CN107055574A - A kind of method of purification of lithium hexafluoro phosphate - Google Patents
A kind of method of purification of lithium hexafluoro phosphate Download PDFInfo
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- CN107055574A CN107055574A CN201710231212.4A CN201710231212A CN107055574A CN 107055574 A CN107055574 A CN 107055574A CN 201710231212 A CN201710231212 A CN 201710231212A CN 107055574 A CN107055574 A CN 107055574A
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- hexafluoro phosphate
- lithium hexafluoro
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/005—Lithium hexafluorophosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to a kind of method of purification of lithium hexafluoro phosphate, belong to technical field of lithium ion.The method of purification of the lithium hexafluoro phosphate of the present invention comprises the following steps：1) under protective atmosphere, into lithium hexafluoro phosphate to be purified, addition organic solvent is dissolved, and is filtered, is obtained filtrate；2) add silazane into filtrate to carry out removing acid reaction, crystallization obtains crystal, is drying to obtain.The method of purification of the present invention, lithium hexafluoro phosphate crude product is purified using ether solvent, carbonate-based solvent or acetonitrile as organic solvent, remove the insoluble substance in lithium hexafluoro phosphate, then free acid is removed by adding HF acid effect of the silazane with being remained in lithium hexafluoro phosphate crude product, then metal impurities is removed through recrystallization process；The method of purification can be handled the lithium hexafluoro phosphate of inferior quality, effectively remove lithium hexafluoro phosphate crystals be mingled with or surface attachment acid and metal impurities, reduce insolubles content, improve lithium hexafluoro phosphate product quality.
Description
Technical field
The present invention relates to a kind of method of purification of lithium hexafluoro phosphate, belong to technical field of lithium ion.
Background technology
Nearly ten years, the electric industry development of lithium is swift and violent, drives upstream industry to develop rapidly, lithium ion battery electrolyte demand
Improve constantly.Lithium hexafluoro phosphate, as current internationally recognized excellent electrolyte, is the key core material for manufacturing lithium ion battery
One of material, the cycle life of lithium ion battery, rate charge-discharge performance, high temperature performance all with hexafluorophosphoric acid lithium electrolyte quality
There is the performance of the meeting extreme influence positive and negative electrode in cell operation of the impurity in direct relation, electrolyte.Lithium hexafluoro phosphate one
As be prepared from by anhydrous hydrogen fluoride, phosphorus pentoxide and lithium fluoride, in its finished product inevitably contain hydrogen fluoride impurity, separately
Outside, lithium hexafluoro phosphate easily absorbs water generation hydrolysis, resolves into insoluble fluorine oxygen phosphorus lithium compound, and these impurity lithium from
Sub- battery in use, the performance of lithium ion battery can be reduced, therefore how to obtain high-purity, low free acid, low-moisture height
Purity lithium hexafluoro phosphate is current urgent problem to be solved.
Chinese patent (publication number CN 1850593A) discloses a kind of purification process of lithium hexafluoro phosphate, by phosphorus pentafluoride
It is passed through with after hydrogen fluoride mixed gas purification in the drying equipment of lithium hexafluoro phosphate, phosphorus pentafluoride is being prepared with lithium hexafluoro phosphate
During the lithium fluoride and fluorine oxygen phosphorus lithium LiPO carried secretlyxFyReacted and be converted into lithium hexafluoro phosphate, so that lithium hexafluoro phosphate
Purified, but this method can not reduce lithium hexafluoro phosphate crystals be mingled with or surface attachment acid and metal impurities.
