CN108046233A - A kind of preparation method of LiBF4 - Google Patents
A kind of preparation method of LiBF4 Download PDFInfo
- Publication number
- CN108046233A CN108046233A CN201711137961.7A CN201711137961A CN108046233A CN 108046233 A CN108046233 A CN 108046233A CN 201711137961 A CN201711137961 A CN 201711137961A CN 108046233 A CN108046233 A CN 108046233A
- Authority
- CN
- China
- Prior art keywords
- libf4
- lithium
- hydrogen fluoride
- boric acid
- obtains
- 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.)
- Pending
Links
Classifications
-
- 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
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/455—Phosphates containing halogen
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
Abstract
The present invention relates to a kind of methods for preparing LiBF4, are as follows：(1) synthesize：Fluoborate aqueous solution is heated up after mixing with aqueous hydrogen fluoride solution；Solid powdery lithium carbonate is added in, reacts 1~2h；(2) concentrate：Mixture heating is concentrated, centrifugation obtains tetrafluoro boric acid crystalline lithium of the moisture content 20~30%；(3) it is dry：Tetrafluoro boric acid crystalline lithium is put into rotary dryer, tetrafluoro boric acid crystalline lithium is dried, obtains LiBF4 crude product；(4) purify.This method is the danger of difficulty and production technology that equipment is reduced using aqueous solution as medium, and entire reaction process is more steady, in the process without side reaction, also there is no by-product, the purity for the LiBF4 being prepared is higher, and quality grade reaches high-purity grade.
Description
Technical field
The present invention relates to a kind of preparation methods of LiBF4.
Background technology
Lithium ion battery is as a kind of environment-protecting clean energy, with fuel cell together as the main electricity of 21 century electric car
Pond, the broad based growth prospect of lithium ion battery carry out huge development space for lithium ion battery material industrial zone.Lithium ion battery
The middle inorganic electrolyte salt used mainly has LiPF6, LiCLO4, LiAsF6, LiBOB, LiBF4 etc., wherein LiPF6 electrolysis
Plastidome has many advantages, such as high conductivity and high electrochemical stability, becomes the main of current lithium ion battery electrolyte field
Product.But this electrolyte of LiPF6 is met water and is easily decomposed, and thermal stability is poor, it is difficult to meet the need of high performance lithium ion battery
It will.And LiBF4 with it in the advantage of moisture, temperature sensitivity and security performance etc., catered to high-performance lithium ion
The needs of battery become the hot spot of lithium salts research and development.
LiBF4, appearance are white or yellowish mobility powder, and fusing point is 293~300 DEG C, easily absorbs moisture,
Chemical property is stablized, and can be used as a lithium electricity (pacemaker batteries, lithium-manganese cell etc.) or secondary lithium ion cell electrolyte solution
Conductive salt can improve the security performance of the high temperature of battery, low temperature and battery, while also quite outstanding to the passivation ability of aluminium foil,
Film for additive can be used as, but LiBF4 is used alone there is significant limitation as electrolytic salt.
Less to the research in terms of the preparation of LiBF4 at home at present, existing Chinese patent CN104692405A is public
A kind of preparation method of LiBF4 have been opened, has been using hydrofluoric acid as solvent, preparation process is more demanding to process equipment,
The danger of technique is higher, and reaction is not easy to control；In addition, it is necessary to be concentrated under vacuum conditions, operating condition is more harsh；
Chinese patent CN104326482A also discloses that a kind of method for preparing LiBF4, is first prepared into lithium metaborate, then and fluorine
Change ammonium or ammonium acid fluoride hybrid reaction, it is also necessary to carry out under vacuum, not only condition is harsh for this method, and reacts and its not
Stablize, it is difficult to control, more most important, in the process there are side reaction and by-product, separating-purifying and its complexity are unfavorable for protecting
The quality of product is demonstrate,proved, is unfavorable for industrialization promotion.
