For pretreatment of solid waste, firstly shred and/or crushed agricultural residues and agro-industrial wastes to fine powder, and introduced into the reactor, and added concentrate sulphuric acid (55 wt%), heated and stirred for 30 min. A second stage hydrolysis performed by a dilution of H2SO4 from 55 wt% to 6.7 wt%, and keep the solution for another 20 min stirring, then add the equivalent moles of calcium hydroxide to neutralize, and then continues stirred for 20 h. After completion of the hydrolysis reaction, the mother liquid carried out by vacuum filtration to separate the solid and liquid products. The liquid hydrolyzate used as substrate for biological fermentation. The hydrolyzate was analyzed for total sugar concentrations, furfural and 5-HMF (5-Hydroxymethylfurfural). The hydrolysis of agricultural residues and agro-industrial wastes can produce 40e50 g total-sugar/L (50e60 g COD/L) [22,26,35]. Agricultural residues and agro-industrial wastes were analyzed and shown in Table 4.