Chinese patent (publication number CN 103539168A) discloses the purification process of lithium hexafluoro phosphate, and this method is in dehydration
The lower progress of protective gas protection afterwards, lithium hexafluoro phosphate is dissolved in carbonic ester and (or) ether solvent, is filtered to remove insoluble
Thing obtains transparency liquid, adds the alkane or ether solvent of 0.1~10 volume and makes lithium hexafluoro phosphate nucleation and crystallization, repeats the above steps
At least one times, finally it is dried in vacuo, obtains high purity lithium hexafluorophosphate.This method, which needs to be repeated several times to crystallize, could remove hexafluoro phosphorus
Inorganic impurity and organic impurities in sour lithium, and purified without the hydrogen fluoride impurity remained for lithium hexafluoro phosphate.
The content of the invention
It is an object of the invention to provide a kind of method of purification of lithium hexafluoro phosphate, this method can remove lithium hexafluoro phosphate
The insoluble matter and metal impurities of inner inclusion or adsorption, especially remove the sour impurity of the HF contained in lithium hexafluoro phosphate.
To achieve these goals, the technical scheme of the method for purification of lithium hexafluoro phosphate of the present invention is as follows：
A kind of method of purification of lithium hexafluoro phosphate, comprises the following steps：
1) under protective atmosphere, into lithium hexafluoro phosphate to be purified, addition organic solvent is dissolved, and is filtered, is filtered
Liquid；
2) add silazane into filtrate to carry out removing acid reaction, crystallization obtains crystal, is drying to obtain.
The form that free acid in lithium hexafluoro phosphate to be purified is mainly HF acid is present, and the content of free acid is lower, right
It is purified all the more difficult, and the be particularly suitable for use in free acid content of lithium hexafluoro phosphate to be purified of method of the invention is not more than
100ppm is purified.
Step 1) in, the organic solvent is ether solvent, carbonate-based solvent or acetonitrile.The ether solvent is preferably
Ether；The carbonate-based solvent is preferably dimethyl carbonate.During dissolving, the matter of organic solvent and lithium hexafluoro phosphate to be purified
Measure ratio preferably 100：(40~90).
The temperature of the dissolving is not higher than below the boiling point of organic solvent 10 DEG C.When organic solvent is ether, dissolve controllable
System is carried out in 10 DEG C~25 DEG C；When organic solvent is dimethyl carbonate, dissolving can be controlled in 15 DEG C~40 DEG C and carried out.
The moisture of the organic solvent is not more than 50ppm.Organic solvent can be purified by the method steamed again, with
Reduce moisture, free acid and various trace impurity contents.
Step 2) in, the silazane is HMDS or the silazane of nine methyl three.
Step 2) in, counted using in lithium hexafluoro phosphate to be purified using the free acid content that HF is counted as 80~100ppm, often
The addition of the corresponding silazane of lithium hexafluoro phosphate to be purified 100g is 0.05~0.7mL.
Step 2) in, except the temperature of acid reaction is not higher than below the boiling point of organic solvent 10 DEG C, except the time of acid reaction is
More than 20min.Except in acid reaction, the purity of silazane can be to analyze pure or higher purity rank, and fusing point or boiling point are higher,
Do not reacted with solvent and lithium hexafluoro phosphate, stable chemical performance under normal temperature, the performance to lithium battery has no adverse effects.The step
In, the addition of silazane can be adjusted according to the size of acidity in the property of silazane and lithium hexafluoro phosphate to be purified
Section.
Step 2) in, the crystallization is decrease temperature crystalline and/or vacuumizes crystallization.
The decrease temperature crystalline comprises the following steps：- 25 DEG C~-15 DEG C are cooled to be not more than 5 DEG C/min speed, then
More than 20min is crystallized at such a temperature.The mother liquor of decrease temperature crystalline process can obtain concentrated solution by being concentrated by evaporation, by the concentrated solution
The lithium hexafluoro phosphate remained to reclaim in mother liquor is mixed with filtrate；The organic solvent of evaporation is condensed to can return to step 1) repeat to make
With.Can also by the mother liquor of decrease temperature crystalline process directly and part organic solvent mix return to step 1) reuse.