The content of the invention
It is an object of the present invention to overcome the above-mentioned technical problems, and to provide a kind of method for preparing LiBF4, the party
Method only needs to react in aqueous solution, reduces the difficulty of equipment, and concentration can prepare purity height, yield under room temperature
High LiBF4 product, and raw material is easy to get, operating procedure is simple, is completely suitable for industrialized production, is worthy to be popularized.Solution
Certainly the technical solution of above-mentioned technical problem is as follows：
A kind of preparation method of LiBF4, is as follows：
(1) synthesize：
By the pure grade fluoborate aqueous solution of analysis of 40% mass concentration and the aqueous hydrogen fluoride solution of 55% mass concentration according to
Certain proportion after mixing, raises the temperature to 40~80 DEG C；By the way of continuous charging, added in into mixed solution solid
The powdered lithium carbonate of body, the addition of the lithium carbonate are to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.16~
0.19；The feed time of lithium carbonate is controlled to react 1~2h again after the completion of charging for 3~6h；The purpose of the step is fluoboric acid
For labile acid, itself adds in hydrofluoric acid and is allowed to property stabilization, it is easier to generate target product there are reversible reaction；Feed intake speed
The speed of degree determines the amount for generating by-product, and speed influences production efficiency slowly excessively, and excessive velocities easily generate by-product fluorination
Lithium influences product purity；
(2) concentrate：
The mixture that step (1) obtains is warming up to 110~150 DEG C to concentrate, mixture is concentrated into volume as original
Come 1/3~1/4 when mother liquor is released, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtain moisture content 20
~30% tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, it will be in the chuck of rotary dryer
Conduction oil is warming up to 110~150 DEG C, and tetrafluoro boric acid crystalline lithium is dried, and obtains purity more than 98.5%, acid is divided into
2000ppm, the LiBF4 crude product that moisture is 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0
Dissolving ratio is 100~260gLiBF4/1kgAHF under~10 DEG C of environment, is then while agitating blown hydrogen fluoride with nitrogen
It is dry, conduction oil in chuck is warming up to 110~150 DEG C of convection dryings, pure LiBF4 is dried to obtain by crushing, it is pure
Degree more than 99.5%, acid divide below 50ppm, below moisture 20ppm.The process can dramatically improve product quality, from
And target product is obtained, the hydrofluoric acid in addition generated in the process can reach high-purity grade, and product purity is high, and effect is extensive.
Further say, the ratio of fluoborate aqueous solution and aqueous hydrogen fluoride solution in step (1) for ensure fluoboric acid with
The mass ratio of anhydrous hydrogen fluoride is 1:0.01~0.05.
It further says, the temperature described in step (1) is preferably 50~60 DEG C.
The beneficial effects of the invention are as follows：
The present invention devises a kind of method for preparing LiBF4, and this method is using aqueous solution as medium, reduces and sets
Standby difficulty and the danger of production technology, entire reaction process is more steady, and in the process without side reaction, also there is no pairs
Product, the purity for the LiBF4 being prepared is higher, and quality grade reaches high-purity grade, is conducive to industrialized production.
The present invention will be further described in detail with reference to the specific embodiments.
Specific embodiment
Embodiment 1：
A kind of method of four lithium fluophosphate of quick preparation, is as follows：
(1) synthesize：
By the pure grade fluoborate aqueous solution of analysis of 40% mass concentration and the aqueous hydrogen fluoride solution of 55% mass concentration according to
Mass ratio is 1:0.01 after mixing, raises the temperature to 40 DEG C；By the way of continuous charging, added in into mixed solution
Solid powdery lithium carbonate, the addition of lithium carbonate are to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.16；Control carbon
The feed time of sour lithium is 3h, reacts 1h again after the completion of charging；
(2) concentrate：
The mixture that step (1) obtains is warming up to 110 DEG C to concentrate, mixture is concentrated into volume as original 1/
Mother liquor is released when 3~1/4, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtains moisture content 20~30%
Tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, it will be in the chuck of rotary dryer
Conduction oil is warming up to 110 DEG C, and tetrafluoro boric acid crystalline lithium is dried, obtain purity more than 98.5%, acid is divided into 2000ppm,
Moisture is the LiBF4 crude product of 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0
Dissolving ratio is 100gLiBF4/1kgAHF under~10 DEG C of environment, is then while agitating dried up hydrogen fluoride with nitrogen, will
Conduction oil is warming up to 110 DEG C of convection dryings in chuck, and pure LiBF4 is dried to obtain by crushing, purity 99.6%,
Acid divides below 50ppm, below moisture 20ppm, yield 98.5%.
Embodiment 2
A kind of method of four lithium fluophosphate of quick preparation, is as follows：
(1) synthesize：
By the pure grade fluoborate aqueous solution of analysis of 40% mass concentration and the aqueous hydrogen fluoride solution of 55% mass concentration according to
Mass ratio is 1:0.05 after mixing, raises the temperature to 50 DEG C；By the way of continuous charging, added in into mixed solution
Solid powdery lithium carbonate, the addition of lithium carbonate are to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.19；Control carbon
The feed time of sour lithium is 6h, reacts 2h again after the completion of charging；
(2) concentrate：
The mixture that step (1) obtains is warming up to 150 DEG C to concentrate, mixture is concentrated into volume as original 1/
Mother liquor is released when 3~1/4, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtains moisture content 20~30%
Tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, it will be in the chuck of rotary dryer
Conduction oil is warming up to 150 DEG C, and tetrafluoro boric acid crystalline lithium is dried, obtain purity more than 98.5%, acid is divided into 2000ppm,
Moisture is the LiBF4 crude product of 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0
Dissolving ratio is 260gLiBF4/1kgAHF under~10 DEG C of environment, is then while agitating dried up hydrogen fluoride with nitrogen, will
Conduction oil is warming up to 150 DEG C of convection dryings in chuck, and pure LiBF4 is dried to obtain by crushing, purity 99.6%,
Acid divides below 50ppm, below moisture 20ppm, yield 97.7%.
