CN107585776A - A kind of method of Rheological Phase Method synthesis LiBF4 - Google Patents
A kind of method of Rheological Phase Method synthesis LiBF4 Download PDFInfo
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- CN107585776A CN107585776A CN201710949506.0A CN201710949506A CN107585776A CN 107585776 A CN107585776 A CN 107585776A CN 201710949506 A CN201710949506 A CN 201710949506A CN 107585776 A CN107585776 A CN 107585776A
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- libf4
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Abstract
The invention discloses a kind of method of Rheological Phase Method synthesis LiBF4, the present invention is using boron chloride as raw material, it is fluorinated to obtain intermediate product boron trifluoride through anhydrous hydrogen fluoride, the rheology precursor reactant formed again with high-purity lithium fluoride solid powder and anhydrous hydrofluoric acid modulation, the step such as concentrated crystallization, separation, purification obtains finished product LiBF4 again, wherein anhydrous hydrofluoric acid flaorination process is ripe and simple to operate, compare using boron trifluoride as raw material for cost savings production cost；Wherein the mass fraction of lithium fluoride anhydrous hydrofluoric acid rheology body weight lithium fluoride is 1 2%, can utilize the ratio surface of solid to a greater extent, react more abundant；Crude product is wherein obtained using the method for condensing crystallizing combination low temperature crystallization, crystal can be allowed to separate out to greatest extent；The Methods For Purification crude product of secondary crystallization is wherein used, the finished product purity drawn is higher, and moisture is less, and acidity is lower.
Description
Technical field
The present invention relates to lithium battery raw material LiBF4 technical field, more particularly to a kind of Rheological Phase Method synthesis tetrafluoro
The method of lithium borate.
Background technology
With the continuous development of scientific technology and the people's material and cultural life level raising, people are to novel lithium battery
Demand it is increasing, while the also more and more higher of the requirement to lithium battery performance.Electrolyte is can not in lithium battery electrolytes
Or scarce part, it is one of important determinant of performance of lithium ion battery.It is most widely used in current battery industry
For lithium hexafluoro phosphate base lithium battery because with higher ionic conductivity and steady when lithium hexafluoro phosphate is as electrolyte lithium salt
Fixed chemical property.However, lithium hexafluoro phosphate still have to water sensitive, low temperature generation SEI membrane impedances it is excessive, 80 DEG C open
Begin the distinct disadvantages such as decomposition, causes its condition of work to be greatly limited.
LiBF4 can be applied simultaneously as a kind of new electrolyte lithium salt as additive with lithium hexafluoro phosphate
, can be with the premise of the physical behavior and the high rate performance of battery for not interfering with lithium hexafluorophosphate electrolyte solution in lithium battery
Improve the discharge performance and cycle performance of battery.The research and development of four lithium fluophosphates can provide the skill of strength for the development of lithium battery
Art is supported.
Known LiBF4 synthetic method mainly has solid-gas phase method, aqua-solution method, non-aqueous fusion agent in the market
Method, lithium metaborate method.Wherein solid-gas phase method is reacted with solid lithium source and boron triflouride gas, and principle is simple and operation difficulty is small,
But solid material specific surface area is small, raw material cannot be utilized fully, it is difficult to obtain the higher product of purity.Aqua-solution method with
Water is medium, and reaction is abundant, but obtained product has the larger problems such as dehydration, purification.Non-aqueous flux method uses organic
Solvent（Such as ether）For medium, suspension is formed with lithium source, reaction is more abundant, but side reaction easily occurs, and is difficult to
Separation.Lithium metaborate method needs to react at a higher temperature, and energy consumption is larger and the substantial amounts of moisture of simultaneous generates.
CN104326482A discloses a kind of method for preparing LiBF4, comprises the following steps：By lithium carbonate, Dan Shui
After lithium hydroxide or anhydrous lithium hydroxide and boric acid, boron oxide mixing, calcination, you can obtain lithium metaborate, crush and obtain metaboric acid
Lithium powder, lithium metaborate powder and ammonium fluoride or ammonium acid fluoride are mixed, vacuum pressure negative pressure calcination reaction, you can obtain tetrafluoro
Lithium borate product.
