Vinylidene fluoride → Hfp tfe

A VF2/HFP/TFE fluoroelastomer polymer was prepared by a continuous emulsion polymerization process of the invention in a well-stirred 4.0-liter stainless steel liquid full reaction vessel at 115° C. An aqueous solution, consisting of 3.74 g/hour (g/h) ammonium persulfate, 2.33 g/h sodium hydroxide, 13.4 g/h Zonyl® FS-62 fluorosurfactant (25 wt. % A.I.) solution, and 2.4 g/h isopropanol in deionized water, was fed to the reactor at a rate of 10 L/hour. The reactor was maintained at a liquid-full level at a pressure of 6.2 MPa by means of a back-pressure control valve in the effluent line. After 30 minutes, polymerization was initiated by introduction of a gaseous monomer mixture consisting of 632 g/h tetrafluoroethylene (TFE), 1147 g/h vinylidene fluoride (VF2), and 939 g/h hexafluoropropylene (HFP) fed through a diaphragm compressor. After 2.0 hours collection of the resulting fluoroelastomer latex was begun and continued for 6 hours. The latex, which had a pH of 4.57 and contained 20.4 wt. % solids, was separated from residual monomers in a degassing vessel at atmospheric pressure. Fluoroelastomer crumb product was isolated using aluminum sulfate solution. The coagulated fluoroelastomer polymer was allowed to settle, supernatant serum was removed, and the polymer was washed by reslurrying in water three times before filtering. The wet crumb was dried in an air oven at approximately 50°-65° C. to a moisture content of less than 1 wt. %. About 15.35 kg of fluoroelastomer was recovered at an overall conversion of 95.6%. The product, containing 24.28 wt. % TFE units, 43.70 wt. % VF2 units, and 32.02 wt. % HFP units, was an amorphous elastomer having a glass transition temperature of −13° C., as determined by DSC (heating mode, 10° C./minute, inflection point of transition). Inherent viscosity of the elastomer was 0.72 dL/g, measured at 30° C. in methyl ethyl ketone, and Mooney viscosity, ML (1+10), was 62.

1. temperatureThe reactor was maintained at a liquid-full level at a pressure of 6.2 MPa by means of a back-pressure control valve in the effluent line
2. custompolymerization
3. customAfter 2.0 hours collection of the resulting fluoroelastomer
4. waitcontinued for 6 hours
5. customwas separated from residual monomers in a degassing vessel at atmospheric pressure

ORD 기록

ord-fbf5fbf03e6c455085b695f9ebc21245

출처 데이터셋

uspto-grants-2004_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06774164B2