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Preparation method of trifluoroacetate

A technology of trifluoroacetate and trifluoroacetyl fluoride, which is applied in the field of preparation of trifluoroacetate, can solve the problems affecting the working environment of production and research personnel, high requirements for equipment and materials, and low synthesis yield, so as to solve the problem of environmental protection Protection issues, simplification of synthesis process, and low requirements for reaction equipment

Active Publication Date: 2015-03-11
SANMING HEXAFLUO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional preparation method of trifluoroacetate is to use trifluoroacetic acid as raw material, and carry out esterification reaction with alcohol under the catalysis of concentrated sulfuric acid, and this method synthesis yield is low, and produces more waste water containing waste sulfuric acid; In recent years Recently, there has been a process of using strongly acidic cation exchange resin instead of concentrated sulfuric acid as a catalyst. For example, in the Chinese patent with the authorized announcement number CN101397249A and the title of invention "a preparation method of trifluoroacetate", a method using strong The acidic cation exchange resin is used as a catalyst to prepare trifluoroacetic ester, which reduces the discharge of waste acid, but there are still problems with the disposal of spent catalyst, and the process uses highly corrosive trifluoroacetic acid, which has relatively high requirements for equipment materials
Publication No. CN102351694A also discloses a preparation method of ethyl trifluoroacetate, but it uses amine compounds as acid-binding agents, and the organic amine used in the reaction has a pungent stench, which affects the labor of production and research personnel. surroundings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a reactor with a stirrer, add 12 kilograms of propanol, slowly add 5.8 kilograms of potassium fluoride under stirring to make the two evenly mixed, and add C 2 H 4 Cl 2 , C 2 H 4 Cl 2 The volume ratio to propanol is 1:1, and then the mixture is transferred to a closed reactor with a stirrer, stirring is started, and 11.6 kg of trifluoroacetyl fluoride gas is introduced into the mixture of propanol and potassium fluoride for reaction The reaction temperature is room temperature (25°C), and the reaction time is controlled at 5 hours. After the reaction is completed, filter to remove KHF 2 , The reaction product was transferred to a rectification tower for rectification, to obtain 14.9 kg of propyl trifluoroacetate (yield 95.5%). KHF removed 2 It is a solid. After water is dissolved, it is neutralized with KOH and all converted into KF. After removing water and drying, it is recycled and reused as a raw material.

Embodiment 2

[0026] In a reactor with a stirrer, add 12 kilograms of propanol, slowly add 5.8 kilograms of potassium fluoride under stirring to make the two evenly mixed, and add C 2 H 4 Cl 2 Organic solvent blended with ether (1:1 by volume), C 2 H 4 Cl 2 The volume ratio of the mixed solvent with ether and the volume of propanol is 1:1, and then the mixture is transferred to a closed reactor with a stirrer, stirring is started, and 11.6 kg of trifluoroacetyl fluoride gas is introduced into propanol and fluorinated The reaction is carried out in a potassium mixture, the reaction temperature is room temperature (25°C), and the reaction time is controlled at 5 hours. After the reaction is completed, filter to remove KHF 2 , The reaction product was transferred to the rectification tower for rectification, to obtain 15.5 kg of propyl trifluoroacetate (yield 99.4%). KHF removed 2 It is a solid. After water is dissolved, it is neutralized with KOH and all converted into KF. After removing water ...

Embodiment 3

[0028] In a reactor with a stirrer, add 12 kg of propanol, slowly add 5.8 kg of potassium fluoride under stirring to make the two evenly mixed, add ether, the volume ratio of ether to propanol is 1:1, and then Transfer the mixture to a closed reactor with a stirrer, start stirring, and pass 11.6 kg of trifluoroacetyl fluoride gas into the mixture of propanol and potassium fluoride for reaction. The reaction temperature is room temperature (25°C). The time is controlled at 5 hours. After the reaction is completed, filter to remove KHF 2 , The reaction product was transferred to a rectification tower for rectification, to obtain 14.8 kg of propyl trifluoroacetate (yield 94.8%). KHF removed 2 It is a solid. After water is dissolved, it is neutralized with KOH and all converted into KF. After removing water and drying, it is recycled and reused as a raw material.

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Abstract

The invention relates to a preparation method of trifluoroacetate. The preparation method of trifluoroacetate is characterized by comprising the following steps: (1) uniformly mixing potassium fluoride with alcohol, adding an organic solvent and then adding trifluoroacetyl fluoride to react; (2) filtering potassium fluoride-potassium hydrofluoride solid out of a reaction mixture; (3) rectifying to obtain trifluoroacetate, wherein the organic solvent in the step (1) is selected from one or mixture of both of C2H4C12 and ethyl ether; the volume ratio of the organic solvent to the alcohol is (1:0.5)-(1:4). By virtue of the method, the preparation process of the trifluoroacetate is simplified; waste acid and waste catalyst are not generated in the reaction process; reaction byproducts can be recycled and reused; the problem of the environmental protection of synthesis of the trifluoroacetate can be solved.

Description

Technical field [0001] The invention relates to the field of fine chemicals, in particular to a preparation method of trifluoroacetate. Background technique [0002] Trifluoroacetate is an important organic fluorine intermediate. It has a wide range of applications in the synthesis of a variety of fluorine-containing medicines, pesticides, liquid crystals, fuels and other products. For example, it is used to synthesize cardio-cerebral vascular drugs-Linopril . [0003] The traditional preparation method of trifluoroacetic acid ester is obtained by using trifluoroacetic acid as a raw material and carrying out an esterification reaction with alcohol under the catalysis of concentrated sulfuric acid. This method has a low synthesis yield and produces more waste water containing waste sulfuric acid; The process of using strongly acidic cation exchange resin instead of concentrated sulfuric acid as a catalyst has recently appeared. For example, in the Chinese patent with the authorized...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C69/63
CPCY02P20/584C07C67/54C07C67/14C07C67/48
Inventor 曹伟吕涛谢伟东张威
Owner SANMING HEXAFLUO CHEM CO LTD
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