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A kind of preparation method of ethyl trifluoroacetate

A technology of ethyl trifluoroacetate and trifluoroacetic acid, applied in the field of preparation of ethyl trifluoroacetate, can solve the problems of high equipment requirements, adverse environmental impact, low yield, etc., and achieves reduced corrosiveness, reduced dosage, and reduced reaction high conversion rate

Active Publication Date: 2021-06-04
江山鑫隆化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The traditional preparation method of ethyl trifluoroacetate is to use trifluoroacetic acid as a raw material, which is obtained by esterification with ethanol under the catalysis of concentrated sulfuric acid. Due to the unreasonable arrangement between the various reaction steps, the synthesis yield of the whole process is relatively low. Low, high requirements on equipment, and will have adverse effects on the environment

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  • A kind of preparation method of ethyl trifluoroacetate

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Effect test

Embodiment 1

[0026] 1) Pass 2kg of sulfur trioxide from the storage tank through the oxygen reaction kettle through the internal pressure, and pass 2kg of trifluorotrichloroethane through the oxygen reaction kettle, wherein the sulfur trioxide is passed through a jacket at about 70°C Heating with hot water, controlling the temperature in the oxo reactor to 58°C, and reacting for 20 minutes;

[0027] 2) Pass 3kg of sulfur trioxide from the storage tank through the oxo reactor through internal pressure, pass 6kg of trifluorotrichloroethane through the oxo reactor, control the temperature in the oxo reactor to be 60°C, and react 10 minutes;

[0028] 3) The reaction product trifluoroacetyl chloride in step 1) and 2) and the by-product sulfuryl chloride, pyrothionyl chloride, along with part of the raw materials sulfur trioxide, trifluorotrichloroethane, enter the vapor phase from the gas phase outlet of the oxo reactor. Stripping still, carry out stripping condensation separation at 63 ℃;

...

Embodiment 2

[0041] 1) Pass 4kg of sulfur trioxide from the storage tank through the oxygen reaction kettle through the internal pressure, and pass 4kg of trifluorotrichloroethane through the oxygen reaction kettle, wherein the sulfur trioxide is passed through a jacket at about 70°C Heating with hot water, controlling the temperature in the oxo reactor to 60°C, and reacting for 25 minutes;

[0042] 2) Pass 2kg of sulfur trioxide from the storage tank through the oxo reactor through the internal pressure, pass 4kg of trifluorotrichloroethane through the oxo reactor, control the temperature in the oxo reactor to be 62°C, and react 15 minutes;

[0043] 3) The reaction product trifluoroacetyl chloride in step 1) and 2) and the by-product sulfuryl chloride, pyrothionyl chloride, along with part of the raw materials sulfur trioxide, trifluorotrichloroethane, enter the vapor phase from the gas phase outlet of the oxo reactor. Stripping still, carry out stripping condensation separation at 64 ℃;...

Embodiment 3

[0056] 1) Pass 2.5kg of sulfur trioxide from the storage tank through the oxo reaction kettle through internal pressure, and pass 2.5kg of trifluorotrichloroethane through the oxo reaction kettle, wherein the sulfur trioxide is passed through 70°C with a jacket Heating with hot water from left to right, controlling the temperature in the oxo reactor to 61°C, and reacting for 28 minutes;

[0057] 2) Pass 2kg of sulfur trioxide from the storage tank through the oxo reactor through internal pressure, pass 4kg of trifluorotrichloroethane through the oxo reactor, control the temperature in the oxo reactor to be 64°C, and react 25 minutes;

[0058] 3) The reaction product trifluoroacetyl chloride in step 1) and 2) and the by-product sulfuryl chloride, pyrothionyl chloride, along with part of the raw materials sulfur trioxide, trifluorotrichloroethane, enter the vapor phase from the gas phase outlet of the oxo reactor. Stripping still, carry out stripping condensation separation at ...

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Abstract

The invention discloses a preparation method of ethyl trifluoroacetate, which comprises the following steps: 1) passing sulfur trioxide and trifluorotrichloroethane into an oxygenation reactor twice; 2) trifluoroacetyl chloride and By-products and some raw materials enter the stripping kettle for stripping, condensation and separation; 3) The separated trifluoroacetyl chloride is transported to the hydrolysis absorption system, and part of the raw materials are condensed and refluxed to the oxo reactor; 4) The raw materials after rectification are returned to the oxygen reactor. generation reaction kettle; sulfuryl chloride, pyrothionyl chloride and impurities to be hydrolyzed; 5) obtain crude trifluoroacetic acid, and rectify to obtain trifluoroacetic acid; 6) add trifluoroacetic acid to the esterification kettle; 7) obtain ethyl trifluoroacetic acid finished product . The present invention adds reactants in stages, the reaction conversion rate is higher, and lays a good reaction foundation for subsequent reactions. The reaction conditions are mild, the amount of concentrated sulfuric acid is greatly reduced, and the corrosion to equipment is reduced; adding fibers in frozen brine, Separation of trifluoroacetyl chloride is more efficient.

Description

technical field [0001] The invention belongs to the technical field of preparation of ethyl trifluoroacetate, in particular to a preparation method of ethyl trifluoroacetate. Background technique [0002] Ethyl trifluoroacetate is an important organic fluorine intermediate, which is widely used in the synthesis of various fluorine-containing medicines, pesticides, liquid crystals, fuels, etc. . [0003] The traditional preparation method of ethyl trifluoroacetate is to use trifluoroacetic acid as a raw material, which is obtained by esterification with ethanol under the catalysis of concentrated sulfuric acid. Due to the unreasonable arrangement between the various reaction steps, the synthesis yield of the whole process is relatively low. Low, high requirements on equipment, and will have adverse effects on the environment. Contents of the invention [0004] In order to overcome the deficiencies of the prior art, the present invention provides a method for preparing eth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/63C07C51/64
CPCC07C51/04C07C51/58C07C51/64C07C67/08C07C53/48C07C53/18C07C69/63
Inventor 孙其洪张建华唐志萍卢毅
Owner 江山鑫隆化工有限公司
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