CN110010890A - A kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate - Google Patents
A kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate Download PDFInfo
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- CN110010890A CN110010890A CN201811616650.3A CN201811616650A CN110010890A CN 110010890 A CN110010890 A CN 110010890A CN 201811616650 A CN201811616650 A CN 201811616650A CN 110010890 A CN110010890 A CN 110010890A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- H—ELECTRICITY
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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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- H—ELECTRICITY
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The purpose of the present invention is to provide the normal-temperature reaction preparation methods of ball shaped nano ferric phosphate, belong to battery material field.It is characterized by: certain density trivalent iron salt aqueous solution, phosphate aqueous solution and a certain amount of citric acid, surfactant is added in the reactor with stirring, and solution ph is adjusted to 1.0 with nitric acid, then it is passed through ammonia under stiring, control is passed through the flow of ammonia, gradually rise solution ph, until stopping is passed through ammonia when solution ph is increased to 3.5, milky slurry is obtained.It is filtered after slurry is stood 30 minutes, is washed with deionized filter cake 3 times, filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then crushed through airslide disintegrating mill, the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Description
Technical field
The present invention relates to a kind of normal-temperature reaction preparation methods of ball shaped nano ferric phosphate, belong to battery material field.
Background technique
Lithium ion battery has both good high rate performance and cycle life is widely used due to its excellent energy density
Into the electronic equipment of daily life.As the LiFePO4 of anode material for lithium-ion batteries, raw material environmentally friendly with its
Abundance, specific capacity be high, cycle performance and the distinguishing features such as has a safety feature, and prospect is wide in terms of lithium ion battery applications
It is wealthy.But electronic conductivity lower than lithium ion diffusion velocity and tap density it is small cause lithium ion battery electric conductivity it is undesirable be system
About two big key problems of its development.For the electric conductivity for improving LiFePO4, following three kinds of approach are generallyd use: (1) in particle
Surface carries out coating modification, such as passes through carbon coated (graphene oxide, three-dimensional grapheme)；(2) doped metal ion such as adulterates
The metal ions such as cobalt, nickel, manganese；(3) the small lithium iron phosphate particles of synthesis partial size.Packet carbon will lead to the reduction of its tap density, in addition
The technique of carbon coated especially packet graphene is relatively complicated, and cost is also higher.The electricity of the metal ions such as cation doping, nickel, manganese
Pond can bring environmental issue, and battery security is also declined.For many years studies have shown that being using spherical, nanoscale ferric phosphate
Precursor preparation LiFePO4 is the effective means for improving its tap density and electric conductivity.Nano ferric phosphate is mainly at present
Using hydro-thermal method, injection the methods of high temperature drying techniques and homogeneous precipitation method preparation, hydro-thermal method and injection high temperature drying techniques need height
It is difficult big to carry out scale industrial production for warm high pressure or hot conditions.It needs to be added when preparing using homogeneous precipitation method homogeneous
Precipitating reagent such as urea is simultaneously heated to about 85 DEG C~100 DEG C and is reacted, and the raising and the extension in reaction time of reaction temperature can make
Product grain increases.
Summary of the invention is to overcome the shortcomings of existing nano ferric phosphate precursor preparation method, and the invention proposes a kind of normal
The lower method for preparing nano ferric phosphate by liquid-phase precipitation reaction of temperature, resulting ferric phosphate product particle pattern is spherical shape, partial size
100~150 nanometers.The technical solution used in the present invention is: certain density ferric iron is added in the reactor with stirring
Saline solution, phosphate aqueous solution and a certain amount of citric acid, surfactant, and solution ph is adjusted to 1.0, then with nitric acid
It is passed through ammonia under stiring, control is passed through the flow of ammonia, gradually rises solution ph, until solution ph is increased to 3.5
When, stopping is passed through ammonia, obtains milky slurry.It filters, is washed with deionized filter cake 3 times after slurry is stood 30 minutes,
Then filter cake is placed in 105 DEG C of drying boxes to dry 3 hours, after cooling, then is crushed through airslide disintegrating mill, partial size, which can be obtained, is
100~150 nanometers of white ball shape ferric phosphate.
Trivalent iron salt as described above is ferric nitrate or iron chloride or ferric sulfate or the mixture between them.
