CN108376782A - A kind of catalysis preparation method of difluorophosphate - Google Patents
A kind of catalysis preparation method of difluorophosphate Download PDFInfo
- Publication number
- CN108376782A CN108376782A CN201810068170.1A CN201810068170A CN108376782A CN 108376782 A CN108376782 A CN 108376782A CN 201810068170 A CN201810068170 A CN 201810068170A CN 108376782 A CN108376782 A CN 108376782A
- Authority
- CN
- China
- Prior art keywords
- preparation
- lithium
- added
- difluorophosphate
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
Abstract
The present invention relates to a kind of catalysis preparation methods of difluorophosphate, include the following steps：Non-protonic solvent, lithium carbonate and catalyst are sequentially added in the reaction kettle for being connected with inert gas, stirring is configured to suspension and is heated to reaction kettle.Lithium hexafluorophosphate solution is added drop-wise to dropwise in above-mentioned system and is reacted, good solvent is added after reaction and dissolves product, is filtered to remove insoluble matter, solvent is removed under reduced pressure, difluorophosphate product is obtained after dry.Raw material of the present invention is easy to get, reaction condition is mild, catalyst amount is few, product purification be easy, products obtained therefrom acidity is low, moisture is low, it is simple for process, be suitble to large-scale production.
Description
[technical field]
A kind of catalysis preparation method of difluorophosphate, belongs to lithium-ion battery electrolytes additive technology field.
[background technology]
With the exacerbation of exhaustion and the environmental pollution of petroleum resources, the new energy electric motor vehicle of power lithium-ion battery driving at
For the direction of future automobile development, while it being also the commanding elevation that competitively competes of various countries.Wherein ternary NCM and NCA batteries have height
Energy density, low cost the features such as, become power lithium-ion battery research hot spot, but its cycle life and high/low temperature cycle and
There is also some defects for storage performance.Difluorophosphate is a kind of important lithium carbonate, the lithium containing difluorophosphate from
Sub- battery electrolyte can be obviously improved the cycle life and high temperature performance of ternary battery.But the synthesis of current difluorophosphate
And large-scale production there is also some problems, such as the cost of raw material is high, reaction yield is low, product purity is low.Therefore it explores new
The difluorophosphate preparation method of type has very big theoretical and actual production meaning.Currently, CN101847753A is disclosed
A method of difluorophosphate, difluoro prepared by this method are prepared in aprotic solvent using lithium hexafluoro phosphate and lithium carbonate
The lithium fluoride that residual is slightly soluble in solvent is easy in lithium phosphate solution, this will increase the impedance of battery and is generated to battery performance bad
It influences；CN107381531A, which discloses to react under high-temperature and high-pressure conditions with lithium hexafluoro phosphate using lithium carbonate, prepares difluorophosphoric acid
The method of lithium, but this method is high to equipment requirement, is not suitable for large-scale production；This patent Te Open 2014-62036, which are disclosed, to be adopted
Difluorophosphate is prepared with halide, lithium hexafluoro phosphate, the water other than fluorine removal compound, this method is not easily controlled, and will produce
LiPO4F, HF etc. influences the impurity of battery performance.
[invention content]
In view of this, the technical problem to be solved in the present invention is to improve the deficiencies in the prior art, it is easy to provide a kind of raw material
, simple for process, the reaction time is short, easy to operate, and by-product is less, environmental-friendly, the high difluorophosphate system of product purity
Standby method.
In order to achieve the above object, the present invention adopts the following technical scheme that：
Catalyst is added in lithium carbonate suspension, is heated to certain temperature, lithium hexafluorophosphate solution is added drop-wise to reaction
In system, normal heating reaction prepares difluorophosphate.For wherein using water as catalyst, chemical equation is：
Reaction mechanism is：
LiPF6+H2O→POF3+2HF+LiF
POF3+H2O→HPO2F2+HF
HPO2F2+2Li2CO3+3HF→2CO2+LiPO2F2+2H2O+3LiF
In above-mentioned preparation method, include the following steps：
(1) under room temperature, a certain amount of non-protonic solvent, lithium carbonate are sequentially added in the reaction kettle for being connected with inert gas
And catalyst, stirring are configured to suspension.
