CN108751234A - A kind of method of purification of lithium fluoride - Google Patents
A kind of method of purification of lithium fluoride Download PDFInfo
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- CN108751234A CN108751234A CN201810699570.2A CN201810699570A CN108751234A CN 108751234 A CN108751234 A CN 108751234A CN 201810699570 A CN201810699570 A CN 201810699570A CN 108751234 A CN108751234 A CN 108751234A
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- lithium
- lithium fluoride
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- fluoride
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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
- C01D15/04—Halides
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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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- 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
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a kind of methods of purification of lithium fluoride, include the following steps：S1 provides the lithium salt mixture of lithium carbonate containing, lithium fluoride and difluorophosphate；Carbonic acid fluorine and/or trifluoro-acetic fluoride are passed through the acidic aqueous solution that pH < 4 are formed in water by S2；The lithium salt mixture is added in the acidic aqueous solution, is stirred to react by S3, is separated by solid-liquid separation, and then carries out pure water, detaches, dries again, packing, obtains product lithium fluoride.The advantages that lithium fluoride method of purification of the present invention is more excellent, has product purity height, simple for process easy to operate, and reaction process is mildly controllable, environmental protection and saving, reduction production cost.
Description
Technical field
The present invention relates to lithium fluoride preparation, specially a kind of method of purification of lithium fluoride.
Background technology
Lithium metal belongs to novel energy goods and materials, " important element for pushing the world to advance " is known as, in recent years, electronic
Automobile, energy storage, etc. fields application it is further extensive.As the whole world is to the surging of clean energy resource demand, lithium strategic position highlights, fluorination
Lithium is a kind of important lithium basic material, is to prepare other salts chemical combination such as lithium-ion battery electrolytes solute lithium hexafluoro phosphate
The important source material of object, in addition lithium fluoride be also widely used in ceramic industry reduce kiln temperature and improve thermal shock resistance, abrasion
Property and sour corrosion, can act as the fluxing agent etc. that metal welding connects with other fluorides, chloride and borate one.
In the prior art, a kind of preparation method about battery-grade lithium fluoride, the weight that party's normal direction has configured are disclosed
It is passed through CO in the lithium carbonate slurry that percent concentration is 5~30%2After be prepared into lithia water, then be saturated with ammonium fluoride molten
Liquid carries out reaction and prepares battery-grade lithium fluoride, and the ammonia that generation is reacted in said program needs to recycle.Meanwhile prior art side
Case requires material quality high, and usually slurry corrodes equipment into centrifuge very big, and it is exceeded to easily cause very much product iron ion,
In addition, ceaselessly solid has reached required pH value in pure water elution centrifuge, effect is poor, and consumption is big, and production cost is high.
Invention content
The technical problem to be solved by the present invention is to be directed to existing prepare in lithium fluoride technology to raw material requirement height, production
The problems such as cost is big, preparation process is complicated, equipment requirement is high, purification difficulty is big provides a kind of lithium fluoride purification of economical and efficient
Method.
Specifically, the present invention can be achieved through the following technical solutions：
A kind of method of purification of lithium fluoride, includes the following steps：
S1 provides the lithium salt mixture of lithium carbonate containing, lithium fluoride and difluorophosphate；
Carbonic acid fluorine and/or trifluoro-acetic fluoride are passed through the acidic aqueous solution that pH < 4 are formed in water by S2；
The lithium salt mixture is added in the acidic aqueous solution, is stirred to react by S3, is separated by solid-liquid separation, then carries out pure water
It washs, detaches, dries again, packing, obtain product lithium fluoride.
For lithium salt mixture of the present invention with sour reaction process, charging sequence influences quite the final product quality obtained after reaction
Greatly, if being first added to the water solid matter, it is being passed through sour gas, stirring is uneven, and it is incomplete to be likely to result in local reaction, shadow
Ring the main content of product；Same lithium salt mixture is added at one time equally can cause local reaction incomplete too much, be slowly added to lithium
Salt mixture makes it fully be reacted in acidic aqueous solution, and entire reaction process carries out under constant temperature, have controllability and
Reaction is mild.
