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A kind of preparation method of bisfluorosulfonimide potassium

A technology of potassium bisfluorosulfonimide and bisfluorosulfonimide, applied in the field of chemical synthesis, can solve the problems of waste of raw materials, high cost of industrialization of products, and low yield of intermediate bischlorosulfonimide

Active Publication Date: 2018-10-19
SHANGHAI CHEMSPEC CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method uses excessive chlorosulfonic acid, resulting in waste of raw materials, and the low yield of the intermediate bischlorosulfonimide, which leads to high industrial costs of the product and does not have a competitive advantage

Method used

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  • A kind of preparation method of bisfluorosulfonimide potassium
  • A kind of preparation method of bisfluorosulfonimide potassium
  • A kind of preparation method of bisfluorosulfonimide potassium

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preparation example Construction

[0049] One aspect of the present invention provides a method for preparing potassium bisfluorosulfonyl imide. The preparation method of potassium bisfluorosulfonyl imide may include: reacting chlorosulfonic acid and chlorosulfonyl isocyanate in the presence of a catalyst to obtain bisfluorosulfonyl isocyanate Chlorosulfonimide (HClSI), the specific reaction equation is as follows:

[0050]

[0051] In the above reaction process, the catalyst may be an acid, more specifically, the catalyst may be a protonic acid and / or a Lewis acid. The Lewis acid is usually based on the Lewis acid-base theory, and generally refers to a substance that can accept electron pairs. Examples of specific Lewis acids that can be used include but are not limited to NiCl 2 , FeCl 2 , FeCl 3 、CoCl 3 , ZnCl 2 , MnCl 2 The combination of one or more of them; the protonic acid is usually based on the Bronster-Lowry acid-base theory, usually refers to the proton (hydrogen ion, H + ) molecules or ion...

Embodiment 1

[0082] Preparation of bischlorosulfonimide:

[0083] In the 1000mL reaction flask, add 478.6g of chlorosulfonic acid, NiCl 2 2.1g, start stirring, raise the temperature to 105-115°C, and add 679.2g of chlorosulfonyl isocyanate dropwise. After the dropwise addition, gradually raise the temperature to 130-140°C, and continue stirring for 20 hours. Distilled under reduced pressure, 738 g of stable fractions were collected, with a yield of 83.9%. The product is a white solid with a melting point of about 36°C.

Embodiment 2

[0085] Preparation of bisfluorosulfonimide:

[0086] In the 1000mL tetrafluoro reaction bottle, add the HClSI 738g that embodiment 1 makes, MoCl 5 0.48g, heat up to 100-105°C, slowly introduce about 130g of HF gas under stirring, cool down to room temperature after 12 hours of reaction, blow nitrogen for 16 hours, and obtain about 612g of crude product, short-distilled to obtain 516g of product, yield 82.6%, The product is a colorless liquid.

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Abstract

The invention relates to the field of chemical synthesis, in particular to a preparation method of potassium bis(fluorosulfonyl)imide. The preparation method comprises the following steps: 1) carrying out a reaction between chlorosulfonic acid and chlorosulfonyl isocyanate to obtain bis(chlorosulfonyl)imide in the presence of a catalyst; 2) carrying out a reaction between the bis(chlorosulfonyl)imide and hydrogen fluoride in the presence of a catalyst to obtain bis(fluorosulfonyl)imide; 3) carrying out a reaction between the bis(fluorosulfonyl)imide and an alkaline potassium compound to obtain the potassium bis(fluorosulfonyl)imide. According to the preparation method provided by the invention, the chlorosulfonic acid and the chlorosulfonyl isocyanate can be used as raw materials in the first step, so that generation of waste gases such as SO2, HCl and the like is avoided, and thus a requirement on environment friendliness can be met better.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of a fluorine-containing compound (potassium bis(fluorosulfonyl)imide, KFSI). Background technique [0002] In recent years, the use of potassium bisfluorosulfonyl imide in molten salt batteries, hard coating films, conductive films, and antistatic adhesives has attracted attention. [0003] Patent JP2013087019 uses sulfamic acid, chlorosulfonic acid and thionyl chloride to react to prepare dichlorosulfonimide, and then reacts with potassium fluoride. This method will generate a large amount of acid gas hydrogen chloride and sulfur dioxide in the first step reaction, which is not conducive to environmental protection. The second step reaction requires a large excess of anhydrous potassium fluoride, which is costly and complicated to purify. [0004] Patent WO2015143866 still adopts the process of sulfamic acid, chlorosulfonic acid and thionyl chloride to pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/086
CPCC01B21/086
Inventor 杨东何立林盛平刘俊
Owner SHANGHAI CHEMSPEC CORP
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