(2) reaction kettle is heated to certain temperature, lithium hexafluorophosphate solution is added drop-wise in reaction kettle within a certain period of time,
The reaction was continued after being added dropwise a period of time；
(3) after reaction, the good solvent of difluorophosphate is added, is filtered to remove insoluble matter, filtrate is depressurized
Distillation obtains wet product, finally carries out vacuum high-temperature drying to solid, obtains difluorophosphate sterling.
Preferably, in the above preparation method, the lithium carbonate suspension, lithium carbonate concentration 2.5
~5mol/L；Preferably 4.5~5mol/L.
Preferably, in the above preparation method, the catalyst is one or more in methanol, ethyl alcohol, water
Arbitrary proportion mixes.
Preferably, in the above preparation method, the catalyst loading is 600~2000ppm；Preferably
1200ppm~1500ppm.
Preferably, in the above preparation method, 20~85 DEG C of the heating temperature, preferably 45~50 DEG C；
Preferably, in the above preparation method, the lithium hexafluorophosphate solution a concentration of 1~3.5mol/L is excellent
It is selected as 2.0~2.6mol/L.
Preferably, in the above preparation method, the ratio of the lithium hexafluoro phosphate and lithium carbonate is 1:2.0~
2.5。
Preferably, in the above preparation method, the lithium hexafluorophosphate solution rate of addition is 20~50mL/
Min, preferably 22~30mL/min.
Preferably, in the above preparation method, the reaction time is 3~5h；Preferably 4h.
Preferably, in the above preparation method, the good solvent of the difluorophosphate be glycol dimethyl ether,
Diethylene glycol dimethyl ether, acetonitrile, Isosorbide-5-Nitrae-dioxane, tetrahydrofuran.
Preferably, in the above preparation method, the filter type is closed pressure filtration, decompression filters.
Preferably, in the above preparation method, the vacuum distillation, temperature is 30~70 DEG C, preferably 40~
50℃；Pressure is -0.09~-0.1MPa.
Preferably, in the above preparation method, the vacuum drying temperature is 70~120 DEG C, preferably 85~
90℃。
Preferably, in the above preparation method, the aprotic solvent be methyl ethyl carbonate, dimethyl carbonate,
Diethyl carbonate, ethyl acetate.
Preferably, in the above preparation method, vacuum distillation gained solvent is recyclable and carries out rectifying separation, repeats
It utilizes.
The present invention provides a kind of compared with the method for efficiently preparing difluorophosphate under mild reaction conditions, this method
It is：Under the action of catalyst, lithium hexafluorophosphate solution is added drop-wise in the lithium carbonate suspension of certain temperature, prepared by synthesis under normal pressure
Difluorophosphate, then dissolved difluorophosphate with good solvent, it is filtered to remove insoluble matter, vacuum distillation removes solvent, dry
Obtain the difluorophosphate of high-purity.This method raw material is easy to get, mild condition, and yield is higher (92.3%), and product purity is high
(99.9% or more) meets electrolysis additive quality requirements, and used solvent recoverable, environmental protection pressure is small, is one
The method of the feasible industrialized production difluorophosphate of kind.
[description of the drawings]
Fig. 1 is the XRD characterization figure of difluorophosphate of the present invention.
[specific implementation mode]
Below in conjunction with specific case study on implementation, the present invention is further elaborated：
Embodiment 1：
(1) in a nitrogen environment, 1.1kg lithium carbonates are added in 10L glass reaction kettles, then add 4.0kg carbonic acid
Methyl ethyl ester, adds 12.0g water, and raw material is uniformly mixed by mechanical agitation.
