CN108439362A - A kind of preparation method of high-end lithium hexafluoro phosphate - Google Patents
A kind of preparation method of high-end lithium hexafluoro phosphate Download PDFInfo
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- CN108439362A CN108439362A CN201810482302.5A CN201810482302A CN108439362A CN 108439362 A CN108439362 A CN 108439362A CN 201810482302 A CN201810482302 A CN 201810482302A CN 108439362 A CN108439362 A CN 108439362A
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- lithium
- 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
- C01D15/005—Lithium hexafluorophosphate
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Abstract
The invention discloses a kind of preparation methods of high-end lithium hexafluoro phosphate comprising (1) by distilling the hydrogen fluoride liquid for obtaining purity in 99.99wt% or more；(2), lithium fluoride input anhydrous liquid hydrogen fluoride is prepared into side reaction solution (3), phosphorus pentachloride is put into obtained high-end lithium hexafluorophosphate solution in the anhydrous hydrogen fluoride solution containing lithium fluoride；(4), high-end lithium hexafluorophosphate solution is filtered, filtrate is sent into partial crystallization slot, and lithium hexafluoro phosphate is precipitated, and filtering, mother liquor is sent into mother liquid tank, recycles；(5) high-end lithium hexafluoro phosphate product is obtained through primary drying and redrying.The preparation method of the high-end lithium hexafluoro phosphate, the present invention is safe and reliable, raw material is easy to get, easy to operate, obtains high-end lithium hexafluoro phosphate product purity 99.98% or more, moisture content is less than 10ppm, acid point is less than 50ppm, and insoluble point is less than 60ppm, and total metal is less than 1ppm, the production requirement for meeting lithium ion battery meets electric automobile market demand.
Description
Technical field
The present invention relates to high-end lithium hexafluoro phosphate preparing technical field, specially a kind of preparation of high-end lithium hexafluoro phosphate
Method.
Background technology
Lithium ion battery is high with operating voltage, energy density big (light-weight), self-discharge rate is low, memory-less effect, follows
Ring long lifespan and it is pollution-free outstanding advantages of.In recent years, many has been captured rapidly with the incomparable advantage of other batteries
Field is widely used in the products such as well known mobile phone, laptop, electric bicycle, electric vehicle.With
The industrialization of electric vehicle, the dosage of lithium ion battery is bound to increasing.Using showing that lithium ion battery is a kind of reason
The small-sized green power supply thought.
Important electrolytic salt of the lithium hexafluoro phosphate as lithium-ion battery electrolytes, it is desirable that it has very high purity (logical
Often otherwise it is less than 99.5%), impurity therein such as moisture content, alkali metal, heavy metal and other impurity such as PCl3 and POCl3
Content must be strictly controlled, otherwise the internal resistance of cell will be caused to increase, battery capacity decaying is fast, and cycle life shortens or even shadow
Ring the safety of battery.The high-end lithium hexafluoro phosphate product for obtaining the objectionable impurities of high-purity and low content is of great significance.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, it the present invention provides a kind of preparation method of high-end lithium hexafluoro phosphate, solves and leads
The cause internal resistance of cell increases, and battery capacity decaying is fast, and cycle life shortens, or even the problem of influence battery security.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs：A kind of system of high-end lithium hexafluoro phosphate
Preparation Method, which is characterized in that include the following steps：
Step 1: the preparation of high pure raw material：Anhydrous hydrogen fluoride is sent to destilling tower and is refined, vapo(u)rizing temperature control 20~
25 DEG C, the hydrogen fluoride gas steamed the anhydrous hydrogen fluoride liquid of obtained purity in 99.99wt% or more after condenser condenses
Body；The control of its moisture is in 10ppm hereinafter, metal ion control is in 10ppm or less；
Step 2: the preparation of side reaction solution：Lithium fluoride is put into the secondary reacting kettle of anhydrous liquid hydrogen fluoride, it will be warm
Between -10 DEG C~0 DEG C, pressure controls between 0.1Mpa~0.15Mpa for degree control.It prepares and completes to be sent into main reaction kettle；
Step 3: the preparation of high-end lithium hexafluoro phosphate：Phosphorus pentachloride is added in the main reaction kettle of side reaction solution,
Between temperature controls 0 DEG C~50 DEG C, pressure controls between 0.5Mpa~0.8Mpa, and it is molten to obtain lithium hexafluoro phosphate for synthetic reaction
Liquid, anhydrous hydrogen fluoride, lithium fluoride, phosphorus pentachloride, and lithium hexafluorophosphate solution, anhydrous hydrogen fluoride, lithium fluoride, phosphorus pentachloride
It feeds intake according to a certain percentage, the condensed recovery system of acid tail gas that synthetic reaction generates handles to obtain by-product hydrochloric acid；
Step 4: Crystallization Separation process：Lithium hexafluorophosphate solution obtained by step 3 is removed not by high-precision filter
Solubility impurity, filtrate are sent into crystallization tank, are cooled to -80 DEG C hereinafter, high-end lithium hexafluoro phosphate is made to crystallize out, filtering obtains height
Hold hexafluorophosphoric acid crystalline lithium；
Step 5: refining step：Primary drying, removal residual acid point are carried out at 25 DEG C~50 DEG C of temperature, then are divided
Grade screening obtains the consistent high-end hexafluorophosphoric acid crystalline lithium of granular size, is carried out at 120 DEG C~140 DEG C of temperature secondary dry
It is dry, obtain high-end lithium hexafluoro phosphate product.
