CN107634200A - A kind of inorganic dispersant is used for the method for preparing lithium iron phosphate cell material - Google Patents
A kind of inorganic dispersant is used for the method for preparing lithium iron phosphate cell material Download PDFInfo
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- CN107634200A CN107634200A CN201710807896.8A CN201710807896A CN107634200A CN 107634200 A CN107634200 A CN 107634200A CN 201710807896 A CN201710807896 A CN 201710807896A CN 107634200 A CN107634200 A CN 107634200A
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- lithium
- iron phosphate
- cell material
- lithium iron
- inorganic dispersant
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a kind of method that inorganic dispersant is used to prepare lithium iron phosphate cell material, belongs to field of energy source materials.The present invention mixes in proportion ferric phosphate, lithium carbonate, carbon source, talcum powder, lithium position doped metal ion and iron position doped metal ion, it is placed in ball mill, add the 300min of novel dispersant ball milling 150, ball milling product is put into tube furnace, in nitrogen atmosphere, after 150 250 DEG C preheat 100 250min, heated up with the 5 40 DEG C/min rates of heat addition, in 500 800 DEG C of 200min of constant temperature calcining 30, then room temperature is cooled to 5 20 DEG C/min rate of temperature fall, lithium iron phosphate cell material is made.The present invention solves the problems such as difficult solvent recovery in lithium iron phosphate positive material sintering process, atmosphere is difficult to control.
Description
Technical field
The present invention relates to a kind of method that inorganic dispersant is used to prepare lithium iron phosphate cell material.Belong to energy and material neck
Domain.
Background technology
1997, as Padhi and Goodenough et al. have found olivine phase lithium iron phosphate（LiFePO4）Have excellent
Chemical property, its theoretical specific capacity are of a relatively high（170mAh/g）, 3.4V can be produced（VS. Li/Li+）Voltage, filling entirely
There is good heat endurance, less hygroscopicity and excellent charge-discharge performance under electricity condition；Meanwhile with it is nontoxic,
The features such as raw material sources are extensive, cost is low, heat endurance is good, it is a kind of lithium for integrating many merits since the dawn of human civilization to be described as
Ion battery positive electrode, a great sensation is caused in battery circle.Due to many merits of LiFePO4 so that its
Various movable power source fields, the large-sized power field of power supplies particularly needed for electric car have great market prospects.
But organic solvent batch mixing is used in LiFePO4 batch mixing and sintering process, as patent CN101150191A is used
Organic dispersing agent and inorganic dispersant mixing batch mixing, CN101162776A is then using ethanol as dispersion solvent；Cause as follows
Problem：（1）Using organic solvent batch mixing mixed phosphate iron lithium presoma, it is necessary to increase solvent recovery unit, cost increase；（2）
The organic solvent of recovery not yet in effect vaporizes under the conditions of sintering high temperature, produces the compounds such as carbon, nitrogen, is done after being mixed with inert gas
The Accurate Determining of atmosphere content in atmosphere furnace is disturbed, has a strong impact on the stability of sintering atmosphere, it is final to influence the life of LiFePO4 crystal
Long and electrochemistry uniformity；（3）Organic solvent can produce certain corrosion in preheating and sintering process to sintering furnace, on the one hand
Cause equipment depreciation rate high, on the other hand can bring production safety sex chromosome mosaicism.Therefore, to develop one kind and do not have to recovery, cost is low,
For uncorruptible batch mixing solvent to improving LiFePO4 product quality, promoting the development of China's ferric phosphate lithium cell industry has weight
The meaning wanted.
For the problem of organic solvent, mainly there is following three kinds of methods to change in LiFePO4 batch mixing and sintering process at present
It is apt to its performance：
（1）Using inoganic solids powdered rubber or inorganic solvent mixing presoma；CN101152960A use containing iron ion and/
Or the aqueous solution of ferrous ion and the aqueous solution containing phosphate anion mix, CN101152961A is using deionized water as mixed
Close dispersion solvent；（2）It is that the rate of recovery reaches more than 99% by improving solvent recovery unit, if CN102173402A is in drying machine
Upper end one is surveyed according to solvent condensate recycling device；（3）Preheating temperature is improved, organic solvent is removed before sintering.
The content of the invention
It is an object of the invention to cause sintering atmosphere unstable for above-mentioned LiFePO4 organic solvent, product is influenceed
The problems such as lot stability, there is provided a kind of inorganic dispersant is used for the method for preparing LiFePO 4 material.
Technical scheme is used by the present invention solves the above problems：A kind of inorganic dispersant is used to prepare LiFePO4 electricity
The method of pond material, it is by ferric phosphate, lithium carbonate, carbon source, talcum powder, lithium position doping metals compound and iron position doping metals
Compound mixes in proportion, and is placed in ball mill, adds batch mixing dispersant ball milling 150-300min, ball milling product is put into
In tube furnace, in nitrogen atmosphere, after 150-250 DEG C preheats 100-250min, heated up with the 5-40 DEG C/min rates of heat addition, in
500-800 DEG C of constant temperature calcining 30-200min, room temperature is then cooled to 5-20 DEG C/min rate of temperature fall, LiFePO4 electricity is made
Pond dusty material.