(2) reaction kettle is heated, temperature is set as 45 DEG C.
(3) lithium hexafluoro phosphate/methyl ethyl carbonate ester solution 3.2kg of 2.05mol/L is added into reaction kettle, time for adding is
1h；After lithium hexafluorophosphate solution is added dropwise, 45 DEG C of reaction 4h are kept；There are a large amount of CO in reaction process2Gas overflowing.
(4) into (3), 2kg glycol dimethyl ethers are added in reaction kettle, and mechanical agitation 1h fully dissolves difluorophosphate.
(5) pressurization closed formula filter (pressure is used：0.2MPa, filter：The polytetrafluoroethylstephanoporate stephanoporate that 10 μm of aperture
Film) suspension in (4) is filtered, collect filtrate.
(6) Rotary Evaporators of 10L are used to carry out rotary evaporation, temperature is 50 DEG C.It is recycled after solvent condensation, gained difluoro
Lithium phosphate solid is wet product.
(7) the difluorophosphate wet product in (6) is transferred in vacuum drying chamber to dry, pressure -0.1MPa, temperature 90
DEG C, dry 2h；Finished product 593.8g, yield 83.1%, acidity 193ppm, moisture 72ppm, as shown in Figure 1, passing through XRD
Identify the crystal form of difluorophosphate, XRD:2θ:21.5；22.0；23.5；27.0；34.2；43.2.Nuclear-magnetism further identifies that its is pure
Degree, purity 99.91%,19F-NMR is presented two and meets again, and chemical shift is respectively -83.3ppm and -85.2ppm；31P-NMR is in
Existing triplet, chemical shift are respectively -12.3ppm, 16.9ppm and 21.5ppm.
Embodiment 2：
(1) in a nitrogen environment, 1.1kg lithium carbonates are added in 10L glass reaction kettles, then add 4.0kg carbonic acid
Methyl ethyl ester, adds 24.0g water, and raw material is uniformly mixed by mechanical agitation.
(2) reaction kettle is heated, temperature is set as 45 DEG C.
(3) lithium hexafluoro phosphate-methyl ethyl carbonate ester solution 3.2kg of 2.05mol/L, time for adding are added into reaction kettle
For 2h；After lithium hexafluorophosphate solution is added dropwise, 45 DEG C of reaction 4h are kept；There is bulk gas spilling in reaction process.
(4) into (3), 2kg glycol dimethyl ethers are added in reaction kettle, and mechanical agitation 1h fully dissolves difluorophosphate.
(5) pressurization closed formula filter (pressure is used：0.2MPa, filter：The polytetrafluoroethylstephanoporate stephanoporate that 10 μm of aperture
Film) suspension in (4) is filtered, collect filtrate.
(6) Rotary Evaporators of 10L are used to carry out rotary evaporation, temperature is 50 DEG C.It is recycled after solvent condensation, gained difluoro
Lithium phosphate solid is wet product.
(7) the difluorophosphate wet product in (6) is transferred in vacuum drying chamber to dry, pressure -0.1MPa, temperature 90
DEG C, dry 2h；Finished product 628.9g, yield 88.1%, purity 99.90%, acidity 167ppm, moisture 73ppm.
Embodiment 3：
(1) in a nitrogen environment, 1.1kg lithium carbonates are added in 10L glass reaction kettles, then add 4.0kg carbonic acid
Methyl ethyl ester, adds 24.0g ethyl alcohol, and raw material is uniformly mixed by mechanical agitation.
(2) reaction kettle is heated, temperature is set as 45 DEG C.
(3) lithium hexafluoro phosphate-methyl ethyl carbonate ester solution 3.2kg of 2.05mol/L, time for adding are added into reaction kettle
For 2h；After lithium hexafluorophosphate solution is added dropwise, 45 DEG C of reaction 4h are kept；
(4) into (3), 2kg glycol dimethyl ethers are added in reaction kettle, and mechanical agitation 1h fully dissolves difluorophosphate.
