CN108275702A - A kind of preparation method for the high-purity lithium fluoride producing lithium hexafluoro phosphate - Google Patents
A kind of preparation method for the high-purity lithium fluoride producing lithium hexafluoro phosphate Download PDFInfo
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- CN108275702A CN108275702A CN201711435252.7A CN201711435252A CN108275702A CN 108275702 A CN108275702 A CN 108275702A CN 201711435252 A CN201711435252 A CN 201711435252A CN 108275702 A CN108275702 A CN 108275702A
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- lithium fluoride
- lithium
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- hexafluoro phosphate
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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
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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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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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to the preparation methods of lithium fluoride, disclose a kind of preparation method for the high-purity lithium fluoride producing lithium hexafluoro phosphate, the method includes the steps of：1）Pure Lithium Carbonate or lithium hydroxide are added in hydrofluoric acid solution and reacted, lithium fluoride is precipitated, obtains lithium fluoride suspension；2）Lithium fluoride suspension is injected into crystallization kettle, crystallization kettle is warming up to 60 80 DEG C；3）Crystallization kettle is cooled to 10 20 DEG C again；4）Repeat step 2）With 3）After 15 times, lithium fluoride crystallite is obtained by filtration；5）Lithium fluoride crystallite is washed with deionized, up to high-purity lithium fluoride after drying.The present invention purifies lithium fluoride using dynamic crystallization principle, simple for process, easy to control, cost is relatively low, and product purity can reach 99.99% or more, and particle is smaller and particle diameter distribution is uniform, using effect is good, is a kind of high-purity lithium fluoride being suitable for producing lithium hexafluoro phosphate.
Description
Technical field
The present invention relates to the preparation method of lithium fluoride more particularly to a kind of high-purity lithium fluoride producing lithium hexafluoro phosphate
Preparation method.
Background technology
Lithium hexafluoro phosphate is most common electrolyte in current lithium ion battery, high comprehensive performance, at present hexafluorophosphoric acid
In the industrialized production of lithium, how to obtain the lithium hexafluoro phosphate of high-purity is critical issue, if the purity of lithium hexafluoro phosphate is not
It is up to standard, the internal resistance of cell will be caused to increase, battery capacity decaying is fast, and cycle life shortens, or even influences the safety of battery.Due to
The purification of lithium hexafluoro phosphate is extremely difficult, therefore prepares the raw material of lithium hexafluoro phosphate --- and the purity of lithium fluoride just seems heavy to closing
It has wanted.
Application No. is 201510714659.8 Chinese patents to disclose a kind of purification process of super-active lithium fluoride, leads to
It crosses ball milling removing Dendritic TiC and dry release cleans twice, between high low specific surface area is mutually converted, reach changing for microstructure
Become, but this method needs additionally to use a large amount of hydrofluoric acid solutions, and ball milling machine seriously corroded, cost is increased, and not
Conducive to environmental protection.
Invention content
In order to solve the above technical problem, the present invention provides a kind of high-purity lithium fluoride producing lithium hexafluoro phosphate
Preparation method purifies lithium fluoride using dynamic crystallization principle, and simple for process, easy to control, product purity is high, is that one kind being suitable for life
Produce the high-purity lithium fluoride of lithium hexafluoro phosphate.
The specific technical solution of the present invention is：The method includes the steps of：
1）Pure Lithium Carbonate or lithium hydroxide are added in hydrofluoric acid solution and reacted, lithium fluoride is precipitated, obtains lithium fluoride suspension；
2）Lithium fluoride suspension is injected into crystallization kettle, crystallization kettle is warming up to 60-80 DEG C；
3）Crystallization kettle is cooled to 10-20 DEG C again；
4）Repeat step 2）With 3）After 1-5 times, lithium fluoride crystallite is obtained by filtration；
5）Lithium fluoride crystallite is washed with deionized, up to high-purity lithium fluoride after drying.
After lithium carbonate or lithium hydroxide are reacted with hydrofluoric acid solution, lithium fluoride precipitation can quickly be precipitated, but in the precipitation
What the elements such as Fe, Ca, Zn, Mg, the Cr brought in impurity, including raw material or production equipment there are many containing generated after being reacted with HF
Metal fluoride further includes the HF that compound is formed with lithium fluoride, and after heating, the lithium fluoride precipitation surface of script can be molten again
Solution, due to impurity and the different solubility of lithium fluoride in a solution of hydrofluoric acid, during gradually heating up, impurity and fluorine
Changing lithium will not dissolve simultaneously, effectively separate impurity and lithium fluoride, and after cooling down again, lithium fluoride can be preferentially not complete
Fully dissolved grain surface is precipitated, this process is repeated several times, can obtain the lithium fluoride particle that purity more arrives.