A kind of preparation methods of LiBF4 of CN104030310A, feature include：From tetrafluoroborate MBF4 wherein M
For Na, K, NH4, Ag；Or selected from tetramethyl ammonium tetrafluoroborate, tetraethyl ammonium tetrafluoroborate ammonium tetrafluoroborate type organic in
One or more；And react with starting halo lithium salts such as LiF and product MF, LiBF4, the difference of solubility is utilized, is utilized
Ion-exchange process prepares LiBF4；The reaction temperature is carried out between 0-15 DEG C, filtering, and the heated concentration of filtrate is cold
But LiBF4 crystal is obtained afterwards, and LiBF4 product is produced after vacuum rapid draing；Purified to obtain final four with organic solvent again
Lithium fluoroborate product.
CN104291347A provides a kind of preparation method of LiBF4, including boron triflouride gas is passed into fluorine
Change lithium anhydrous hydrogen fluoride solution in, reaction obtain the mixture of tetrafluoro boric acid crystalline lithium and anhydrous hydrogen fluoride, by crystallization,
Filtering, drying obtain LiBF4 finished product.
The content of the invention
A kind of the defects of it is an object of the invention to for traditional lithium hexafluoro phosphate base lithium battery performance, there is provided excellent performance
New lithium salts LiBF4 synthetic method, final product quality batch is stable, purity is high.
A kind of method of Rheological Phase Method synthesis LiBF4 according to embodiments of the present invention, comprises the following steps：
（1）Under inert gas shielding, high-purity lithium fluoride solid is added into anhydrous liquid hydrogen fluoride, it is agitated to be modulated into stream
Variant；
（2）Boron trichloride gas are passed through into anhydrous liquid hydrogen fluoride, reaction obtains boron triflouride gas；
（3）By step（2）The middle obtained boron triflouride gas that reacts is passed into step（1）In obtained lithium fluoride-anhydrous fluorination
In hydrogen rheological body, reaction at a certain temperature obtains the solidliquid mixture of LiBF4 crystallite and hydrogen fluoride；
（4）Will（3）In the solidliquid mixture of obtained LiBF4 crystallite and hydrogen fluoride be warming up to 30-40 DEG C, remove 80%
Anhydrous hydrogen fluoride medium, then low temperature crystallization is carried out, the substandard products of LiBF4 one are obtained, while anhydrous hydrogen fluoride is collected, it can follow
Ring is used in dissolving high-purity lithium fluoride solid；
（5）LiBF4 finished product is obtained using the organic solvent purification substandard products of LiBF4 one.
On the basis of such scheme, described inert gas is from one kind in nitrogen, helium, argon gas, xenon.
On the basis of such scheme, step（1）In, the mass fraction of lithium fluoride is 1-2% in described rheological body.
On the basis of such scheme, step（1）In, described high-purity lithium fluoride solid is more than 99.5% from purity
Battery-grade lithium fluoride solid powder.
On the basis of such scheme, step（1）In, described stirring modulated process needs to stir more than 40min.
On the basis of such scheme, step（2）In, be 5-15 DEG C in temperature, pressure be 50-100KPa under conditions of to nothing
Boron trichloride gas are passed through in water hydrogen fluoride liquid.
On the basis of such scheme, step（3）In, reaction temperature is 5-15 DEG C.
On the basis of such scheme, step（4）In, described low temperature crystallization is Cryogenic Temperature Swing stationary crystallization, temperature range
For 15~-40 DEG C, cool 3-5 DEG C per hour.
On the basis of such scheme, step（5）In, described organic solvent is from ethyl acetate, propene carbonate, carbonic acid
One kind in dimethyl ester, diethyl carbonate, methyl ethyl carbonate.
On the basis of such scheme, in step（5）Described in purification include dissolving, concentration, recrystallization, filtering, vacuum
Dry.
