Low-chloride electrolyte
A technology for chloride ions and chloride ion content, applied in non-aqueous electrolytes, non-aqueous electrolyte batteries, circuits, etc., can solve problems such as inability to meet purity requirements
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[0173] In the following, the symbols "%" and "ppm" are always understood to mean % by weight and "ppm by weight", respectively.
[0174] "Inert gas conditions" or inert gas means that the water and oxygen content of the atmosphere is below 1 ppm.
[0175] Determination of chloride ion and hexafluorophosphate content:
[0176]For the ion chromatography method used in the context of this work, reference publication, L. Terborg, S. Nowak, S. Passerini, M. Winter, U. Karst, P. R. Haddad, P. N. Nesterenko, Hydrolysates of hexafluorophosphate Ion chromatographic determination of hydrolysis products of hexafluorophosphate salts in a queous solution, Analytica Chimica Acta 714 (2012) 121 - 126 and references cited therein.
[0177] Analysis of the chloride and hexafluorophosphate ions present was performed by ion chromatography. For this purpose, the following instruments and settings were used:
[0178] Instrument type: DionexICS2100
[0179] column: AS202*250-mm "Analytical co...
example 1
[0211] Example 1: Preparation of lithium hexafluorophosphate (saturated) in acetonitrile
[0212] 250 ml of acetonitrile and 25.61 g of lithium fluoride were charged at room temperature into a 500 ml Teflon apparatus filled with argon. Into the resulting suspension were introduced first 180 g of hydrogen chloride gas and then 186.58 g of gaseous phosphorus pentafluoride. The obtained reaction mixture was stirred for one hour. The reaction mixture was filtered and the solid obtained was blown dry under a flow of argon. This yielded 153 g of solid (44% yield).
[0213] Characterization of solids:
example 2
[0214] Example 2: Preparation of lithium hexafluorophosphate in acetonitrile and subsequent precipitation with toluene
[0215] 250 ml of acetonitrile and 6.49 g of lithium fluoride were charged at room temperature into a 500 ml Teflon apparatus filled with argon. Into the resulting suspension were introduced first 27.35 g of hydrogen chloride gas (chloride ion content of the suspension after introduction: 12.1% by weight) and then 47.24 g of gaseous phosphorus pentafluoride. The obtained reaction mixture was stirred for one hour. The reaction mixture is metered into 500 ml of toluene. The precipitated solid was filtered off and blown dry under a stream of argon. This yielded 34.7 g of solid (91% yield).
[0216] Characterization of solids:
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