Preferably, the step 1）A concentration of 10-30wt% of middle hydrofluoric acid solution.
Preferably, the step 1）The solid-liquid ratio of middle pure Lithium Carbonate or lithium hydroxide and hydrofluoric acid solution is 1:1.3-
1.5。
The ratio Ruo Taigao of HF can form a large amount of compounds with lithium fluoride, increase loss, if ratio is too low, be fluorinated
The solubility of lithium and impurity is inadequate, is unfavorable for purifying, and within the scope of the invention, is ensureing that lithium fluoride yield is higher simultaneously,
Also there can be preferable solubility.
Preferably, the step 2）Middle heating rate is 2-5 DEG C/min, and temperature-rise period needs mechanical agitation.
When heating, stirring can promote grain dissolution and diffusion, and impurity is precipitated again in particle surface when preventing from being precipitated.
Preferably, the step 2）Heat preservation 1-2h is needed after middle heating.
Preferably, the step 3）Middle rate of temperature fall is 0.1-2 DEG C/min, and temperature-fall period needs mechanical agitation.
Stirring can weaken the mass-and heat-transfer destabilizing factor that industrial enlarge-effect is brought, and can obtain of uniform particle sizes
Grain.
Preferably, the step 3）Heat preservation 0.5-1h is needed after middle cooling.
Preferably, the step 5）Middle drying is vacuum drying, and temperature is 80-120 DEG C.
It is compared with the prior art, the beneficial effects of the invention are as follows：The present invention purifies lithium fluoride, work using dynamic crystallization principle
Skill is simple, easy to control, and cost is relatively low, and product purity can reach 99.99% or more, and particle is smaller and particle diameter distribution is uniform, makes
It is good with effect, it is a kind of high-purity lithium fluoride being suitable for producing lithium hexafluoro phosphate.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
Pure Lithium Carbonate or lithium hydroxide are pressed into solid-liquid ratio 1:It reacts, is precipitated in the hydrofluoric acid solution of 1.5 a concentration of 10wt% of addition
Lithium fluoride obtains lithium fluoride suspension；Lithium fluoride suspension is injected into crystallization kettle, crystallization kettle is by heating rate 5 DEG C/min heatings
To 80 DEG C, 1h is kept the temperature；Crystallization kettle is cooled to 15 DEG C by 1 DEG C/min of rate of temperature fall again, keeps the temperature 0.8h；Repeat heating and cooling 3
After secondary, lithium fluoride crystallite is obtained by filtration；Lithium fluoride crystallite is washed with deionized, up to high-purity fluorine after 120 DEG C of vacuum drying
Change lithium, the lithium fluoride rate of recovery is 90%, purity 99.99%.
Embodiment 2
Pure Lithium Carbonate or lithium hydroxide are pressed into solid-liquid ratio 1:It reacts, is precipitated in the hydrofluoric acid solution of 1.3 a concentration of 30wt% of addition
Lithium fluoride obtains lithium fluoride suspension；Lithium fluoride suspension is injected into crystallization kettle, crystallization kettle is by heating rate 2 DEG C/min heatings
To 60 DEG C, 2h is kept the temperature；Crystallization kettle is cooled to 20 DEG C by 0.1 DEG C/min of rate of temperature fall again, keeps the temperature 0.5h；It repeats to heat up and cool down
After 4 times, lithium fluoride crystallite is obtained by filtration；Lithium fluoride crystallite is washed with deionized, up to high-purity fluorine after 80 DEG C of vacuum drying
Change lithium, the lithium fluoride rate of recovery is 92%, purity 99.99%.
Embodiment 3
Pure Lithium Carbonate or lithium hydroxide are pressed into solid-liquid ratio 1:It reacts, is precipitated in the hydrofluoric acid solution of 1.4 a concentration of 20wt% of addition
Lithium fluoride obtains lithium fluoride suspension；Lithium fluoride suspension is injected into crystallization kettle, crystallization kettle is by heating rate 3 DEG C/min heatings
To 70 DEG C, 1.5h is kept the temperature；Crystallization kettle is cooled to 10 DEG C by 2 DEG C/min of rate of temperature fall again, keeps the temperature 1h；Repeat heating and cooling 5
After secondary, lithium fluoride crystallite is obtained by filtration；Lithium fluoride crystallite is washed with deionized, up to high-purity fluorine after 100 DEG C of vacuum drying
Change lithium, the lithium fluoride rate of recovery is 95%, purity 99.99%.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit still falls within the technology of the present invention side to any simple modification, change and equivalent transformation made by above example
The protection domain of case.