Preferably, in step 2, the anhydrous liquid hydrogen fluoride being related to is that hydrogen fluoride gas process is steamed in step 1
Condenser condensation generates.
Preferably, in step 3, lithium hexafluorophosphate solution, anhydrous hydrogen fluoride, lithium fluoride, phosphorus pentachloride feed intake weight
Amount is than being 1:0.12~0.22:1.12~1.22.
(3) advantageous effect
The present invention provides a kind of preparation methods of high-end lithium hexafluoro phosphate.Has following advantageous effect：The high-end hexafluoro
The preparation method of lithium phosphate, present invention process is simple, and raw material is easy to get, securely and reliably, the high-end lithium hexafluoro phosphate product yield of gained
Height, quality are high.Therefore, the present invention has good economic value and social value, application easy to spread.
(1), rectifying purifying is carried out to anhydrous hydrogen fluoride, obtains high-purity anhydrous hydrogen fluoride, moisture is controlled in 10ppm
Hereinafter, metal ion control is in 10ppm or less.
(2), prepared by side reaction solution, and amount of heat can be discharged in anhydrous hydrogen fluoride solution since lithium fluoride dissolves in, need pair
Secondary reacting kettle carry out cooling treatment, by temperature control between -10 DEG C~0 DEG C, pressure control 0.1Mpa~0.15Mpa it
Between.
(3), phosphorus pentachloride is added in side reaction solution, should be noted that rate is added in control, and need to be carried out to main reaction kettle
Cooling treatment, between temperature controls 0 DEG C~50 DEG C, pressure controls between 0.5Mpa~0.8Mpa, anhydrous hydrogen fluoride, fluorination
Lithium, phosphorus pentachloride charged material weight ratio be 1:0.12~0.22:1.12~1.22.
(4), it should be noted when crystallizing and be cooled to -80 DEG C hereinafter, high-end lithium hexafluoro phosphate is made to crystallize out, filtering obtains height
Hold hexafluorophosphoric acid crystalline lithium.
(5), refining step does not need the pulverizing process of tradition preparation, and entire refining step, which should be noted to use, is mainly
The gas of N2 carries out whole process protection.
(6), the mother liquor being separated by solid-liquid separation in present invention process can be recycled, the acid tail gas that synthetic reaction generates
Condensed recovery system handles to obtain by-product hydrochloric acid.With good environment protection significance.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment one
Technical problems based on background technology, the present invention provide a kind of technical solution：A kind of high-end lithium hexafluoro phosphate
Preparation method, include the following steps：
Step 1: the preparation of high-pure anhydrous hydrogen fluoride liquid：In closed steel lining fluorine plastic containers, in nitrogen protection
Lower addition 500kg anhydrous hydrogen fluorides, are heated by fluoroplastics reboiler, and temperature controls the hydrogen fluoride gas distilled out at 25 DEG C
It is condensed by condenser, condensation temperature is controlled at -15 DEG C, and condensation obtains the hydrogen fluoride liquid of high-purity.Distilling condensation time is
4 hours.
Step 2: the modulation of lithium fluoride solution：Hydrogen fluoride liquid 300kg obtained by step 1 is taken to be added to steel lining fluoroplastics
In reactor, then by 12 kg of high purity lithium fluoride of automatic charging equipment 99.9% or more purity of addition, it is sufficiently stirred, temperature control
Near 0 DEG C, pressure is controlled in 0.1Mpa system.