The present invention has an advantageous effect in that compared with prior art：Using boron chloride as raw material, through anhydrous hydrogen fluoride fluorine
Change obtains intermediate product boron trifluoride, then anti-with rheological body that high-purity lithium fluoride solid powder and anhydrous hydrogen fluoride modulation form
Answer, then the step such as concentrated crystallization, separation, purification obtains finished product LiBF4, wherein anhydrous hydrogen fluoride flaorination process is ripe
And it is simple to operate, compare using boron trifluoride as raw material for cost savings production cost；Wherein lithium fluoride-anhydrous fluorination
The mass fraction of hydrogen rheology body weight lithium fluoride is 1-2%, can utilize the ratio surface of solid to a greater extent, react more abundant；Wherein
Crude product is obtained using method of the condensing crystallizing plus low temperature crystallization, crystal can be allowed to separate out to greatest extent；Wherein using secondary
The Methods For Purification crude product of crystallization, the finished product purity drawn is higher, and moisture is less, and acidity is lower；Material is uniformly distributed in media as well,
The surface of solids can efficiently be utilized, and heat exchange is good, be advantageous to temperature control；Reaction is abundant, efficiently, section
Can, it is environment-friendly.Boron chloride is fluorinated generation boron trifluoride by anhydrous hydrogen fluoride, and intermediate product boron trifluoride is passed into lithium fluoride
With the equally distributed rheology body weight of anhydrous hydrogen fluoride, generation LiBF4 is fully reacted with lithium fluoride, by low temperature crystallization,
The steps such as separation, purification obtain LiBF4 finished product, and final product quality batch is stable, purity is high.
Brief description of the drawings
Fig. 1 is the process chart for the method that a kind of Rheological Phase Method proposed by the present invention synthesizes LiBF4.
Embodiment
For feature, technological means and the concrete function reached of the present invention can be further appreciated that, below with accompanying drawing, specific
Embodiment is described in further detail to the present invention.
As shown in figure 1, the present invention provides a kind of method of Rheological Phase Method synthesis LiBF4, comprise the following steps：
（1）Under inert gas shielding, high-purity lithium fluoride solid, agitated modulation are added into anhydrous liquid hydrogen fluoride
More than 40min becomes rheological body, and wherein inert gas is fluorinated in rheological body from one kind in nitrogen, helium, argon gas, xenon
The mass fraction of lithium is 1-2%, and high-purity lithium fluoride solid is more than 99.5% battery-grade lithium fluoride solid powder from purity；
（2）It it is 5-15 DEG C in temperature, pressure is passed through boron chloride gas into anhydrous liquid hydrogen fluoride under conditions of being 50-100KPa
Body, reacted at 5-15 DEG C and obtain boron triflouride gas；
（3）By step（2）The middle obtained boron triflouride gas that reacts is passed into step（1）In obtained lithium fluoride-anhydrous fluorination
In hydrogen rheological body, reaction obtains the solidliquid mixture of LiBF4 crystallite and hydrogen fluoride；
（4）Will（3）In the solidliquid mixture of obtained LiBF4 crystallite and hydrogen fluoride be warming up to 30-40 DEG C, remove 80%
Anhydrous hydrogen fluoride medium, then low temperature crystallization is carried out, the substandard products of LiBF4 one are obtained, while anhydrous hydrogen fluoride is collected, it can follow
Ring is used in dissolving high-purity lithium fluoride solid, wherein, low temperature crystallization be Cryogenic Temperature Swing stationary crystallization, temperature range for 15~-
40 DEG C, cool 3-5 DEG C per hour；
（5）LiBF4 finished product is obtained using the organic solvent purification substandard products of LiBF4 one, organic solvent selects acetic acid second
One kind in ester, propene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, purification include dissolving, concentration, tied again
Brilliant, filtering, vacuum drying.
The present invention is further elaborated by the following examples.
Embodiment 1：
（1）1.5kg lithium fluoride and 100kg anhydrous hydrogen fluorides are taken, common under inert nitrogen gas protection to add in synthesis reactor, temperature
Degree is arranged to 10 DEG C, is sufficiently stirred 1h and is modulated into lithium fluoride-anhydrous hydrogen fluoride rheological body.
（2）Take 4kg anhydrous hydrogen fluorides（Excessive 14%）Adding in reactor, temperature setting is 10 DEG C, pressure 70KPa, then
6.8kg boron chlorides are taken slowly at the uniform velocity to be passed through in reactor, the boron triflouride gas generated in reactor is passed into synthesis reactor
Lithium fluoride-anhydrous hydrogen fluoride rheological body in, control temperature a length of 3h at 10 DEG C, reaction, obtain LiBF4 crystallite and
The solidliquid mixture of hydrogen fluoride.
