Vinylidene fluoride → Hfp tfe

HRID 2422990Notes

Reaction equation

HRID 2422990 reaction equation
S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+].[OH-].[Na+].C(S([O-])(=O)=O)CCCCCCC.[Na+].C(F)(F)=C.[F:32][C:33]([F:40])([F:39])[C:34]([F:38])=[C:35]([F:37])[F:36].[F:41][C:42]([F:46])=[C:43]([F:45])[F:44]>O>[F:32][C:33]([F:40])([F:39])[C:34]([F:38])=[C:35]([F:37])[F:36].[F:41][C:42]([F:46])=[C:43]([F:45])[F:44]

Participants

8

Reactant 6

HCID 6369Vinylidene fluorideHCID 8301TetrafluoroethyleneHCID 8302HexafluoropropyleneHCID 14798Sodium HydroxideHCID 62648Ammonium PersulfateHCID 23669624Sodium caprylyl sulfonate

Product 1

HCID 18927062Hfp tfe

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A VF2/HFP/TFE copolymer fluoroelastomer was prepared by a continuous emulsion polymerization process of the invention, carried out at 110° C. in a well-stirred 2.0-liter stainless steel liquid full reaction vessel. An aqueous solution, consisting of 2.16 g/hour (g/h) ammonium persulfate initiator, 0.87 g/h sodium hydroxide, 1.31 g/h sodium octyl sulfonate, and 0.98 g/h isopropanol chain transfer agent in deionized water, was fed to the reactor at a rate of 5.0 L/hour. The reactor was maintained at a liquid-full level at a pressure of 6.2 MPa by means of a backpressure control valve in the effluent line. After 30 minutes, polymerization was initiated by introduction of a gaseous monomer mixture consisting of 395 g/h vinylidene fluoride (VF2), 507 g/h hexafluoropropylene (HFP), and 309 g/h tetrafluoroethylene (TFE) fed through a diaphragm compressor. After 2.0 hours, collection of effluent dispersion was begun and collection continued for 5 hours. The effluent polymer latex, which had a pH of 2.67 and contained 18.5 wt. % solids, was separated from residual monomers in a degassing vessel at atmospheric pressure.

Workup

  1. customcarried out at 110° C. in a well-stirred 2.0-liter stainless steel liquid full reaction vessel
  2. temperatureThe reactor was maintained at a liquid-full level at a pressure of 6.2 MPa by means of a backpressure control valve in the effluent line
  3. custompolymerization
  4. waitAfter 2.0 hours
  5. customcollection of effluent dispersion
  6. customcollection
  7. waitcontinued for 5 hours
  8. customwas separated from residual monomers in a degassing vessel at atmospheric pressure

Sources & evidence

ORD record
ord-20f8ac89bcf246029b751812ae44ee03
Source dataset
uspto-grants-2011_06
Patent number
US07960480B2

Reaction notes

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