CN107768646A - A kind of cobaltosic oxide preparation method of doped chemical gradient distribution - Google Patents
A kind of cobaltosic oxide preparation method of doped chemical gradient distribution Download PDFInfo
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- CN107768646A CN107768646A CN201710995198.5A CN201710995198A CN107768646A CN 107768646 A CN107768646 A CN 107768646A CN 201710995198 A CN201710995198 A CN 201710995198A CN 107768646 A CN107768646 A CN 107768646A
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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Abstract
The invention discloses a kind of cobaltosic oxide preparation method of doped chemical gradient distribution, using cobalt salt solution as raw material, pass through sodium hydroxide solution, add a certain proportion of ammoniacal liquor, and the amount of doped chemical soluble salt solution and the hydrogen peroxide solution prepared are calculated according to quantity, synthetic reaction is carried out, then filtered, washed and is dried, obtains final products；The present invention adds the amount gradient increase of dopant in reactor, makes doped chemical distribution gradient in cobaltosic oxide product, prepared the cobaltosic oxide product of doped chemical gradient distribution first by extending with synthesising reacting time.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of modification four for anode material for lithium-ion batteries
The preparation method of Co 3 O.
Background technology
From Sony corporation of Japan in 1992 successfully by after lithium ion battery commercialization, lithium ion battery relies on its operating voltage
It is high, energy density is high, have extended cycle life, self discharge is low, it is pollution-free, unique advantage such as have a safety feature, be widely used as moving
The power supply of mobile phone, portable computer, video camera, camera etc. and in space flight, navigation, artificial satellite, small medical
And progressively develop into the energy battery of mainstream applications in military communication apparatus.
Cobalt acid lithium is the main positive electrode of current commercial Li-ion battery.But cobalt acid lithium actual specific capacity only has
140mAh./g or so, it is only its theoretical capacity（274mAh./g）50% or so；And the anti-over-charging poor-performing of cobalt acid lithium,
Reduced rapidly compared with specific capacity under high charge voltage.The problem of to overcome cobalt acid lithium to exist, people's research take a variety of modifications and arranged
Apply and method.Research has shown that, in terms of positive electrode performance, particularly cycle performance is improved, doping be most efficient method it
One, doping can not only improve the stability of lattice, and the cycle performance of material can be greatly improved.
Existing doping cobalt acid lithium production technology mainly mixes doped chemical oxide, cobaltosic oxide, lithium carbonate,
Grinding, high-temperature calcination.This method not only high energy consumption, and Elemental redistribution is uneven in the cobalt acid lithium product prepared, uniformity
Difference, it is impossible to meet requirement of the battery industry to doping cobalt acid lithium.
Chinese invention patent CN201210486483.1, disclose a kind of " preparation side of doping spherical cobaltosic oxide
Method ", specifically doped chemical ion is incorporated into cobalt salt solution be configured to adulterate mixed solution, with hydroxide solution and
Air is passed into reaction unit simultaneously, and is constantly stirred and is made its reaction, prepares doping spherical cobaltosic oxide.China
Patent of invention CN200810110753.2, " a kind of preparation method of doped cobaltic-cobaltous oxide " is disclosed, specifically will doping member
Plain ion, which is incorporated into cobalt salt solution, to be configured to adulterate mixed solution, is passed into simultaneously with the hydroxide solution containing ammoniacal liquor anti-
Answering makes its reaction in device, then prepares doping spherical cobaltosic oxide by washing, dry, calcining.Made in upper two kinds of patents
Gradient distribution can not be presented in Doped ions in standby cobaltosic oxide.Chinese invention patent CN201410091324.0 is disclosed
" a kind of preparation method of rare earth doped compound lithium cobaltate cathode material ", the present invention relates to a kind of rare earth doped
The preparation method of compound lithium cobaltate cathode material, this method include the compound lithium cobaltate forerunner that coprecipitation prepares the doping containing neodymium
Body, then neodymium doped and compounded cobalt acid lithium presoma is mixed with lithium oxalate, double sintering, cooling processing, crush, screening, produced
Product.The invention reaction process is cumbersome.
The content of the invention
To overcome above-mentioned deficiency, it is an object of the invention to provide a kind of cobaltosic oxide preparation of doped chemical gradient distribution
Method.
In order to meet above-mentioned purpose, the technical solution used in the present invention is：
A kind of cobaltosic oxide preparation method of doped chemical gradient distribution, it is concretely comprised the following steps：
A, solution A is prepared
Using cobalt salt solution as raw material, the solution A that concentration is 50~150g/L is configured to, precise volume is that x A is standby；
B, B solution is prepared
Compound concentration is 50~400g/L sodium hydroxide solution, and it is B solution to add a certain proportion of ammoniacal liquor, and ammoniacal liquor and hydrogen-oxygen
The volume ratio of compound is 1：5~1：20.