（3）After reaction completely, by the LiBF4 crystallite and the solidliquid mixture of hydrogen fluoride in synthesis reactor, 30 are warming up to
DEG C, remove 80% anhydrous hydrogen fluoride medium, concentrating low-temperature alternating temperature stationary crystallization is simultaneously filtrated to get the substandard products of LiBF4 one
5.3kg, take 100kg ethyl acetate to dissolve the substandard products of LiBF4 one, LiBF4 finished product 5.2kg is obtained after purification, produce
Rate 96%.After after testing, finished product purity is 99.8%, moisture 17ppm.
Embodiment 2：
（1）3.0kg lithium fluoride and 200kg anhydrous hydrogen fluorides are taken, inert gas helium protection is lower to be added in synthesis reactor jointly, temperature
10 DEG C are arranged to, 1h is sufficiently stirred and is modulated into lithium fluoride-anhydrous hydrogen fluoride rheological body.
（2）Take 8kg anhydrous hydrogen fluorides（Excessive 15%）Adding in reactor, temperature setting is 10 DEG C, pressure 80KPa, then
Take 13.6kg boron chlorides to be slowly at the uniform velocity passed through in reactor, the boron triflouride gas generated in reactor is passed into synthesis reactor
In lithium fluoride-anhydrous hydrogen fluoride rheological body in, control temperature a length of 3h at 10 DEG C, reaction, obtain LiBF4 crystallite
With the solidliquid mixture of hydrogen fluoride.
（3）After reaction completely, by the LiBF4 crystallite and the solidliquid mixture of hydrogen fluoride in synthesis reactor, 30 are warming up to
DEG C, remove 80% anhydrous hydrogen fluoride medium, concentrating low-temperature alternating temperature stationary crystallization is simultaneously filtrated to get the substandard products of LiBF4 one
10.6kg, take 100kg ethyl acetate to dissolve the substandard products of LiBF4 one, LiBF4 finished product 10.3kg obtained after purification,
Yield 95%.After after testing, finished product purity is 99.9%, moisture 18ppm.
By can be seen that in above-described embodiment use the present invention preparation method prepare LiBF4 yield 95% with
On, for finished product purity more than 99.8%, moisture is less than 18ppm, and final product quality batch is stable, purity is high.
Part is not described in detail by the present invention, is the known technology of those skilled in the art.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
- A kind of 1. method of Rheological Phase Method synthesis LiBF4, it is characterised in that comprise the following steps：（1）Under inert gas shielding, high-purity lithium fluoride solid is added into anhydrous liquid hydrogen fluoride, it is agitated to be modulated into stream Variant；（2）Boron trichloride gas are passed through into anhydrous liquid hydrogen fluoride, reaction obtains boron triflouride gas；（3）By step（2）The middle obtained boron triflouride gas that reacts is passed into step（1）In obtained lithium fluoride-anhydrous fluorination In hydrogen rheological body, reaction obtains the solidliquid mixture of LiBF4 crystallite and hydrogen fluoride；（4）Will（3）In the solidliquid mixture of obtained LiBF4 crystallite and hydrogen fluoride be warming up to 30-40 DEG C, remove 80% Anhydrous hydrogen fluoride medium, then low temperature crystallization is carried out, the substandard products of LiBF4 one are obtained, while anhydrous hydrogen fluoride is collected, it can follow Ring is used in dissolving high-purity lithium fluoride solid；（5）LiBF4 finished product is obtained using the organic solvent purification substandard products of LiBF4 one.
- 2. the method for a kind of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that described is lazy Property gas from nitrogen, helium, argon gas, one kind in xenon.
- A kind of 3. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（1） In, the mass fraction of lithium fluoride is 1-2% in described rheological body.
- A kind of 4. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（1） In, described high-purity lithium fluoride solid is more than 99.5% battery-grade lithium fluoride solid powder from purity.
- A kind of 5. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（1） In, described stirring modulated process needs to stir more than 40min.
- A kind of 6. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（2） In, it is 5-15 DEG C in temperature, pressure is passed through boron trichloride gas into anhydrous liquid hydrogen fluoride under conditions of being 50-100KPa.
- A kind of 7. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（3） In, reaction temperature is 5-15 DEG C.
- A kind of 8. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（4） In, described low temperature crystallization is Cryogenic Temperature Swing stationary crystallization, and temperature range is 15~-40 DEG C, is cooled 3-5 DEG C per hour.