Embodiment 3
A kind of method of four lithium fluophosphate of quick preparation, is as follows：
(1) synthesize：
By the pure grade fluoborate aqueous solution of analysis of 40% mass concentration and the aqueous hydrogen fluoride solution of 55% mass concentration according to
Mass ratio is 1:0.02 after mixing, raises the temperature to 60 DEG C；By the way of continuous charging, added in into mixed solution
Solid powdery lithium carbonate, the addition of lithium carbonate are to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.17；Control carbon
The feed time of sour lithium is 4h, reacts 1h again after the completion of charging；
(2) concentrate：
The mixture that step (1) obtains is warming up to 120 DEG C to concentrate, mixture is concentrated into volume as original 1/
Mother liquor is released when 3~1/4, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtains moisture content 20~30%
Tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, it will be in the chuck of rotary dryer
Conduction oil is warming up to 130 DEG C, and tetrafluoro boric acid crystalline lithium is dried, obtain purity more than 98.5%, acid is divided into 2000ppm,
Moisture is the LiBF4 crude product of 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0
Dissolving ratio is 200gLiBF4/1kgAHF under~10 DEG C of environment, is then while agitating dried up hydrogen fluoride with nitrogen, will
Conduction oil is warming up to 130 DEG C of convection dryings in chuck, and pure LiBF4 is dried to obtain by crushing, purity 99.6%,
Acid divides below 50ppm, below moisture 20ppm, yield 94.5%.
Embodiment 4
A kind of method of four lithium fluophosphate of quick preparation, is as follows：
(1) synthesize：
By the pure grade fluoborate aqueous solution of analysis of 40% mass concentration and the aqueous hydrogen fluoride solution of 55% mass concentration according to
Mass ratio is 1:0.04 after mixing, raises the temperature to 70 DEG C；By the way of continuous charging, added in into mixed solution
Solid powdery lithium carbonate, the addition of lithium carbonate are to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.18；Control carbon
The feed time of sour lithium is 5h, reacts 1.5h again after the completion of charging；
(2) concentrate：
The mixture that step (1) obtains is warming up to 140 DEG C to concentrate, mixture is concentrated into volume as original 1/
Mother liquor is released when 3~1/4, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtains moisture content 20~30%
Tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, it will be in the chuck of rotary dryer
Conduction oil is warming up to 140 DEG C, and tetrafluoro boric acid crystalline lithium is dried, obtain purity more than 98.5%, acid is divided into 2000ppm,
Moisture is the LiBF4 crude product of 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0
Dissolving ratio is 180gLiBF4/1kgAHF under~10 DEG C of environment, is then while agitating dried up hydrogen fluoride with nitrogen, will
Conduction oil is warming up to 140 DEG C of convection dryings in chuck, and pure LiBF4 is dried to obtain by crushing, purity 99.6%,
Acid divides below 50ppm, below moisture 20ppm, yield 96.7%.
Embodiment 5
A kind of method of four lithium fluophosphate of quick preparation, is as follows：
(1) synthesize：
By the pure grade fluoborate aqueous solution of analysis of 40% mass concentration and the aqueous hydrogen fluoride solution of 55% mass concentration according to
Mass ratio is 1:0.035 after mixing, raises the temperature to 80 DEG C；By the way of continuous charging, add into mixed solution
Enter solid powdery lithium carbonate, the addition of lithium carbonate is to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.185；Control
The feed time of lithium carbonate is 4h, reacts 2h again after the completion of charging；
(2) concentrate：
The mixture that step (1) obtains is warming up to 145 DEG C to concentrate, mixture is concentrated into volume as original 1/
Mother liquor is released when 3~1/4, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtains moisture content 20~30%
Tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, it will be in the chuck of rotary dryer
Conduction oil is warming up to 145 DEG C, and tetrafluoro boric acid crystalline lithium is dried, obtain purity more than 98.5%, acid is divided into 2000ppm,
Moisture is the LiBF4 crude product of 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0
Dissolving ratio is 230gLiBF4/1kgAHF under~10 DEG C of environment, is then while agitating dried up hydrogen fluoride with nitrogen, will
Conduction oil is warming up to 145 DEG C of convection dryings in chuck, and pure LiBF4 is dried to obtain by crushing, purity 99.6%,
Acid divides below 50ppm, below moisture 20ppm, yield 93.3%.