Described ferric phosphate, lithium carbonate, carbon source, talcum powder, lithium position doping metals compound and iron position doping metals
The molar ratio of compound is：2:1:1:0.1:(0.005~0.2):(0.01~0.1).
Described carbon source is selected from sucrose, the one or several kinds in glucose, citric acid.
Described lithium position doped compound is Nb2O5, TiO2In one kind；Iron position doped compound is MgO, Mg (OH)2,
One kind in NiO.
Described batch mixing dispersant is the one or more in zinc oxide, magnesia, distilled water, ethylenediamine inorganic solvent.
Inventive dispersant uses inorganic solvent, exists so as to avoid the organic solvent of recovery not yet in effect in traditional dispersant
Vaporized under the conditions of sintering high temperature, the compound such as produced carbon, nitrogen disturbs atmosphere content in atmosphere furnace after being mixed with inert gas
Accurate Determining, cause the stability for having a strong impact on sintering atmosphere, it is final to influence LiFePO4 crystal growth and electrochemistry uniformity
The problem of.
The preparation method of lithium iron phosphate positive material of the present invention solves solvent in lithium iron phosphate positive material sintering process
The problems such as recovery is difficult, and atmosphere is difficult to control, obtains the LiFePO 4 material that product batches stability has well.
Embodiment
The method that a kind of inorganic dispersant of the present invention is used to preparing lithium iron phosphate cell material be by ferric phosphate, lithium carbonate,
Carbon source, talcum powder, lithium position doping metals compound and iron position doping metals compound mix in proportion, and are placed in ball mill
In, novel dispersant ball milling 150-300min is added, ball milling product is put into tube furnace, in nitrogen atmosphere, in 150-250
After DEG C preheating 100-250min, heated up with the 5-40 DEG C/min rates of heat addition, in 500-800 DEG C of constant temperature calcining 30-200min, then
Room temperature is cooled to 5-20 DEG C/min rate of temperature fall, iron phosphate powder is made.
Ferric phosphate, lithium carbonate, carbon source, talcum powder, lithium position doping metals compound and iron position doping metals compound
Molar ratio is：2:1:1:0.1:(0.005~0.2):(0.01~0.1).
Carbon source is selected from sucrose, the one or more in glucose, citric acid.
In lithium position doped compound be Nb2O5, one kind in TiO2；Iron position doped compound is MgO, Mg (OH) 2, NiO
In one kind.
Novel mixing dispersant is zinc oxide, magnesia, distilled water, the one or more in ethylenediamine.
Embodiment 1
151g ferric phosphates, 37g lithium carbonates, 171g sucrose, 10g talcum powder, 2.6gNb2O5 and 2gMgO are mixed in proportion
It is even, it is placed in ball mill, adds zinc oxide ball milling 200min, ball milling product is put into tube furnace, in nitrogen atmosphere, in
After 180 DEG C of preheating 150min, heated up with the 12 DEG C/min rates of heat addition, in 650 DEG C of constant temperature calcining 100min, then with 8 DEG C/min
Rate of temperature fall is cooled to room temperature, and iron phosphate powder is made.Solves solvent recovery in lithium iron phosphate positive material sintering process
Difficulty, the problems such as atmosphere is difficult to control.
Embodiment 2
By 226.5g ferric phosphates, 55.5g lithium carbonates, 135g glucose, 10g talcum powder, 2.4gNb2O5 and 3.5gNiO press than
Example is well mixed, is placed in ball mill, adds magnesia and ethylenediamine ball milling 150min, ball milling product is put into tube furnace,
In nitrogen atmosphere, after 200 DEG C preheat 200min, heated up with the 30 DEG C/min rates of heat addition, in 800 DEG C of constant temperature calcining 80min,
Then room temperature is cooled to 15 DEG C/min rate of temperature fall, iron phosphate powder is made.
Embodiment 3
302g ferric phosphates, 74g lithium carbonates, 192g citric acids, 10g talcum powder, 7gTiO2 and 1.9gMg (OH) 2 are mixed in proportion
Close uniformly, be placed in ball mill, add distilled water and diethylamine ball milling 300min, ball milling product is put into tube furnace, in nitrogen
In gas atmosphere, after 250 DEG C preheat 250min, heated up with the 40 DEG C/min rates of heat addition, in 800 DEG C of constant temperature calcining 200min, so
Room temperature is cooled to 20 DEG C/min rate of temperature fall afterwards, iron phosphate powder is made.
Embodiment 4
45.3g ferric phosphates, 11.1g lithium carbonates, 51.3g sucrose, 10g talcum powder, 2gTiO2 and 1.5gNiO are mixed in proportion
Uniformly, it is placed in ball mill, adds distillation water for ball milling 150min, ball milling product is put into tube furnace, in nitrogen atmosphere, in
After 150 DEG C of preheating 100min, heated up with the 5 DEG C/min rates of heat addition, in 500 DEG C of constant temperature calcining 30min, then dropped with 5 DEG C/min
Warm speed is cooled to room temperature, and iron phosphate powder is made.
