CN110305153A - A kind of synthetic method and application of double oxalic acid Boratexes - Google Patents
A kind of synthetic method and application of double oxalic acid Boratexes Download PDFInfo
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- CN110305153A CN110305153A CN201910686922.5A CN201910686922A CN110305153A CN 110305153 A CN110305153 A CN 110305153A CN 201910686922 A CN201910686922 A CN 201910686922A CN 110305153 A CN110305153 A CN 110305153A
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- oxalic acid
- sodium
- boratexes
- double
- double oxalic
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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 155
- 235000006408 oxalic acid Nutrition 0.000 title claims abstract description 52
- 238000010189 synthetic method Methods 0.000 title claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 20
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004327 boric acid Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 16
- 239000011734 sodium Substances 0.000 claims abstract description 16
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 35
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 206010013786 Dry skin Diseases 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005253 cladding Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000003388 sodium compounds Chemical class 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 235000013495 cobalt Nutrition 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 2
- 239000007774 positive electrode material Substances 0.000 claims description 2
- LMHHRCOWPQNFTF-UHFFFAOYSA-N s-propan-2-yl azepane-1-carbothioate Chemical compound CC(C)SC(=O)N1CCCCCC1 LMHHRCOWPQNFTF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 3
- 208000012839 conversion disease Diseases 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 235000010338 boric acid Nutrition 0.000 description 12
- 229960002645 boric acid Drugs 0.000 description 12
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002001 electrolyte material Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 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 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- WYWLPUYJUPVXSK-UHFFFAOYSA-N boron;oxalic acid Chemical compound [B].OC(=O)C(O)=O WYWLPUYJUPVXSK-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 150000005686 dimethyl carbonates Chemical class 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 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 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a kind of synthetic methods of double oxalic acid Boratexes, according to the stoichiometric ratio of each element in double oxalic acid Boratexes, after the compound of a certain amount of boric acid, oxalic acid and sodium is dried at high temperature, it mixes, tabletting carries out solid-solid reaction under the high temperature conditions and obtains white solid, then carries out white solid after thoroughly drying, it is extracted in nonaqueous solvents, extract liquor evaporative crystallization is finally obtained into the double oxalic acid Boratexes of final products.The reaction conversion ratio of process route provided by the present invention is high, and yield is up to 70% or more, and the reaction time is short, and reaction condition is simple to operation, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to electrochemical material fields, and in particular to a kind of synthetic method and application of double oxalic acid Boratexes.
Background technique
The lithium ion secondary battery for developing comparative maturity at present has energy density high, has extended cycle life, self discharge is small etc.
Advantage is widely used as the working power (mobile phone, palm PC etc.) of various portable electronic products, and gradually application is mobile dress
Standby power battery (electric vehicle, submarine etc.).But global lithium resource is not rich, abundance is only 0.006% in the earth's crust, simultaneously
It is unevenly distributed, becomes the suffering of the following large-scale application.
Compared with lithium resource, sodium reserves very abundant, crustal abundance is about 2.64%, also there is a large amount of sodium in seawater.Simultaneously
Sodium and lithium are same major element, and chemical property is close, and the recycling of sodium is more mature cheap, substitutes lithium with sodium, opens
Hair sodium ion secondary battery has broad application prospects.For sodium-ion battery, developing high performance electrolyte is to close very much
The link of key, and high performance sodium salt is the important component for forming electrolyte.It is applied to sodium ion electrolyte material at present
Sodium salt in material mainly has sodium hexafluoro phosphate and sodium perchlorate, and the two is bad for the resistance of micro-moisture, therefore is electrolysed material
Although expecting that ionic conductivity is higher, stability is poor, so that the final cycle performance of battery is bad, requirement is not achieved.
In lithium-ion electrolyte material, boron system lithium salts such as di-oxalate lithium borate and difluorine oxalic acid boracic acid lithium has moisture preferable
Resistance, excellent combination property.So preparing corresponding sodium salt just has very high practical value.
Summary of the invention
The purpose of the present invention is to provide one kind to realize reactant homogeneous reaction in solid middle mixing, in conjunction with organic solvent reality
The extraction of existing active constituent, finally obtains the synthetic method of double oxalic acid Boratexes of high quality of products.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of synthetic method of double oxalic acid Boratexes will be a certain amount of according to the stoichiometric ratio of each element in double oxalic acid Boratexes
Boric acid, oxalic acid and sodium compound be dried at high temperature after, mix, tabletting, carry out under the high temperature conditions solid
Reaction obtains white solid, then carries out after thoroughly drying white solid, is extracted in nonaqueous solvents, finally will extraction
Liquid evaporative crystallization obtains the double oxalic acid Boratexes of final products.
Further, the compound of the sodium can be sodium hydroxide, sodium chloride, sodium isopropylate, sodium sulphate, sodium nitrate, cobalt
One of sour sodium etc..
Further, the molar ratio of the compound of the sodium and oxalic acid is 1:2.5.
