A method for synthesizing difluoroethanol with 2,2-difluoro-1-chloroethane as raw material
A technology of difluoroethanol and ethyl chloride, which is applied in the field of synthesizing difluoroethanol, can solve the problems of harsh reaction conditions, low purity, and low product yield, and achieve the effect of easy recovery and mild reaction conditions
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Embodiment 1
[0019] Add 1105g of 2,2-difluoro-1-chloroethane, 5L of N,N-dimethylacetamide and 1380g of potassium acetate into a 10L self-boosting reactor in sequence, keep stirring at 600r / min and gradually raise the temperature to 150 ℃, reacted for 4h, and cooled naturally. The resulting reaction solution was filtered and distilled to obtain difluoroethyl acetate with a purity of 99.63%.
[0020] Then add 1523g methanol and 35.8g 80%-H 2 SO 4 -Silicate-1, after stirring evenly, gradually raise the temperature to 85°C, and react for 5 hours. The resulting reaction solution was filtered and distilled to obtain difluoroethanol with a yield of 89.9% and a purity of 99.73%.
Embodiment 2
[0022] Add 1168g of 2,2-difluoro-1-chloroethane, 5L of N,N-dimethylacetamide and 1402g of potassium acetate into a 10L self-boosting reactor in sequence, keep stirring at 600r / min and gradually raise the temperature to 140 ℃, react for 5h, and cool naturally. The resulting reaction solution was filtered and distilled to obtain difluoroethyl acetate with a purity of 99.52%.
[0023] Then add 1426g methanol and 50.55g 55%-H 2 SO 4 - Chromatographic SiO 2 , after stirring evenly, gradually raise the temperature to 80°C, and react for 6h. The resulting reaction solution was filtered and distilled to obtain difluoroethanol with a yield of 87.7% and a purity of 99.76%.
Embodiment 3
[0025] Add 1200g of 2,2-difluoro-1-chloroethane, 5L of N,N-dimethylacetamide and 1389g of potassium acetate into a 10L self-boosting reactor in sequence, keep stirring at 600r / min and gradually raise the temperature to 140 ℃, reacted for 6h, and cooled naturally. The resulting reaction solution was filtered and distilled to obtain difluoroethyl acetate with a purity of 99.33%.
[0026] Then add 2138g methanol and 42.8g 65%-H 2 SO 4 - Silica sol, after stirring evenly, gradually raise the temperature to 75° C., and react for 5 hours. The resulting reaction solution was filtered and distilled to obtain difluoroethanol with a yield of 89.3% and a purity of 99.80%.
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