And the method for purification of lithium fluoride of the present invention is to reacting the lithium salt mixture containing lithium fluoride in acid condition, and
Pure water is carried out again after separation of solid and liquid to detach again, will be water-soluble in impurity further dissolve, then detach, heating is dried
Dry, packaging can be obtained high-purity lithium fluoride, and processing step is simple, can be easily separated, and entire reaction process uncontaminated gases production
It is raw, it is environmentally protective.
Further, lithium carbonate and difluorophosphate amount to content 1%~50%, fluorination in lithium salt mixture described in step S1
Lithium 50%~99%, preferably lithium carbonate 10%~20%, lithium fluoride 80%~90%, difluorophosphate 0~5%.The present invention can purify content
For the lithium salt mixture of 50%~99% lithium fluoride, when lithium fluoride 80%~90% in lithium salt mixture, refining effect is best.Due to
Lithium carbonate is not soluble in water, solid-liquid it is heterogeneous it is more difficult the reaction was complete, and in method provided by the invention, by above-mentioned carbonic acid fluorine and/or
Trifluoro-acetic fluoride is passed through the specific acidic aqueous solution formed in water and is reacted with the lithium salt mixture of special component, is being fluorinated
Lithium and/or difluorophosphate exist and in the environment of above-mentioned specific acid reactant aqueous solution, lithium carbonate not soluble in water can have
Effect react, and it is not necessary that lithium carbonate is first carried out reaction dissolving, effectively raises the reaction of lithium carbonate in aqueous solution and lives
Property, so that lithium carbonate reaction is generated lithium fluoride, to improve the purity of lithium fluoride after processing.
Further, acidic aqueous solution described in step S2 also can be the hydrogen fluoride solution of pH < 4.Acidic aqueous solution pH value is small
Accelerate reaction rate in 4, keeps raw material reaction more abundant, and new as the avoidable introducing of reaction dissolvent using hydrogen fluoride solution
Impurity.
Further, it is 50~2000g/h that the acidic aqueous solution medium velocity, which is added, in lithium salt mixture described in step S3.Control
Speed is added in lithium salt mixture processed, if addition is too fast, lithium salt mixture, which is easy localized clusters, to be caused to react insufficient, if being added
It is slow to extend reaction duration, reduce reaction efficiency.
Further, it is 10~80 DEG C of reaction temperature that condition is stirred to react described in step S3, and the reaction time is 1~8 hour.
It is stirred to react the time according to reaction temperature control, fluorination lithium mixture can be fully obtained by the reaction in lithium salt mixture, and reaction temperature is low
Extend reaction duration in 10 DEG C, reduce reaction efficiency, reaction temperature causes reaction excessively fierce higher than 80 DEG C, easy tos produce by-product
Object reduces the purity of finished product；Persistently stirring ensures to come into full contact between reactant in reaction process, ensures that the reaction was complete, instead
It answers temperature low time delay length to be stirred to react duration to 8 hours, ensures that the reaction was complete, can shorten being stirred to react the time when reaction temperature is high
To 1 hour, avoided the reaction of long-time high-temperature stirring from generating lithium fluoride under excessive by-product and hot conditions and be easy to decompose, reduced
Yield.
Further, it is separated by solid-liquid separation described in step S3 in selection filtering, precipitation or horizontal type screw settling centrifuge separation
One or more combinations.It can guarantee that the lithium fluoride being prepared is sufficiently separated using multiple combinations solid-liquid separation method, improve
Yield.
Further, by reaction system adjusting pH value to 6.5~7.5, the reaction before being separated by solid-liquid separation described in step S3
System is added lithium hydroxide or adds water gradient sedimentation.Reaction system adjusts pH value to being separated by solid-liquid separation again after 6.5~7.5, can
Avoid because of solution acidic deep-etching separation equipment, while reducing the introducing of other metal ions in equipment, so as to get lithium fluoride
Purity is high, and other metals content impurities are below 50ppm.Lithium hydroxide is added and adjusts the avoidable new impurity of introducing of reaction system,
Or add water gradient sedimentation, stratification is stirred after water is added, water stirring is added after upper solution is discharged and is stood, is operated repeatedly
To pH value of reaction system to 6.5~7.5, water-solubility impurity can be dissolved and be removed.