Step 3: the preparation of high-end lithium hexafluorophosphate solution：It is slowly added to 100kg phosphorus pentachlorides by automatic charging equipment
Solid enters step in two steel lining fluorine plastic reactor, using the cycle of pump, synthesis is made fully to be reacted, and obtains high-end
The solution of lithium hexafluoro phosphate.Temperature controls near 0 DEG C, and pressure is controlled in 0.6Mpa.The acid tail gas generated is reacted through supercooling
It is solidifying, hydrogen fluoride gas is recycled, hydrogen chloride gas becomes by-product hydrochloric acid through water absorption.
Step 4: the preparation of lithium hexafluoro phosphate product：High-end lithium hexafluorophosphate solution obtained by step 3 is moved into crystallization tank
Depth cooling is carried out, final temperature reaches -42 DEG C, by filter plant, collects mother liquor and enters steel lining fluorine plastics mother liquid tank,
Crystal stays in filter plant.
Step 5: crystal obtained by step 4, which is blown into N2, carries out primary drying, N2 flow controls are in 20ml/min, drying
Time is 0.5h.It is transferred to drying device after crystal is sieved again, carries out redrying, temperature is controlled at 130 DEG C, done
The dry time is 1h.
Step 6: finally obtaining high-end lithium hexafluoro phosphate product 66kg.It is 94%, by analysis, institute to calculate ultimate yield
The purity for obtaining product is 99.98%, free acid 42ppm, moisture 4.4ppm, insoluble matter 53ppm, and total metal is less than
1ppm is in domestic and international top standard.
Embodiment two
Technical problems based on background technology, the present invention provide a kind of technical solution：A kind of high-end lithium hexafluoro phosphate
Preparation method, include the following steps：
Step 1: the preparation of high-pure anhydrous hydrogen fluoride liquid：In closed steel lining fluorine plastic containers, in nitrogen protection
Lower addition 500kg anhydrous hydrogen fluorides, are heated by fluoroplastics reboiler, and temperature controls the hydrogen fluoride gas distilled out at 25 DEG C
It is condensed by condenser, condensation temperature is controlled at -15 DEG C, and condensation obtains the hydrogen fluoride liquid of high-purity.Distilling condensation time is
4 hours.
Step 2: the modulation of lithium fluoride solution：Hydrogen fluoride liquid 400kg obtained by step 1 is taken to be added to steel lining fluoroplastics
In reactor, then by 15 kg of high purity lithium fluoride of automatic charging equipment 99.9% or more purity of addition, it is sufficiently stirred, temperature control
Near 0 DEG C, pressure is controlled in 0.1Mpa system.
Step 3: the preparation of high-end lithium hexafluorophosphate solution：It is slowly added to 128kg phosphorus pentachlorides by automatic charging equipment
Solid enters step in two steel lining fluorine plastic reactor, using the cycle of pump, synthesis is made fully to be reacted, and obtains high-end
The solution of lithium hexafluoro phosphate.Temperature controls near 0 DEG C, and pressure is controlled in 0.6Mpa.The acid tail gas generated is reacted through supercooling
It is solidifying, hydrogen fluoride gas is recycled, hydrogen chloride gas becomes by-product hydrochloric acid through water absorption.
Step 4: the preparation of lithium hexafluoro phosphate product：High-end lithium hexafluorophosphate solution obtained by step 3 is moved into crystallization tank
Depth cooling is carried out, final temperature reaches -44 DEG C, by filter plant, collects mother liquor and enters steel lining fluorine plastics mother liquid tank,
Crystal stays in filter plant.
Step 5: crystal obtained by step 4, which is blown into N2, carries out primary drying, N2 flow controls are in 20ml/min, drying
Time is 0.5h.It is transferred to drying device after crystal is sieved again, carries out redrying, temperature is controlled at 130 DEG C, done
The dry time is 1h.
Step 6: finally obtaining high-end lithium hexafluoro phosphate product 85kg.It is 97%, by analysis, institute to calculate ultimate yield
The purity for obtaining product is 99.98%, free acid 35ppm, moisture 2.8ppm, insoluble matter 50ppm, and total metal is less than
1ppm is in domestic and international top standard.
To sum up, preparation method of the present invention compared with prior art, has following advantage：
1, the addition of the raw material fluorinated lithium solid of present invention process, phosphorus pentachloride solid is to enter solution system, and reaction becomes
In mild, no high temperature risk, it is conducive to control, securely and reliably.
2, present invention process device therefor main material is steel lining plastic plastics, solves the problems, such as metal ion influence, is conducive to
The safety of lithium battery.
