Nitric Acid → Nitric Acid
Reaction equation
[C:1]([CH2:5][OH:6])([F:4])([F:3])[F:2].[N+:7]([O-:10])([OH:9])=[O:8].[O:11]=O>>[N+:7]([O-:10])([OH:9])=[O:8].[C:5]([OH:11])([C:1]([F:4])([F:3])[F:2])=[O:6]Participants
Procedure
CF3CH2OH (200.00 g, 2.00 moles), 55% nitric acid (114.55 g, 1.00 mole) and FeCl2.nH2O (0.0020 g) were placed into the autoclave used in Example 1. The mixture was heated with stirring in the same manner as in Example 1. 3.0 hours after the start of heating, the reaction temperature rose to 125° C. and the reaction pressure increased to 0.75 MPa. From that time, oxygen was fed into the gas phase in the same manner as in Example 1, whereby the reaction pressure was controlled at 0.75 MPa. 6.0 hours after the start of heating, complete consumption of the starting fluoroalkyl alcohol was confirmed by gas chromatography to confirm the completion of the reaction [CF3CH2OH conversion: 100.0 g.c. %; CF3COOH selectivity: 98.5 g.c. % or higher]. The same procedure as in Example 1 was followed, thus giving an aqueous nitric acid solution of CF3COOH (361.18 g, a material balance of 99.43 mass %).
Workup
- temperatureThe mixture was heated
- temperature3.0 hours after the start of heating
- customrose to 125° C.
- customthe reaction pressure
- temperatureincreased to 0.75 MPa
- customthe reaction pressure
- temperature6.0 hours after the start of heating
- customcomplete consumption of the starting fluoroalkyl alcohol
- customthe completion of the reaction [CF3CH2OH conversion: 100.0 g.c. %; CF3COOH selectivity: 98.5 g.c. % or higher]
Sources & evidence
- ORD record
- ord-f8c57a4df89e49fbacca81e370f797a3
- Source dataset
- uspto-grants-2005_05
- Patent number
- US06891064B1
Reaction notes
Loading…