Recycling method of waste containing ethyl acetate and ethyl alcohol in production process of ethyl trifluoroacetoacetate

A technology of ethyl trifluoroacetoacetate and ethyl trifluoroacetate, which is applied in the field of recycling ethyl acetate and ethanol, can solve the problems of high energy consumption per unit product separation, high safety risk of pressurized rectification, and high equipment investment cost , to achieve the effect of improving atom economy, no waste liquid residue, and convenient operation

Active Publication Date: 2015-06-03
中化蓝天氟材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process adopts a two-stage rectification system, which has high equipment investment costs, high safety risks in pressurized rectificati...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 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. The condenser condenses and recovers the unreacted trifluoroacetyl chloride in the rectification tail gas, and then absorbs the hydrogen chloride gas through the absorption device to produce hydrochloric acid by-product. 80.0g mixed waste containing ethyl acetate and ethanol (the content of ethanol is 44.8%, and the content of ethyl acetate is 54.2%). After rising to 40°C, start feeding trifluoroacetyl chloride gas to maintain the feeding speed of trifluoroacetyl chloride 2.0g / min. After ventilating for 20 minutes, start to add the mixed waste containing ethyl acetate and ethanol dropwise at a rate of 1.3 g / min, gradually warming up to an internal temperature of 60°C while adding, and carry out reactive distillation to ge...

Embodiment 2

[0031] 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. The condenser condenses and recovers the unreacted trifluoroacetyl chloride in the rectification tail gas, and then absorbs the hydrogen chloride gas through the absorption device to produce hydrochloric acid by-product. 90.0g mixed waste containing ethyl acetate and ethanol (the content of ethanol is 37.6%, and the content of ethyl acetate is 61.6%). After rising to 50°C, start to feed trifluoroacetyl chloride gas to maintain the feeding speed of trifluoroacetyl chloride It is 1.5g / min. After ventilating for 15 minutes, start to add the mixed waste containing ethyl acetate and ethanol dropwise at a rate of 0.8 g / min, gradually warming up to an internal temperature of 65°C while adding, and carry out reactive distillation...

Embodiment 3

[0033] 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. The condenser condenses and recovers the unreacted trifluoroacetyl chloride in the rectification tail gas, and then absorbs the hydrogen chloride gas through the absorption device to produce hydrochloric acid by-product. 100.0g of mixed waste containing ethyl acetate and ethanol (the content of ethanol is 31.7%, and the content of ethyl acetate is 67.5%). After rising to 45°C, start to feed trifluoroacetyl chloride gas to maintain the feeding speed of trifluoroacetyl chloride It is 1.0g / min. After ventilating for 30 minutes, start to add the mixed waste containing ethyl acetate and ethanol dropwise at a rate of 0.5 g / min, gradually warming up to an internal temperature of 65°C while adding, and carry out reactive distilla...

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PUM

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Abstract

The invention discloses a recycling method of waste containing ethyl acetate and ethyl alcohol in a production process of ethyl trifluoroacetoacetate. A mixture of ethyl trifluoroacetate and ethyl acetate is obtained by reaction of trifluoroacetyl chloride, ethyl acetate and ethyl alcohol under the operation condition of reactive rectification. The method disclosed by the invention has the advantages of low cost, safety, environmental friendliness, simple technology and the like.

Description

technical field [0001] The invention relates to a method for recycling ethyl acetate and ethanol from a mixture containing ethyl acetate and ethanol. Background technique [0002] Ethyl trifluoroacetoacetate is an important raw material for the synthesis of pesticides such as fluprofen-methyl, pyrimaben-methyl, fluthiofos, dithiopyr, thiflufen, and amiflumezone. At present, the main industrial production method is to use ethyl trifluoroacetate and ethyl acetate as raw materials, under the action of sodium ethoxide, to prepare ethyl trifluoroacetoacetate through Claisen condensation reaction. This production process can produce a large amount of mixture of ethyl acetate and ethanol, if not recycled, on the one hand it will cause production cost increase, on the other hand it will cause environmental pollution. [0003] Since ethyl acetate is easy to form an azeotrope with ethanol, the azeotrope point is 71.8°C, and the azeotrope composition (wt%): ethanol 31%, ethyl acetate ...

Claims

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Application Information

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IPC IPC(8): C07C69/738C07C67/343C01B7/01
CPCC01B7/01C07C67/14C07C67/343C07C69/63C07C69/716Y02P20/10
Inventor 蒋强徐卫国李华洪健缪水斌马小红吴华明
Owner 中化蓝天氟材料有限公司
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