Further, heating, drying method described in step S3 is decompression gradient-heated processing method, with 1~2 DEG C/min
Heating rate 5~10min of heating, then stops 120~180min, repeats above-mentioned temperature-rise period, until the maximum temperature that heats up
To 120~200 DEG C.Gradually low boiling impurity, high-boiling-point impurity and solvent can be removed using the drying of decompression gradient-heated, ensured
It obtains fully dry being in powdered lithium fluoride, can avoid direct high temperature drying causes lithium fluoride to lump, and ensures product quality.
Further, the lithium salt mixture is prepared with the following method：
Lithium hexafluoro phosphate is dissolved in nonaqueous solvents by S'1；
Lithium carbonate is added under 120~200r/min stirring conditions in S'2；
S'3, the solidliquid mixture having to step S'2 reactions realize separation of solid and liquid by modes such as filtering, precipitation or centrifugations,
It is molten to obtain the non-aqueous solvent system containing lithium fluoride, the solid material of carbonic acid lithium mixture and the material of hybrid solid containing difluorophosphate
Liquid；
S'4 is dried in vacuo drying to above-mentioned solid material and removes organic component to get lithium salt mixture.
Lithium salt mixture preparation process is simple, and can be needed to select self-control or outsourcing according to the method described above according to production,
The by-product in difluorophosphate production process also can be selected, the product purity being prepared is high, and the other impurities of introducing are few.
Further, product fluorination lithium content is 99.5% or more, foreign metal ion content be 50ppm hereinafter,
Na, K, Ca, Fe content are 10ppm or less.The lithium fluoride purity handled by above-mentioned purification step is high, and foreign metal
Ion introduction volume is few, can be widely applied to the emerging industries such as new energy, new material field.
The preparation method of high-purity lithium fluoride of the present invention has following advantageous effect：
The first, preparation method is more excellent, and product purity is high；Reaction condition of the present invention is mild, reduces in reaction process and generates by-product,
Adjust pH value to being separated by solid-liquid separation again after 6.5~7.5 by adjusting reaction system after the completion of reaction, avoid acid ion with from
The contact of heart equipment introduces metal impurities, and gained lithium fluoride wet product is by pure water, then detaches, further will be water-soluble miscellaneous
Matter removes, and the lithium fluoride purity being prepared can reach 99.5% or more, and foreign metal ion content is 50ppm hereinafter, wherein
Na, K, Ca, Fe etc. are within 10ppm；
The second, simple for process easy to operate；The present invention is mainly completed by three step process step, and operating process is routine operation, and
It is generated without waste water,waste gas and industrial residue in entire technical process, wherein fluorine-containing acid solution recoverable, is suitble to industrialized production；
Third, reaction process are mildly controllable；The entire reaction process controlling reaction temperature of the present invention and reaction time, by reaction system
PH value is adjusted to 6.5~7.0 reduction equipment rates of corrosion, impurity is removed using mode of washing and passes through and depressurize gradient-heated drying
Product avoids the dry influence to product quality that rapidly heats up, and the mild condition of entire reaction process is controllable, and it is dangerous to reduce production
Property；
4th, environmental protection and saving reduces production cost；The entire reaction process of the present invention is generated without exhaust gas, and the acid after separation of solid and liquid
Property aqueous solution can be with Recycling, environmental protection and saving substantially reduces production cost, has good economic value and social valence
Value.
Specific implementation mode
In order that those skilled in the art will better understand the technical solution of the present invention, with reference to embodiment to this hair
It is bright to be described in further detail.
Embodiment 1
The present embodiment is used to illustrate the method for purification of lithium fluoride disclosed by the invention.
