CN109232625A - A kind of preparation method of difluorine oxalic acid boracic acid lithium - Google Patents
A kind of preparation method of difluorine oxalic acid boracic acid lithium Download PDFInfo
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- CN109232625A CN109232625A CN201811246050.2A CN201811246050A CN109232625A CN 109232625 A CN109232625 A CN 109232625A CN 201811246050 A CN201811246050 A CN 201811246050A CN 109232625 A CN109232625 A CN 109232625A
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- oxalic acid
- reaction
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- difluorine oxalic
- acid lithium
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims abstract description 174
- 235000006408 oxalic acid Nutrition 0.000 title claims abstract description 58
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 37
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 title claims abstract description 35
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229960002645 boric acid Drugs 0.000 title claims abstract description 35
- 235000010338 boric acid Nutrition 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 85
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 238000002425 crystallisation Methods 0.000 claims abstract description 32
- 230000008025 crystallization Effects 0.000 claims abstract description 32
- 239000003960 organic solvent Substances 0.000 claims abstract description 27
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- -1 reaction promoter Substances 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- 239000012141 concentrate Substances 0.000 claims description 10
- 239000012046 mixed solvent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 244000025254 Cannabis sativa Species 0.000 description 4
- 229910013188 LiBOB Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 229910015900 BF3 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/022—Boron compounds without C-boron linkages
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a kind of preparation method of difluorine oxalic acid boracic acid lithium, the reaction raw materials of difluorine oxalic acid boracic acid lithium of the invention are LiBF4, oxalic acid, reaction promoter, organic solvent, crystallization solvent；By pretreatment of raw material, reactor vessel processes, reaction process one, reaction process two, filtering and concentrating and etc. prepared.The preparation of difluorine oxalic acid boracic acid lithium of the invention, simple process is easy to operate, and difluorine oxalic acid boracic acid lithium can be obtained without complicated equipment；Nonhazardous product generates in the preparation process of difluorine oxalic acid boracic acid lithium of the invention, safety and environmental protection, the readily treated absorption of exhaust gas that reaction process generates, and offal treatment is at low cost.
Description
Technical field
The invention belongs to technical field of lithium batteries, more particularly to a kind of preparation method of difluorine oxalic acid boracic acid lithium.
Background technique
Lithium ion battery is a kind of novel high-energy secondary cell to grow up the 1990s.It has specific energy
High, small in size, light weight, can the excellent properties such as high rate discharge, self-discharge rate low (500 times), nontoxic, memory-less effect,
Portable electronic products and household appliance technical field are widely used.Difluorine oxalic acid boracic acid lithium (LiODFB) is as a kind of novel
Lithium salts not only combines the respective advantage of LiBOB and LiBF4 [3]: having good film forming function as LiBOB, as electricity
Solution matter lithium salts is added in electrolyte that effectively inhibit PC embedding altogether on graphite, prevents graphite from falling off, and assembled with it
Battery has the comprehensive performances such as excellent high temperature performance, multiplying power discharging property;LiODFB also compensates for LiBOB not simultaneously
Foot: the SEI film formed on graphite is more stable, impedance is smaller, and, wetability lower than LiBOB viscosity is more preferable, it is linear to be more soluble in
In carbonate solvent, also there is superior security performance.
But have in the prior art to the raw material boron trifluoride ether solution used in the preparation of difluorine oxalic acid boracic acid lithium strong
Strong irritation and aggressive meets open fire burning, harm is brought to staff's health and environment, to the corrosion resistance of equipment
Energy requirement with higher, cost of investment are big.
Summary of the invention
The object of the invention is that overcoming above-mentioned deficiency, a kind of preparation method of difluorine oxalic acid boracic acid lithium is provided.
