Richard 1. Holzmann Thiokol Chemical Corporation Denville, New Jersey
In this laboratory it has been necessary to have available a reactor capable of use with reactive fluorine-containing gases and liquids. I n addition, the use of elemental fluorine itself a t low pressures demonstrated the need for such equipment. Efforts to do synthesis studies on a milliiole scale are frequently defeated because even slight attack of the reactor by active intermediates yields products which make accurate material balances impossible. Several preliminary models of our own design were tested preceding that shown in the figure. With this reactor it is possible to study systems a t reduced pressure equally as well as a t several atmospheres. The reactor is designed so that reagents come in contact only with Teflon. The body was machined from a single piece of 2I/,-in. Teflon rod. The reactor was threaded in the center to allow ready access to solid or liquid products under glove-box conditions. The thermoplastic properties of Teflon eliminated the need for a gasket. The thermal conductivity of bulk Teflon is such that an inordinate amount of time is required to cool the reactor with liquid nitrogen to - 196'C for the purpose of transferring and condensing gases. Consequently, the freeze-out tip was incorporated in the design. The snug-fit aluminum ring was used to prevent sagging a t the threads. Failure to use this ring caused substantial leaks after only several runs. The Teflon diaphragm valve was found to be the simplest way of confining the gases. The author is pleased to acknowledge the assistance of T. Macherione and K. Cooper.
All-Teflon Reactor
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KNURLEO lUlYlNUY
XNURED 1L. RIP4
T
T-
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la
REACTOR HEAD FREEZE-OUT
TWEIDED TO FIT
REACTOR BoTrnM
Volume 39, Number 7, July 1962
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373