The above is only presently preferred embodiments of the present invention, not does limitation in any form to the present invention, it is every according to
According to above example is made in the technical spirit of the present invention any simple modification, equivalent variations, each fall within the guarantor of the present invention
Within the scope of shield.
Claims (3)
1. a kind of preparation method of LiBF4, which is characterized in that be as follows：
(1) synthesize：
40% mass concentration is analyzed into pure grade fluoborate aqueous solution with the aqueous hydrogen fluoride solution of 55% mass concentration according to certain
Ratio after mixing, raises the temperature to 40~80 DEG C；By the way of continuous charging, solid powder is added in into mixed solution
Last shape lithium carbonate, the addition of the lithium carbonate are to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.16~0.19；
The feed time of lithium carbonate is controlled to react 1~2h again after the completion of charging for 3~6h；
(2) concentrate：
The mixture that step (1) obtains is warming up to 110~150 DEG C to concentrate, it is original that mixture is concentrated into volume
Mother liquor is released when 1/3~1/4, crystallisation by cooling is carried out under room temperature industrial water, finally centrifugation obtain moisture content 20~
30% tetrafluoro boric acid crystalline lithium；
(3) it is dry：
The tetrafluoro boric acid crystalline lithium that step (2) obtains is put into rotary dryer, by heat conduction in the chuck of rotary dryer
Oil is warming up to 110~150 DEG C, and tetrafluoro boric acid crystalline lithium is dried, obtain purity more than 98.5%, acid is divided into 2000ppm,
Moisture is the LiBF4 crude product of 2000ppm；
(4) purify：
The LiBF4 crude product that step (3) obtains is placed in dissolving tank, and adds in anhydrous hydrogen fluoride to make its dissolving, 0~10
Dissolving ratio is 100~260gLiBF4/1kgAHF under DEG C environment, is then while agitating dried up hydrogen fluoride with nitrogen, will
Conduction oil is warming up to 110~150 DEG C of convection dryings in chuck, and pure LiBF4, purity are dried to obtain by crushing
More than 99.5%, acid divides below 50ppm, below moisture 20ppm.
2. the preparation method of LiBF4 according to claim 1, which is characterized in that the fluoboric acid water in step (1)
The ratio of solution and aqueous hydrogen fluoride solution is to ensure that the mass ratio of fluoboric acid and anhydrous hydrogen fluoride is 1:0.01~0.05.
3. the preparation method of LiBF4 according to claim 1, which is characterized in that the temperature described in step (1)
For 50~60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711137961.7A CN108046233A (en) | 2017-11-16 | 2017-11-16 | A kind of preparation method of LiBF4 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711137961.7A CN108046233A (en) | 2017-11-16 | 2017-11-16 | A kind of preparation method of LiBF4 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108046233A true CN108046233A (en) | 2018-05-18 |
Family
ID=62118843
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711137961.7A Pending CN108046233A (en) | 2017-11-16 | 2017-11-16 | A kind of preparation method of LiBF4 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108046233A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811407A (en) * | 2019-11-15 | 2021-05-18 | 多氟多化工股份有限公司 | Preparation method of lithium difluorophosphate |
| CN116102028A (en) * | 2022-12-12 | 2023-05-12 | 湖南法恩莱特新能源科技有限公司 | Preparation method of lithium tetrafluoroborate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318664A (en) * | 2008-05-09 | 2008-12-10 | 中国科学院青海盐湖研究所 | Method of preparing waterless lithium terafluoroborate |
| CN102030339A (en) * | 2011-01-12 | 2011-04-27 | 新疆有色金属研究所 | Preparation method of battery-grade anhydrous lithium tetrafluoroborate |
| CN103342372A (en) * | 2013-07-23 | 2013-10-09 | 森田化工(张家港)有限公司 | Method for preparing lithium tetrafluoroborate |
| CN104310421A (en) * | 2014-10-20 | 2015-01-28 | 多氟多化工股份有限公司 | Preparation method of high-purity lithium tetrafluoroborate |
| CN104692405A (en) * | 2015-02-04 | 2015-06-10 | 多氟多化工股份有限公司 | Preparation method of lithium tetrafluoroborate |
-
2017