In PE reaction kettles of the 3L with stirring, under room temperature, pure water 2L is added, 40% aqueous hydrogen fluoride solution 120g is added,
Stirring is opened, by-product lithium salt mixture 500g (mass fraction lithium carbonate 14.5%, the fluorine for preparing difluorophosphate are slowly added into
Change lithium 82.1%, difluorophosphate 3.4%), it is stirred to react, is added and finishes in 2h, system pH is detected as 1.42, stops stirring,
4h is stood, solid-liquid layering is apparent, pours out supernatant liquor, collects barrelling, supplements new pure water 1.5L, this reciprocal operation 3 times, system
PH value is detected as 7.50, is injected into 5L stainless steel pressure filters and carries out press filtration, and filter sizes are 0.25 μm.Obtain paste lithium fluoride
Then solid wet feed 705g is stopped 120~180min, is repeated above-mentioned with 1~2 DEG C/min heating rates, 5~10min of heating
Temperature-rise period after standing vacuum drying 4h, obtains white small blocks of solid 460g, after testing until being warming up to 120 DEG C of maximum temperature
Product water score value 800ppm, fluorination lithium content 99.6% (anion chromatographic quantitative analysis), is computed lithium fluoride and prepares product yield
About 98.8%.
Embodiment 2
The present embodiment is used to illustrate the method for purification of lithium fluoride disclosed by the invention.
In PE reaction kettles of the 3L with stirring, under room temperature, the carbonyl fluoride tail gas absorber aqueous solution for being derived from production is added
2.5L, pH value is 0.83 after testing, opens stirring, is slowly added into the by-product lithium salt mixture 500g for preparing difluorophosphate
(mass fraction lithium carbonate 11.5%, lithium fluoride 83.9%, difluorophosphate 4.6%), is stirred to react, is added dropwise in 2h, system pH
Value is detected as 2.58, stops stirring, stands 4h, solid-liquid layering is apparent, pours out supernatant liquor, collects barrelling, supplements new pure water
2.0L, this reciprocal operation 4 times, system pH is detected as 6.96, is injected into 5L stainless steel pressure filters and carries out press filtration, filter hole
Diameter is 0.25 μm.Paste lithium fluoride solid wet feed 745g is obtained, with 1~2 DEG C/min heating rates, 5~10min of heating, is then stopped
120~180min repeats above-mentioned temperature-rise period, until being warming up to 150 DEG C of maximum temperature, after standing vacuum drying 4h, obtains white
The small blocks of solid 455g of color, product water score value 280ppm, is fluorinated lithium content 99.5% (anion chromatographic quantitative analysis) after testing,
It is computed lithium fluoride and prepares product yield about 97.8%.
Embodiment 3
The present embodiment is used to illustrate the method for purification of lithium fluoride disclosed by the invention.
In PE reaction kettles of the 3L with stirring, under room temperature, the trifluoro-acetic fluoride tail gas absorber water for being derived from production is added
Solution 2.5L, pH value is 0.45 after testing, opens stirring, lithium salt mixture is prepared as follows：S'1, by lithium hexafluoro phosphate
It is dissolved in nonaqueous solvents；Lithium carbonate is added under 120~200r/min stirring conditions in S'2；S'3 has step S'2 reactions
Obtained solidliquid mixture realizes separation of solid and liquid by modes such as filtering, precipitation or centrifugations, obtains mixing containing lithium fluoride, lithium carbonate
The non-aqueous solvent system solution of the solid material of object and the material of hybrid solid containing difluorophosphate；S'4, it is dry to above-mentioned solid material vacuum
Dry drying removes organic component to get mass fraction lithium carbonate 11.5%, lithium fluoride 83.9%, and the lithium salts of difluorophosphate 4.6% is mixed
Object is closed, lithium salt mixture 400g is slowly added into, is stirred to react, be added dropwise in 2h, system pH is detected as 1.38, stops stirring
It mixes, stands 4h, solid-liquid layering is apparent, pours out supernatant liquor, collects barrelling, supplements new pure water 2.0L, this reciprocal operation 4 times,
System pH is detected as 6.96, is injected into 5L stainless steel pressure filters and carries out press filtration, and filter sizes are 0.25 μm, obtain paste fluorine
Change lithium solid wet feed 685g, with 1~2 DEG C/min heating rates, 5~10min of heating, then stops 120~180min, repeat
Above-mentioned temperature-rise period obtains white powdery solids until being warming up to 120 DEG C of maximum temperature after decompression rotary evaporation dries 4h
350g, product water score value 183ppm, fluorination lithium content 99.8% (anion chromatographic quantitative analysis) are computed lithium fluoride after testing
Product yield is prepared about 94.3%.
Embodiment 4
The present embodiment is used to illustrate the method for purification of lithium fluoride disclosed by the invention.
