CN109232629A - The preparation method of di-oxalate lithium borate - Google Patents
The preparation method of di-oxalate lithium borate Download PDFInfo
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- CN109232629A CN109232629A CN201811430406.8A CN201811430406A CN109232629A CN 109232629 A CN109232629 A CN 109232629A CN 201811430406 A CN201811430406 A CN 201811430406A CN 109232629 A CN109232629 A CN 109232629A
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- lithium borate
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- temperature
- oxalate
- filtrate
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- DEUISMFZZMAAOJ-UHFFFAOYSA-N lithium dihydrogen borate oxalic acid Chemical compound B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] DEUISMFZZMAAOJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 78
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 75
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 25
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004327 boric acid Substances 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 16
- 230000008020 evaporation Effects 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000002274 desiccant Substances 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 description 9
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical group O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 238000002329 infrared spectrum Methods 0.000 description 4
- 159000000002 lithium salts Chemical class 0.000 description 4
- 244000025254 Cannabis sativa Species 0.000 description 3
- 229910003867 O—B—O Inorganic materials 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 3
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 2
- 229910013188 LiBOB Inorganic materials 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- RVWKVYGFLYAWBZ-UHFFFAOYSA-M [Li+].[OH-].OB(O)O Chemical compound [Li+].[OH-].OB(O)O RVWKVYGFLYAWBZ-UHFFFAOYSA-M 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Secondary Cells (AREA)
Abstract
The present invention provides a kind of preparation methods of di-oxalate lithium borate, lithium hydroxide is weighed by certain mol proportion, oxalic acid and boric acid, later respectively by lithium hydroxide, oxalic acid and boric acid drying, again by the lithium hydroxide after drying, oxalic acid and boric acid are placed in ball milling in ball mill and form mixture, then by mixture, dry-pressing is fitted into that temperature is first placed in container is that 5~8h is reacted under 105~130 DEG C of vacuum environment afterwards in flakes under certain pressure P, being placed in temperature again is reaction 12 under 140~170 DEG C of vacuum environment~for 24 hours, di-oxalate lithium borate crude product is made, then di-oxalate lithium borate crude product is pulverized last be substantially soluble in the processed anhydrous acetonitrile of distillation, filtrate is obtained after filtering, filtrate is concentrated by evaporation to 1~2% that residual liquid is filtrate total amount, finally outwell residual liquid, it will filter Liquid is concentrated by evaporation product drying obtained and di-oxalate lithium borate is made.The method of the present invention, simple process, raw material is cheap and easy to get, and product purity obtained is higher.
Description
Technical field
The present invention relates to a kind of preparation methods of di-oxalate lithium borate.
Background technique
Main electrolyte lithium salt used in lithium battery electrolytes has on the market at present: 1, lithium hexafluoro phosphate, manufacture
Complex process, preparation condition is very harsh, very sensitive to moisture, and cost of material is relatively high, and thermal stability is poor, with
Lithium hexafluoro phosphate is not especially good as the battery cryogenic property that electrolyte lithium salt forms；2, LiBF4: due to preparing item
The limitation of part, existing technique hardly result in the LiBF4 of high-purity, now obtained to typically contain very more impurity,
It is easy to react with the active material of lithium ion secondary battery in use, prevent battery is from normal use etc..And double grass
Sour lithium borate is compared as a kind of novel electrolytes lithium salts with LiPF6, has that filming performance is good, thermal stability is strong, high-temperature behavior
Good, decomposition voltage is formally applied in lithium battery electrolytes compared with high, environmental pollution is small.Therefore, how to prepare purity compared with
High di-oxalate lithium borate also just becomes a current research direction.
Summary of the invention
The present invention is intended to provide a kind of preparation method of the higher di-oxalate lithium borate of simple process, product purity.
