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Method for preparing ethyl trifluoroacetate through continuous non-catalytic method

A technology of ethyl trifluoroacetate and trifluoroacetyl chloride, which is applied in the field of preparation of ethyl trifluoroacetate, can solve the problems of low product purity, uneconomical reaction, and high energy consumption

Active Publication Date: 2014-06-18
中化蓝天氟材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The continuous production of ethyl trifluoroacetate can be realized through gas phase reaction using trifluoroacetyl chloride and ethanol as raw materials, but the ethanol must be gasified in advance and then reacted through a gas phase reaction tube, the energy consumption of the reaction is high, and the reaction is slow. Economical, and the product purity is lower

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  • Method for preparing ethyl trifluoroacetate through continuous non-catalytic method

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Effect test

Embodiment 1

[0034] The reactor is a three-necked flask with a volume of 250ml, equipped with stirring, a thermometer, an air guide tube, a dropping funnel and a rectification column, and the rectification column is connected with a condenser and an HCl absorption device. Add 38 g of ethanol into the reactor, and start feeding trifluoroacetyl chloride gas after the temperature rises to 35° C., keeping the feed rate of trifluoroacetyl chloride at 1 g / min. After reacting at 35°C for 60 minutes, start to add ethanol dropwise. The drop rate of ethanol is 0.22g / min. While adding dropwise, the temperature is gradually raised to 60°C, and the reaction distillation is carried out to rectify the generated ethyl trifluoroacetate. Go out, absorb hydrogen chloride gas with HCl absorption device, generate by-product hydrochloric acid. After 360 minutes of reactive distillation, a total of 415.3 g of rectified products were obtained. The purity of ethyl trifluoroacetate was 98.51% and the yield was 96.0...

Embodiment 2

[0036] The reactor is a three-necked flask with a volume of 250ml, equipped with stirring, a thermometer, an air guide tube, a dropping funnel and a rectification column, and the rectification column is connected with a condenser and an HCl absorption device. Add 38 g of ethanol into the reactor, and start feeding trifluoroacetyl chloride gas after the temperature rises to 20° C., keeping the feed rate of trifluoroacetyl chloride at 1 g / min. After reacting at 20°C for 65 minutes, start to add ethanol liquid dropwise. The drop rate of ethanol is 0.2g / min. Distill it out, absorb hydrogen chloride gas with an HCl absorption device, and generate hydrochloric acid as a by-product. After 360 minutes of reactive distillation, a total of 420.4 g of rectified products were obtained. According to chromatographic analysis, the purity of ethyl trifluoroacetate was 99.05%, and the yield was 97.75%.

Embodiment 3

[0038] The reactor is a three-necked flask with a volume of 250ml, equipped with stirring, thermometer, air duct and rectification column, and the rectification column is connected with a condenser and an HCl absorption device. Add 88g of ethanol into the reactor, and start to feed trifluoroacetyl chloride gas after the temperature rises to 40° C., the feeding speed of trifluoroacetyl chloride is 2 g / min. After reacting at 40°C for 60 minutes, start to add ethanol liquid dropwise. The drop rate of ethanol is 0.35g / min. Distill it out, absorb hydrogen chloride gas with an HCl absorption device, and generate hydrochloric acid as a by-product. After 145 min of reactive distillation, 421.3 g of the rectified product was obtained. The purity of ethyl trifluoroacetate was 98.52% and the yield was 97.43% according to chromatographic analysis.

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Abstract

The invention provides a process for preparing ethyl trifluoroacetate through a continuous non-catalytic method reaction of trifluoroacetyl chloride and ethanol under a reactive rectification condition. The process has the characteristics of conveniently and easily available raw materials, simple process, mild reaction conditions, low reaction energy consumption, and no waste liquid residue in the procedure, and is suitable for amplification production. The prepared ethyl trifluoroacetate can be used for synthesis of fluorine-containing pesticides, fluorine-containing medicines, fluorine-containing liquid crystals, fluorine-containing dyes and the like.

Description

technical field [0001] The invention relates to a method for preparing ethyl trifluoroacetate, in particular to a method for preparing ethyl trifluoroacetate by a continuous non-catalytic method using trifluoroacetyl chloride and ethanol as raw materials. Background technique [0002] Ethyl trifluoroacetate, an important organic synthesis intermediate, is used as an organic synthesis building block for the synthesis of fluorine-containing pesticides, fluorine-containing medicines, fluorine-containing liquid crystals, and fluorine-containing dyes. Ethyl trifluoroacetate can also be used as a reaction solvent for the synthesis of pesticides and medicines. [0003] The synthetic method of ethyl trifluoroacetate is divided into following several kinds: [0004] Patent CN102276463 reports that trifluoroacetic acid and absolute ethanol are used as raw materials, and concentrated sulfuric acid is used as a catalyst to prepare ethyl trifluoroacetate through esterification. After t...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/14
CPCC07C67/14C07C69/63Y02P20/10
Inventor 李华徐卫国蒋强戴佳亮杨汪松
Owner 中化蓝天氟材料有限公司
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