It is described to vacuumize crystallization and comprise the following steps：To be not more than 0.5bar/min speed, to be evacuated to vacuum little
In -1bar, more than 30min is then crystallized under the vacuum.The gas produced in crystallization process is vacuumized to reclaim by condensation
Organic solvent, can directly or through again steam after return to step 1) realize recycle.
The crystalline rate and crystal of lithium hexafluoro phosphate can be improved decrease temperature crystalline and by way of vacuumizing crystalline phase combination
Quality.
The method of purification of the lithium hexafluoro phosphate of the present invention, using ether solvent, carbonate-based solvent or acetonitrile as organic molten
Agent purifies lithium hexafluoro phosphate crude product, the insoluble substance in lithium hexafluoro phosphate is removed, then by adding silazane and hexafluoro phosphorus
The HF acid effects remained in sour lithium crude product remove free acid, then remove metal impurities through recrystallization process；The method of purification can be right
The lithium hexafluoro phosphate of inferior quality is handled, effectively remove lithium hexafluoro phosphate crystals be mingled with or surface attachment acid and
Metal impurities, reduce insolubles content, improve the quality of lithium hexafluoro phosphate product.
The method of purification of the lithium hexafluoro phosphate of the present invention, extensively, production cost is low, non-hazardous, product quality for raw material sources
Height, can be achieved semi-industrial production, with good social value and economic value, it is easy to promote and use.
Embodiment
In the present invention organic solvent used using preceding needing to be pre-processed, remove moisture therein, free acid with
And metal impurities, its moisture should be less than 50ppm after solvent is treated.
Embodiment 1
The method of purification of the present embodiment lithium hexafluoro phosphate, lithium hexafluoro phosphate to be purified is big production product, quality testing knot
It is really：Product purity is more than 99.9%, product free acid (in terms of HF) 80ppm, moisture (with karr Fei Xiufa) 5ppm, alkali metal
Ion concentration (in terms of K, Na) 2ppm, heavy metal ion content (in terms of Fe) 2ppm, insolubles content 220ppm；Purification operations are such as
Under：
1) there is a glove box of enough operating spaces full of nitrogen, adding 150mL second into 500mL reaction vessel
Ether, is down to 15 DEG C by ether temperature using refrigerator, opens stirring, adds 90g lithium hexafluoro phosphates to be purified and is dissolved, often
Add 5g and determine system temperature, keep course of dissolution temperature at 10 DEG C~25 DEG C, finish continuation and stir 20min so as to dissolve
Entirely, insoluble matter is filtered off using 500 eye mesh screens, obtains filtrate；
2) 0.5mL HMDSs are added into filtrate, the stirring reaction 20min at 20 DEG C closes stirring；Then
System is cooled to -20 DEG C with 1 DEG C/min speed, 20min, isolated crystal, through being dried to obtain 75g products is kept.
The purity of lithium hexafluoro phosphate is more than 99.9%, free acid (in terms of HF) 30ppm obtained by the present embodiment, and moisture is (with card
Er Feixiufa) 3ppm, alkali metal ion content measured (in terms of Ka, Na) 2ppm, heavy metal ion content (in terms of Fe) 1ppm, insoluble matter
Content 200ppm.