In order to achieve the above objectives, the present invention is implemented according to following technical scheme:
A kind of preparation method of difluorine oxalic acid boracic acid lithium, the reaction raw materials of the difluorine oxalic acid boracic acid lithium are LiBF4, grass
Acid, reaction promoter, organic solvent, crystallization solvent；
The preparation process the following steps are included:
A pretreatment of raw material: being put into vacuum drying furnace for oxalic acid and dry, and guarantees the moisture of oxalic acid less than 1 × 10-4；It will reaction
Auxiliary agent, organic solvent, crystallization solvent are carried out dehydrating respectively, guarantee reaction promoter, organic solvent, crystallization solvent moisture contain
Amount is 2 × 10-5Below；
B reactor vessel processes: all reaction vessels used high pure nitrogen is purged into 15-30min, removes reaction vessel surface
Moisture；Gas in glove box is replaced, the dry high pure nitrogen of cleaning is passed through；
C reaction process one: in glove box, by a certain amount of LiBF4 be added in the reaction vessel of organic solvent into
Row stirring obtains mixed solvent until dissolution；
D reaction process two: a certain amount of oxalic acid is taken to be added to the in the mixed solvent of step C acquisition, in 20 DEG C 55 DEG C of reaction
At a temperature of, stir 2h 4h；It continues thereafter with and a certain amount of reaction promoter is added, after reaction promoter addition, continue to stir
It mixes, under 20 DEG C 55 DEG C of reaction temperature, stirs 2h 4h；Obtain mixing liquid；
E filtering and concentrating: after obtained mixing liquid is filtered, filtered fluid will be obtained and be concentrated, concentrate is obtained；It will be dense
After a certain amount of crystallization solvent is added in contracting liquid, solid is obtained by filtration；Under vacuum conditions by the solid being obtained by filtration, dry
For 24 hours after 36h, difluorine oxalic acid boracic acid lithium is obtained.
Preferably, the reaction promoter is silicon tetrachloride.
Preferably, the organic solvent is dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, one in ethyl acetate
Kind.
Preferably, the crystallization solvent is one of methylene chloride, toluene, normal heptane, carbon tetrachloride.
Preferably, the ratio between oxalic acid and the amount of LiBF4 substance are 0.90:1 1.2:1.
Preferably, the mass ratio 1:50 1:80 of the concentrate and crystallization solvent.
Preferably, the ratio between reaction promoter and the amount of LiBF4 substance are 0.6:1 0.8:1.
Action principle of the invention:
The raw material that the present invention uses is LiBF4, oxalic acid, reaction promoter, organic solvent, crystallization solvent, several raw materials.
Key reaction process of the invention is as follows:
2C2H2O4+SiCl4+2LiBF4=2LiBF2(C2O4)+SiF4+4HCl
Nonhazardous product generates in reaction process, and the sour gas for reacting generation only needs to be absorbed using lye, whole
A reaction process and traditional technical process comparatively more safety and environmental protection.
Compared with prior art, the invention has the benefit that
The preparation of difluorine oxalic acid boracic acid lithium of the invention, simple process is easy to operate, can be obtained without complicated equipment
Difluorine oxalic acid boracic acid lithium；Nonhazardous product generates in the preparation process of difluorine oxalic acid boracic acid lithium of the invention, safety and environmental protection, reaction
The readily treated absorption of exhaust gas that process generates, offal treatment are at low cost.
Specific embodiment
With specific embodiment, the invention will be further described below, the invention illustrative examples and illustrate to use
Explain the present invention, but not as a limitation of the invention.
Embodiment 1
A kind of preparation method of difluorine oxalic acid boracic acid lithium, the reaction raw materials of the difluorine oxalic acid boracic acid lithium are LiBF4, grass
Acid, reaction promoter, organic solvent, crystallization solvent；
The preparation process the following steps are included:
A pretreatment of raw material: being put into vacuum drying furnace for oxalic acid and dry, and guarantees the moisture of oxalic acid less than 1 × 10-4；It will reaction
Auxiliary agent, organic solvent, crystallization solvent are carried out dehydrating respectively, guarantee reaction promoter, organic solvent, crystallization solvent moisture contain
Amount is 2 × 10-5Below；
B reactor vessel processes: all reaction vessels used high pure nitrogen is purged into 20min, removes reaction vessel surface
Moisture；Gas in glove box is replaced, the dry high pure nitrogen of cleaning is passed through；
C reaction process one: in glove box, by a certain amount of LiBF4 be added in the reaction vessel of organic solvent into
Row stirring obtains mixed solvent until dissolution；
D reaction process two: taking a certain amount of oxalic acid to be added to the in the mixed solvent of step C acquisition, under 37 DEG C of reaction temperature,
Stir 3h；It continues thereafter with and a certain amount of reaction promoter is added, after reaction promoter addition, continue to stir, at 37 DEG C
Under reaction temperature, 3h is stirred；Obtain mixing liquid；
E filtering and concentrating: after obtained mixing liquid is filtered, filtered fluid will be obtained and be concentrated, concentrate is obtained；It will be dense
After a certain amount of crystallization solvent is added in contracting liquid, solid is obtained by filtration；Under vacuum conditions by the solid being obtained by filtration, dry
After 30h, difluorine oxalic acid boracic acid lithium is obtained.
Wherein, reaction promoter is silicon tetrachloride；Organic solvent selects dimethyl carbonate；Crystallization solvent selects methylene chloride.
