CN112758904A - Preparation method of lithium difluorophosphate - Google Patents

Preparation method of lithium difluorophosphate Download PDF

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Publication number
CN112758904A
CN112758904A CN201911159657.1A CN201911159657A CN112758904A CN 112758904 A CN112758904 A CN 112758904A CN 201911159657 A CN201911159657 A CN 201911159657A CN 112758904 A CN112758904 A CN 112758904A
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fluorine
lithium difluorophosphate
lithium
gas
preparation
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CN112758904B (en
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李世江
薛旭金
杨明霞
于贺华
张照坡
于洋
刘海霞
耿梦湍
张扬
李迪
周苏
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Duo Fluoride Chemicals Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/10—Halides or oxyhalides of phosphorus
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to the technical field of lithium ion battery additives, in particular to a preparation method of lithium difluorophosphate. The preparation method specifically comprises the steps of reacting lithium phosphate with fluorine-containing reaction gas, and purifying to obtain the lithium phosphate. The preparation method of the lithium difluorophosphate adopts the fluorine-containing reaction gas and the lithium phosphate to synthesize the lithium difluorophosphate through fluorination, has few byproducts, high utilization rate of raw materials, direct solid-gas reaction, simple treatment after reaction, almost zero discharge of three wastes in the production process, green and environment-friendly preparation process, can obviously shorten the preparation period of the lithium difluorophosphate and reduce the preparation cost.