- A kind of 9. method of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that step（5） In, described organic solvent is from ethyl acetate, propene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate It is a kind of.
- 10. the method for a kind of Rheological Phase Method synthesis LiBF4 according to claim 1, it is characterised in that in step （5）Described in purification include dissolving, concentration, recrystallization, filtering, vacuum drying.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110774A (en) * | 2018-10-25 | 2019-01-01 | 河南省法恩莱特新能源科技有限公司 | A kind of preparation method of LiBF4 |
| CN109659608A (en) * | 2018-11-16 | 2019-04-19 | 湖北锂诺新能源科技有限公司 | A kind of preparation method and application of tetrafluoro lithium aluminate |
| CN112480153A (en) * | 2019-09-12 | 2021-03-12 | 多氟多化工股份有限公司 | Preparation method of lithium difluoroborate |
| CN113912075A (en) * | 2021-11-25 | 2022-01-11 | 山东中顼技术研究有限公司 | Preparation method of lithium tetrafluoroborate |
| CN116041377A (en) * | 2022-12-31 | 2023-05-02 | 九江天赐高新材料有限公司 | Method for co-producing lithium tetrafluoroborate and lithium bisfluooxalate borate based on rheological phase reaction and lithium salt |
| CN116462205A (en) * | 2023-03-29 | 2023-07-21 | 宜春国轩电池有限公司 | Synthesis method of lithium tetrafluoroborate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291347A (en) * | 2014-02-17 | 2015-01-21 | 多氟多化工股份有限公司 | Preparation method of lithium tetrafluoroborate |
| CN105293512A (en) * | 2014-11-11 | 2016-02-03 | 汕头市金光高科有限公司 | Direct synthesis method of lithium tetrafluoroborate |
| CN105883840A (en) * | 2014-09-10 | 2016-08-24 | 常德市金佰特节能环保科技有限公司 | Method for producing boron fluoride and hydrochloric acid from boron mud waste liquid |
-
2017
- 2017-10-13 CN CN201710949506.0A patent/CN107585776A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291347A (en) * | 2014-02-17 | 2015-01-21 | 多氟多化工股份有限公司 | Preparation method of lithium tetrafluoroborate |
| CN105883840A (en) * | 2014-09-10 | 2016-08-24 | 常德市金佰特节能环保科技有限公司 | Method for producing boron fluoride and hydrochloric acid from boron mud waste liquid |
| CN105293512A (en) * | 2014-11-11 | 2016-02-03 | 汕头市金光高科有限公司 | Direct synthesis method of lithium tetrafluoroborate |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110774A (en) * | 2018-10-25 | 2019-01-01 | 河南省法恩莱特新能源科技有限公司 | A kind of preparation method of LiBF4 |
| CN109110774B (en) * | 2018-10-25 | 2022-02-01 | 河南省法恩莱特新能源科技有限公司 | Preparation method of lithium tetrafluoroborate |
| CN109659608A (en) * | 2018-11-16 | 2019-04-19 | 湖北锂诺新能源科技有限公司 | A kind of preparation method and application of tetrafluoro lithium aluminate |
| CN112480153A (en) * | 2019-09-12 | 2021-03-12 | 多氟多化工股份有限公司 | Preparation method of lithium difluoroborate |
| CN112480153B (en) * | 2019-09-12 | 2023-10-31 | 多氟多新材料股份有限公司 | Preparation method of lithium difluoro oxalate borate |
| CN113912075A (en) * | 2021-11-25 | 2022-01-11 | 山东中顼技术研究有限公司 | Preparation method of lithium tetrafluoroborate |
| CN116041377A (en) * | 2022-12-31 | 2023-05-02 | 九江天赐高新材料有限公司 | Method for co-producing lithium tetrafluoroborate and lithium bisfluooxalate borate based on rheological phase reaction and lithium salt |
| CN116041377B (en) * | 2022-12-31 | 2023-10-20 | 九江天赐高新材料有限公司 | Method for co-producing lithium tetrafluoroborate and lithium bisfluooxalate borate based on rheological phase reaction and lithium salt |
| CN116462205A (en) * | 2023-03-29 | 2023-07-21 | 宜春国轩电池有限公司 | Synthesis method of lithium tetrafluoroborate |
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