The present invention is realized by the following scheme:
A kind of preparation method of di-oxalate lithium borate weighs lithium hydroxide, oxalic acid and boric acid, Zhi Houfen by certain mol proportion
Lithium hydroxide, oxalic acid and boric acid are not dried, then that lithium hydroxide, oxalic acid and the boric acid after drying is placed in ball milling in ball mill is equal
Even formation mixture, then by mixture under certain pressure P dry-pressing be fitted into afterwards in container in flakes be first placed in temperature be 105~
5~8h is reacted under 130 DEG C of vacuum environment, then being placed in temperature is reaction 12 under 140~170 DEG C of vacuum environment~for 24 hours, is made
Then di-oxalate lithium borate crude product is pulverized and last is substantially soluble in the processed nothing of distillation by di-oxalate lithium borate crude product
In water-acetonitrile, filtrate is obtained after filtering, and filtrate is concentrated by evaporation to 1~2% that residual liquid is filtrate total amount, is finally outwelled residual
Filtrate is concentrated by evaporation product drying obtained and di-oxalate lithium borate (LiBOB) is made by liquid stay.
Further, the molar ratio of the lithium hydroxide, oxalic acid and boric acid is 1:2:1.
Further, the lithium hydroxide, oxalic acid and boric acid drying specifically comprises the processes of: the lithium hydroxide, oxalic acid and
Boric acid drying specifically comprises the processes of: lithium hydroxide and boric acid are placed in the baking oven that temperature is 50~70 DEG C and shelve 4~6h, it will be careless
Acid is placed in the baking oven that temperature is 105~130 DEG C and shelves 4~6h.
Further, the filtrate is concentrated by evaporation the drying process of product obtained specifically: is concentrated by evaporation filtrate and makes
The product obtained is placed in dry 8~12h in the vacuum oven that temperature is 105~130 DEG C.
Further, the pressure P is 0.18~0.25MPa.
Further, the preparation process of the processed anhydrous acetonitrile of distillation specifically: anhydrous acetonitrile is placed in container
In, desiccant is added into container later, 4~5h of reflow treatment under the conditions of temperature is 90~96 DEG C is finally 100 in temperature
Distillation processing is until be evaporated obtained under the conditions of~110 DEG C.
Further, the desiccant is phosphorus pentoxide.
Further, the lithium hydroxide, oxalic acid and boric acid are placed in ball milling in ball mill and form the specific of mixture
Technique are as follows: lithium hydroxide and oxalic acid are first placed in ball milling certain time in ball mill, ball in ball mill is added in boric acid again later
Certain time is ground, until forming uniform mixture.Ball-milling Time can be adjusted as needed, generally 10~30min.
The preparation method of di-oxalate lithium borate of the invention, simple process is feasible, and the purity of product obtained is higher, can
Up to 99.9% or more, product obtained is used as the lithium salts of lithium battery electrolytes, can be reduced the impedance of electrolyte, be can be improved
Filming performance, thermal stability of electrolyte etc..The raw material that the method for the present invention uses is cheap and easy to get, and preparation process is simple, to ring
Border is substantially pollution-free.
Detailed description of the invention
Fig. 1 is the infrared spectrum of di-oxalate lithium borate made from preparation method using di-oxalate lithium borate in embodiment 1.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited to the statements of embodiment.
Embodiment 1
A kind of preparation method of di-oxalate lithium borate is that 1:2:1 is weighed respectively by the molar ratio of lithium hydroxide, oxalic acid and boric acid
Lithium hydroxide and boric acid are placed in the baking oven that temperature is 60 DEG C shelve 4h later by substance, and it is 120 DEG C that oxalic acid, which is placed in temperature,
Shelve 4h in baking oven, then by after drying lithium hydroxide and oxalic acid be placed in ball milling 15min in ball mill, later by the boron after drying
Ball milling 15min in ball mill is added in acid, until uniform mixture is formed, then by mixture dry-pressing under the pressure of 0.2MPa
Being fitted into after in flakes and being first placed in temperature in container is that 6h is reacted in 120 DEG C of vacuum tank, and height-regulating vacuum tank temperature is to 150 DEG C later,
So that mixture, which is placed in the vacuum tank that temperature is 150 DEG C, reacts 15h, di-oxalate lithium borate crude product is made, then by double grass
Sour lithium borate crude product pulverize it is last be substantially soluble in the processed anhydrous acetonitrile of distillation, filtrate is obtained after filtering, will be filtered
Liquid is concentrated by evaporation to 1% that residual liquid is filtrate total amount, finally outwells residual liquid, and filtrate is concentrated by evaporation product obtained
It is placed in dry 10h in the vacuum oven that temperature is 120 DEG C and di-oxalate lithium borate (LiBOB) is made.
