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Method for preparing ethyl trifluoroacetate

A technology of ethyl trifluoroacetate and trifluoroacetic acid, which is applied in the field of preparation of ethyl trifluoroacetate, an organic chemical raw material, to achieve the effects of improving product quality and yield, convenient operation, and no environmental pollution

Inactive Publication Date: 2012-05-30
申少星
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the deficiencies of the existing production process, provide a kind of operation specification, easy to control the reaction end point, the quality analysis method in the distillation process is simple and reliable, the quality is stable, and the high boiling ethanol can be reused after distillation for The dehydrated drying tower filler can be recycled and used repeatedly, the production cost is low, the environment is not polluted, the resource is not wasted, and the preparation method of ethyl trifluoroacetate can improve product quality and yield

Method used

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  • Method for preparing ethyl trifluoroacetate

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Experimental program
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Effect test

Embodiment 1

[0010] According to the mass ratio 1:0.8 of trifluoroacetic acid and anhydrous acetic acid, 500 grams of metered trifluoroacetic acid are put into the esterification reaction device, and 400 grams of dehydrated alcohol are put into the high-level drip metering tank, and then the mass ratio of trifluoroacetic acid and catalyzer is 1: 0.6 Measure 300 grams of 732 type strongly acidic cation exchange resin into the esterification reaction device. Start stirring, raise the temperature to 40°C and start adding absolute ethanol dropwise at a rate of 0.30g-0.80g / s, and control the temperature of the reaction solution between 40°C-50°C. After the dropwise addition, keep stirring at 40° C. to 50° C. for 10 minutes. The temperature was raised to reflux for esterification. The end point of the esterification reaction is controlled with the water in the water separator of the esterification reaction device reaching a theoretical calculation value of 78.9ml, and the esterification reactio...

Embodiment 2

[0013] According to the mass ratio 1:3.2 of trifluoroacetic acid and absolute ethanol, 50 kg of trifluoroacetic acid is put into the esterification reaction device, and 270 grams of the residual high boiling point of embodiment 1, that is, 0.27 kg, is put into the high-level dripping metering tank, and the calculation should be put into Dehydrated alcohol is 160kg, deducts the ethanol amount 0.269kg in the residual high boiling of throwing embodiment 1, throws dehydrated alcohol 159.73kg again and enters the high position dropwise metering tank. Then measure 40 kg of D72 type strongly acidic cation exchange resin according to the mass ratio of trifluoroacetic acid and catalyst of 1:0.8, and put it into the esterification reaction device. Start stirring, raise the temperature to 45°C and start adding absolute ethanol dropwise at a rate of 0.4g~0.6g / s, control the temperature of the reaction solution between 45°C~49°C, keep stirring at 45°C~49°C for 10 minutes after the addition ...

Embodiment 3

[0016] According to the mass ratio of trifluoroacetic acid and dehydrated alcohol 1:1.8, measure 150kg of trifluoroacetic acid and put it into the esterification reaction device, first put the residual high boiling 144.7kg of embodiment 2 into the high-level dripping metering tank, and calculate that it should be dropped into dehydrated ethanol 270kg, subtracted the ethanol amount 144.35kg in the residual high boiling of throwing embodiment 2, throws dehydrated ethanol 125.65kg again and enters the high position dripping metering tank. Then measure 45 kg of 732 type strongly acidic cation exchange resin according to the mass ratio of trifluoroacetic acid and catalyst of 1:0.3, and put it into the esterification reaction device. Start stirring, raise the temperature to 46°C and start adding absolute ethanol dropwise at a rate of 0.45g-0.55g / s, control the temperature of the reaction solution between 46°C-48°C, keep stirring at 46°C-48°C for 10 minutes after the addition . The ...

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Abstract

The invention relates to a preparation method of ethyl trifuoroacetate, trifluoroacetic acid and anhydrous ethanol are taken as main raw materials, a strong acid cation exchange resin is taken as a catalyst, and the anhydrous ethanol is dripped at the temperature which is lower than 50 DEG C and the atmospheric pressure and maintained for a period of time for complete reaction. The catalyst is filtered, the drying in a drying tower which is filled with solid silica gel particles is carried out for removing the residual water, the atmospheric distillation is carried out, and a fraction which is collected at 58 DEG C to 64 DEG C is a finished product. The production process is carried out under the completely sealed state, the catalyst can be recycled for circulating use, and the fraction after collecting the finished product can be recycled. The preparation method is used for preparing the ethyl trifuoroacetate, and the product is an importable organic chemical raw material which is mainly used for synthesizing organic fluorine compounds and can be used for preparing pesticides, medicines, dyes, liquid crystals and industrial chemicals. The preparation method has complete and standard process and convenient operation, and the preparation method is applicable to the industrial production and can effectively improve the purity and the yield of the product, reduce the production cost and has no environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of ethyl trifluoroacetate, an organic chemical raw material used for synthesizing organic fluorinated compounds and preparing pesticides and medicines, which is prepared from trifluoroacetic acid and absolute ethanol as main raw materials. Background technique [0002] Ethyl trifluoroacetate is an important organic chemical raw material, mainly used in the synthesis of organic fluorine compounds and the preparation of industrial chemicals such as pesticides, medicines, dyes, and liquid crystals. In medicine, it is used to manufacture anti-inflammatory drugs for rheumatoid arthritis and osteoarthritis and anti-tumor drugs for colorectal cancer. Pesticides are used in the manufacture of cell division inhibitors, and are used in cotton and peanut fields to kill grasses and broad-leaved weeds. Development and application prospects are broad. In the past, concentrated sulfuric acid was often used to catalyze t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/63C07C67/08B01J31/08
CPCY02P20/584
Inventor 申少星尤小文
Owner 申少星
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