Abstract: A polymeric dicyanoketene acetal (DCKA), prepared from a styrene monomer bearing dicyanoketene acetal functionality, was found to be an effective and recyclable catalyst in the chemoselective deprotection of acetals and silyl ethers. A remarkable acceleration accountable for the polymer effect was observed. Key words: polymeric p-acid catalyst, chemoselective deprotection, acetal, silyl ether, polymer effect