3, present invention process crystallographic is uniform, and no bulky grain is formed, and is not necessarily to pulverizing process, and yield improves, production cost
It reduces.
4, drying of the present invention process after high-end lithium hexafluoro phosphate is prepared, packaging overall process use nitrogen protection,
It avoids finished product from being hydrolyzed because absorbing moisture content, increases impurity.And the hydrogen chloride gas generated in the reaction can also take away part water
Point, to greatly reduce the moisture in mother liquor, production process.Control temperature in the reaction, pressure can effectively inhibit
The generation of side reaction, greatly improves product quality.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, without necessarily requiring or implying between these entities or operation
There are any actual relationship or orders.Moreover, the terms "include", "comprise" or its any other variant are intended to
Cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements includes not only that
A little elements, but also include other elements that are not explicitly listed, or further include for this process, method, article or
The intrinsic element of equipment.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited to
This, any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention
And its inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of preparation method of high-end lithium hexafluoro phosphate, which is characterized in that include the following steps：
Step 1: the preparation of high pure raw material：Anhydrous hydrogen fluoride to be sent to destilling tower and is refined, vapo(u)rizing temperature is controlled at 20~25 DEG C,
The hydrogen fluoride gas steamed the anhydrous liquid hydrogen fluoride of obtained purity in 99.99wt% or more after condenser condenses；Its water
Sub-control system is in 10ppm hereinafter, metal ion control is in 10ppm or less；
Step 2: the preparation of side reaction solution：Lithium fluoride is put into the secondary reacting kettle of anhydrous liquid hydrogen fluoride, temperature is controlled
Between -10 DEG C~0 DEG C, pressure controls between 0.1Mpa~0.15Mpa.It prepares and completes to be sent into main reaction kettle；
Step 3: the preparation of high-end lithium hexafluoro phosphate：Phosphorus pentachloride is added in the main reaction kettle of side reaction solution, temperature control
Between 0 DEG C~50 DEG C of system, pressure controls between 0.5Mpa~0.8Mpa, and synthetic reaction obtains lithium hexafluorophosphate solution, anhydrous
Hydrogen fluoride, lithium fluoride, phosphorus pentachloride, and lithium hexafluorophosphate solution, anhydrous hydrogen fluoride, lithium fluoride, phosphorus pentachloride are according to certain
Ratio feed intake, synthetic reaction generate the condensed recovery system of acid tail gas handle to obtain by-product hydrochloric acid；
Step 4: Crystallization Separation process：Lithium hexafluorophosphate solution obtained by step 3 is insoluble by high-precision filter removal
Impurity, filtrate are sent into crystallization tank, are cooled to -80 DEG C hereinafter, high-end lithium hexafluoro phosphate is made to crystallize out, filtering obtains high-end six
Lithium fluophosphate crystal；
Step 5: refining step：Primary drying, removal residual acid point are carried out at 25 DEG C~50 DEG C of temperature, then carry out classifying screen
Choosing obtains the consistent high-end hexafluorophosphoric acid crystalline lithium of granular size, carries out redrying at 120 DEG C~140 DEG C of temperature, obtains
High-end lithium hexafluoro phosphate product.
2. a kind of preparation method of high-end lithium hexafluoro phosphate according to claim 1, it is characterised in that：In step 2,
The anhydrous liquid hydrogen fluoride being related to is to steam hydrogen fluoride gas in step 1 to generate by condenser condensation.
3. a kind of preparation method of high-end lithium hexafluoro phosphate according to claim 1, it is characterised in that：In step 3,
Lithium hexafluorophosphate solution, anhydrous hydrogen fluoride, lithium fluoride, phosphorus pentachloride charged material weight ratio be 1:0.12~0.22:1.12~
1.22。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110690503A (en) * | 2019-12-10 | 2020-01-14 | 中化蓝天集团有限公司 | High-stability fluorine-containing electrolyte and lithium ion battery |
| CN113321228A (en) * | 2021-06-11 | 2021-08-31 | 厚成科技（南通）有限公司 | Lithium hexafluorophosphate purification method |
| CN115872385A (en) * | 2022-12-22 | 2023-03-31 | 张家港博威新能源材料研究所有限公司 | Method for purifying sodium hexafluorophosphate |
| WO2023094368A1 (en) * | 2021-11-24 | 2023-06-01 | Gujarat Fluorochemicals Limited | A method for preparing lithium hexafluorophosphate |
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