Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of difluoroborate

A technology of difluorooxalate borate and hydrogen oxalate, which is applied in the field of preparation of difluorooxalate borate, can solve the problems of unfeasible economy, high cost, and many steps, and achieve the control of metal ion and anion impurity content, The effect of short reaction time and simple process

Inactive Publication Date: 2018-11-30
苏州松湖新能源材料有限公司
View PDF7 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As one of them, the preparation method of lithium difluorooxalate borate, such as patent document 1 (Chinese patent: a synthesis process for obtaining lithium difluorooxalate borate and lithium bisoxalate borate; patent number: CN200910144760.9), the method It reacts fluorine-containing compounds, boron-containing compounds, lithium-containing compounds and oxalate-containing compounds in the reaction medium to obtain a solution containing difluorooxalate lithium borate and bisoxalate lithium borate. In this patent, it needs to be filtered The two substances of lithium difluorooxalate borate and bisoxalate lithium borate are separated by organic solvent extraction, and the product is purified by cooling crystallization and recrystallization. There are many steps, the process is very complicated, and it is not easy for industrial production.
Patent Document 2 (European Patent: Process for synthesizing ionic metal complex; Patent No.: EP1308449A2) uses oxalic acid, lithium tetrafluoroborate, lithium fluoride and boron trichloride or trimethoxyboron to react in dimethyl carbonate to obtain di Lithium fluorooxalate borate, but the raw material lithium tetrafluoroborate itself is an additive for lithium-ion batteries, it is difficult to obtain in large quantities, and the cost is high, so it is not economically feasible

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of difluoroborate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a glove box filled with dry argon, add dry lithium hydrogen oxalate (LiHC 2 o 4 ) 48.0g (0.5mol), and phosphorus pentachloride (PCl 5 ) 20.8g (0.1mol), and then add 108g of dry tetrahydrofuran (THF) to the three-necked flask. The flask was taken out from the glove box, placed in a water bath at 35°C and stirred, and boron trifluoride tetrahydrofuran (BF 3 · THF) 73.5g (0.525mol), the reaction started to proceed, the generated gas flowed through the device equipped with sodium hydroxide solution to be absorbed, and the dropwise addition took 2 hours. The solid dissolves slowly, the solution becomes transparent, and is kept at 35°C for one hour, and no gas is emitted from the reaction, indicating that the reaction is complete. Under the protection of argon flow, dichloroethane (CH 2 Cl 2 ) 800mL, stirred slowly at 25°C until crystals precipitated, stopped stirring, after the crystals settled, filtered, and dichloroethane (CH 2 Cl 2 ), and the obtained crystals w...

Embodiment 2

[0029] In a glove box filled with dry argon, add 67.5 g of dry dimethyl carbonate (DMC) to a three-necked flask, and add boron trifluoride dimethyl carbonate (BF 3 DMC) 41.0g, dissolve, then add dry lithium hydrogen oxalate (LiHC 2 o 4 ) 24.0g (0.25mol). The flask was taken out from the glove box, immersed in a 35°C water bath, and kept stirring. Phosphorus trichloride (PCl) was slowly added using a constant pressure dropping funnel 3 ) 13.7g (0.1mol), the reaction began to take place. The generated gas flows into the device equipped with sodium hydroxide solution for absorption. Phosphorus trichloride (PCl 3) took 1.5 hours, and then kept at 35°C for one hour, the reaction solution became clear, and no gas was released, indicating the end of the reaction. The reaction solution was evacuated, while the temperature was raised to 50°C, concentrated and evaporated. Under the protection of argon flow, 800 mL of cyclohexane was added into the flask, and stirred slowly until ...

Embodiment 3

[0032] In a dry argon glove box, add 55.6 g of dry ether (Ether) to the three-necked flask, and then put 24.0 g (0.25 mol) of fully dried lithium hydrogen oxalate and 36.9 g of boron trifluoride ether into the flask, One mouth of the flask was connected to a gas conduit with a valve, and the other two mouths were plugged with stoppers. The flask was taken out of the glove box, immersed in a water bath at 40 °C, and the mixture was continuously stirred. Silicon tetrachloride (SiCl) was slowly added dropwise using a constant pressure dropping funnel 4 ) 11.9g (0.07mol), the reaction began to take place. The generated gas flows into the device equipped with sodium hydroxide solution for absorption. Silicon tetrachloride (SiCl 4 ) for 1 hour, and then kept at 40°C for 1 hour, the reaction solution became clear, and no gas was released, indicating the end of the reaction. The temperature was raised to 40°C, and the solvent was evaporated. Under the protection of argon flow, di...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
crystallization temperatureaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of a difluoroborate. The preparation method comprises following steps: 1, a boron trifluoride complex is dissolved in an aprotic solvent, a dioxalate and achloride are added, and reaction is carried out so as to obtain a difluoroborate solution; and 2, the difluoroborate solution is subjected to degassing concentration, a poor solvent is added for crystallization precipitation of the difluoroborate, and filtering, washing, and drying are carried out so as to obtain the difluoroborate. The preparation method is simple; reaction time is short; yieldis high; the contents of metal ions and negative ion impurities can be controlled effectively, and the high purity difluoroborate target product can be prepared.

Description

technical field [0001] The invention relates to a method for preparing difluorooxalate borate which can be used as an additive for non-aqueous electrolyte batteries. Background technique [0002] Difluorooxalate borate can be used as an additive for non-aqueous electrolyte batteries. For example, lithium difluorooxalate borate can be used as an additive for non-aqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors, and sodium difluorooxalate borate can be used as an additive for sodium ion batteries. As one of them, the preparation method of lithium difluorooxalate borate, such as patent document 1 (Chinese patent: a synthesis process for obtaining lithium difluorooxalate borate and lithium bisoxalate borate; patent number: CN200910144760.9), the method It reacts fluorine-containing compounds, boron-containing compounds, lithium-containing compounds and oxalate-containing compounds in the reaction medium to obtain a solution containing diflu...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 周文超赵喜波
Owner 苏州松湖新能源材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com