Distill the preparation process of processed anhydrous acetonitrile specifically: anhydrous acetonitrile is placed in container, later toward container
Middle addition phosphorus pentoxide, reflow treatment 4h under the conditions of temperature is 94 DEG C, finally distillation is handled under the conditions of temperature is 100 DEG C
Until being evaporated obtained.
Will use 1 method of embodiment made from di-oxalate lithium borate carry out infrared analysis, infrared spectrum as shown in Figure 1,
Go out peak position according to the infrared spectrum of Fig. 1 di-oxalate lithium borate obtained and its corresponding functional group's list is as shown in table 1, ties
Table 1 and Fig. 1 are closed it is found that functional using di-oxalate lithium borate made from 1 method of embodiment, meets lithium battery electrolytes use
It is required that.
The infrared spectrum of 1 di-oxalate lithium borate of table goes out peak position and its corresponding functional group's list
| Peak position/(cm out-1) | Corresponding functional group |
| 3432.5 | OH in the crystallization water |
| 1818.2 | C=O asymmetric stretch |
| 1778.72 | C=O symmetrically stretches |
| 1638.1 | COO-Asymmetric stretch |
| 1442.33 | COO-It is symmetrical flexible |
| 1364.06 | B-O stretching vibration |
| 1307.6 | C-O-B-O-C stretching vibration |
| 1220.64 | C-O-C asymmetric stretching vibration |
| 1088.42 | O-B-O symmetrical stretching vibration |
| 997.88 | O-B-O symmetrical stretching vibration |
| 983.31 | O-B-O asymmetric stretching vibration |
| 710.1 | COO-Symmetrical stretching vibration |
| 609.13 | B-O deformation vibration |
| 490.97 | BO4The vibration of key |
Embodiment 2
A kind of preparation method of di-oxalate lithium borate in the preparation method of di-oxalate lithium borate, step and embodiment 1
The step of it is essentially identical, the difference is that:
1, lithium hydroxide and boric acid, which are placed in the baking oven that temperature is 50 DEG C, shelves 6h, and oxalic acid is placed in the baking that temperature is 130 DEG C
4.5h is shelved in case；
2, the Ball-milling Time of lithium hydroxide and oxalic acid is 25min, the ball milling 25min after boric acid addition；
3, mixture dry-pressing under the pressure of 0.22MPa is fitted into afterwards first is placed in the vacuum that temperature is 130 DEG C in container in flakes
5h is reacted in case, vacuum tank temperature is turned up later to 170 DEG C, so that mixture is placed in reaction in the vacuum tank that temperature is 170 DEG C
Di-oxalate lithium borate crude product is made in 12h；
4, filtrate is concentrated by evaporation to 2% that residual liquid is filtrate total amount；
5, filtrate is concentrated by evaporation product obtained and is placed in the dry obtained double grass of 8h in the vacuum oven that temperature is 130 DEG C
Sour lithium borate；
6, the preparation process of processed anhydrous acetonitrile is distilled specifically: anhydrous acetonitrile is placed in container, later toward appearance
Phosphorus pentoxide is added in device, reflow treatment 4.5h under the conditions of temperature is 96 DEG C finally distills under the conditions of temperature is 105 DEG C
Processing is until be evaporated obtained.
