Preparation method of bifluorosulfonyl imide onium salt

A technology of bisfluorosulfonimide onium salt and bisfluorosulfonimide, which is applied in the field of preparation of fluorine-containing compounds, can solve the problems that hinder the large-scale application of bisfluorosulfonimide onium salt, impurity ions and onium ions. Separation, preparation and purification process are long and other problems, to achieve the effect of large-scale industrial production, reduce material consumption, and reduce waste generation

Inactive Publication Date: 2014-12-24
SHENZHEN CAPCHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: the preparation and purification process is too long, resulting in too much material consumption and high production costs; it is difficult to separate impurity ions and onium ions in the cation exchange reaction, resulting in low product yield and purity
If the above problems are not solved, it will hinder the large-scale application of bisfluorosulfonylimide onium salt, especially hinder it from becoming the mainstream electrolyte material in new energy devices such as lithium-ion batteries and supercapacitors.

Method used

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  • Preparation method of bifluorosulfonyl imide onium salt

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preparation example Construction

[0017] Concretely, the preparation method of the bisfluorosulfonimide onium salt provided by the present invention comprises reacting the bischlorosulfonimide represented by the structural formula (A), the onium ion halide represented by the structural formula (B) and hydrogen fluoride to prepare The step of obtaining bisfluorosulfonylimide salt.

[0018]

[0019] Among them, M + represents the onium cation, X - Indicates a halide ion.

[0020] In the above preparation method, the bischlorosulfonimide can be a commercially available product, or can be obtained by a method recorded in literature (R.Appel et al, Chem.Ber.1962,95,625; M.Goehring et al, Inorg. Synth.1966,8,105; J.Ruff,Inorg.Chem.1967,6,2108; M.Berran et al, Z.Anorg.Allg.Chem.2005,631,55) synthesized. Preferably, the dichlorosulfonimide is prepared by the mixed reaction of sulfonamide, thionyl chloride and chlorosulfonic acid, and the reaction equation is as follows:

[0021]

[0022] Wherein, the reactio...

Embodiment 1

[0031] Embodiment 1: Preparation of bisfluorosulfonimide

[0032]Under stirring, 679 g of sulfonamide (7 mol), 1785 g of thionyl chloride (15 mol), and 815.5 g of chlorosulfonic acid (7 mol) were successively added into a dry 5 L reaction vessel to obtain a mixed solution. Heat the mixed solution to 140°C for reaction, and the sulfur dioxide and hydrogen chloride acid gas produced will be absorbed by the lye. After reacting for 20 hours, the brownish-yellow liquid crude product obtained was vacuum-distilled under reduced pressure, and the fraction at 110-114°C / 2mmHg was collected to obtain 1438 g of dichlorosulfonimide colorless liquid, with a yield of 96% and a purity of 99%.

[0033] Embodiment 1: Preparation of bisfluorosulfonimide ammonium salt

[0034] Under constant temperature stirring at 5°C, add 1,600 grams of hydrogen fluoride (80 mol) into a 3L dry reaction vessel, and slowly add 1,284 grams of bischlorosulfonimide (6 mol) for a chemical reaction, and the generated...

Embodiment 2

[0035] Example 2: Preparation of bisfluorosulfonimide tetraethylammonium salt

[0036] Under constant temperature stirring at 8°C, add 500 grams of hydrogen fluoride (25 mol) into a 1L dry reaction vessel, slowly add 165.5 grams of tetraethylammonium chloride (1 mol) and 214 grams of dichlorosulfonimide (1 mol) for a chemical reaction to produce The hydrogen chloride acid gas is absorbed by the lye. The reaction was continued at a constant temperature of 8°C for 5 hours, and then heated to 50°C to distill and recover 450 g of hydrogen fluoride, and continue to heat and dry in vacuum to obtain 307 g of bisfluorosulfonimide tetraethylammonium salt with a yield of 99% and a purity of 99%.

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Abstract

The invention relates to a preparation method of bifluorosulfonyl imide onium salt. The preparation method comprises the following step: by adopting hydrogen fluoride as a fluorination reagent and a reaction solvent, reacting with dichlorosulfonyl imide and an onium ion halide to obtain bifluorosulfonyl imide onium salt. Therefore, by adopting the preparation method disclosed by the invention, the raw material cost can be reduced, the material consumption and waste generation can be reduced, the raw material utilization rate and the product yield and purity can be improved, products can be more easily purified, a preparation technological process can be simpler and more efficient, and a good technological base for preparing bifluorosulfonyl imide onium salt massively and industrially can be provided.

Description

technical field [0001] The invention relates to a preparation method of a fluorine-containing compound, in particular to a preparation method of bisfluorosulfonylimide onium salt. Background technique [0002] Bisfluorosulfonylimide onium salt is an important class of ionic compounds. As a high-performance electrolyte material, it plays a key role in electrochemical new energy devices such as lithium-ion batteries and supercapacitors, so it has a high industrial application value. [0003] Japan Soda Co., Ltd. patent CN103391896A, first reacts chlorosulfonyl isocyanate and chlorosulfonic acid to obtain dichlorosulfonimide, then reacts with ammonium fluoride in acetonitrile and then filters to remove the solvent to obtain difluorosulfonimide ammonium salt. Finally, cation exchange with the onium compound results in the bisfluorosulfonimide onium salt. The method reported in this patent has problems such as too long reaction and purification process flow, difficult separatio...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/68C07D295/037C07D295/023C07D487/10C01C1/00
CPCC07D295/037C01B21/0935C07C209/68C07D295/023C07D487/10C07C211/63
Inventor 陈群
Owner SHENZHEN CAPCHEM TECH
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