Embodiment 2
Addition ether obtains 100mL mixed liquors in the mother liquor 35mL obtained after being crystallized in the present embodiment into embodiment 1, takes
45g is big to produce lithium hexafluoro phosphate product, and quality measurements are：Product purity is more than 99.9%, product free acid (in terms of HF)
75ppm, moisture (with karr Fei Xiufa) 5ppm, alkali metal ion content measured (in terms of Ka, Na) 2ppm, heavy metal ion content (with
Fe is counted) 2ppm, insolubles content 230ppm；
The technological parameter pressed by organic solvent of above-mentioned mixed liquor in embodiment 1 carries out purification operations, obtains 45g hexafluoro phosphorus
Sour lithium product, testing result is：Product purity is more than 99.9%, and product free acid (in terms of HF) 20ppm, moisture is (luxuriant and rich with fragrance with karr
Not method) 3ppm, alkali metal ion content measured (in terms of Ka, Na) 1ppm, heavy metal ion content (in terms of Fe) 1ppm, insolubles content
180ppm。
Embodiment 3
The method of purification of the present embodiment lithium hexafluoro phosphate, lithium hexafluoro phosphate to be purified is big production product, quality testing knot
It is really：Product purity is more than 99.9%, product free acid (in terms of HF) 90ppm, moisture (with karr Fei Xiufa) 6ppm, alkali metal
Ion concentration (in terms of K, Na) 2ppm, heavy metal ion content (in terms of Fe) 2ppm, insolubles content 200ppm；Purification operations are such as
Under：
1) there is a glove box of enough operating spaces full of nitrogen, adding 150mL carbon into 500mL reaction vessel
Dimethyl phthalate, is down to 20 DEG C by dimethyl carbonate temperature using refrigerator, opens stirring, adds 80g hexafluorophosphoric acids to be purified
Lithium is dissolved, and is often added 5g and is determined system temperature, keeps course of dissolution temperature at 15 DEG C~40 DEG C, is finished continuation and is stirred
20min is so that dissolving completely, filters off insoluble matter using 500 eye mesh screens, obtains filtrate；
2) silazane of nine methyl of 0.05mL three is added into filtrate, the stirring reaction 20min at 25 DEG C closes stirring；So
System is cooled to -15 DEG C with 3 DEG C/min speed afterwards, 20min, isolated crystal, through being dried to obtain 65g products is kept.
The purity of lithium hexafluoro phosphate is more than 99.9%, product free acid (in terms of HF) 26ppm, moisture obtained by the present embodiment
(with karr Fei Xiufa) 2ppm, alkali metal ion content measured (in terms of Ka, Na) 2ppm, heavy metal ion content (in terms of Fe) 1ppm,
Insolubles content 180ppm.
In the present embodiment, the mother liquor of the decrease temperature crystalline process of decrease temperature crystalline process can be obtained dense molten by being concentrated by evaporation
Liquid, the concentrated solution is mixed with filtrate the lithium hexafluoro phosphate remained to reclaim in mother liquor；The organic solvent of evaporation is condensed to be returned
Step 1) reuse.
In other embodiments of the invention, also silazane reaction can specially be added by the way of crystallization is vacuumized
Afterwards, vacuum is evacuated to as -1bar using 0.5bar/min speed, keeps more than 30min, product quality can be obtained suitable
Lithium hexafluoro phosphate product, can be directly or through return to step 1 steam again after after the gas of vacuum generation is condensed) realize
Recycle.
Claims (10)
1. a kind of method of purification of lithium hexafluoro phosphate, it is characterised in that comprise the following steps：
1) under protective atmosphere, into lithium hexafluoro phosphate to be purified, addition organic solvent is dissolved, and is filtered, is obtained filtrate；
2) add silazane into filtrate to carry out removing acid reaction, crystallization obtains crystal, is drying to obtain.
2. the method for purification of lithium hexafluoro phosphate as claimed in claim 1, it is characterised in that step 1) in, the organic solvent
For ether solvent, carbonate-based solvent or acetonitrile.
3. the method for purification of lithium hexafluoro phosphate as claimed in claim 1 or 2, it is characterised in that the temperature of the dissolving is not high
10 DEG C below the boiling point of organic solvent.
4. the method for purification of lithium hexafluoro phosphate as claimed in claim 1 or 2, it is characterised in that the moisture of the organic solvent
Content is not more than 50ppm.
5. the method for purification of lithium hexafluoro phosphate as claimed in claim 1, it is characterised in that step 2) in, the silazane is
HMDS or the silazane of nine methyl three.