Wherein, the ratio between amount of oxalic acid and LiBF4 substance is 1.1:1；The amount of reaction promoter and LiBF4 substance
The ratio between be 0.7:1.
In step E, the mass ratio 1:65 of concentrate and crystallization solvent.
Embodiment 2
A kind of preparation method of difluorine oxalic acid boracic acid lithium, the reaction raw materials of the difluorine oxalic acid boracic acid lithium are LiBF4, grass
Acid, reaction promoter, organic solvent, crystallization solvent；
The preparation process the following steps are included:
A pretreatment of raw material: being put into vacuum drying furnace for oxalic acid and dry, and guarantees the moisture of oxalic acid less than 1 × 10-4；It will reaction
Auxiliary agent, organic solvent, crystallization solvent are carried out dehydrating respectively, guarantee reaction promoter, organic solvent, crystallization solvent moisture contain
Amount is 2 × 10-5Below；
B reactor vessel processes: all reaction vessels used high pure nitrogen is purged into 15min, removes reaction vessel surface
Moisture；Gas in glove box is replaced, the dry high pure nitrogen of cleaning is passed through；
C reaction process one: in glove box, by a certain amount of LiBF4 be added in the reaction vessel of organic solvent into
Row stirring obtains mixed solvent until dissolution；
D reaction process two: taking a certain amount of oxalic acid to be added to the in the mixed solvent of step C acquisition, under 20 DEG C of reaction temperature,
Stir 4h；It continues thereafter with and a certain amount of reaction promoter is added, after reaction promoter addition, continue to stir, at 20 DEG C
Under reaction temperature, 4h is stirred；Obtain mixing liquid；
E filtering and concentrating: after obtained mixing liquid is filtered, filtered fluid will be obtained and be concentrated, concentrate is obtained；It will be dense
After a certain amount of crystallization solvent is added in contracting liquid, solid is obtained by filtration；Under vacuum conditions by the solid being obtained by filtration, dry
For 24 hours after h, difluorine oxalic acid boracic acid lithium is obtained.
Wherein, reaction promoter is silicon tetrachloride；Organic solvent selects diethyl carbonate；Crystallization solvent selects normal heptane.
Wherein, the ratio between amount of oxalic acid and LiBF4 substance is 0.90:1；Reaction promoter and LiBF4 substance
The ratio between amount is 0.6:1.
In step E, the mass ratio 1:50 of concentrate and crystallization solvent.
Embodiment 3
A kind of preparation method of difluorine oxalic acid boracic acid lithium, the reaction raw materials of the difluorine oxalic acid boracic acid lithium are LiBF4, grass
Acid, reaction promoter, organic solvent, crystallization solvent；
The preparation process the following steps are included:
A pretreatment of raw material: being put into vacuum drying furnace for oxalic acid and dry, and guarantees the moisture of oxalic acid less than 1 × 10-4；It will reaction
Auxiliary agent, organic solvent, crystallization solvent are carried out dehydrating respectively, guarantee reaction promoter, organic solvent, crystallization solvent moisture contain
Amount is 2 × 10-5Below；
B reactor vessel processes: all reaction vessels used high pure nitrogen is purged into 30min, removes reaction vessel surface
Moisture；Gas in glove box is replaced, the dry high pure nitrogen of cleaning is passed through；
C reaction process one: in glove box, by a certain amount of LiBF4 be added in the reaction vessel of organic solvent into
Row stirring obtains mixed solvent until dissolution；
D reaction process two: taking a certain amount of oxalic acid to be added to the in the mixed solvent of step C acquisition, under 55 DEG C of reaction temperature,
Stir 2h；It continues thereafter with and a certain amount of reaction promoter is added, after reaction promoter addition, continue to stir, at 55 DEG C
Under reaction temperature, 2h is stirred；Obtain mixing liquid；
E filtering and concentrating: after obtained mixing liquid is filtered, filtered fluid will be obtained and be concentrated, concentrate is obtained；It will be dense
After a certain amount of crystallization solvent is added in contracting liquid, solid is obtained by filtration；Under vacuum conditions by the solid being obtained by filtration, dry
After 36h, difluorine oxalic acid boracic acid lithium is obtained.
Wherein, reaction promoter is silicon tetrachloride；Organic solvent selects methyl ethyl carbonate；Crystallization solvent selects toluene.
Wherein, the ratio between amount of oxalic acid and LiBF4 substance is 1.2:1；The amount of reaction promoter and LiBF4 substance
The ratio between be 0.8:1.
