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Preparation method of heptafluorobutyric acid and derivatives thereof

A technology of heptafluorobutyric acid and heptafluorobutyryl, which is applied in the field of preparation of heptafluorobutyric acid and its derivatives, and can solve the problems of restricting large-scale industrial production of heptafluorobutyric acid and its derivatives and low yield

Active Publication Date: 2019-06-25
阜新瑞宁化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, for a long time, the problem of low yield has limited the large-scale industrial production of heptafluorobutyric acid and its derivatives

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0041] The invention provides a kind of preparation method of heptafluorobutyric acid, comprises the following steps:

[0042] A) Electrochemical fluorination reaction of n-butyric acid, n-butyryl chloride or n-butyryl fluoride and anhydrous hydrogen fluoride to obtain electrolytic mixed gas;

[0043] The current density of the electrochemical fluorination reaction is 0.025-0.033A / cm 2 , the reaction temperature is 9~13℃;

[0044] The electrochemical fluorination reaction is provided with a cooling reflux device, and the cooling medium temperature of the cooling reflux device is -45°C;

[0045] B) passing the electrolytic mixed gas prepared in step A) into a reaction kettle equipped with an acid-binding agent to obtain heptafluorobutyryl fluoride, and the acid-binding agent is triethylamine;

[0046] C) mixing the heptafluorobutyryl fluoride obtained in step B) with water, and hydrolyzing to generate an aqueous solution of heptafluorobutyric acid;

[0047] D) Mix the above ...

Embodiment 1

[0103] In the electrolytic fluorination tank, 600 kg of n-butyryl fluoride and anhydrous hydrogen fluoride electrolytic liquid, the mass concentration of n-butyryl fluoride is 40%, and the electrolytic fluorination reaction is carried out under the following conditions, the electrolysis temperature is 10 ° C, and the voltage and current are respectively 7V and 2000A, current density 0.03A / cm 2 , Reflux condensation temperature -45 ℃. Perfluorobutyryl fluoride accounted for 31% by weight of the mixed gas generated during the electrolysis process, entrained hydrogen fluoride accounted for 20% by weight, and other gases accounted for 49%. As the electrolysis proceeds, the electrolyte should be regularly replenished in the electrolytic cell, but the concentration of the electrolyte should be adjusted according to the current and voltage, and the adjustment range is between 23% and 45%.

[0104] The electrolytic mixed gas enters the reaction kettle filled with 300 kg of triethylam...

Embodiment 2

[0125] In the electrolytic fluorination tank, 600 kg of n-butyryl fluoride and anhydrous hydrogen fluoride electrolytic liquid, the mass concentration of n-butyryl fluoride is 40%, and the electrolytic fluorination reaction is carried out under the following conditions, the electrolysis temperature is 10 ° C, and the voltage and current are respectively 7V and 2000A, current density 0.03A / cm 2 , Reflux condensation temperature -45 ℃. Perfluorobutyryl fluoride accounted for 31% by weight of the mixed gas generated during the electrolysis process, entrained hydrogen fluoride accounted for 20% by weight, and other gases accounted for 49%. As the electrolysis proceeds, the electrolyte should be regularly replenished in the electrolytic cell, but the concentration of the electrolyte should be adjusted according to the current and voltage, and the adjustment range is between 23% and 45%.

[0126] Pass the electrolysis mixed gas into the reactor of n-butyric acid and n-butyric anhyd...

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Abstract

The invention provides a preparation method of heptafluorobutyric acid, comprising the following steps: A) performing electrochemical fluorination reaction with n-butyric acid, n-butyryl chloride or n-butyryl fluoride and anhydrous hydrogen fluoride to obtain electrolytic mixed gas; The current density of electrochemical fluorination reaction is 0.025~0.033A / cm 2 , the reaction temperature is 9 to 13°C; the electrochemical fluorination reaction is provided with a cooling reflux device, and the cooling medium temperature of the cooling reflux device is -45°C; B) the electrolytic mixed gas prepared in step A) is passed into A reaction kettle equipped with an acid-binding agent to obtain heptafluorobutyryl fluoride, the acid-binding agent being triethylamine; C) mixing the heptafluorobutyryl fluoride obtained in step B) with water, and hydrolyzing to generate an aqueous solution of heptafluorobutyric acid D) mixing the above-mentioned heptafluorobutyric acid aqueous solution with KOH until the KOH concentration is 40% to 45%, and naturally crystallizing to obtain potassium heptafluorobutyrate; E) acidifying the above-mentioned potassium heptafluorobutyrate with sulfuric acid to obtain heptafluorobutyrate acid.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of heptafluorobutyric acid and derivatives thereof. Background technique [0002] Heptafluorobutyric acid and its derivatives are a class of chemical intermediates, which can be used as intermediates for new medicines, gunpowder, and spices, and can also be used as raw materials or additives for the synthesis of new organic polymer materials. At the same time, they can also be used as organic solvents. For example, after perfluorooctanoic acid is added to polymer molecules as a reagent providing fluorine-containing groups, fiber textiles with waterproof and dustproof properties can be produced by modifying the polymer. In addition, trifluoroacetic acid can be used as a catalyst and is an important intermediate in medicine, pesticide and industrial production. [0003] The research on the synthesis of heptafluorobutyric acid and its derivatives at home and ab...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/04C07C53/21C07C51/41C07C51/02C07C51/58C07C53/50C07C67/14C07C67/08C07C69/63C07C41/01C07C43/12C07C29/147C07C31/38C25B3/08C25B3/28
CPCC07C29/147C07C41/01C07C51/02C07C51/04C07C51/412C07C51/58C07C67/08C07C67/14C25B3/28
Inventor 王奎王然张晓东
Owner 阜新瑞宁化工有限公司
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