6. the method for purification of the lithium hexafluoro phosphate as described in claim 1 or 5, it is characterised in that step 2) in, with to be purified
Counted in lithium hexafluoro phosphate using the free acid content that HF is counted as 80~100ppm, per the corresponding silicon of lithium hexafluoro phosphate to be purified 100g
The addition of azane is 0.05~0.7mL.
7. the method for purification of the lithium hexafluoro phosphate as described in claim 1 or 5, it is characterised in that step 2) in, except acid reaction
Temperature is not higher than below the boiling point of organic solvent 10 DEG C, except the time of acid reaction is more than 20min.
8. the method for purification of lithium hexafluoro phosphate as claimed in claim 1, it is characterised in that step 2) in, the crystallization is drop
Temperature crystallizes and/or vacuumized crystallization.
9. the method for purification of lithium hexafluoro phosphate as claimed in claim 8, it is characterised in that the decrease temperature crystalline includes following step
Suddenly：- 25 DEG C~-15 DEG C are cooled to be not more than 5 DEG C/min speed, more than 20min is then crystallized at such a temperature.
10. the method for purification of lithium hexafluoro phosphate as claimed in claim 8 or 9, it is characterised in that described to vacuumize crystallization and include
Following steps：Vacuum is evacuated to be not more than 0.5bar/min speed and is not more than -1bar, is then tied under the vacuum
Brilliant more than 30min.
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Cited By (6)
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|---|---|---|---|---|
| CN108147386A (en) * | 2017-12-25 | 2018-06-12 | 衢州北斗星化学新材料有限公司 | A kind of preparation method of dynamic crystallization lithium hexafluoro phosphate |
| CN108569710A (en) * | 2017-12-26 | 2018-09-25 | 衢州北斗星化学新材料有限公司 | A kind of purification process preparing high purity lithium hexafluorophosphate |
| CN110562949A (en) * | 2019-09-17 | 2019-12-13 | 珠海市赛纬电子材料股份有限公司 | Method for purifying lithium difluorophosphate |
| CN111153917A (en) * | 2019-10-12 | 2020-05-15 | 湖北省宏源药业科技股份有限公司 | Purification process of lithium bis (oxalato) borate |
| CN113060718A (en) * | 2021-03-29 | 2021-07-02 | 兰州理工大学 | Method for preparing lithium difluorophosphate by recycling electrolyte from waste lithium ion battery |
| CN113479914A (en) * | 2021-08-12 | 2021-10-08 | 浙江三美化工股份有限公司 | Purification process of lithium hexafluorophosphate |
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Cited By (8)
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|---|---|---|---|---|
| CN108147386A (en) * | 2017-12-25 | 2018-06-12 | 衢州北斗星化学新材料有限公司 | A kind of preparation method of dynamic crystallization lithium hexafluoro phosphate |
| CN108147386B (en) * | 2017-12-25 | 2020-06-09 | 衢州北斗星化学新材料有限公司 | Preparation method of dynamic crystalline lithium hexafluorophosphate |
| CN108569710A (en) * | 2017-12-26 | 2018-09-25 | 衢州北斗星化学新材料有限公司 | A kind of purification process preparing high purity lithium hexafluorophosphate |
| CN110562949A (en) * | 2019-09-17 | 2019-12-13 | 珠海市赛纬电子材料股份有限公司 | Method for purifying lithium difluorophosphate |
| CN111153917A (en) * | 2019-10-12 | 2020-05-15 | 湖北省宏源药业科技股份有限公司 | Purification process of lithium bis (oxalato) borate |
| CN113060718A (en) * | 2021-03-29 | 2021-07-02 | 兰州理工大学 | Method for preparing lithium difluorophosphate by recycling electrolyte from waste lithium ion battery |
| CN113479914A (en) * | 2021-08-12 | 2021-10-08 | 浙江三美化工股份有限公司 | Purification process of lithium hexafluorophosphate |
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Application publication date: 20170818 |