The molality of trivalent iron salt as described above are as follows: 0.1~1.0molkg-1。
Phosphoric acid and ferric ion (Fe as described above3+) the ratio between the amount of substance be 1~1.3: 1.
The mass percent concentration of citric acid as described above are as follows: 1~10% (in terms of the quality of phosphate aqueous solution).
Surfactant as described above are as follows: dodecyl trimethyl ammonium chloride or tetradecyl trimethyl ammonium chloride or
Person's hexadecyltrimethylammonium chloride or dodecyl trimethyl ammonium bromide or tetradecyltrimethylammonium bromide or ten
Six alkyl trimethyl ammonium chlorides or their mixture.
The mass percent concentration of surfactant as described above are as follows: 0.1~5% (with the quality of phosphate aqueous solution
Meter).
Ball shaped nano ferric phosphate reaction condition prepared by the present invention is mild, and preparation method is simple, with prepared phosphoric acid
Iron is predecessor, and the LiFePO4 being prepared using carbothermic method/C positive electrode material is under the conditions of 0.5C, discharge capacity
Reach 155~163mAh/g.
Detailed description of the invention
Attached drawing 1 is the scanning electron microscope (SEM) photograph of prepared ball shaped nano ferric phosphate.
Specific embodiment
It will be further elucidated by the following examples the present invention, but the present invention is not only limited to following embodiment.
Embodiment 1
100kg 0.1mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 100kg 0.1mol/kg phosphorus
Aqueous acid, 1kg citric acid, 0.1kg dodecyl trimethyl ammonium chloride, and solution ph is adjusted to 1.0 with nitric acid.Then exist
Ammonia is passed through under stirring, control is passed through the flow of ammonia, gradually rises solution ph, until when solution ph is increased to 3.5,
Stopping is passed through ammonia, obtains milky slurry.Will slurry stand 30 minutes after filter, be washed with deionized filter cake 3 times, then
Filter cake is placed in 105 DEG C of drying boxes to dry 3 hours, after cooling, then is crushed through airslide disintegrating mill, can be obtained partial size be 100~
150 nanometers of white ball shape ferric phosphate.
Embodiment 2
100kg 0.2mol/kg FeCl is added in the reactor with stirring3Aqueous solution, 100kg 0.2mol/kg phosphoric acid
Aqueous solution, 1kg citric acid, 1kg tetradecyl trimethyl ammonium chloride, and solution ph is adjusted to 1.0 with nitric acid.Then it is stirring
Under be passed through ammonia, control is passed through the flow of ammonia, gradually rises solution ph, until stopping when solution ph is increased to 3.5
It is passed through ammonia, obtains milky slurry.It filters, is washed with deionized filter cake 3 times after slurry is stood 30 minutes, it then will filter
Cake is placed in 105 DEG C of drying boxes and dries 3 hours, after cooling, then crushes through airslide disintegrating mill, and it is 100~150 to receive that partial size, which can be obtained,
The white ball shape ferric phosphate of rice.
Embodiment 3
50kg 0.5mol/kg Fe is added in the reactor with stirring2(SO4)3Aqueous solution, 100kg 0.5mol/kg phosphorus
Aqueous acid, 5kg citric acid, 2.5kg hexadecyltrimethylammonium chloride, and solution ph is adjusted to 1.0 with nitric acid.Then exist
Ammonia is passed through under stirring, control is passed through the flow of ammonia, gradually rises solution ph, until when solution ph is increased to 3.5,
Stopping is passed through ammonia, obtains milky slurry.Will slurry stand 30 minutes after filter, be washed with deionized filter cake 3 times, then
Filter cake is placed in 105 DEG C of drying boxes to dry 3 hours, after cooling, then is crushed through airslide disintegrating mill, can be obtained partial size be 100~
150 nanometers of white ball shape ferric phosphate.
