Method for electrochemical synthesis of lithium imidodifluorosulfonate

A technology of lithium bisfluorosulfonate imide and bisfluorosulfonate imide is applied in the field of electrochemical synthesis of lithium bisfluorosulfonate imide, which can solve the problem that the purity of bisfluorosulfonate imide is difficult to meet the battery-grade standard , can not directly enter the large-scale industrial application and other problems, to achieve the effect of low cost, low energy consumption and simple process

Active Publication Date: 2020-02-04
LANZHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Above-mentioned synthesis method uses fluorine or chloride metal salt as the catalyzer of dichlorosulfonic acid imide (HClSI) fluorination, has introduced other heteroatoms in th...

Method used

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  • Method for electrochemical synthesis of lithium imidodifluorosulfonate
  • Method for electrochemical synthesis of lithium imidodifluorosulfonate
  • Method for electrochemical synthesis of lithium imidodifluorosulfonate

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Embodiment 1

[0030] A method for electrochemically synthesizing lithium bisfluorosulfonate, comprising the following steps:

[0031] Step 1, synthesis of dichlorosulfonate imide: under magnetic stirring (1000-1500 rpm), add 300g thionyl chloride (SOCl 2 ) and 500g chlorosulfonic acid (CISO 3 H) Add 110g of ammonium chloride (NH 4 Cl), heating the temperature of the mixed solution to 100°C to react and generate SO 2 And HCl gas, brought out with nitrogen, absorbed with sodium hydroxide (1M NaOH) aqueous solution; distilled after 30 hours of reaction, collected fractions at 115-120°C, and cooled to obtain 185g of colorless dichlorosulfonic acid imide (HCSI) liquid , the yield of dichlorosulfonic acid imide (HCSI) is 89.6%;

[0032] Step 2, reduce the water content of anhydrous hydrofluoric acid: the temperature of polytetrafluoroethylene electrolytic cell is adjusted to 18 ℃, with two nickel plates respectively as anode and negative electrode, add 300ml anhydrous hydrofluoric acid ( HF),...

Embodiment 2

[0040] A method for electrochemically synthesizing lithium bisfluorosulfonate, comprising the following steps:

[0041] Step 1, synthesis of dichlorosulfonic acid imide: under magnetic stirring (1000-1500 rev / min), add 350g thionyl chloride (SOCl 2 ) and 450g chlorosulfonic acid (CISO 3 H) Add 100g ammonium chloride (NH 4 Cl), heating to raise the temperature of the mixed solution to 100°C to react, generate SO2 and HCl gas, take it out with nitrogen, and absorb it with sodium hydroxide (1M NaOH) aqueous solution; distill after 40 hours of reaction, collect 115-120°C Fraction, after cooling, obtain 200g colorless dichlorosulfonic acid imide (HClSI) liquid, and the yield of dichlorosulfonic acid imide (HClSI) is 90.6%;

[0042] Step 2, reduce the water content of anhydrous hydrofluoric acid: the temperature of polytetrafluoroethylene electrolytic cell is adjusted to 18 ℃, with two nickel plates respectively as anode and negative electrode, add 300ml anhydrous hydrofluoric aci...

Embodiment 3

[0049] A method for electrochemically synthesizing lithium bisfluorosulfonate, comprising the following steps:

[0050] Step 1, synthesis of dichlorosulfonic acid imide: under magnetic stirring (1000-1500 rpm), add 320g thionyl chloride (SOCl 2 ) and 480g chlorosulfonic acid (CISO 3 H) Add 105g ammonium chloride (NH 4 Cl), heating the temperature of the mixed solution to 80°C to react and generate SO 2 And HCl gas, carried out with nitrogen, absorbed with sodium hydroxide (NaOH) aqueous solution; distilled after 35 hours of reaction, collected fractions at 115-120 ° C, and obtained 190 g of colorless dichlorosulfonic acid imide (HClSI) liquid after cooling, The yield of dichlorosulfonic acid imide (HClSI) is 91.5%;

[0051] Step 2, reduce the water content of anhydrous hydrofluoric acid: the temperature of polytetrafluoroethylene electrolytic cell is adjusted to 18 ℃, with two nickel plates respectively as anode and negative electrode, add 300ml anhydrous hydrofluoric acid ...

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Abstract

The invention discloses a method for electrochemical synthesis of lithium imidodifluorosulfonate. The preparation method comprises: regulating the temperature of an electrolytic tank to 0-18 DEG C, respectively taking two nickel plates as an anode and a cathode, adding a proper amount of anhydrous hydrofluoric acid into the electrolytic tank, and carrying out electrolysis; after the current in theelectrolytic tank is stabilized, adding a proper amount of imidodichlorosulfonate into the electrolytic tank, and after the imidodichlorosulfonate is dissolved, adjusting the working voltage of the electrolytic tank to 5-8 V; when the current is reduced to below 5 mA, taking out the solution in the electrolytic tank; distilling the solution taken out from the electrolytic tank under normal pressure to separate the imidodifluorosulfonate from the anhydrous hydrofluoric acid, and cooling to obtain the high-purity colorless liquid imidodifluorosulfonate; and reacting with lithium hydroxide, filtering, and re-crystallizing to obtain high-purity lithium imidodifluorosulfonate. According to the invention, water and chlorine ions are electrochemically pre-removed while fluorination is performedthrough electrochemistry without introduction of a metal halide as a catalyst, so that the method is simple in process, low in energy consumption and low in cost, and the prepared LiFSI is high in purity.

Description

technical field [0001] The invention relates to the technical field of chemical reagent preparation, in particular to a method for electrochemically synthesizing lithium bisfluorosulfonate imide. Background technique [0002] As a new type of green energy equipment, lithium batteries have gradually been widely used. The key materials of lithium-ion batteries include: positive electrodes, negative electrodes, binders, separators, and electrolytes. It is a key component of lithium-ion batteries, which significantly affects battery cycle and life, safety performance and energy. Lithium bisfluorosulfonyl imide (LiFSI) is a new type of electrolyte lithium salt used in lithium battery electrolytes, which is environmentally friendly and Good safety performance. As bisfluorosulfonyl imide (HFSI) is used as a raw material for the synthesis of lithium bisfluorosulfonimide (LiFSI), its purity and cost are crucial to battery performance and whether the industrial production of lithium ...

Claims

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Application Information

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IPC IPC(8): C01B21/093C01B21/092C25B1/24
CPCC01B21/0935C01B21/0926C25B1/245C01P2006/80Y02E60/10
Inventor 靳军
Owner LANZHOU UNIVERSITY
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