Elsevier

Journal of Fluorine Chemistry

Volume 58, Issues 2–3, August–September 1992, Page 188
Journal of Fluorine Chemistry

Purification procedures for electrochemical fluorination products

https://doi.org/10.1016/S0022-1139(00)80638-7Get rights and content

Abstract

Electrochemical fluorination of organic compounds (tertiary alkylamines, dialkyl ethers, cyclic and acyclic hydrocarbons, aromatic and heterocyclic compounds) leads to a mixture of perfluorinated analogues with preserved carbon frame, partially fluorinated compounds, unsaturated compounds and considerable amounts of paraffins with variable length of carbon chain.

The paper discusses two approaches to isolation of high-purity perfluorinated compounds. The first involves treatment of the crude product with alkaline solutions in solvents more basic than water, isolation of the desired product by rectification and final fluorination with elementary fluorine. The second treats the crude product with elementary fluorine on a catalyst, and subsequent fractionation. Experimental data are given for these approaches as applied to production of perfluorinated amines (tributyl-, tripropyl-, and triamylamines), perfluorodialkyl ethers, perfluorodecalin and pentane, and perfluoro-1-ethylcyclohexane.

The paper compares product quality, economics and production procedure. Processes occurring on treatment with aqueous alkalis are discussed. Impurities are analyzed: their structure and relationship with the structure of products taken as substrates for fluorination, GC/MS, 13C and 19F NMR data are discussed.

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