Further, include the following steps:
S1, according to the stoichiometric ratio of each element in double oxalic acid Boratexes, by the boric acid, oxalic acid and sodium hydroxide of certain mass；
S2, weighed oxalic acid is handled into 3h in 100 DEG C of vacuum and heating dryings, and boric acid and sodium hydroxide is antivacuum at 65 DEG C
Heat drying handles 3 h；
S3, the boric acid by after the completion of drying, oxalic acid and sodium compound mix, tabletting, 120~180 DEG C of solid-solid reactions 12~
15h obtains white solid；
S4, it after thoroughly drying resulting white solid, is extracted in acetonitrile or dimethyl carbonate solvent, it finally will extraction
Liquid evaporative crystallization obtains double oxalic acid Boratexes that purity reaches 98% or more.
Further, the boric acid, oxalic acid, sodium hydroxide molar ratio be 1:2:1.
Its raw material that can be used as secondary cell of double oxalic acid Boratexes synthesized by the present invention: as secondary battery positive electrode material
Cladding, the raw material of doping or the raw material as secondary cell electrolyte；And it can also be used to synthesize some new materials.
The invention has the following advantages:
The reaction conversion ratio of process route provided by the present invention is high, and yield is up to 70% or more, and the reaction time is short, reaction condition
It is simple to operation, it is easy to accomplish industrialized production.
Detailed description of the invention
Fig. 1 is the infrared spectrogram for double oxalic acid Boratexes that embodiment 1 is prepared.
Fig. 2 is the liquid that double oxalic acid Boratexes that embodiment 2 is prepared are dissolved in mixed solvent SL/DEC=1:1 preparation
The conductivity temperature curve of state electrolyte.
Fig. 3 is the XRD spectra for double oxalic acid Boratexes that embodiment 2 is prepared.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment 1
S1,20.83 g oxalic acid, 4.74 g boric acid, 1.99 g sodium hydroxides are weighed；
S2, weighed oxalic acid is handled into 3h in 100 DEG C of vacuum and heating dryings, and boric acid and sodium hydroxide is antivacuum at 65 DEG C
Heat drying handles 3 h.
S3, the oxalic acid by after the completion of drying, boric acid, sodium hydroxide are placed in round bottom beaker, shake up (about 1 h), 10 M
Pa tabletting, is transferred in beaker, is placed in vacuum oven, after 120 DEG C of 30 min of reaction, is evacuated to 0.07 M pa,
Temperature reacts 12 h under conditions of being 180 DEG C, obtains white solid.
S4, obtained white solid grind into powder is transferred in the beaker equipped with 500 mL acetonitriles, stirs 15 min
After filter, obtained filtrate is evaporated into solvent under the conditions of 65 DEG C, obtains double oxalic acid Boratexes of about 11.5 g, a conversion ratio
About 76%, purity about 99%.
Double oxalic acid boron are provided as shown in Figure 1, in figure by double oxalic acid Boratex infrared spectrograms that the present embodiment is prepared
The infrared spectrogram of sour lithium is for reference.
Embodiment 2
S1,19.33 g oxalic acid, 4.74 g boric acid, 1.99 g sodium hydroxides are weighed；
S2, weighed oxalic acid is handled into 3 h in 110 DEG C of vacuum and heating dryings, and by boric acid and 65 DEG C of antivacuum addings of sodium hydroxide
Heated drying handles 3 h.
S3, the oxalic acid by after the completion of drying, boric acid, sodium hydroxide are placed in round-bottomed flask, are shaken up (about 1h), 10 M
Pa tabletting, is transferred in beaker, is placed in vacuum oven, after 120 DEG C of 45 min of reaction, is evacuated to 0.07 M pa,
12 h are reacted under conditions of temperature is 150 DEG C, obtain white solid.
S4, obtained white solid grind into powder is transferred in the volumetric flask of 500 mL dimethyl carbonates, stirring 15
It is filtered after min, obtained filtrate is evaporated into solvent under the conditions of 65 DEG C, obtains the bis- oxalic acid Boratexes of about 10.5g, it is primary to convert
Rate about 70%, purity about 98%.
Fig. 2 shows double oxalic acid Boratex XRD spectras that the present embodiment 2 is prepared, diffraction maximum is sharply obtained
Preferable double oxalic acid Boratex bodies, and occur without apparent dephasign peak, it can be used as the raw material of positive electrode cladding, doping.
Fig. 3 is the liquid that double oxalic acid Boratexes that the present embodiment is prepared are dissolved in mixed solvent SL/DEC=1:1 preparation
The conductivity temperature curve of electrolyte, it can be seen that its conductivity at room temperature reaches 10~3More than, meet secondary cell for
The requirement of electrolytic conductivity.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (8)
1. a kind of synthetic method of double oxalic acid Boratexes, it is characterised in that: counted according to the chemistry of each element in double oxalic acid Boratexes
Ratio is measured, after the compound of a certain amount of boric acid, oxalic acid and sodium is dried at high temperature, is mixed, tabletting, in high temperature item
Solid-solid reaction is carried out under part and obtains white solid, and then white solid is carried out after thoroughly drying, is extracted in nonaqueous solvents
It takes, extract liquor evaporative crystallization is finally obtained into the double oxalic acid Boratexes of final products.
