Method for preparing fluorine-containing sulphonyl (phosphoryl) imine and alkali metal salt thereof

A technology containing fluorine-containing sulfonyl and perfluoroalkylsulfonyl fluoride, which is applied in the field of fluorine chemical synthesis, and can solve problems such as strong corrosion, harsh reaction conditions, and cumbersome product separation operations

Active Publication Date: 2010-02-24
HUAZHONG UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The task of the present invention is to provide a method for preparing fluorine-containing sulfonyl (phosphoryl) imide and alkali metal salt of fluorine-containing sulfonyl (phosphoryl) imide, which has the advantages of simple operation steps, mild reaction conditions and low cost. , easy separation and purification of the product, high purity a

Method used

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  • Method for preparing fluorine-containing sulphonyl (phosphoryl) imine and alkali metal salt thereof
  • Method for preparing fluorine-containing sulphonyl (phosphoryl) imine and alkali metal salt thereof
  • Method for preparing fluorine-containing sulphonyl (phosphoryl) imine and alkali metal salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0073] Example 1: Preparation of bis(fluorosulfonyl)imide

[0074] The reaction formula is as follows:

[0075]

[0076] Into a 500mL autoclave with reflux condenser (PTFE lining), add 214g (1mol) bis(chlorosulfonyl)imide (HN(SO 2 Cl) 2 ), 100g anhydrous hydrogen fluoride (HF) (5mol), 8.9g (0.05mol) antimony trifluoride (SbF) 3 ) As a catalyst, keep the condenser temperature at -20°C and the heating temperature at 50°C, and stop the reaction after 10 hours of reaction. Remove excess anhydrous hydrogen fluoride and hydrogen chloride and other volatile components at 50°C with a stream of dry nitrogen. Discharge and distill under reduced pressure. Collect 82-84°C / 30mmHg fractions to obtain 159g (0.88mol) colorless and transparent Liquid product bis(fluorosulfonyl)imide (HN(SO 2 F) 2 ), the yield is 88%.

Example

[0077] Comparative Examples and Examples 2-12

[0078] Comparative example and Examples 2-12, the reaction device used is the same as that of Example 1, and other experimental conditions (catalyst type, feed, reaction time, reaction temperature) and product yield are shown in Table 1.

[0079] Table 1 Different Lewis acid systems catalyze anhydrous hydrogen fluoride fluorination of bis(chlorosulfonyl)imide (HN(SO) 2 Cl) 2 ) Experimental results

[0080]

[0081]

Example Embodiment

[0082] Example 13: Preparation of bis(difluorophosphoryl)imide

[0083] The reaction formula is as follows:

[0084]

[0085] Into a 500mL autoclave (PTFE lined) with reflux condenser, add 252g (1mol) bis(dichlorophosphoryl)imide (HN(POCl) 2 ) 2 ), 160g anhydrous hydrogen fluoride (HF) (8mol), 15g (0.05mol) antimony pentachloride (SbCl 5 ), keep the condenser temperature at -20°C, slowly increase the temperature to 50°C and react for 4 hours, then stop the reaction. After removing excess anhydrous hydrogen fluoride and hydrogen chloride and other volatile components at 50℃ with a stream of dry nitrogen, the material was discharged and distilled under reduced pressure. The fraction at 96-100℃ / 30mmHg was collected to obtain 148g of colorless and transparent bis(difluoro) Phosphorimide product with a yield of 80%.

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Abstract

The invention provides a method for preparing fluorine-containing sulphonyl (phosphoryl) imine and fluorine-containing sulphonyl (phosphoryl) imine alkali metal salt. The method comprises the following steps: taking one or two or more than two of Lewis acid, perfluoro-alkyl sulfuryl fluoride and perfluoro-alkyl acyl fluoride as a catalyst, catalyzing anhydrous hydrogen fluoride to react with chlorine-containing sulphonyl (phosphoryl) imine in a high-pressure kettle and then obtaining the fluorine-containing sulphonyl (phosphoryl) imine by depressurization distilling; taking Lewis base as a catalyst, catalyzing the anhydrous hydrogen fluoride to react with the chlorine-containing sulphonyl (phosphoryl) imine, then acting with different alkali metal carbonate and obtaining the correspondingfluorine-containing sulphonyl (phosphoryl) imine alkali metal salt. Compared with the prior art, the method has the characteristics of simple operation steps, mild reaction conditions, low cost, easyseparation and purification of the product, high purity and yield and the like and is suitable for industrialized mass production.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical synthesis, and synthesizes fluorine-containing sulfonyl (phosphoryl) imides and fluorine-containing sulfonyl (phosphoryl) imide alkali metal salts by catalyzing the fluorination of anhydrous hydrogen fluoride, and specifically relates to bis(fluorine Sulfonyl)imide HN(SO 2 f) 2 , Bis(difluorophosphoryl)imide HN(POF 2 ) 2 , (perfluoroalkylsulfonyl fluorosulfonyl) imine (HN(SO 2 F)(SO 2 R f ), (difluorophosphoryl) (fluorosulfonyl) imide HN (POF 2 )(SO 2 F), (perfluoroalkylsulfonyl) (difluorophosphoryl) imide HN (POF 2 )(SO 2 R f )(R f =C m f 2m+1 , m is an integer, m=1-8) and the preparation of the above-mentioned fluorine-containing sulfonyl (phosphoryl) imide alkali metal salt. Background technique [0002] Fluorine-containing sulfonyl (phosphoryl) imides are precursors for the preparation of various fluorine-containing sulfonyl (phosphoryl) imide salts, and have important ...

Claims

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Application Information

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IPC IPC(8): C01B21/096C01B21/097C07C311/48C07C303/40C07F9/26B01J27/12B01J27/10B01J27/135B01J31/02B01J31/26
Inventor 周志彬韩鸿波聂进
Owner HUAZHONG UNIV OF SCI & TECH
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