Description

Preparation method of lithium difluorophosphate
Technical Field
The invention relates to the technical field of lithium ion battery additives, in particular to a preparation method of lithium difluorophosphate.
Background
At present, the lithium ion power battery anode material mainly takes a lithium iron phosphate and nickel cobalt manganese ternary material as a main material, and the electrolyte mainly takes a liquid electrolyte system of lithium hexafluorophosphate compounded with a carbonate organic solvent. In a ternary positive electrode material system, proper amount of lithium difluorophosphate is added to reduce the internal resistance of the battery, and a protective film is formed on the positive electrode of the battery, so that the cycle performance of the battery is obviously improved; meanwhile, in a lithium iron phosphate anode system with high compaction density, lithium difluorophosphate is taken as an additive of electrolyte, so that the high-low temperature cycle storage performance and the cycle stability of the battery can be obviously improved, and the lithium difluorophosphate is a novel lithium salt additive with great industrial value and is widely concerned. The industrial preparation of the lithium difluorophosphate is researched, the manufacturing cost of the lithium difluorophosphate is reduced, and the method plays an important role in popularizing the industrial application of the lithium difluorophosphate.
For example, chinese patent application publication No. CN106829909A discloses a method for preparing lithium difluorophosphate, which uses lithium hexafluorophosphate and tris (trimethylsilane) borate or tris (trimethylsilyl) borate as raw materials to prepare lithium difluorophosphate, and on one hand, the method generates byproducts, which easily causes product coating and affects product quality; on the other hand, the cost of raw materials is high, which causes high production cost of products.
The Chinese patent application with publication number CN108689395A discloses a preparation method of lithium difluorophosphate, which takes a lithium hexafluorophosphate complex and lithium carbonate as raw materials to prepare the lithium difluorophosphate, and on one hand, the method can cause a complexing reagent of the lithium hexafluorophosphate complex to be dissociated, which can cause the reduction of the product yield and also can increase the raw material cost of the product; on the other hand, the product is also coated with impurities, the quality of the product is influenced, and the reaction time is longer.
Chinese patent application with publication number CN108640096A discloses a method for preparing difluorophosphoric acid and lithium difluorophosphate, which takes dichlorophosphoric acid, a fluorination reagent and a lithium source substance as raw materials to prepare lithium difluorophosphate, and the method has the advantages of side reaction, low utilization rate of the raw materials and high requirement on equipment on one hand; on the other hand, the produced industrial wastewater is more and is not beneficial to environmental protection.
Chinese patent application publication No. CN104445133A discloses a method for preparing lithium difluorophosphate, in which pyrophosphate reacts with fluorine gas to generate a mixed gas, the obtained mixed gas is introduced into an anhydrous hydrogen fluoride solution of lithium fluoride to react, and after the reaction is finished, a product is crystallized, filtered and dried to obtain a lithium difluorophosphate product. However, this method produces a large amount of by-product harmful gases, such as CoF produced when cobalt pyrophosphate is used as a raw material2And OF2The raw material utilization rate is low, two-step reaction is needed, the process flow is complex and is not easy to control.
Disclosure of Invention
The invention aims to provide a preparation method of lithium difluorophosphate, so as to solve the problems of low lithium difluorophosphate yield, low preparation efficiency and high preparation cost of the existing preparation method.
In order to achieve the purpose, the technical scheme of the preparation method of the lithium difluorophosphate is as follows:
a preparation method of lithium difluorophosphate is specifically characterized by reacting lithium phosphate with fluorine-containing reaction gas, and purifying to obtain the lithium difluorophosphate, wherein the fluorine-containing reaction gas consists of 20-100% of fluorine gas and 0-80% of inert gas.
The invention adopts fluorine-containing reaction gas and lithium phosphate to synthesize lithium difluorophosphate by fluorination, and byproducts are inert gas, lithium fluoride and oxygen, so that the method can be recycled, the reaction yield is high and can reach 78.5%, and the product purity is more than 99.95%. The preparation method of the invention has direct solid-gas contact reaction, and lithium phosphate is pretreated into powder state in order to increase the solid-gas contact area and make the reaction more sufficient. The preparation method has simple treatment after reaction, almost zero discharge of three wastes and green and environment-friendly preparation process.
The inert gas may be any gas which does not react with the substance in the reaction system, and is selected from, for example, nitrogen, helium and argon, which are commonly used. From the viewpoint of production cost, nitrogen gas is preferred.
The reaction product contains a large amount of lithium difluorophosphate and lithium fluoride as a byproduct, and the lithium difluorophosphate can be obtained by conventional purification steps, such as recrystallization from an organic solvent and drying.
The organic solvent is selected from organic solvents having good solubility for lithium difluorophosphate, and preferably, the organic solvent is one of ester solvents, ether solvents and alcohol solvents. Further preferably, the ester solvent is ethyl acetate, the ether solvent is methyl tert-butyl ether, and the alcohol solvent is ethanol.
And the step of recrystallization is to concentrate the mixed solution of the organic solvent and the reaction product to 1/5-1/3 of the original volume, then cool and crystallize, and then carry out solid-liquid separation to obtain the lithium difluorophosphate crystal. The cooling temperature is preferably-10 to-30 ℃.
In order to ensure that the partial pressure of fluorine gas in the mixed gas in the reactor is proper to reduce the generation of side reaction, excessive fluorine-containing reaction gas is introduced into lithium phosphate, the volume of the fluorine gas in the fluorine-containing reaction gas accounts for 20-100%, the volume of the fluorine-containing reaction gas introduced per minute is 10-500 times of the mass of the lithium difluorophosphate, the volume of the fluorine-containing reaction gas is calculated by mL, and the mass of the lithium difluorophosphate is calculated by g.
Preferably, the flow rate of the fluorine-containing reaction gas is 200-1000 mL/min.