2. a kind of synthetic method of double oxalic acid Boratexes as described in claim 1, it is characterised in that: the compound of the sodium can
For one of sodium hydroxide, sodium chloride, sodium isopropylate, sodium sulphate, sodium nitrate, cobalt acid sodium.
3. a kind of synthetic method of double oxalic acid Boratexes as described in claim 1, it is characterised in that: the compound of the sodium with
The molar ratio of oxalic acid is 1:2.5.
4. a kind of synthetic method of double oxalic acid Boratexes as described in claim 1, characterized by the following steps:
S1, according to the stoichiometric ratio of each element in double oxalic acid Boratexes, by the boric acid, oxalic acid and sodium hydroxide of certain mass；
S2, weighed oxalic acid is handled into 3h in 100 DEG C of vacuum and heating dryings, and boric acid and sodium hydroxide is antivacuum at 65 DEG C
Heat drying handles 3 h；
S3, the boric acid by after the completion of drying, oxalic acid and sodium compound mix, tabletting, 120~180 DEG C of solid-solid reactions 12~
15h obtains white solid；
S4, it after thoroughly drying resulting white solid, is extracted in acetonitrile or dimethyl carbonate solvent, it finally will extraction
Liquid evaporative crystallization obtains double oxalic acid Boratexes that purity reaches 98% or more.
5. a kind of synthetic method of double oxalic acid Boratexes as claimed in claim 4, it is characterised in that: the boric acid, oxalic acid, hydrogen
The molar ratio of sodium oxide molybdena is 1:2:1.
6. the application of double oxalic acid Boratexes of synthetic method synthesis as claimed in any one of claims 1 to 5, it is characterised in that:
Its raw material that can be used as secondary cell.
7. application as claimed in claim 6, it is characterised in that: it can be used as secondary battery positive electrode material cladding, the original of doping
Material.
8. application as claimed in claim 6, it is characterised in that: its raw material that can be used as secondary cell electrolyte.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115304629A (en) * | 2022-10-09 | 2022-11-08 | 江苏国泰超威新材料有限公司 | Preparation method of sodium difluorooxalate |
| CN115557980A (en) * | 2022-12-06 | 2023-01-03 | 江苏华盛锂电材料股份有限公司 | Synthesis and purification process of sodium bisoxalato |
| CN115850312A (en) * | 2022-12-16 | 2023-03-28 | 山东海科创新研究院有限公司 | Preparation method of sodium bisoxalato borate and obtained product |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627661A (en) * | 2011-09-09 | 2012-08-08 | 兰州理工大学 | Preparation method of lithium bis(oxalato)borate |
| CN103030657A (en) * | 2011-10-10 | 2013-04-10 | 中国科学院福建物质结构研究所 | Preparation method of electrolyte double-oxalate based lithium borate for lithium ion battery |
| KR101358682B1 (en) * | 2013-06-26 | 2014-02-07 | 주식회사 천보정밀 | Synthetic method of lithium bis(oxalato) borate |
| JP2014154446A (en) * | 2013-02-12 | 2014-08-25 | Toyota Motor Corp | Nonaqueous electrolyte secondary battery and method for manufacturing the same |
| CN105732682A (en) * | 2016-03-24 | 2016-07-06 | 洛阳和梦科技有限公司 | Solid-phase production method of lithium-borate-base electrolyte |
| US20160268661A1 (en) * | 2013-11-27 | 2016-09-15 | Unist(Ulsan National Institute Of Science And Technology) | Secondary battery |
-
2019
- 2019-07-29 CN CN201910686922.5A patent/CN110305153A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627661A (en) * | 2011-09-09 | 2012-08-08 | 兰州理工大学 | Preparation method of lithium bis(oxalato)borate |
| CN103030657A (en) * | 2011-10-10 | 2013-04-10 | 中国科学院福建物质结构研究所 | Preparation method of electrolyte double-oxalate based lithium borate for lithium ion battery |
| JP2014154446A (en) * | 2013-02-12 | 2014-08-25 | Toyota Motor Corp | Nonaqueous electrolyte secondary battery and method for manufacturing the same |
| KR101358682B1 (en) * | 2013-06-26 | 2014-02-07 | 주식회사 천보정밀 | Synthetic method of lithium bis(oxalato) borate |
| US20160268661A1 (en) * | 2013-11-27 | 2016-09-15 | Unist(Ulsan National Institute Of Science And Technology) | Secondary battery |
| CN105732682A (en) * | 2016-03-24 | 2016-07-06 | 洛阳和梦科技有限公司 | Solid-phase production method of lithium-borate-base electrolyte |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115304629A (en) * | 2022-10-09 | 2022-11-08 | 江苏国泰超威新材料有限公司 | Preparation method of sodium difluorooxalate |
| CN115557980A (en) * | 2022-12-06 | 2023-01-03 | 江苏华盛锂电材料股份有限公司 | Synthesis and purification process of sodium bisoxalato |
| CN115850312A (en) * | 2022-12-16 | 2023-03-28 | 山东海科创新研究院有限公司 | Preparation method of sodium bisoxalato borate and obtained product |
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