Embodiment 5
By 86.7g ferric phosphates, 21.25g lithium carbonates, 37.6g sucrose, 10g talcum powder, 42.4g glucose, 3.6gTiO2 and
1.8gNiO is mixed in proportion, and is placed in ball mill, adds magnesia and distillation water for ball milling 190min, ball milling product is put
Enter in tube furnace, in nitrogen atmosphere, after 200 DEG C preheat 170min, heated up with the 16 DEG C/min rates of heat addition, in 780 DEG C of perseverances
Temperature roasting 60min, is then cooled to room temperature with 15 DEG C/min rate of temperature fall, iron phosphate powder is made.
Embodiment 6
By 169.5g ferric phosphates, 41.5g lithium carbonates, 61.1g sucrose, 10g talcum powder, 18.9g citric acids, 4.2gTiO2 and
3.6gNiO is mixed in proportion, and is placed in ball mill, adds zinc oxide ball milling 210min, ball milling product is put into tube furnace
In, in nitrogen atmosphere, after 230 DEG C preheat 210min, heated up with the 28 DEG C/min rates of heat addition, in 700 DEG C of constant temperature calcinings
160min, room temperature is then cooled to 20 DEG C/min rate of temperature fall, iron phosphate powder is made.
Claims (5)
1. a kind of inorganic dispersant is used for the method for preparing lithium iron phosphate cell material, it is characterised in that：By ferric phosphate, carbonic acid
Lithium, carbon source, talcum powder, lithium position doping metals compound and iron position doping metals compound mix in proportion, and are placed in ball
In grinding machine, batch mixing dispersant ball milling 150-300min is added, ball milling product is put into tube furnace, in nitrogen atmosphere, in
After 150-250 DEG C of preheating 100-250min, heated up with the 5-40 DEG C/min rates of heat addition, in 500-800 DEG C of constant temperature calcining 30-
200min, room temperature is then cooled to 5-20 DEG C/min rate of temperature fall, ferric phosphate lithium cell dusty material is made.
2. inorganic dispersant according to claim 1 is used for the method for preparing lithium iron phosphate cell material, it is characterised in that：
Ferric phosphate, lithium carbonate, carbon source, talcum powder, the molar ratio of lithium position doping metals compound and iron position doping metals compound
For：2:1:1:0.1:(0.005~0.2):(0.01~0.1).
3. inorganic dispersant according to claim 1 is used for the method for preparing lithium iron phosphate cell material, it is characterised in that：
Carbon source is selected from sucrose, the one or several kinds in glucose, citric acid.
4. inorganic dispersant according to claim 1 is used for the method for preparing lithium iron phosphate cell material, it is characterised in that：
Lithium position doped compound is Nb2O5, TiO2In one kind；Iron position doped compound is MgO, Mg (OH)2, one kind in NiO.
5. inorganic dispersant according to claim 1 is used for the method for preparing lithium iron phosphate cell material, it is characterised in that
Batch mixing dispersant is the one or more in zinc oxide, magnesia, distilled water, ethylenediamine inorganic solvent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109192948A (en) * | 2018-08-29 | 2019-01-11 | 深圳市德方纳米科技股份有限公司 | A kind of high compacted density LiFePO4 and preparation method thereof |
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| CN103682363A (en) * | 2013-12-30 | 2014-03-26 | 云南磷化集团有限公司 | Method for using novel material mixing dispersing agents for preparing lithium iron phosphate battery materials |
| CN103779565A (en) * | 2014-02-12 | 2014-05-07 | 云南磷化集团有限公司 | Preparation method of lithium iron phosphate composite battery material |
| CN106242603A (en) * | 2016-08-23 | 2016-12-21 | 江西省安源化工填料有限公司 | A kind of sintering supporting body and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103682363A (en) * | 2013-12-30 | 2014-03-26 | 云南磷化集团有限公司 | Method for using novel material mixing dispersing agents for preparing lithium iron phosphate battery materials |
| CN103779565A (en) * | 2014-02-12 | 2014-05-07 | 云南磷化集团有限公司 | Preparation method of lithium iron phosphate composite battery material |
| CN106242603A (en) * | 2016-08-23 | 2016-12-21 | 江西省安源化工填料有限公司 | A kind of sintering supporting body and preparation method thereof |
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| 朱洪法: "《生活化学品与健康》", 1 April 2013 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109192948A (en) * | 2018-08-29 | 2019-01-11 | 深圳市德方纳米科技股份有限公司 | A kind of high compacted density LiFePO4 and preparation method thereof |
| CN109192948B (en) * | 2018-08-29 | 2021-05-07 | 深圳市德方纳米科技股份有限公司 | High-compaction-density lithium iron phosphate and preparation method thereof |
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