The synthesis of poly (butyl vinyl ether) and poly (butyl vinyl ether 2-chloroethyl vinyl ether) random copolymers was accomplished through the use of the aluminum hydrogen sulfate catalyst (AHS). In this system, AHS acts as a heterogeneous catalyst in the cationic polymerization of vinyl alkyl ethers. Highly isotactic polymers (greater than 70%) have been prepared and characterized by IH and 13C NMR. DSC characterization of poly(butyl vinyl ether) also reveals that these polymers are semicrystalline. Gel permeation chromatography characterization and intrinsic viscosity data of poly(butyl vinyl ether), and poly{butyl vinyl ether-2-chloroethyl vinyl ether) homopolymers and copolymers indicate fairly narrow polydispersities, and very high molecular weights. A study of this copolymerization by lH NMR revealed that the 2-chloroethyl ether monomer was being incorporated along the chain with the greater percentage of the 2-chloroethyl vinyl ether monomer near the chain ends. Reactions on the pendent chlorine group are currently under investigation in our laboratories. It is anticipated that a range of pendent functional groups can be obtained. / Master of Science