In this Paper,the solid acid hydrolysis method was established to prepare κ-carrageenan oligosaccharides by the orthogonal experiment.The results showed that the oligosaccharide distribution width was narrow under the following condition of 100 mg/mL 732# resin,3% κ-carrageenan,60 ℃,reacting for 3 hours.The degree of polymerization was under 25 by PAGE analysis,and their structure was confirmed to be series of odd-numbered κ-carrigeenan oligosaccharides by ESI-MS.