C, C solution is prepared
Compound concentration is 5~20g/L doped chemical soluble salt solution C, is produced according to the concentration of cobalt, x amount, preparation in solution A
Doped chemical concentration in the doped chemical doping and C solution of product requirement, according to formula：C solution volume=（X*A solution cobalts are molten
Spend * dopings）/（Cobalt content in C solution doped chemical concentration * cobaltosic oxides）, be calculated needed for C solution volume, this
Volume is set to y；
D, compound concentration is 1~5mol/L hydrogen peroxide solution D；
E, synthetic reaction
When synthetic reaction starts, according to the generated time t of preparation technology determination, C solution is added in solution A with y/t flow
Mixing, while with（x+y）/ t flow velocity adds A, C mixed solution and B solution, solution D cocurrent in reactor, it is strong in stirring
Spend to be reacted under 200~500 revs/min, the temperature of reaction system is 50~90 DEG C, the flow control reaction of regulation B solution
PH value, the pH value of reaction system is 7~10, and the flow of solution D is A, C mixed solution flow（x+y）The 1/10~1/2 of/t, close
It is 8~40h into the time；
F, filtering, washing and drying
Material is filtered after the completion of reaction, pulping and washing, dry, obtain final products.
Preferably, in the step (a), the cobalt salt is that the one or more in cobaltous sulfate, cobalt nitrate and cobalt chloride are mixed
Compound.
Preferably, in the step (c), the doped chemical soluble salt is Mg, Al, Mn, Cu, Cr, Zr, Ce, Y, Nb, Ni
In one in or several chlorides or nitric acid thing.
Preferably, in the step (f), washing material is washed to pH value and is using 80~100 DEG C of deionized water
7~7.5.
Preferably, in the step (f), the temperature of dried material is 100~400 DEG C.
Preferably, in the step (f), the physical and chemical indexes of the final products include：Doped chemical content 0~2%,
The distribution of doped chemical gradient, laser grain are in 1~10 micron, Zhen Shi Mi Du≤2.0g/cm3, 0.5~3.0m of specific surface area2/ g, shape
Looks are spherical or spherical.
Beneficial effects of the present invention are：
（1）The present invention adds the amount gradient increase of dopant in reactor, makes doping first by extending with synthesising reacting time
Element distribution gradient in cobaltosic oxide product, has prepared the cobaltosic oxide product of doped chemical gradient distribution first.
（2）Synthetic product is direct oxidation into four oxygen by the present invention by way of adding oxidant hydrogen peroxide into reactor
Change three cobalts, without calcining, liquid phase one-step has synthesized the doped cobaltic-cobaltous oxide product of doped chemical gradient distribution, avoids
The step of needing to be passed through compressed air or other oxidizing gas in calcination process, production process is set not produce dust, no dirt
It is dye, environment-friendly, and it also avoid that calcination process is passed through unclean compressed air or other oxidizing gas cause four oxygen
Change the risk of three cobalt product impurity content exceeding indexs.
（3）The product prepared using the present invention simply can readily prepare the cobalt acid lithium of doped chemical gradient distribution
Product.
Brief description of the drawings
Fig. 1 is the testing result of the synthetic product of embodiment 1；
Fig. 2 is the 2-in-1 testing result into product of embodiment；
Fig. 3 is the testing result of the synthetic product of embodiment 3.
Embodiment
Embodiment one
Production stage is same as above, and the design parameter in each step is as follows：
The solution A of preparation is cobalt chloride solution, concentration 60g/L, volume 120L.
180g/L ammonia spirit, and sodium hydroxide and ammoniacal liquor are added in the sodium hydroxide that the B solution of preparation is 100g/L
Volume ratio be 1：20.
The magnesium chloride solution 10L that C solution is 5g/L is prepared, the total amount of magnesium is about the 0.5% of end product quality.
Prepare the hydrogen peroxide solution that solution D is 1mol/L.
When synthetic reaction starts, reaction time 16h is determined according to preparation technology, C solution is added with 0.625L/h flow
Enter in solution A, while added A, C mixed solution, B solution, solution D cocurrent in reactor with 8.125L/h flow velocity, strong
Both are reacted under strong stirring, the temperature of reaction system is 70 DEG C, and the flow velocity of B solution is adjusted according to pH value in reaction to be determined,
The pH value of reaction system is 10.0, and the flow of solution D is 1L/h.
Pulping and washing material requires washing to pH7.3 using 90 DEG C of deionized water;The temperature of dried material is
150℃。
The product indices of preparation are shown in accompanying drawing 1.
Embodiment two
This example and embodiment one are essentially identical, and simply following adjustment parameter is different：
The solution A of preparation is cobalt nitrate solution, concentration 100g/L, volume 250L.
180g/L ammonia spirit, and sodium hydroxide and ammoniacal liquor are added in the sodium hydroxide that the B solution of preparation is 200g/L
Volume ratio be 3：25.
The aluminium and nickel solution 35L that C solution is 10g/L are prepared, and the total amount of Al and nickel is the 1% of end product quality.
Prepare the hydrogen peroxide solution that solution D concentration is 2mol/L.
