, cobalt chloride, cobalt nitrate, cobalt acetate.
5. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, is characterized in that, the water-soluble salt of described Mn is the mixing of one or more in manganese sulfate, manganese chloride, manganese nitrate, manganese acetate.
6. the nickel electrolyte that utilizes according to claim 1 or 4 or 5 directly prepares the method for nickel-cobalt-manganternary ternary anode material presoma, it is characterized in that, needed for nickel-cobalt-manganternary ternary anode material, proportioning is as follows: Ni:Co:Mn mol ratio is 1:1:1 or 5:2:3 or 6:2:2 or 8:1:1.
7. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, is characterized in that, described precipitation reagent is the mixing of one or more in ammonium carbonate, carbonic hydroammonium, ammoniacal liquor.
8. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, is characterized in that, is regulated and controled in 8 ~ 12 scopes by the pH of mixed liquor, stirring reaction 0.5 ~ 5h under the condition of 20 ~ 90 DEG C with alkali lye.
9. the nickel electrolyte that utilizes according to claim 1 or 8 directly prepares the method for nickel-cobalt-manganternary ternary anode material presoma, it is characterized in that, described alkali lye is the mixing of one or more in NaOH, KOH, ammoniacal liquor.
10. the method utilizing nickel electrolyte directly to prepare nickel-cobalt-manganternary ternary anode material presoma according to claim 1, it is characterized in that, to react gained sedimentation and filtration in step (2), after spending deionized water, drying can obtain nickel-cobalt-manganternary ternary anode material presoma.
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Application publication date: 20150610 |