(5) pressurization closed formula filter (pressure is used：0.2MPa, filter：The polytetrafluoroethylstephanoporate stephanoporate that 10 μm of aperture
Film) suspension in (4) is filtered, collect filtrate.
(6) Rotary Evaporators of 10L are used to carry out rotary evaporation, temperature is 50 DEG C.It is recycled after solvent condensation, gained difluoro
Lithium phosphate solid is wet product.
(7) the difluorophosphate wet product in (6) is transferred in vacuum drying chamber to dry, pressure -0.1MPa, temperature 80
DEG C, dry 2h；Finished product 579.9g, yield 81.3%, purity 99.96%, acidity 90ppm, moisture 32ppm.
Embodiment 4：
(1) in a nitrogen environment, 1.1kg lithium carbonates are added in 10L glass reaction kettles, then add 4.0kg carbonic acid
Methyl ethyl ester, adds 24.0g methanol, and raw material is uniformly mixed by mechanical agitation.
(2) reaction kettle is heated, temperature is set as 45 DEG C.
(3) lithium hexafluoro phosphate-methyl ethyl carbonate ester solution 3.2kg of 2.05mol/L, time for adding are added into reaction kettle
For 2h；After lithium hexafluorophosphate solution is added dropwise, 45 DEG C of reaction 4h are kept；
(4) into (3), 2kg glycol dimethyl ethers are added in reaction kettle, and mechanical agitation 1h fully dissolves difluorophosphate.
(5) pressurization closed formula filter (pressure is used：0.2MPa, filter：The polytetrafluoroethylstephanoporate stephanoporate that 10 μm of aperture
Film) suspension in (4) is filtered, collect filtrate.
(6) Rotary Evaporators of 10L are used to carry out rotary evaporation, temperature is 50 DEG C.It is recycled after solvent condensation, difluorophosphoric acid
Lithium solid is wet product.
(7) the difluorophosphate wet product in (6) is transferred in vacuum drying chamber to dry, pressure -0.1MPa, temperature 80
DEG C, dry 2h；Finished product 650.9g, yield 90.3%, purity 99.98%, acidity 65ppm, moisture 25ppm.
Above-mentioned specific implementation mode is only explained in detail technical scheme of the present invention, and the present invention not merely limits to
In above-described embodiment, it will be understood by those skilled in the art that every changing on the basis of the present invention according to above-mentioned principle and spirit
Into, substitute, all should be within protection scope of the present invention.
Claims (13)
1. a kind of catalysis preparation method of difluorophosphate, which is characterized in that including：It is added in the suspension containing lithium carbonate
Catalyst simultaneously heats, and lithium hexafluorophosphate solution is added drop-wise in reaction system, and normal heating reaction prepares difluorophosphate.
2. preparation method according to claim 1, which is characterized in that include the following steps：
(1) under room temperature, lithium carbonate is added in aprotic solvent and is made into suspension, catalyst is added, is heated to temperature extremely
20~85 DEG C, preferably 45~50 DEG C；
(2) lithium hexafluorophosphate solution is added drop-wise in reaction kettle dropwise, 3~5h of reaction is further continued for after being added dropwise；
(3) after reaction, good solvent is added, filters insoluble matter, filtrate is evaporated under reduced pressure to obtain crude product, finally to solid
Body is dried in vacuo, and difluorophosphate sterling is obtained.
3. preparation method according to claim 2, which is characterized in that the aprotic solvent is methyl ethyl carbonate, carbon
Dimethyl phthalate, diethyl carbonate, ethyl acetate.
4. preparation method according to claim 2, which is characterized in that the catalyst is one in methanol, ethyl alcohol, water
Kind or the mixing of a variety of arbitrary proportions.
5. preparation method according to claim 2, which is characterized in that the suspension of the lithium carbonate, lithium carbonate concentration
For 2.5~5mol/L.
