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

Preparation of difluoro chelato borate salts

A borate and chelating technology, applied in the field of preparation of difluoro chelate borate, can solve the problems of unfavorable fluorine, low efficiency loss and the like, and achieve the effects of easy acquisition, avoidance of purification steps and high yield

Inactive Publication Date: 2018-12-21
GOTION INC
View PDF8 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This results in an unfavorable and inefficient loss of fluorine
In addition, fluorine-containing by-products must be removed from the product

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 of difluoro chelato borate salts
  • Preparation of difluoro chelato borate salts
  • Preparation of difluoro chelato borate salts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0155] 38 g of oxalic acid dihydrate, 6 g of boric acid and 30 g of triethylamine were mixed with 150 mL of acetonitrile. 21 g of boron trifluoride-dihydrate were added and the reaction mixture was heated to 120-130° C. while distilling off volatile components. The residue was further dried at 120° C. and 10 mbar for 2 hours. After cooling, triethylammonium difluoro(oxalatoborate) was obtained as a colorless, solidified melt. Quantitative F-NMR showed a purity of 92%, the corresponding tetrafluoroborate (2%) and 6% bis(oxalatoborate) salt.

Embodiment 2

[0157] 38 g of oxalic acid dihydrate, 6 g of boric acid and 30 g of triethylamine were mixed with 150 mL of acetic acid. 21 g of boron trifluoride-dihydrate were added and the reaction mixture was heated to 120-130° C. while distilling off volatile components. The residue was further dried at 120° C. and 10 mbar for 2 hours. After cooling, triethylammonium difluoro(oxalatoborate) was obtained as a colorless, solidified melt. Quantitative F-NMR showed a purity of 93%, the corresponding tetrafluoroborate (3%) and 4% bis(oxalatoborate) salt.

Embodiment 3

[0159] 38 g of oxalic acid dihydrate, 6 g of boric acid and 30 g of triethylamine were mixed with 150 mL of methanol. 21 g of boron trifluoride-dihydrate were added and the reaction mixture was heated to 120-130° C. while distilling off volatile components. The residue was further dried at 120° C. and 10 mbar for 2 hours. After cooling, triethylammonium difluoro(oxalatoborate) was obtained as a colorless, solidified melt. Quantitative F-NMR showed a purity of 88%, the corresponding tetrafluoroborate (6%) and 6% bis(oxalatoborate) salt.

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
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
Login to View More

Abstract

A process for preparing a difluoro chelato borate salt comprising an anion A of formula (I) wherein (I)' is a bidentate radical derived from a 1,2-, 1,3- or 1,4-diol, from a 1,2-, 1,3- or 1,4- dicarboxylic acid or from a 1,2-, 1,3- or 1,4-hydroxycarboxylic acid by abstracting the two H atoms of pairs of adjacent OH groups of the respective diol, hydroxycarboxylic acid or dicarboxylic acid; comprising step (i) reacting (a) one or more BF3 sources; (b) a dihydric compound selected from 1,2-, 1,3- and 1,4-diols, 1,2-, 1,3- and 1,4-dicarboxylic acids, and 1,2-, 1,3- and 1,4-hydroxycarboxylic acids; (c) one or more second boron sources which do not contain F; and (d) one or more proton acceptors.

Description

technical field [0001] The present invention relates to the preparation method of difluorochelate borates (difluorochelatoborates salts). Background technique [0002] Difluorochelate borates such as lithium difluorooxalate borate and ammonium difluorooxalate borate are used in electrolyte compositions for electrochemical cells, see for example US6,783,896B2 and WO2013 / 026854A1. The synthesis of difluoroborate anions usually involves compounds containing fluorine and boron, such as tetrafluoroborate or BF 3 compound. [0003] US 6,783,896 B2 describes by making LiBF 4 Reaction with lithium alkoxide followed by addition of oxalic acid to synthesize lithium difluorooxalate borate. In addition to the desired lithium difluorooxalate borate, LiF is formed which must be removed from the product. [0004] J.L.Allen et al., Journal of Power Sources 196 (2011), pages 9737 to 9742 disclose 3 - ether) with lithium oxalate to prepare difluorooxalate borate. [0005] DE 10 2006 008...

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): C07F5/02H01G9/022H01M6/16
CPCH01G11/62H01M10/0525H01M10/0568C07F5/022C07D213/20C07D295/037Y02E60/10Y02E60/13C07C211/63H01M2300/0025
Inventor 妮可·赫鲁伯于尔根·赫柏林
Owner GOTION INC
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