- 2017-11-16 CN CN201711137961.7A patent/CN108046233A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318664A (en) * | 2008-05-09 | 2008-12-10 | 中国科学院青海盐湖研究所 | Method of preparing waterless lithium terafluoroborate |
| CN102030339A (en) * | 2011-01-12 | 2011-04-27 | 新疆有色金属研究所 | Preparation method of battery-grade anhydrous lithium tetrafluoroborate |
| CN103342372A (en) * | 2013-07-23 | 2013-10-09 | 森田化工(张家港)有限公司 | Method for preparing lithium tetrafluoroborate |
| CN104310421A (en) * | 2014-10-20 | 2015-01-28 | 多氟多化工股份有限公司 | Preparation method of high-purity lithium tetrafluoroborate |
| CN104692405A (en) * | 2015-02-04 | 2015-06-10 | 多氟多化工股份有限公司 | Preparation method of lithium tetrafluoroborate |
Non-Patent Citations (2)
| Title |
|---|
| 兰倩倩等: "电池级四氟硼酸锂制备工艺的优化及电化学性能研究", 《化工新型材料》 * |
| 彭静红等: "溶液法制备四氟硼酸锂的研究", 《化工新型材料》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811407A (en) * | 2019-11-15 | 2021-05-18 | 多氟多化工股份有限公司 | Preparation method of lithium difluorophosphate |
| CN112811407B (en) * | 2019-11-15 | 2023-10-31 | 多氟多新材料股份有限公司 | Preparation method of lithium difluorophosphate |
| CN116102028A (en) * | 2022-12-12 | 2023-05-12 | 湖南法恩莱特新能源科技有限公司 | Preparation method of lithium tetrafluoroborate |
| CN116102028B (en) * | 2022-12-12 | 2023-12-12 | 湖南法恩莱特新能源科技有限公司 | Preparation method of lithium tetrafluoroborate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105731399B (en) | A kind of preparation method of double fluorine sulfimide lithiums | |
| EP3353841B1 (en) | Method of preparing and application of carbon-selenium composites | |
| CN101643481B (en) | Synthesis technique for obtaining difluoro oxalate lithium borate and di-oxalate lithium borate | |
| CN100593515C (en) | Method of preparing waterless lithium terafluoroborate | |
| CN111224164B (en) | Preparation method of lithium difluorophosphate | |
| CN102702243B (en) | Method for preparation and purifying lithium difluoroborate | |
| CN103682251A (en) | Porous ferric oxide/carbon nanometer plate composite material as well as preparation method thereof and application in preparing lithium ion battery | |
| CN104409715A (en) | Preparation method of high-performance nitrogen-doped carbon-coated lithium titanate composite anode material of lithium ion battery | |
| CN104445133A (en) | Preparation method of difluoro-lithium phosphate and lithium ion battery non-aqueous electrolyte | |
| CN103030657A (en) | Preparation method of electrolyte double-oxalate based lithium borate for lithium ion battery | |
| CN102074686A (en) | Method for synthesizing manganese lithium phosphate/carbon serving as positive material of lithium ion battery | |
| CN105859760A (en) | A synthetic method of electronic grade lithium difluoro(oxalato)borate | |
| CN109503635A (en) | A kind of di-oxalate lithium borate purification process | |
| CN102496705A (en) | Preparation method of spinel lithium titanate | |
| CN103265002A (en) | Preparation method of lithium hexafluorophosphate | |
| CN102299325A (en) | Ionothermal process of manganese lithium phosphate anode material | |
| CN110615480A (en) | Method for preparing layered lithium manganate material by dynamic hydrothermal method | |
| CN104557995B (en) | Preparation method of lithium oxalyldifluoroborate | |
| CN107017399A (en) | A kind of doping type lithium vanadate anode material and its synthetic method | |
| CN103647041A (en) | Carbon-covering ferroferric oxide nanowire as well as preparation method thereof and application in preparation of lithium ion battery | |
| CN104037412A (en) | Preparation method of multilevel-structured hollow nano-sphere of negative electrode material of high-performance lithium ion secondary battery | |
| CN108046233A (en) | A kind of preparation method of LiBF4 | |
| CN103227326B (en) | Synthesis method of lithium hexafluorozirconate and new application thereof | |
| CN102976303A (en) | Method for preparing lithium hexafluorophosphate | |
| Liu et al. | Research progress on preparation and purification of fluorine-containing chemicals in lithium-ion batteries |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180926 Address after: 213000 room 2502, unit 48, Li Cheng, Longhu, Tianning District, Changzhou, Jiangsu Applicant after: Gu Fei Address before: 213000 No. 240 central flower garden, Changzhou, Jiangsu Applicant before: Changzhou Hongzheng new energy Limited by Share Ltd |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180518 |