Claims (8)
1. a kind of preparation method for the high-purity lithium fluoride producing lithium hexafluoro phosphate, it is characterised in that：This method includes following
Step：
1）Pure Lithium Carbonate or lithium hydroxide are added in hydrofluoric acid solution and reacted, lithium fluoride is precipitated, obtains lithium fluoride suspension；
2）Lithium fluoride suspension is injected into crystallization kettle, crystallization kettle is warming up to 60-80 DEG C；
3）Crystallization kettle is cooled to 10-20 DEG C again；
4）Repeat step 2）With 3）After 1-5 times, lithium fluoride crystallite is obtained by filtration；
5）Lithium fluoride crystallite is washed with deionized, up to high-purity lithium fluoride after drying.
2. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate as described in claim 1, which is characterized in that institute
State step 1）A concentration of 10-20wt% of middle hydrofluoric acid solution.
3. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate, feature exist as claimed in claim 1 or 2
In the step 1）The solid-liquid ratio of middle pure Lithium Carbonate or lithium hydroxide and hydrofluoric acid solution is 1:1.3-1.5.
4. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate as described in claim 1, which is characterized in that institute
State step 2）Middle heating rate is 2-5 DEG C/min, and temperature-rise period needs mechanical agitation.
5. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate as described in claim 1 or 4, feature exist
In the step 2）Heat preservation 1-2h is needed after middle heating.
6. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate as described in claim 1, which is characterized in that institute
State step 3）Middle rate of temperature fall is 0.1-2 DEG C/min, and temperature-fall period needs mechanical agitation.
7. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate as described in claim 1 or 6, feature exist
In the step 3）Heat preservation 0.5-1h is needed after middle cooling.
8. the preparation method of the high-purity lithium fluoride of production lithium hexafluoro phosphate as described in claim 1, which is characterized in that institute
State step 5）Middle drying is vacuum drying, and temperature is 80-120 DEG C.
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| CN201711435252.7A CN108275702A (en) | 2017-12-26 | 2017-12-26 | A kind of preparation method for the high-purity lithium fluoride producing lithium hexafluoro phosphate |
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| CN201711435252.7A CN108275702A (en) | 2017-12-26 | 2017-12-26 | A kind of preparation method for the high-purity lithium fluoride producing lithium hexafluoro phosphate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570337A (en) * | 2008-04-28 | 2009-11-04 | 多氟多化工股份有限公司 | Production method of battery- grade lithium fluoride |
| CN101723413A (en) * | 2009-11-20 | 2010-06-09 | 江西赣锋锂业股份有限公司 | Method for preparing lithium fluoride |
| CN101723414A (en) * | 2009-12-11 | 2010-06-09 | 多氟多化工股份有限公司 | Method for producing battery-grade lithium fluoride |
| CN103449480A (en) * | 2013-08-30 | 2013-12-18 | 新疆有色金属研究所 | Battery-grade high-purity lithium fluoride and preparation method thereof |
-
2017
- 2017-12-26 CN CN201711435252.7A patent/CN108275702A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570337A (en) * | 2008-04-28 | 2009-11-04 | 多氟多化工股份有限公司 | Production method of battery- grade lithium fluoride |
| CN101723413A (en) * | 2009-11-20 | 2010-06-09 | 江西赣锋锂业股份有限公司 | Method for preparing lithium fluoride |
| CN101723414A (en) * | 2009-12-11 | 2010-06-09 | 多氟多化工股份有限公司 | Method for producing battery-grade lithium fluoride |
| CN103449480A (en) * | 2013-08-30 | 2013-12-18 | 新疆有色金属研究所 | Battery-grade high-purity lithium fluoride and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 于宝青等: "利用工业碳酸锂提纯制备高纯度氟化锂", 《创新技术》 * |
| 孟繁智: "《新编精细化工应用配方10000例与生产工艺实用手册》", 28 February 2004 * |
| 抚顺市教育学院教研部化学组: "《初中化学复习资料》", 31 January 1980 * |
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Application publication date: 20180713 |