6. preparation method according to claim 2, which is characterized in that the catalyst loading be 600~
3000ppm。
7. preparation method according to claim 2, which is characterized in that the lithium hexafluorophosphate solution a concentration of 1~
3.5mol/L, preferably 2.0~2.6mol/L.
8. preparation method according to claim 2, which is characterized in that the ratio of the lithium hexafluoro phosphate and lithium carbonate is
1:2.0~2.5.
9. preparation method according to claim 2, which is characterized in that the lithium hexafluorophosphate solution rate of addition is 20
~50mL/min.
10. preparation method according to claim 2, which is characterized in that the good solvent is glycol dimethyl ether, two
One or more arbitrary proportions mixing in glycol dimethyl ether, acetonitrile, Isosorbide-5-Nitrae-dioxane, tetrahydrofuran.
11. preparation method according to claim 2, which is characterized in that the filter type can be closed pressurizeed
Filter, decompression filter.
12. preparation method according to claim 2, which is characterized in that the vacuum distillation, temperature are 30~70 DEG C,
Preferably 40~50 DEG C；Pressure is -0.09~-0.1Mpa.
13. preparation method according to claim 2, which is characterized in that the vacuum drying pressure be -0.09~-
0.1MPa；Drying temperature is 70~120 DEG C, preferably 85~90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810068170.1A CN108376782A (en) | 2018-01-23 | 2018-01-23 | A kind of catalysis preparation method of difluorophosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810068170.1A CN108376782A (en) | 2018-01-23 | 2018-01-23 | A kind of catalysis preparation method of difluorophosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108376782A true CN108376782A (en) | 2018-08-07 |
Family
ID=63016709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810068170.1A Withdrawn CN108376782A (en) | 2018-01-23 | 2018-01-23 | A kind of catalysis preparation method of difluorophosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108376782A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108910857A (en) * | 2018-09-26 | 2018-11-30 | 王静静 | A kind of preparation method of difluorophosphate |
| CN112320783A (en) * | 2020-11-24 | 2021-02-05 | 多氟多化工股份有限公司 | Catalytic preparation method of lithium difluorophosphate |
| CN113336214A (en) * | 2021-07-15 | 2021-09-03 | 西安荣岩科技发展有限公司 | Preparation method of lithium difluorophosphate |
| CN116715215A (en) * | 2023-08-02 | 2023-09-08 | 深圳新宙邦科技股份有限公司 | Preparation method of sodium difluorophosphate and sodium ion battery |
| CN116715214A (en) * | 2023-07-06 | 2023-09-08 | 中国科学院兰州化学物理研究所 | Method for preparing lithium difluorophosphate and co-producing lithium tetrafluoroborate by ultrasonic promotion |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101208266A (en) * | 2005-06-20 | 2008-06-25 | 三菱化学株式会社 | Method for producing difluorophosphate, non-aqueous electrolyte for secondary cell and non-aqueous electrolyte secondary cell |
| CN101626978A (en) * | 2007-03-12 | 2010-01-13 | 中央硝子株式会社 | Method for producing lithium difluorophosphate and nonaqueous electrolyte battery using the same |
| 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 |
| CN107381530A (en) * | 2017-08-23 | 2017-11-24 | 中山大学 | A kind of method of purification of difluorophosphate |
-
2018
- 2018-01-23 CN CN201810068170.1A patent/CN108376782A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101208266A (en) * | 2005-06-20 | 2008-06-25 | 三菱化学株式会社 | Method for producing difluorophosphate, non-aqueous electrolyte for secondary cell and non-aqueous electrolyte secondary cell |
| CN101626978A (en) * | 2007-03-12 | 2010-01-13 | 中央硝子株式会社 | Method for producing lithium difluorophosphate and nonaqueous electrolyte battery using the same |
| 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 |
