The cost of pretreatment process for saccharification from biomass and the cost of dilute ethanol purification are significant components of the overall cost for fuel grade ethanol production through fermentation or other biological routes. This work focuses on developing optimal designs of dilute ethanol purification process and the new acid hydrolysis technology for the production of fermentable sugars from biomass where the overarching goal is to reduce the cost of ethanol production from biomass. In this thesis, the ethanol separation process with the reverse osmosis membrane pretreatment is developed to reduce separation cost and energy consumption especially when the feed is dilute. In addition, the new solid phase reactive separation system for biomass saccharification via acid hydrolysis is proposed. This new process is applied for both dilute and concentrated acid hydrolysis where the goal is to increase sugar yield and to reduce byproduct formation. The reaction kinetics of the concentrated acid hydrolysis is investigated through batch experiment. All of these use optimization approaches for seeking the best process designs and for parameter estimations.