Prepn process of 2,2,2-trifluoroethyl acetate
A technology of trifluoroethyl acetate and potassium acetate, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve problems such as equipment corrosion, equipment corrosion, and health hazards to operators, and achieve Reduced production costs, mild reaction conditions, and less equipment corrosion
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Embodiment 1
[0017] In a dry 1L stainless steel autoclave equipped with magnetic stirring, put in 98g (1.0mol) of dry anhydrous potassium acetate, 198g (2.0mol) of polar aprotic solvent N-methylpyrrolidone and 1.0g of phase transfer catalyst After 6000 ethylene glycol, close the kettle, then press in 178g (1.5mol) of HCFC133a, and close the valve. Control the stirring speed at 200-250 rpm, raise the temperature to 200°C within 1h, react at this temperature for 2h, and after the pressure drops from 1.80Mpa to 1.30Mpa, flash the product at 170-160°C to another In the receiving bottle of packed column and condenser, liquid product 191g is obtained, and after analysis, its component composition (percentage by weight) is:
[0018] 1,1,1-Trifluoro-2-chloroethane (R133a) 29.50%
[0019] 2,2,2-Trifluoroethyl acetate (ATE) 63.72%
[0020] N-Methylpyrrolidone (NMP) 6.78%
[0021] After calculation, the yield of ATE is 85.7%, and the conversion rate of raw material potassium acetate is 95.6%. [Ex...
Embodiment 2
[0022]In a dry 1L stainless steel autoclave equipped with magnetic stirring, put in 98g (1.0mol) of dry anhydrous potassium acetate, 198g (2.0mol) of polar aprotic solvent N-methylpyrrolidone and 3.0g of phase transfer catalyst After 6000 ethylene glycol, close the kettle, then press in 178g (1.5mol) of HCFC133a, and close the valve. Control the stirring speed at 200-250 rpm, raise the temperature to 180°C within 1h, react at this temperature for 6h, and after the pressure drops from 1.05Mpa to 0.9Mpa, flash the product at 170-160°C to another In the receiving bottle of packing column and condenser, obtain liquid product 189g, after analysis, its component composition (percentage by weight) is:
[0023] 1,1,1-Trifluoro-2-chloroethane (R133a) 20.69%
[0024] 2,2,2-Trifluoroethyl acetate (ATE) 72.73%
[0025] N-Methylpyrrolidone (NMP) 6.17%
[0026] After calculation, the yield of ATE is 96.8%, and the refined ATE with a purity of more than 98% can be obtained through rectifi...
Embodiment 3
[0027] Except that the phase-transfer catalyst was changed to sodium dodecylsulfonate (2.7g), others were implemented according to the steps of Example 2. The conversion rate of raw material potassium acetate is 92.6%, and the yield of ATE is 70.7%. 【Example 4】
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