Abstract: A depolymerization and purification process, by which a poly(alkyl-.alpha.-cyanoacrylate) feed is depolymerized into high-purity cyanoacrylate monomers without the use of a high-boiling heat transfer medium such as tricresyl phosphate. The poly(alkyl-.alpha.-cyanoacrylate) feed, which contains one or more polymerization inhibitors such as hydroquinone and phosphorus pentoxide, is first introduced into a thin-film evaporator for a depolymerization reaction. The temperature of the film evaporator is maintained at about 200.degree..about.260.degree. C., and operated under a vacuum of 1.about.20 mm Hg. The produced gas stream from the depolymerization reactor is subject to a two-stage heat transfer process for condensation and purification. The first stage involves a very-high temperature condenser (about 150.degree. C.). The residue collected in the first stage condenser contains primarily dimers of .alpha.-cyanoacrylate.