Embodiment 4
100kg 1mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 100kg 1mol/kg phosphoric acid water
Solution, 10kg citric acid, 5kg dodecyl trimethyl ammonium chloride, and solution ph is adjusted to 1.0 with nitric acid.Then it is stirring
Under be passed through ammonia, control is passed through the flow of ammonia, gradually rises solution ph, until stopping when solution ph is increased to 3.5
It is passed through ammonia, obtains milky slurry.It filters, is washed with deionized filter cake 3 times after slurry is stood 30 minutes, it then will filter
Cake is placed in 105 DEG C of drying boxes and dries 3 hours, after cooling, then crushes through airslide disintegrating mill, and it is 100~150 to receive that partial size, which can be obtained,
The white ball shape ferric phosphate of rice.
Embodiment 5
100kg 0.2mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 100kg 0.22mol/kg
Phosphate aqueous solution, 2kg citric acid, 0.5kg tetradecyl trimethyl ammonium chloride, and solution ph is adjusted to 1.0 with nitric acid.Then
It is passed through ammonia under stiring, control is passed through the flow of ammonia, gradually rises solution ph, until solution ph is increased to 3.5
When, stopping is passed through ammonia, obtains milky slurry.It filters, is washed with deionized filter cake 3 times after slurry is stood 30 minutes,
Then filter cake is placed in 105 DEG C of drying boxes to dry 3 hours, after cooling, then is crushed through airslide disintegrating mill, partial size, which can be obtained, is
100~150 nanometers of white ball shape ferric phosphate.
Embodiment 6
100kg 0.2mol/kg FeCl is added in the reactor with stirring3Aqueous solution, 100kg 0.26mol/kg phosphorus
Aqueous acid, 2kg citric acid, 1kg hexadecyltrimethylammonium chloride, and solution ph is adjusted to 1.0 with nitric acid.Then it is stirring
It mixes down and is passed through ammonia, control is passed through the flow of ammonia, gradually rises solution ph, until stopping when solution ph is increased to 3.5
It is only passed through ammonia, obtains milky slurry.It is filtered after slurry is stood 30 minutes, is washed with deionized filter cake 3 times, then will
Filter cake is placed in 105 DEG C of drying boxes and dries 3 hours, after cooling, then crushes through airslide disintegrating mill, it is 100~150 that partial size, which can be obtained,
The white ball shape ferric phosphate of nanometer.
Embodiment 7
50kg 0.1mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 50kg 0.1mol/kg
FeCl3Aqueous solution, 100kg 0.12mol/kg phosphate aqueous solution, 1kg citric acid, 0.2kg dodecyl trimethyl ammonium bromide, and
Solution ph is adjusted to 1.0 with nitric acid.Then be passed through ammonia under stiring, control is passed through the flow of ammonia, make solution ph by
Edge up height, until stopping is passed through ammonia when solution ph is increased to 3.5, obtains milky slurry.After slurry is stood 30 minutes
Filtering is washed with deionized filter cake 3 times, filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then through air-flow
Pulverizer crushes, and the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Embodiment 8
50kg 0.4mol/kg FeCl is added in the reactor with stirring3Aqueous solution, 100kg 0.2mol/kg Fe2
(SO4)3Aqueous solution, 140kg 0.5mol/kg phosphate aqueous solution, 2kg citric acid, 1kg tetradecyltrimethylammonium bromide, are used in combination
Nitric acid adjusts solution ph to 1.0.Then it is passed through ammonia under stiring, control is passed through the flow of ammonia, makes solution ph gradually
It increases, until stopping is passed through ammonia when solution ph is increased to 3.5, obtains milky slurry.Mistake after slurry is stood 30 minutes
Filter is washed with deionized filter cake 3 times, filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then through air-flow powder
Broken machine crushes, and the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Embodiment 9
60kg 0.5mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 50kg 0.2mol/kg Fe2
(SO4)3Aqueous solution, 110kg 0.5mol/kg phosphate aqueous solution, 5kg citric acid, 2.5kg cetyl trimethylammonium bromide, and
Solution ph is adjusted to 1.0 with nitric acid.Then be passed through ammonia under stiring, control is passed through the flow of ammonia, make solution ph by
Edge up height, until stopping is passed through ammonia when solution ph is increased to 3.5, obtains milky slurry.After slurry is stood 30 minutes
Filtering is washed with deionized filter cake 3 times, filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then through air-flow
Pulverizer crushes, and the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Embodiment 10
100kg 1mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 110kg 1mol/kg phosphoric acid water
Solution, 10kg citric acid, 2.5kg dodecyl trimethyl ammonium chloride and 2.5kg hexadecyltrimethylammonium chloride, and use nitric acid