When synthetic reaction starts, reaction time 30h is determined according to preparation technology, C solution is added with 1.17L/h flow
In solution A, while A, C mixed solution, B solution, solution D cocurrent are added in reactor with 9.5L/h flow velocity, stirred strongly
Mixing down is reacted both, and the temperature of reaction system is 80 DEG C, and the flow velocity of B solution is adjusted according to pH value in reaction to be determined, reaction
The pH value of system is 9.0, and the flow of solution D is 2L/h.
Pulping and washing material requires washing to pH7 using 80 DEG C of deionized water;The temperature of dried material is
250℃。
The product indices of preparation are shown in accompanying drawing 2.
Embodiment three
This example and embodiment one are essentially identical, and simply following adjustment parameter is different：
The solution A of preparation is cobalt sulfate solution, concentration 120g/L, volume 500L.
180g/L ammonia spirit, and sodium hydroxide and ammoniacal liquor are added in the sodium hydroxide that the B solution of preparation is 300g/L
Volume ratio be 1：5.
The total amount of the copper nitrate and yttrium chloride solution 84L that preparation C solution is 20g/L, copper and yttrium is about end product quality
2%.
Prepare the hydrogen peroxide solution that solution D concentration is 4mol/L.
When synthetic reaction starts, according to preparation technology, reaction time 60h is determined, C solution is added with 1.4L/h flow
In solution A, while A, C mixed solution, B solution, solution D cocurrent are added in reactor with 9.74L/h flow velocity, stirred strongly
Mixing down is reacted both, and the temperature of reaction system is 75 DEG C, and the flow velocity of B solution is adjusted according to pH value in reaction to be determined, reaction
The pH value of system is 8.0, and the flow of solution D is 3L/h.
Pulping and washing material requires washing to pH7.5 using 95 DEG C of deionized water;The temperature of dried material is
400℃。
The product index of preparation is shown in accompanying drawing 3.
Claims (6)
1. a kind of cobaltosic oxide preparation method of doped chemical gradient distribution, it is characterised in that concretely comprise the following steps：
A, solution A is prepared
Using cobalt salt solution as raw material, the solution A that concentration is 50~150g/L is configured to, precise volume is that x A is standby；
B, B solution is prepared
Compound concentration is 50~400g/L sodium hydroxide solution, and it is B solution to add a certain proportion of ammoniacal liquor, and ammoniacal liquor and hydrogen-oxygen
The volume ratio of compound is 1：5~1：20；
C, C solution is prepared
Compound concentration is 5~20g/L doped chemical soluble salt solution C, is produced according to the concentration of cobalt, x amount, preparation in solution A
Doped chemical concentration in the doped chemical doping and C solution of product requirement, according to formula：C solution volume=（X*A solution cobalts are molten
Spend * dopings）/（Cobalt content in C solution doped chemical concentration * cobaltosic oxides）, be calculated needed for C solution volume, this
Volume is set to y；
D, compound concentration is 1~5mol/L hydrogen peroxide solution D；
E, synthetic reaction
When synthetic reaction starts, according to the generated time t of preparation technology determination, C solution is added in solution A with y/t flow
Mixing, while with（x+y）/ t flow velocity adds A, C mixed solution and B solution, solution D cocurrent in reactor, it is strong in stirring
Spend to be reacted under 200~500 revs/min, the temperature of reaction system is 50~90 DEG C, the flow control reaction of regulation B solution
PH value, the pH value of reaction system is 7~10, and the flow of solution D is A, C mixed solution flow（x+y）The 1/10~1/2 of/t, close
It is 8~40h into the time；
F, filtering, washing and drying
Material is filtered after the completion of reaction, pulping and washing, dry, obtain final products.
A kind of 2. preparation method of grade doping cobalt acid lithium according to claim 1, it is characterised in that：The step (a)
In, the cobalt salt is one or more of mixtures in cobaltous sulfate, cobalt nitrate and cobalt chloride.
A kind of 3. preparation method of grade doping cobalt acid lithium according to claim 1 or 2, it is characterised in that：The step
(c) in, the doped chemical soluble salt be Mg, Al, Mn, Cu, Cr, Zr, Ce, Y, Nb, Ni in one in or several chlorides or
Nitric acid thing.
A kind of 4. preparation method of grade doping cobalt acid lithium according to claim 3, it is characterised in that：The step (f)
In, for washing material using 80~100 DEG C of deionized water, it is 7~7.5 to wash to pH value.
A kind of 5. preparation method of grade doping cobalt acid lithium according to claim 1 or 4, it is characterised in that：The step
(f) in, the temperature of dried material is 100~400 DEG C.
A kind of 6. preparation method of grade doping cobalt acid lithium according to claim 5, it is characterised in that：The step (f)
In, the physical and chemical indexes of the final products include：Doped chemical content is in the distribution of 0~2%, doped chemical gradient, laser grain 1
~10 microns, Zhen Shi Mi Du≤2.0g/cm3, 0.5~3.0m of specific surface area2/ g, pattern are spherical or spherical.
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