A novel copolymer network with acetal structure was prepared using bis [4-(vinyloxy)butyl] (4-methyl-1,3-phenylene)biscarbamate (BECT) as the crosslinking agent. Firstly, a tri-copolymer of maleic anhydride (MAn), n-butyl vinyl ether (BVE) and 4-hydroxybutyl vinyl ether (HBVE) was synthesized via free-radical polymerization with 2,2′-azobisisobutyronitrile as the initiator. The tri-copolymer consisted of two sorts of alternating units, MAn-alt-BVE and MAn-alt-HBVE. The linear copolymer Poly((MAn-alt-BVE)-co-(MAn-alt-HBVE)) with pending hydroxyl groups was then combined with BECT in the presence of pyridinium p-toluenesulfonate, generating a copolymer network comprising acetal components in the crosslinking segment. This polymer network exhibited degradation in acid conditions.