In PE reaction kettles of the 1000L with stirring, under room temperature, the tail gas being derived from difluorophosphate production process is added
Absorption tower aqueous solution 800L, pH value is 2.23 (the fluorine-containing spent acid predominantly decomposed in production process) after testing, opens stirring, slowly
Slow dropwise addition prepares by-product solid slag 200Kg (mass fraction lithium carbonate 5.0%, lithium fluoride 93.9%, the difluorophosphoric acid of difluorophosphate
Lithium 1.1%), it is stirred to react, is added dropwise in 3h, system pH is detected as 2.68, stops stirring, stands 4h, and solid-liquid layering is bright
It is aobvious, it extracts supernatant liquor out, collects barrelling, supplement new pure water 600L, this reciprocal operation 3 times, system pH is detected as 6.56, adopts
It is separated by solid-liquid separation with the bedroom screw settling formula centrifuge of 316 materials, 3500r/min is arranged in the speed of mainshaft, and speed difference is than setting
17,40min centrifugations finish, and solid fluorinated lithium wet feed is heated up into drying in 316 stainless steel ribbon kettles of 500L with 1~2 DEG C/min
Rate 5~10min of heating, then stops 120~180min, above-mentioned temperature-rise period is repeated, until being warming up to maximum temperature 150
DEG C, stirring is opened, after being dried in vacuo 4h, obtains white powdery solids 160Kg, after testing product water score value 300ppm, lithium fluoride
Content 99.6% (anion chromatographic quantitative analysis), is computed lithium fluoride and prepares product yield about 82.4%.
The results are shown in table below for the preparation-obtained lithium fluoride metal impurities ion of above-described embodiment and yield：
| Metal impurities ion（ppm） | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Al | 3.14 | 0.24 | 4.21 | 1.78 |
| Ba | 0.72 | 0.22 | 2.22 | 5.03 |
| Ca | ND | 3.06 | 0.06 | 0.73 |
| Cd | ND | 0.01 | ND | ND |
| Co | 0.06 | 0.02 | ND | ND |
| Cr | 2.22 | 1.82 | 0.82 | 1.11 |
| Cu | ND | 0.02 | ND | ND |
| Fe | 4.26 | 1.65 | 3.654 | 4.76 |
| K | 3.11 | 1.11 | 0.11 | 1.95 |
| Mg | 2.04 | 0.56 | 0.16 | 0.93 |
| Mn | 0.24 | 0.14 | 0.34 | 0.39 |
| Na | 5.73 | 3.73 | 8.73 | ND |
| Ni | 1.47 | 0.15 | 1.85 | 1.51 |
| Pb | ND | 0.01 | 2.01 | 0.54 |
| Zn | 0.36 | 0.06 | 3.06 | 4.43 |
| Content（%） | 99.6 | 99.5 | 99.8 | 99.6 |
From above-described embodiment as can be seen that metal contained by the lithium fluoride that lithium fluoride method of purification provided by the invention is handled from
Sub- impurity is below 10ppm, and is fluorinated lithium content and is not less than 99.5%, illustrates that the present invention can effectively purify acquisition high-purity fluorine
Change lithium.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form；It is all
The those of ordinary skill of the industry can implement the present invention by the above and swimmingly；But all technologies for being familiar with this profession
Personnel without departing from the scope of the present invention, a little change for being made using disclosed above technology contents,
Modification and the equivalent variations developed, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals according to the present invention are to above
The variation, modification and evolution etc. of any equivalent variations made by embodiment still fall within the protection model of technical scheme of the present invention
Within enclosing.
Claims (9)
1. a kind of method of purification of lithium fluoride, it is characterised in that：Include the following steps：
S1 provides the lithium salt mixture of lithium carbonate containing, lithium fluoride and difluorophosphate；
Carbonic acid fluorine and/or trifluoro-acetic fluoride are passed through the acidic aqueous solution that pH < 4 are formed in water by S2；
The lithium salt mixture is added in the acidic aqueous solution, is stirred to react by S3, is separated by solid-liquid separation, then carries out pure water
It washs, detaches, dries again, packing, obtain product lithium fluoride.
