Reaktion #346975

ord-c68e654d7e48499c8b6b631d3f5accb3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat 50° C.
  2. 2
    Temperaturmaintained at a stirring speed of about 1200 rpm
  3. 3
    Sonstigepurged with tetrafluoroethylene gas three times
  4. 4
    TemperaturThen the temperature of the mixture was raised
  5. 5
    Temperaturmaintained
  6. 6
    Sonstigeto be about 90° C
  7. 7
    workup.ADDITIONA mixture of tetrafluoroethylene and hexafluoropropylene gas
  8. 8
    workup.ADDITIONwas charged to the reactor
  9. 9
    Sonstigethe reaction
  10. 10
    SonstigeReaction
  11. 11
    SonstigeAt the end of the reaction

Vorschrift

In a 2-liter reactor were added 1000 gram of deionized water, 70 gram of fluoroacrylate (Zonyl TA-N from dupont), 130 gram of ammonium perfluorooctanoate (Fluororad FC-143, 3M). The mixture is a transparent microemulsion at 50° C. and maintained at a stirring speed of about 1200 rpm. The rector was then vacuumed and purged with tetrafluoroethylene gas three times to ensure oxygen content in the mixture to be below 30 ppm. Then the temperature of the mixture was raised and maintained to be about 90° C. A mixture of tetrafluoroethylene and hexafluoropropylene gas was charged to the reactor and the pressure inside the reactor was about 1500 kPa, in which the mole ratio of tetrafluoroethylene to hexafluoroethylene is about 70:30. Then, 0.4 gram of ammonium persulfate in 40 gram of water was pumped into the reactor to start the reaction. Reaction proceeded for about 234 minutes and was stopped. At the end of the reaction, the pressure of the reactor was about 600 kPa.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05523346uspto-grants-1996_06