| CN107381530A (en) * | 2017-08-23 | 2017-11-24 | 中山大学 | A kind of method of purification of difluorophosphate |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108910857A (en) * | 2018-09-26 | 2018-11-30 | 王静静 | A kind of preparation method of difluorophosphate |
| CN108910857B (en) * | 2018-09-26 | 2020-10-13 | 深圳市研一新材料有限责任公司 | Preparation method of lithium difluorophosphate |
| CN112320783A (en) * | 2020-11-24 | 2021-02-05 | 多氟多化工股份有限公司 | Catalytic preparation method of lithium difluorophosphate |
| CN113336214A (en) * | 2021-07-15 | 2021-09-03 | 西安荣岩科技发展有限公司 | Preparation method of lithium difluorophosphate |
| CN116715214A (en) * | 2023-07-06 | 2023-09-08 | 中国科学院兰州化学物理研究所 | Method for preparing lithium difluorophosphate and co-producing lithium tetrafluoroborate by ultrasonic promotion |
| CN116715215A (en) * | 2023-08-02 | 2023-09-08 | 深圳新宙邦科技股份有限公司 | Preparation method of sodium difluorophosphate and sodium ion battery |
| CN116715215B (en) * | 2023-08-02 | 2024-02-09 | 深圳新宙邦科技股份有限公司 | Preparation method of sodium difluorophosphate and sodium ion battery |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108376782A (en) | A kind of catalysis preparation method of difluorophosphate | |
| CN105800582B (en) | The preparation method and lithium ion battery non-aqueous electrolyte of a kind of difluorophosphate | |
| KR102036924B1 (en) | Method for producing alkali metal hexafluorophosphate, alkali metal hexafluorophosphate, method for producing electrolyte concentrate comprising alkali metal hexafluorophosphate, and method for producing secondary battery | |
| CN102910612B (en) | Method for preparing lithium hexafluorophosphate | |
| CN102803142A (en) | Method for producing tetrafluoroborate | |
| CN102702243A (en) | Method for preparation and purifying lithium difluoroborate | |
| JP5862094B2 (en) | Method for producing lithium hexafluorophosphate concentrate | |
| KR20150016533A (en) | Fluorine-containing esters and methods of preparation thereof | |
| CN107381531A (en) | A kind of preparation method of difluorophosphate | |
| CN114229816A (en) | Method for recycling and preparing anode material from waste lithium iron phosphate battery | |
| CN110343125B (en) | Method for preparing high-purity proportional mixed lithium salt at low cost and application of mixed lithium salt in lithium ion battery | |
| KR20200114963A (en) | Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content | |
| JP3428910B2 (en) | Method for producing electrolyte and method for producing secondary battery | |
| JP5609283B2 (en) | Method for producing electrolytic solution for lithium ion battery and lithium ion battery using the same | |
| CN114275757B (en) | Preparation method of lithium difluorophosphate | |
| CN106384841A (en) | Method for enhancing utilization ratio of electrolyte in lithium ion battery | |
| KR20200114967A (en) | Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content | |
| CN102491305A (en) | Method for preparing lithium hexafluorophosphate by using composite solvent | |
| CN106299473B (en) | A kind of oxalic acid lithium phosphate and preparation method thereof | |
| CN112678795B (en) | Preparation method of lithium difluorophosphate | |
| CN113636534A (en) | Preparation method of lithium difluorophosphate | |
| CN113725430A (en) | Preparation method of lithium tetrafluoro oxalate phosphate and derivative thereof, electrolyte and secondary battery | |
| KR20220135283A (en) | Method for manufacturing sodium bis(fluorosulfonyl)imide | |
| CN112898457A (en) | Single ion conducting polymers for electrochemical devices | |
| KR101321523B1 (en) | Manufacturing of active carbon for capacitor electrode using NaOH chemical activation and a capacitor made thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180807 |
|
| WW01 | Invention patent application withdrawn after publication |