In order to improve the reaction rate and further improve the preparation efficiency, the reaction temperature is 30-150 ℃.
In order to improve the reaction efficiency, the reaction time is 10-300 min.
Drawings
FIG. 1 is an XRD pattern of the reaction product of example 1 of the present invention.
Detailed Description
The following examples are provided to further illustrate the practice of the invention. In the following examples, lithium phosphate was purchased from a Luoyang reagent factory, the purity was 99%, and fluorine-containing reaction gas was prepared by itself.
Example 1
The preparation method of lithium difluorophosphate of the embodiment adopts the following steps:
adding 11.6g of lithium phosphate into a fluorination furnace, replacing with nitrogen, filling nitrogen until the pressure is 0.05MPa, setting the temperature of the fluorination furnace to be 30 ℃, starting to introduce mixed fluorine and nitrogen gas into the fluorination furnace when the temperature reaches a set value, controlling the flow rate to be 200mL/min, introducing the mixed fluorine and nitrogen gas for 300min, and cooling to room temperature after the reaction is finished, wherein the volume ratio of fluorine in the mixed fluorine and nitrogen gas is 20 percent of that of the mixed fluorine and nitrogen gas; then, the solid in the fluorination furnace was subjected to XRD by replacing it with nitrogen, and the results were as follows: all of lithium difluorophosphate and lithium fluoride; then, ethyl acetate is used for recrystallization, and the recrystallization steps are as follows: concentrating at 50 deg.C under-0.1 MPa for 2 hr, reducing the volume of the solution to 1/3, cooling to-20 deg.C, filtering to obtain crystal, and drying to obtain 8.48g lithium difluorophosphate with yield of 78.5% and purity of 99.97%.
The XRD pattern is shown in figure 1, the solid has a group of strong diffraction peaks at 21.623 degrees, 22.008 degrees, 27.216 degrees, 23.526 degrees, 34.187 degrees and 45.170 degrees, and no obvious diffraction peak is observed between 50 and 90 degrees.
Example 2
The preparation method of lithium difluorophosphate of the embodiment adopts the following steps:
adding 11.6g of lithium phosphate into a fluorination furnace, replacing with nitrogen, filling nitrogen until the pressure is 0.05MPa, setting the temperature of the fluorination furnace to 150 ℃, starting to introduce a fluorine-nitrogen mixed gas into the fluorination furnace when the temperature reaches a set value, controlling the flow rate to be 200mL/min, introducing the fluorine-nitrogen mixed gas for 60min, and cooling to room temperature after the reaction is finished, wherein the volume ratio of fluorine in the fluorine-nitrogen mixed gas is 40% of that of the fluorine-nitrogen mixed gas; then, the solid in the fluorination furnace was subjected to XRD by replacing it with nitrogen, and the results were as follows: all of lithium difluorophosphate and lithium fluoride; then using ethanol for recrystallization, wherein the recrystallization steps are as follows: concentrating at 50 deg.C under-0.1 MPa for 3 hr, reducing the volume of the solution to 1/3, cooling to-30 deg.C, filtering to obtain crystal, and drying to obtain 8.5g lithium difluorophosphate with yield of 78.7% and purity of 99.96%.
Example 3
The preparation method of lithium difluorophosphate of the embodiment adopts the following steps:
adding 11.6g of lithium phosphate into a fluorination furnace, replacing with nitrogen, filling nitrogen until the pressure is 0.05MPa, setting the temperature of the fluorination furnace to be 30 ℃, starting to introduce mixed fluorine and nitrogen gas into the fluorination furnace when the temperature reaches a set value, controlling the flow rate to be 1000mL/min, introducing the mixed fluorine and nitrogen gas for 30min, and cooling to room temperature after the reaction is finished, wherein the volume ratio of fluorine in the mixed fluorine and nitrogen gas is 80% of that of the mixed fluorine and nitrogen gas; then, the solid in the fluorination furnace was subjected to XRD by replacing it with nitrogen, and the results were as follows: all of lithium difluorophosphate and lithium fluoride; then recrystallizing by using methyl tert-butyl ether, wherein the recrystallization steps are as follows: concentrating at 45 deg.C under-0.1 MPa for 1.5h, reducing the volume of the solution to 1/3, cooling to-15 deg.C, filtering to obtain crystal, and drying to obtain 8.47g lithium difluorophosphate with yield of 78.4% and purity of 99.98%.
Example 4
The preparation method of lithium difluorophosphate of the embodiment adopts the following steps:
adding 11.6g of lithium phosphate into a fluorination furnace, replacing with nitrogen, filling nitrogen until the pressure is 0.05MPa, setting the temperature of the fluorination furnace to be 150 ℃, starting to introduce a fluorine-nitrogen mixed gas into the fluorination furnace when the temperature reaches a set value, controlling the flow rate to be 1000mL/min, introducing the fluorine-nitrogen mixed gas for 10min, and cooling to room temperature after the reaction is finished, wherein the volume ratio of fluorine in the fluorine-nitrogen mixed gas is 100% of that of the fluorine-nitrogen mixed gas; then, the solid in the fluorination furnace was subjected to XRD by replacing it with nitrogen, and the results were as follows: all of lithium difluorophosphate and lithium fluoride; then using ethyl acetate for recrystallization, wherein the recrystallization steps are as follows: concentrating at 50 deg.C under-0.1 MPa for 2 hr, reducing the volume of the solution to 1/3, cooling to-20 deg.C, filtering to obtain crystal, and drying to obtain 8.52g lithium difluorophosphate with yield of 78.9% and purity of 99.97%.
Example 5
The preparation method of lithium difluorophosphate of the embodiment adopts the following steps:
adding 11.6g of lithium phosphate into a fluorination furnace, replacing with nitrogen, filling nitrogen until the pressure is 0.05MPa, setting the temperature of the fluorination furnace to 70 ℃, starting to introduce a fluorine-nitrogen mixed gas into the fluorination furnace when the temperature reaches a set value, controlling the flow rate to be 300mL/min, introducing the fluorine-nitrogen mixed gas for 90min, and cooling to room temperature after the reaction is finished, wherein the volume ratio of fluorine in the fluorine-nitrogen mixed gas is 50% of that of the fluorine-nitrogen mixed gas; then, the solid in the fluorination furnace was subjected to XRD by replacing it with nitrogen, and the results were as follows: all of lithium difluorophosphate and lithium fluoride; then using ethanol for recrystallization, wherein the recrystallization steps are as follows: under the conditions of 50 ℃ and-0.1 MPa pressure, the solution is concentrated for 3h, the volume of the solution is reduced to 1/3, and the solution is cooled to-30 ℃ to obtain 8.49g of lithium difluorophosphate, the yield is 78.6 percent, and the purity is 99.96 percent.

