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
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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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