Vinylidene fluoride → Hfp tfe

A VF2/HFP/TFE copolymer fluoroelastomer was prepared by a continuous emulsion polymerization process of the invention, carried out at 115° C. in a well-stirred 4.0-liter stainless steel liquid full reaction vessel. An aqueous solution, consisting of 3.74 g/hour (g/h) ammonium persulfate, 11.26 g/h sodium phosphate dibasic heptahydrate, 3.75 g/h sodium octyl sulfonate, 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 594 g/h tetrafluoroethylene (TFE), 1119 g/h vinylidene fluoride (VF2), and 897 g/h hexafluoropropylene (HFP) fed through a diaphragm compressor. After 2.0 hours, collection of effluent dispersion was begun and continued for 5 hours. The effluent polymer dispersion, which had a pH of 4.1 and contained 19.9 wt. % solids, was separated from residual monomers in a degassing vessel at atmospheric pressure. Fluoroelastomer product was isolated using calcium nitrate solution. The coagulated 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%. About 12 kg of polymer was recovered at an overall conversion of 94.6%. The product, comprised of 24.0 wt. % TFE units, 45.0 wt. % VF2 units, and 31.0 wt. % HFP units, was an amorphous elastomer having a glass transition temperature of−14° C., as determined by differential scanning calorimetry (heating mode, 10° C./minute, inflection point of transition). Inherent viscosity of the elastomer was 0.76 dL/g, measured at 30° C. in methyl ethyl ketone, and Mooney viscosity, ML(1+10), was 64.

1. customcarried out at 115° C. in a well-stirred 4.0-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 back-pressure control valve in the effluent line
3. custompolymerization
4. waitAfter 2.0 hours
5. customcollection of effluent dispersion
6. waitcontinued for 5 hours
7. customwas separated from residual monomers in a degassing vessel at atmospheric pressure

ORD 기록

ord-b5650d5c82eb4e5095745490feec5dd6

출처 데이터셋

uspto-grants-2003_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06512063B2