Claims (10)

1. A preparation method of lithium difluorophosphate is characterized in that lithium phosphate is reacted with fluorine-containing reaction gas and purified to obtain the lithium difluorophosphate; the fluorine-containing reaction gas consists of 20-100% by volume of fluorine gas and 0-80% by volume of inert gas, and the proportion is volume percentage.
2. The method of claim 1, wherein the inert gas is one of nitrogen, helium, and argon.
3. The method for preparing lithium difluorophosphate as claimed in claim 1, wherein the purification is carried out by recrystallizing and drying the reaction product with an organic solvent.
4. The method for preparing lithium difluorophosphate according to claim 3, wherein the organic solvent is one of an ester solvent, an ether solvent and an alcohol solvent.
5. The method for preparing lithium difluorophosphate according to claim 4, wherein the ester solvent is ethyl acetate, or the ether solvent is methyl tert-butyl ether, or the alcohol solvent is ethanol.
6. The method for preparing lithium difluorophosphate as claimed in claim 3, wherein the step of recrystallizing is to concentrate the mixture of the organic solvent and the reaction product to 1/5-1/3 volume, and then cool the mixture to-10 to-30 ℃.
7. The method for producing lithium difluorophosphate according to claim 1, wherein an excess amount of a fluorine-containing reaction gas is introduced into lithium phosphate, the fluorine gas in the fluorine-containing reaction gas is 20 to 100% by volume, the fluorine-containing reaction gas is introduced per minute in a volume of 10 to 500 times the mass of lithium difluorophosphate, the fluorine-containing reaction gas is introduced in a volume of mL, and the lithium difluorophosphate is introduced in a mass of g.
8. The method for preparing lithium difluorophosphate as claimed in claim 7, wherein the flow rate of the fluorine-containing reaction gas is 200 to 1000 mL/min.
9. The method for preparing lithium difluorophosphate as claimed in claim 1, wherein the reaction temperature is 30 to 150 ℃.
10. The method for preparing lithium difluorophosphate of claim 9, wherein the reaction time is 10-300 min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115159494A (en) * 2022-09-01 2022-10-11 多氟多新材料股份有限公司 Preparation method of lithium difluorophosphate
CN115771888A (en) * 2023-01-05 2023-03-10 安阳工学院 Preparation method of high-purity lithium difluorophosphate

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JP2004175659A (en) * 2002-11-12 2004-06-24 Santoku Corp Method for producing fluorine-containing lithium compound
CN102985362A (en) * 2010-07-08 2013-03-20 索尔维公司 Manufacture of liPO2F2
WO2015028346A1 (en) * 2013-08-28 2015-03-05 Solvay Sa Production of metal difluorophosphates in an inorganic solvent
CN104692405A (en) * 2015-02-04 2015-06-10 多氟多化工股份有限公司 Preparation method of lithium tetrafluoroborate
CN105731399A (en) * 2016-04-29 2016-07-06 多氟多化工股份有限公司 Preparation method of difluoro-sulfonyl imide lithium
CN205990244U (en) * 2016-08-30 2017-03-01 多氟多化工股份有限公司 A kind of fluorination stove and twin furnace fluorinated systems
CN108751234A (en) * 2018-06-29 2018-11-06 惠州市宙邦化工有限公司 A kind of method of purification of lithium fluoride

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004175659A (en) * 2002-11-12 2004-06-24 Santoku Corp Method for producing fluorine-containing lithium compound
CN102985362A (en) * 2010-07-08 2013-03-20 索尔维公司 Manufacture of liPO2F2
WO2015028346A1 (en) * 2013-08-28 2015-03-05 Solvay Sa Production of metal difluorophosphates in an inorganic solvent
CN104692405A (en) * 2015-02-04 2015-06-10 多氟多化工股份有限公司 Preparation method of lithium tetrafluoroborate
CN105731399A (en) * 2016-04-29 2016-07-06 多氟多化工股份有限公司 Preparation method of difluoro-sulfonyl imide lithium
CN205990244U (en) * 2016-08-30 2017-03-01 多氟多化工股份有限公司 A kind of fluorination stove and twin furnace fluorinated systems
CN108751234A (en) * 2018-06-29 2018-11-06 惠州市宙邦化工有限公司 A kind of method of purification of lithium fluoride

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115159494A (en) * 2022-09-01 2022-10-11 多氟多新材料股份有限公司 Preparation method of lithium difluorophosphate
CN115159494B (en) * 2022-09-01 2023-03-21 多氟多新材料股份有限公司 Preparation method of lithium difluorophosphate
CN115771888A (en) * 2023-01-05 2023-03-10 安阳工学院 Preparation method of high-purity lithium difluorophosphate
CN115771888B (en) * 2023-01-05 2024-01-16 安阳工学院 Preparation method of high-purity lithium difluorophosphate

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