Development of a Pilot-Scale Polymerization Facility and Monomer Preparation for the Determination of Reactivity Ratios for Tetrafluoroethylene (TFE)-Based Copolymers

Author

Daniel A. Hercules, Clemson University

Date of Award

8-2016

Document Type

Dissertation

Degree Name

Doctor of Philosophy (PhD)

Department

Chemistry

Committee Member

Dr. Joseph S. Thrasher, Committee Chair

Committee Member

Dr. Darryl D. DesMarteau

Committee Member

Dr. Stephen E. Creager

Committee Member

Dr. William T. Pennington

Abstract

The addition of a pilot-scale tetrafluoroethylene (TFE) polymerization facility at Clemson University has enabled this academic institution to not only prepare TFE in kilogram quantities but also to store it and copolymerize it in safe conditions. The facility is used to prepare equimolar mixtures of TFE/CO₂ from the pyrolysis of potassium perfluoropropionate in approximately quantitative yields. The TFE is separated from the mixture and stabilized by D-limonene by scrubbing CO₂ from the aforementioned mixture. With the development of high technology software and hardware, the facility has been used to study the relative reactivity ratios of various polymerizations systems like the copolymerization of TFE with sulfonyl fluoride-substituted vinyl ethers [(perfluoro-3-oxa-4-pentene sulfonyl fluoride [DOW monomer] and perfluoro-2-(2-fluorosulfonylethoxy) propyl vinyl ether [PSEPVE]), methyl perfluoro(4-oxa-5-hexanoate) (DEVE), and perfluoro 8-cyano-5-methyl-3,6-dioxa-1-octene (8CNVE)], and vinylidene difluoride (VDF), in the presence and absence of CO₂. Some results from these studies as well as further details on the facility will be presented.

Recommended Citation

Hercules, Daniel A., "Development of a Pilot-Scale Polymerization Facility and Monomer Preparation for the Determination of Reactivity Ratios for Tetrafluoroethylene (TFE)-Based Copolymers" (2016). All Dissertations. 2169.
https://tigerprints.clemson.edu/all_dissertations/2169