2. a kind of method of purification of lithium fluoride according to claim 1, it is characterised in that：Lithium salt mixture described in step S1
Middle lithium carbonate and difluorophosphate amount to content 1%~50%, lithium fluoride 50%~99%, preferably lithium carbonate 10%~20%, lithium fluoride
80%~90%, difluorophosphate 0~5%.
3. a kind of method of purification of lithium fluoride according to claim 2, it is characterised in that：Lithium salt mixture described in step S3
It is 50~2000g/h that the acidic aqueous solution medium velocity, which is added,.
4. a kind of method of purification of lithium fluoride according to claim 3, it is characterised in that：It is stirred to react item described in step S3
Part is 10~80 DEG C of reaction temperature, and the reaction time is 1~8 hour.
5. a kind of method of purification of lithium fluoride according to claim 4, it is characterised in that：It is separated by solid-liquid separation described in step S3
One or more combinations in selection filtering, precipitation or horizontal type screw settling centrifuge separation.
6. a kind of method of purification of lithium fluoride according to claim 5, it is characterised in that：It is separated by solid-liquid separation described in step S3
Preceding that reaction system is adjusted pH value to 6.5~7.5, the reaction system is added lithium hydroxide or adds water gradient sedimentation.
7. a kind of method of purification of lithium fluoride according to claim 6, it is characterised in that：Heating, drying described in step S3
Method be decompression gradient-heated processing method, with 1~2 DEG C/min heating rates heat up 5~10min, then stop 120~
180min repeats above-mentioned temperature-rise period, until heating maximum temperature is to 120~200 DEG C.
8. a kind of method of purification of lithium fluoride according to any one of claims 1 to 7, it is characterised in that：The lithium salts is mixed
Object is closed to prepare with the following method：
Lithium hexafluoro phosphate is dissolved in nonaqueous solvents by S'1；
Lithium carbonate is added under 120~200r/min stirring conditions in S'2；
S'3, the solidliquid mixture having to step S'2 reactions realize separation of solid and liquid by modes such as filtering, precipitation or centrifugations,
It is molten to obtain the non-aqueous solvent system containing lithium fluoride, the solid material of carbonic acid lithium mixture and the material of hybrid solid containing difluorophosphate
Liquid；
S'4 is dried in vacuo drying to above-mentioned solid material and removes organic component to get lithium salt mixture.
9. a kind of method of purification of lithium fluoride according to claim 8, it is characterised in that：The product is fluorinated lithium content
99.5% or more, foreign metal ion content is 50ppm hereinafter, Na, K, Ca, Fe content are 10ppm or less.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498432A (en) * | 2019-09-11 | 2019-11-26 | 江苏容汇通用锂业股份有限公司 | A kind of method that mother liquor prepares battery-grade lithium fluoride |
| CN112551559A (en) * | 2020-12-31 | 2021-03-26 | 江西赣锋循环科技有限公司 | Preparation method of small-particle-size neutral lithium fluoride |
| CN112758904A (en) * | 2019-11-22 | 2021-05-07 | 多氟多化工股份有限公司 | Preparation method of lithium difluorophosphate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829910A (en) * | 2017-03-29 | 2017-06-13 | 东营石大胜华新能源有限公司 | A kind of preparation method of difluorophosphate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106829910A (en) * | 2017-03-29 | 2017-06-13 | 东营石大胜华新能源有限公司 | A kind of preparation method of difluorophosphate |
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| 于剑昆: ""高纯氟化锂的合成工艺进展"", 《无机盐工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498432A (en) * | 2019-09-11 | 2019-11-26 | 江苏容汇通用锂业股份有限公司 | A kind of method that mother liquor prepares battery-grade lithium fluoride |
| CN112758904A (en) * | 2019-11-22 | 2021-05-07 | 多氟多化工股份有限公司 | Preparation method of lithium difluorophosphate |
| CN112758904B (en) * | 2019-11-22 | 2022-12-02 | 多氟多新材料股份有限公司 | Preparation method of lithium difluorophosphate |
| CN112551559A (en) * | 2020-12-31 | 2021-03-26 | 江西赣锋循环科技有限公司 | Preparation method of small-particle-size neutral lithium fluoride |
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