In step E, the mass ratio 1:80 of concentrate and crystallization solvent.
The limitation that technical solution of the present invention is not limited to the above specific embodiments, it is all to do according to the technique and scheme of the present invention
Technology deformation out, falls within the scope of protection of the present invention.
Claims (7)
1. a kind of preparation method of difluorine oxalic acid boracic acid lithium, it is characterised in that: the reaction raw materials of the difluorine oxalic acid boracic acid lithium are
LiBF4, oxalic acid, reaction promoter, organic solvent, crystallization solvent；
The preparation process the following steps are included:
A pretreatment of raw material: being put into vacuum drying furnace for oxalic acid and dry, and guarantees the moisture of oxalic acid less than 1 × 10-4；It will reaction
Auxiliary agent, organic solvent, crystallization solvent are carried out dehydrating respectively, guarantee reaction promoter, organic solvent, crystallization solvent moisture contain
Amount is 2 × 10-5Below；
B reactor vessel processes: all reaction vessels used high pure nitrogen is purged into 15-30min, removes reaction vessel surface
Moisture；Gas in glove box is replaced, the dry high pure nitrogen of cleaning is passed through；
C reaction process one: in glove box, by a certain amount of LiBF4 be added in the reaction vessel of organic solvent into
Row stirring obtains mixed solvent until dissolution；
D reaction process two: a certain amount of oxalic acid is taken to be added to the in the mixed solvent of step C acquisition, in 20 DEG C 55 DEG C of reaction
At a temperature of, stir 2h 4h；It continues thereafter with and a certain amount of reaction promoter is added, after reaction promoter addition, continue to stir
It mixes, under 20 DEG C 55 DEG C of reaction temperature, stirs 2h 4h；Obtain mixing liquid；
E filtering and concentrating: after obtained mixing liquid is filtered, filtered fluid will be obtained and be concentrated, concentrate is obtained；It will be dense
After a certain amount of crystallization solvent is added in contracting liquid, solid is obtained by filtration；Under vacuum conditions by the solid being obtained by filtration, dry
For 24 hours after 36h, difluorine oxalic acid boracic acid lithium is obtained.
2. a kind of preparation method of difluorine oxalic acid boracic acid lithium according to claim 1, it is characterised in that: the reaction promoter
For silicon tetrachloride.
3. a kind of preparation method of difluorine oxalic acid boracic acid lithium according to claim 1, it is characterised in that: the organic solvent
For one of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, ethyl acetate.
4. a kind of preparation method of difluorine oxalic acid boracic acid lithium according to claim 1, it is characterised in that: the crystallization solvent
For one of methylene chloride, toluene, normal heptane, carbon tetrachloride.
5. a kind of preparation method of difluorine oxalic acid boracic acid lithium according to claim 1, it is characterised in that: oxalic acid and tetrafluoro boron
The ratio between the amount of sour lithium substance is 0.90:1 1.2:1.
6. a kind of preparation method of difluorine oxalic acid boracic acid lithium according to claim 1, it is characterised in that: the concentrate with
The mass ratio 1:50 1:80 of crystallization solvent.
7. a kind of preparation method of difluorine oxalic acid boracic acid lithium according to claim 1, it is characterised in that: reaction promoter and four
The ratio between the amount of lithium fluoroborate substance is 0.6:1 0.8:1.
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Cited By (3)
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| CN111533763A (en) * | 2020-07-09 | 2020-08-14 | 山东海科创新研究院有限公司 | Preparation method and preparation device of lithium difluoroborate |
| CN112625055A (en) * | 2019-10-08 | 2021-04-09 | 杉杉新材料（衢州）有限公司 | Method for purifying lithium difluorooxalate borate and lithium tetrafluoroborate mixed lithium salt and application thereof |
| CN114349775A (en) * | 2022-01-12 | 2022-04-15 | 王怀英 | Method for joint production of lithium bis (oxalato) borate and lithium difluoro (oxalato) borate |
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| CN112625055A (en) * | 2019-10-08 | 2021-04-09 | 杉杉新材料（衢州）有限公司 | Method for purifying lithium difluorooxalate borate and lithium tetrafluoroborate mixed lithium salt and application thereof |
| CN111533763A (en) * | 2020-07-09 | 2020-08-14 | 山东海科创新研究院有限公司 | Preparation method and preparation device of lithium difluoroborate |
| CN114349775A (en) * | 2022-01-12 | 2022-04-15 | 王怀英 | Method for joint production of lithium bis (oxalato) borate and lithium difluoro (oxalato) borate |
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