Embodiment 3
A kind of preparation method of di-oxalate lithium borate in the preparation method of di-oxalate lithium borate, step and embodiment 1
The step of it is essentially identical, the difference is that:
1, lithium hydroxide and boric acid, which are placed in the baking oven that temperature is 70 DEG C, shelves 4.5h, and it is 105 DEG C that oxalic acid, which is placed in temperature,
6h is shelved in baking oven；
2, the Ball-milling Time of lithium hydroxide and oxalic acid is 10min, the ball milling 25min after boric acid addition；
3, mixture dry-pressing under the pressure of 0.25MPa is fitted into afterwards first is placed in the vacuum that temperature is 105 DEG C in container in flakes
8h is reacted in case, vacuum tank temperature is turned up later to 140 DEG C, so that mixture is placed in reaction in the vacuum tank that temperature is 140 DEG C
For 24 hours, di-oxalate lithium borate crude product is made；
4, filtrate is concentrated by evaporation to 1.5% that residual liquid is filtrate total amount；
5, filtrate evaporation and concentration product obtained is placed in obtained couple of dry 12h in the vacuum oven that temperature is 105 DEG C
Lithium bis (oxalate) borate；
6, the preparation process of processed anhydrous acetonitrile is distilled specifically: anhydrous acetonitrile is placed in container, later toward appearance
Phosphorus pentoxide is added in device, reflow treatment 5h under the conditions of temperature is 90 DEG C, finally under the conditions of temperature is 110 DEG C at distillation
Reason is until be evaporated obtained.
Claims (8)
1. a kind of preparation method of di-oxalate lithium borate, it is characterised in that: weigh lithium hydroxide, oxalic acid and boron by certain mol proportion
Lithium hydroxide, oxalic acid and boric acid are dried respectively later, then lithium hydroxide, oxalic acid and the boric acid after drying are placed in ball milling by acid
Ball milling forms mixture in machine, and then by mixture, dry-pressing is fitted into container is afterwards first placed in temperature in flakes under certain pressure P
Degree is 5~8h of reaction under 105~130 DEG C of vacuum environment, then is placed under the vacuum environment that temperature is 140~170 DEG C and reacts 12
~for 24 hours, di-oxalate lithium borate crude product is made, then di-oxalate lithium borate crude product is pulverized and last is substantially soluble in distillation
In processed anhydrous acetonitrile, filtrate is obtained after filtering, and filtrate is concentrated by evaporation to 1~2% that residual liquid is filtrate total amount,
Residual liquid is finally outwelled, filtrate is concentrated by evaporation product drying obtained, di-oxalate lithium borate is made.
2. the preparation method of di-oxalate lithium borate as described in claim 1, it is characterised in that: the lithium hydroxide, oxalic acid and
The molar ratio of boric acid is 1:2:1.
3. the preparation method of di-oxalate lithium borate as claimed in claim 2, it is characterised in that: the lithium hydroxide, oxalic acid and
Boric acid drying specifically comprises the processes of: lithium hydroxide and boric acid are placed in the baking oven that temperature is 50~70 DEG C and shelve 4~6h, it will be careless
Acid is placed in the baking oven that temperature is 105~130 DEG C and shelves 4~6h.
4. the preparation method of di-oxalate lithium borate as described in claim 1, it is characterised in that: the filtrate, which is concentrated by evaporation, to be made
Product drying process specifically: filtrate is concentrated by evaporation product obtained and is placed in the vacuum drying that temperature is 105~130 DEG C
Dry 8~12h in case.
5. the preparation method of di-oxalate lithium borate as described in claim 1, it is characterised in that: the pressure P be 0.18~
0.25MPa。
6. the preparation method of di-oxalate lithium borate as described in claim 1, it is characterised in that: the distillation is processed anhydrous
The preparation process of acetonitrile specifically: anhydrous acetonitrile is placed in container, desiccant is added into container later, temperature be 90~
4~5h of reflow treatment under the conditions of 96 DEG C, finally distillation processing is obtained up to being evaporated under the conditions of temperature is 100~110 DEG C.
