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This study used reed and corn stalk which are abundant agricultural wastes as the materials,explored the enzymatic hydrolysis changes of material in liquid hot water pretreatment.The results showed that a large number of cellulose(pentosans)and part of lignin were dissolved out,and amount of cellulose were exposed during the liquid hot water pretreatment process because of the breaking of LLC structure,which is better for the enzymolysis.Along with the rise of temperature,the content of pentosans was significantly reduced to the maximum 15.24%(reed)and 12.84%(corn stalk)at 180℃.the content of glucosans kept stable basically; The content of furfural were significantly reduced after the first increase,and it can respectively reached the maximum 2.06%(reed)and 1.02%(corn stalk)at 200℃.The content of HMF can respectively reached the maximum 7.64%(reed)and 7.42%(corn stalk)at 200℃.The percent conversion of enzyme hydrolysis for reed can reached the maximum 88.2% at 48h.Its percent conversion of enzymolysis increases 84.61% than the untreated reed.And the percent conversion of corn stalk was 24.3% at 24h.