The objective of this research program was to solve the problem of hydrolysis of the s-triazine ring in the perfluoroalkylene s-triazine polymer system by reducing the negative inductive effects and increasing steric blocking of the substituent perfluoroalkyl group with branching on the carbon alpha to the ring. The initial and crucial phase of this program was the synthesis of alpha, omega-sec-perfluoroetherdicarboxylic acid intermediates required for the monomer preparation. Four methods of generating alpha, omega-sec-dihaloperfluoroethers were investigated. Ethylene addition and dehydrohalogenation reactions readily convented the above alpha, omega-sec-dihaloperfluoroethers to alpha, omega-sec-divinylperfluoroethers. These compounds were found to be resistant to KMnO4 oxidation to yield the corresponding alpha, omega-sec-dicarboxylic acids.