Solution ph is adjusted to 1.0.Then it is passed through ammonia under stiring, control is passed through the flow of ammonia, gradually rises solution ph,
Until stopping is passed through ammonia when solution ph is increased to 3.5, milky slurry is obtained.It filters, uses after slurry is stood 30 minutes
Deionized water is washed filter cake 3 times, and filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then through airslide disintegrating mill
It crushes, the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Embodiment 11
100kg 0.2mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 120kg 0.2mol/kg phosphorus
Aqueous acid, 2kg citric acid, 0.5kg tetradecyl trimethyl ammonium chloride and 0.5kg cetyl trimethylammonium bromide, are used in combination
Nitric acid adjusts solution ph to 1.0.Then it is passed through ammonia under stiring, control is passed through the flow of ammonia, makes solution ph gradually
It increases, until stopping is passed through ammonia when solution ph is increased to 3.5, obtains milky slurry.Mistake after slurry is stood 30 minutes
Filter is washed with deionized filter cake 3 times, filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then through air-flow powder
Broken machine crushes, and the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Embodiment 12
100kg 0.3mol/kg Fe (NO is added in the reactor with stirring3)3Aqueous solution, 120kg 0.3mol/kg phosphorus
Aqueous acid, 3kg citric acid, 1kg dodecyl trimethyl ammonium chloride and 0.5kg tetradecyltrimethylammonium bromide, and use nitre
Acid-conditioning solution pH value is to 1.0.Then it is passed through ammonia under stiring, control is passed through the flow of ammonia, rises solution ph gradually
Height obtains milky slurry until stopping is passed through ammonia when solution ph is increased to 3.5.Mistake after slurry is stood 30 minutes
Filter is washed with deionized filter cake 3 times, filter cake is then placed in 105 DEG C of drying boxes and is dried 3 hours, after cooling, then through air-flow powder
Broken machine crushes, and the white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
Claims (7)
1. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate, it is characterised in that: be added in the reactor with stirring
Certain density trivalent iron salt aqueous solution, phosphate aqueous solution and a certain amount of citric acid, surfactant, and it is molten with nitric acid adjusting
Liquid pH value is to 1.0；Then it is passed through ammonia under stiring, control is passed through the flow of ammonia, gradually rises solution ph, until molten
When liquid pH value is increased to 3.5, stopping is passed through ammonia, obtain milky slurry；Will slurry stand 30 minutes after filter, spend from
Then filter cake is placed in 105 DEG C of drying boxes and dried 3 hours by sub- water washing filter cake 3 times, after cooling, then crush through airslide disintegrating mill,
The white ball shape ferric phosphate that partial size is 100~150 nanometers can be obtained.
2. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate according to claim 1, it is characterised in that: trivalent
Molysite is ferric nitrate or iron chloride or ferric sulfate or the mixture between them.
3. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate according to claim 1, it is characterised in that: described
Trivalent iron salt molality are as follows: 0.1~1.0mol/kg.
4. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate according to claim 1, it is characterised in that: phosphoric acid
With ferric ion (Fe3+) the ratio between the amount of substance be 1~1.3: 1.
5. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate according to claim 1, it is characterised in that: lemon
The mass percent concentration of acid are as follows: 1~10% (in terms of the quality of phosphate aqueous solution).
6. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate according to claim 1, it is characterised in that: surface
Activating agent are as follows: dodecyl trimethyl ammonium chloride or tetradecyl trimethyl ammonium chloride or hexadecyltrimethylammonium chloride
Either dodecyl trimethyl ammonium bromide or tetradecyltrimethylammonium bromide or hexadecyltrimethylammonium chloride or
Their mixture.
7. a kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate according to claim 1, it is characterised in that: surface
The mass percent concentration of activating agent are as follows: 0.1~5% (in terms of the quality of phosphate aqueous solution).
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Cited By (1)
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| CN113104829A (en) * | 2021-03-19 | 2021-07-13 | 合肥国轩电池材料有限公司 | Lithium iron phosphate material and preparation method and application thereof |
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