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Production of high-purity lithium difluorophosphate

A technology of lithium difluorophosphate and lithium fluoride, which is applied in the field of low-sodium lithium difluorophosphate, sodium or potassium ions, and can solve problems such as inability to meet purity requirements and complexity

Inactive Publication Date: 2015-06-03
LANXESS DEUTDCHLAND GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The prior art shows that achieving the high purity of lithium difluorophosphate and especially keeping the content of foreign metal ions and chloride ions low is technically very complex
The methods known hitherto for the preparation of lithium difluorophosphate are therefore not able to meet every purity requirement

Method used

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  • Production of high-purity lithium difluorophosphate
  • Production of high-purity lithium difluorophosphate

Examples

Experimental program
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preparation example Construction

[0106] pass figure 1 The preparation of lithium fluoride will be described in detail.

[0107] In a device 1 for preparing lithium fluoride, water (H 2 O) makes solid lithium carbonate (Li 2 CO 3 (s)) suspend and, if the device 1 is not filled for the first time, the filtrate from the filter unit 19 in the reservoir 3, and the lithium carbonate at least partly go into solution. The suspension thus obtained is conveyed via line 4 by pump 5 to a filtration unit 6 (here in the form of a cross-flow filter), wherein undissolved lithium carbonate is recycled via line 7 to storage 3, and The filtrate (aqueous medium containing dissolved lithium carbonate) is introduced from line 8 into reactor 9 . In the reactor 9, a gas stream comprising gaseous hydrogen fluoride (which here comprises gaseous hydrogen fluoride and nitrogen) is introduced via line 10 into the gas space 11 of the reactor (which is above the liquid space 12 of the reactor) . A pump 13 directs the contents of the ...

example

[0191] The unit "%" is to be understood hereinafter always as meaning % by weight.

[0192] Regarding the ion chromatography method used in the course of this study, reference is made to a publication of the TU Bergakademie Freiberg, Faculty of Chemistry and Physics, Department of Analytical Chemistry, March 2002 , and the literature cited therein.

[0193] During the course of this study, LiPO 2 f 2 The concentrations were measured using an ion chromatograph with the following parameters:

[0194] Instrument type: Dionex ICS 2100

[0195] column: AS202*250-mm "analytical column with guard"

[0196] Sample volume: 1μl

[0197] Eluent: KOH Gradient: 0min / 15mM, 10min / 15mM, 13min / 80mM, 27min / 100mM, 27.1min / 15mM, 34min / 15mM

[0198] Eluent flow rate: 0.25ml / min

[0199] Temperature: 30°C

[0200] Self-regenerating suppressors: 300(2-mm)

[0201] For LiPO 2 f 2 The obtained signal is specified by 31 P and 19 Confirmed by FNMR spectroscopy. Separation of LiPO from ...

example 1

[0202] Example 1: Preparation of high-purity lithium fluoride

[0203] on a basis figure 1 In the device, the reservoir 3 is initially loaded with 500 g of industrial grade quality (purity: >98% by weight; Na: 231 ppm, K: 98 ppm, Mg: 66 ppm, Ca: 239 ppm) of solid lithium carbonate and 20 l of water, and prepare a suspension at 20°C. After about five minutes, the suspension is directed to a filtration unit 6 (which takes the form of a cross-flow filter), and the resulting medium comprising dissolved lithium carbonate (here a Aqueous solution of lithium carbonate) is led into reactor 9 via line 8.

[0204] After a total of 4 kg of medium has been pumped into the reactor 9, the feed from the filter unit 6 is stopped and the feed of gaseous hydrogen fluoride into the gas space 11 is started in this reactor 9 via pump 13, line 14 and A column 15 with random packing circulates the medium continuously with pumping. This metering was ended when the pH of the solution circulated by...

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Abstract

Producing lithium fluorophosphate, comprises contacting the solid lithium fluoride having a water content of more than 1500 ppm, preferably 5000-15000 ppm with gas containing phosphorus pentafluoride. An independent claim is included for lithium difluorophosphate having a purity of 99.9-99.9995 wt.%, preferably 99.97-99.9995 based on anhydrous product.

Description

Contents of the invention [0001] The invention relates to a process for the preparation of high-purity, especially low-sodium lithium difluorophosphate, especially in the form of a solution thereof in an organic solvent, starting from lithium fluoride and phosphorus pentafluoride. Background technique [0002] The global spread of portable electronic devices, such as laptop and palmtop computers, mobile phones or video cameras, and thus also the demand for lightweight and high-performance batteries and accumulators, has increased considerably over the past few years. This will increase in the future by equipping electric vehicles with accumulators and batteries of this type. [0003] Lithium difluorophosphate (LiPO 2 f 2 ) has attracted industrial interest as a conductive salt as a substitute for lithium hexafluorophosphate in the production of high-performance batteries because it is quite stable. In order to guarantee the functional capacity and life of such accumulator...

Claims

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Application Information

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IPC IPC(8): C01B25/10C01B25/455C01D15/00C01D15/08
CPCC01B25/10C01B25/455C01D15/005C01D15/04Y02E60/10C01D15/00H01M10/0568H01M2300/0025
Inventor 马蒂亚斯·博尔沃尔夫冈·埃文贝克
Owner LANXESS DEUTDCHLAND GMBH
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