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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 and yield, suitable for industrialized mass production, etc., to overcome the harsh reaction conditions (such as high temperature and strong corrosion) when using a single anhydrous hydrogen fluoride as a fluorination reagent in the existing method , low yield, cumbersome product separation operation, difficult product purification and other deficiencies

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

Embodiment 1

[0073] Embodiment 1: the preparation of two (fluorosulfonyl) imides

[0074] The reaction formula is as follows:

[0075]

[0076] To a 500 mL autoclave (PTFE lined) with a reflux condenser, 214 g (1 mol) of 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, react for 10 hours, and then stop the reaction. At 50°C, use a dry nitrogen flow to remove volatile components such as excess anhydrous hydrogen fluoride and hydrogen chloride, discharge the material, carry out vacuum distillation, collect the fraction at 82-84°C / 30mmHg, and obtain 159g (0.88mol) of colorless and transparent The liquid product bis(fluorosulfonyl)imide (HN(SO 2 f) 2 ), yield 88%.

Embodiment 13

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

[0083] The reaction formula is as follows:

[0084]

[0085] Into a 500 mL autoclave (PTFE lined) with a reflux condenser, add 252 g (1 mol) of bis(dichlorophosphoryl)imide (HN(POCl 2 ) 2 ), 160g anhydrous hydrogen fluoride (HF) (8mol), 15g (0.05mol) antimony pentachloride (SbCl 5 ), keep the temperature of the condenser at -20°C, slowly raise the temperature to 50°C and react for 4 hours, then stop the reaction. After removing volatile components such as excess anhydrous hydrogen fluoride and hydrogen chloride with a dry nitrogen flow at 50°C, discharge the material, carry out vacuum distillation, collect 96-100°C / 30mmHg fractions to obtain 148g colorless and transparent bis(difluoro Phosphoryl) imide product, yield 80%.

Embodiment 14

[0086] Example 14: Preparation of (trifluoromethylsulfonyl)(fluorosulfonyl)imide

[0087] The reaction formula is as follows:

[0088]

[0089] To a 500 mL autoclave (PTFE lined) with a reflux condenser, 248 g (1 mol) of (trifluoromethylsulfonyl)(chlorosulfonyl)imide HN(CF 3 SO 2 )(SO 2 Cl), 30 anhydrous hydrogen fluoride (HF) (1.5mol), 4.5g perfluoroheptyl fluoride (C 7 f 15 COF) as a catalyst, keep the temperature of the condenser at -20°C, slowly raise the temperature to 60°C and react for 8h, then stop the reaction. At 50°C, use a dry nitrogen flow to remove volatile components such as excess anhydrous hydrogen fluoride and hydrogen chloride, discharge the material, carry out vacuum distillation, collect 86-90°C / 30mmHg fractions to obtain 162g colorless and transparent (trifluoromethyl Sulfonyl)(fluorosulfonyl)imide liquid, yield 70%.

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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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