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Method for preparing a halogenocetyl fluoride and the derivatives thereof

A technology of haloacetyl fluoride and haloacetyl halide, which is applied in the field of preparation of haloacetyl fluoride and its derivatives, and can solve the problems of long reaction time and selectivity reduction

Inactive Publication Date: 2012-05-23
RHODIA OPERATIONS SAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The problem is that the reaction is an extremely slow reaction
The complete conversion of tetrachlorethylene to trichloroacetyl chloride requires a very long reaction time
[0009] When high conversions are desired, the reaction is less selective due to the formation of heavy by-products

Method used

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  • Method for preparing a halogenocetyl fluoride and the derivatives thereof
  • Method for preparing a halogenocetyl fluoride and the derivatives thereof
  • Method for preparing a halogenocetyl fluoride and the derivatives thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0146] 500 g of PER was charged into a 2 L jacketed Pyrex reactor with a condenser (-10 °C) and a mercury vapor lamp in a gas stream containing a mixture of pure oxygen (4 l / h) and nitrogen (0.5 l / h) under reflux (110°C) under radiation (210-260 nm).

[0147] A gas chromatographic analysis of the reaction medium (gas analysis detection) after 4 h of reaction showed the presence of 74% TCAC and 26% PER (% by weight).

[0148] Add 210.6 g (0.86 mol) of TCAC / PER (74 / 26 w / w) mixture and 40 g (2 mol) of anhydrous hydrofluoric acid into 0.3 liter of Hastelloy cooled to 0°C C276 autoclave.

[0149] The reactor was then heated to 120°C (temperature increase in about 1 h) and then kept at 120°C for 5 h under autogenous pressure (pressure about 60 bar).

[0150] The reactor was then cooled to 0°C (residual pressure about 15 bar), and the reaction medium was then slowly pumped into a polyvinyl fluoride flask cooled to -30°C.

[0151] The biphasic reaction medium is then degassed with...

Embodiment 2 to 4

[0179] The following examples involving the fluorination of TCAC to give TCAF were carried out under the same general conditions (temperature = 120° C.); only the changed parameters are mentioned in the table (I) below.

[0180] In Examples 3 and 4, the reaction was carried out at autogenous pressure, in Example 4 the control pressure was 22 bar.

[0181] The results obtained are reported in the table below:

[0182] Table (I)

[0183]

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PUM

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Abstract

The present invention relates to a method for preparing a halogenocetyl fluoride and the derivatives thereof. The inventive method for preparing a halogenocetyl fluoride acid is characterised in that said method includes: a step of preparing a halogenoacetyl halide by photo-oxidation of a halogenoethylene compound in conditions such that the transformation rate of the halogenoethylene compound into halogenoacetyl halide is no higher than 80 %, producing a reaction mixture essentially including halogenoacetyl halide and the excess halogenoethylene compound; a step of partial fluorination of the mixture obtained by reacting the latter with hydrofluoric acid suitable for obtaining a mixture of halogenoacetyl fluoride and the excess halogenoethylene compound; a step of separating the halogenoacetyl fluoride and the excess halogenoethylene compound. The invention can be used, specifically, for preparing the trichloroacetyl fluoride used as an intermediate species in the production of trifluoroacetic acid.

Description

technical field [0001] The subject of the present invention is a process for the preparation of haloacetyl fluorides and derivatives thereof. [0002] The present invention relates to the preparation of monohalogenated acetyl fluoride and the preparation of polyhalogenated acetyl fluoride. [0003] The object of the present invention is also to use said haloacetyl fluorides as intermediates for the manufacture of fluoroacetyl fluorides, the corresponding fluorocarboxylic acids and their derivatives. [0004] More specifically, the present invention relates to the preparation of trichloroacetyl fluoride as an intermediate in the manufacture of trifluoroacetyl fluoride from trifluoroacetic acid. Background technique [0005] The conventional route for the preparation of trifluoroacetic acid is the hydrolysis of trifluoroacetyl fluoride. [0006] The method described in the document (GB 976 316) for the preparation of trifluoroacetyl fluoride is the fluorination of trichloroa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C51/58C07C51/60C07C51/62C07C51/64C07C53/48C07C53/18
CPCC07C51/04C07C51/64C07C51/58C07C51/62C07C53/18C07C53/48
Inventor L·圣雅尔默斯F·梅斯
Owner RHODIA OPERATIONS SAS
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