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Production method of ethyl trifluoroacetate

A technology of ethyl trifluoroacetate and trifluoroacetic acid is applied in the field of production technology of ethyl trifluoroacetate, can solve problems such as complex process, and achieve the effects of simple reaction, rapid reaction and high yield

Inactive Publication Date: 2012-07-04
田晓琴
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] A kind of preparation method of ethyl trifluoroacetate disclosed in 00023, take trifluoroacetic acid and dehydrated alcohol as main raw material, make catalyzer with strongly acidic cation exchange resin, catalyzer can recycle after strong acid treatment, although catalyzer can recycle , but the amount of acid required is relatively large, and water is generated in the system. Considering that the water generated by the esterification reaction has an inhibitory effect on the reaction, the water should be removed in time, which is conducive to the conversion of the esterification reaction, and the process is more complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] The production process of ethyl trifluoroacetate comprises the following steps: add 100g trifluoroacetic acid in a 500ml four-necked bottle equipped with mechanical stirring, a thermometer and a condenser tube, cool to 3°C, control the stirring speed to 300r / min, and use 0.4 Add the mixture of 38g ethanol and 0.8g concentrated sulfuric acid dropwise at the speed of g / s, flow for 4 hours, Shimadzu Gc-2010 gas chromatograph detects that the mass percentage content of trifluoroacetic acid is less than 0.1%, install a rectification column, after rectification Obtain product ethyl trifluoroacetate 118g, yield 92%, add 0.8g sulfur trioxide in the distillation residue, can make dilute sulfuric acid become concentrated sulfuric acid again, thereby realize recycling, repeat above-mentioned reaction 3 times, let off distillation residue thing.

Embodiment 2

[0009] The production process of embodiment 2 ethyl trifluoroacetate, comprises the following steps: add 107g trifluoroacetic acid in the 500ml four-necked bottle that is equipped with mechanical stirring, thermometer and condensing tube, cool to 5 ℃, control stirring speed 500r, / min , add dropwise a mixture of 45g ethanol and 0.9g concentrated sulfuric acid at a speed of 0.5g / s, reflux for 5 hours, Shimadzu Lc-20AT high performance liquid chromatography detects that the mass percentage of trifluoroacetic acid is less than 0.1%, and rectifying column, after rectification, 125g of ethyl trifluoroacetate was obtained, with a yield of 92.5%. Adding 0.9g of sulfur trioxide to the distillation residue could turn dilute sulfuric acid into concentrated sulfuric acid again, thereby realizing recycling, and repeating the above reaction 3 times , let off the distillation residue.

Embodiment 3

[0011] The production process of ethyl trifluoroacetate comprises the following steps: add 114g trifluoroacetic acid in a 500ml four-necked bottle equipped with mechanical stirring, a thermometer and a condenser tube, cool to 5°C, control the stirring speed at 600r / min, and set the temperature at 0.6 Add a mixture of 52g ethanol and 1g concentrated sulfuric acid dropwise at a speed of g / s, and reflux for 6 hours. The Shimadzu Gc-2010 gas chromatograph detects that the mass percentage of trifluoroacetic acid is less than 0.1%. A rectification column is installed and obtained after rectification Product ethyl fluoroacetate 132g, yield 93%, add 1g sulfur trioxide in distillation residue, can make dilute sulfuric acid become concentrated sulfuric acid again, thereby realize recycling, repeat above-mentioned reaction 4 times, let off distillation residue.

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Abstract

The invention relates to a production process of ethyl trifluoroacetate, and the production process comprises the following steps of: adding 100-128 parts by mass of trifluoroacetic acid in a four-mouth bottle provided with a mechanical agitator, a thermometer and a condensation tube, cooling to 37 DEG C, controlling an agitation speed to be 300-1000 r / min, adding a mixture of 38-66 parts by mass of ethanol and 0.8-1.2 parts by mass of concentrated sulfuric acid drop by drop at a speed of 0.4-0.7 g / s, refluxing for 48 hours, detecting that the content of the trifluoroacetic acid in percentage by mass is less than 0.1% by a chromatographic instrument, additionally mounting a rectifying column, rectifying to obtain a product ethyl trifluoroacetate, adding 0.8-1.2 parts by mass of sulfur trioxide in a distillation residue, repeating the reaction for 35 times, and discharging the distillation residue. The production process has the advantages that the concentrated sulfuric acid is selected for catalytic esterification; the reaction is quick; as water is generated in a system, the sulfur trioxide is added, so that dilute sulfuric acid can become the concentrated sulfuric acid again, thereby achieving recycle; the reaction is simple; and the yield is high.

Description

technical field [0001] The invention relates to a production process of ethyl trifluoroacetate, which belongs to the field of chemical industry. Background technique [0002] A kind of preparation method of ethyl trifluoroacetate disclosed in 00023, take trifluoroacetic acid and dehydrated alcohol as main raw material, make catalyzer with strongly acidic cation exchange resin, catalyzer can recycle after strong acid treatment, although catalyzer can recycle , but the amount of acid required is relatively large, and water is generated in the system. Considering that the water generated by the esterification reaction has an inhibitory effect on the reaction, the water should be removed in time to facilitate the conversion of the esterification reaction, and the process is more complicated. Therefore, a new technical solution needs to be provided to solve the above problems. Contents of the invention [0003] o0033 The purpose of this invention is to provide a simple, high-y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08
Inventor 田晓琴
Owner 田晓琴
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