7. the preparation method of di-oxalate lithium borate as claimed in claim 6, it is characterised in that: the desiccant is five oxidations two
Phosphorus.
8. the preparation method of the di-oxalate lithium borate as described in claim 1~7 is any, it is characterised in that: the lithium hydroxide,
Oxalic acid and boric acid are placed in ball milling in ball mill and form mixture specifically comprises the processes of: lithium hydroxide and oxalic acid are first placed in ball
Later ball milling certain time in ball mill is added again in boric acid by ball milling certain time in grinding machine, until forming uniform mixture.
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Cited By (9)
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|---|---|---|---|---|
| CN109851640A (en) * | 2019-01-17 | 2019-06-07 | 兰州理工大学 | Double oxalic acid lithium phosphates of a kind of difluoro and the preparation method and application thereof |
| CN111057079A (en) * | 2019-12-16 | 2020-04-24 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium bis (oxalato) borate and lithium bis (oxalato) borate |
| CN111057082A (en) * | 2019-12-26 | 2020-04-24 | 天津金牛电源材料有限责任公司 | Preparation method of lithium bis (oxalato) borate |
| CN111116624A (en) * | 2019-12-26 | 2020-05-08 | 天津金牛电源材料有限责任公司 | Preparation method of lithium bis (oxalato) borate |
| CN112409393A (en) * | 2020-12-11 | 2021-02-26 | 临沂小篆新材料科技有限公司 | Process for preparing lithium bis (oxalato) borate |
| CN114057784A (en) * | 2022-01-17 | 2022-02-18 | 山东海科创新研究院有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN114181240A (en) * | 2021-12-28 | 2022-03-15 | 山东海科创新研究院有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN114671899A (en) * | 2022-03-28 | 2022-06-28 | 珠海市赛纬电子材料股份有限公司 | Preparation method of lithium bis (oxalato) borate and application of lithium bis (oxalato) borate |
| WO2023000198A1 (en) * | 2021-07-21 | 2023-01-26 | 江苏华盛锂电材料股份有限公司 | Method for preparing lithium bisoxalate borate and method for preparing lithium-ion battery electrolyte |
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| CN111057079A (en) * | 2019-12-16 | 2020-04-24 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium bis (oxalato) borate and lithium bis (oxalato) borate |
| CN111057082A (en) * | 2019-12-26 | 2020-04-24 | 天津金牛电源材料有限责任公司 | Preparation method of lithium bis (oxalato) borate |
| CN111116624A (en) * | 2019-12-26 | 2020-05-08 | 天津金牛电源材料有限责任公司 | Preparation method of lithium bis (oxalato) borate |
| CN112409393A (en) * | 2020-12-11 | 2021-02-26 | 临沂小篆新材料科技有限公司 | Process for preparing lithium bis (oxalato) borate |
| WO2023000198A1 (en) * | 2021-07-21 | 2023-01-26 | 江苏华盛锂电材料股份有限公司 | Method for preparing lithium bisoxalate borate and method for preparing lithium-ion battery electrolyte |
| CN114181240A (en) * | 2021-12-28 | 2022-03-15 | 山东海科创新研究院有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN114181240B (en) * | 2021-12-28 | 2023-09-22 | 山东海科创新研究院有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN114057784A (en) * | 2022-01-17 | 2022-02-18 | 山东海科创新研究院有限公司 | Preparation method of lithium bis (oxalato) borate |
| CN114671899A (en) * | 2022-03-28 | 2022-06-28 | 珠海市赛纬电子材料股份有限公司 | Preparation method of lithium bis (oxalato) borate and application of lithium bis (oxalato) borate |
| WO2023184704A1 (en) * | 2022-03-28 | 2023-10-05 | 珠海市赛纬电子材料股份有限公司 | Preparation method for lithium bis(oxalato)borate and use thereof |
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