OZONOLYSISAS A PRE- PRETREATMENT FOR COMPACTED BIOENERGY FEEDSTOCK Nathan S. Mosier, Iman Beheshti Tabar*, Patrick T. Murphy,

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1 OZONOLYSISAS A PRE- PRETREATMENT FOR COMPACTED BIOENERGY FEEDSTOCK Nathan S. Mosier, Iman Beheshti Tabar*, Patrick T. Murphy, *Graduate Research Assistant, Agricultural and Biological Engineering Department, Laboratory of Renewable Resources Engineering (LORRE), Purdue University

2 2 INTRODUCTION Aben -25 million gallon/ year facility in Hugoton, Kansas; Operational. -30 million gallon/year facility in Nevada, Iowa; Operation Q million gallons/year, formally opened September (eia.gov)

3 3 INTRODUCTION Pretreatment - Key to unlocking low cost cellulosic ethanol.

4 4 OUTLINE Introduction Previous Work Methods Results & Discussion Conclusion

5 5 INTRODUCTION Limited harvest window Storage Prepretreatment

6 6 INTRODUCTION Ozone concentration (mg/l) Corona discharge Time (min.)

7 7 METHOD OF REACTION Lignin + O 3 + H 2 O Soluble Lignin Hemicellulose + O 3 + H 2 O Soluble hemicellulose

8 8 OUTLINE Introduction Previous Work Methods Results & Discussion Conclusion

9 9 PREVIOUS WORK Ozone treatment Lignocellulosic material Grains and cereals Animal feed Biofuel pretreatment Disinfect Storability Neely 1984 Mironet al., 1981 Vidal et al., 1988 Lee et al., 2003 Panneerselvam et al., 2013 Murphy et al., 2010

10 10 PREVIOUS WORK Proof of Concept Excessive moisture content/slurry Too high O3 Travaini et al., 2013 Sugarcane bagasse O3 Concentration: mg /l Silverstein et al., 2007 Biomass in water slurry Particle size: mm Ground biomass Fine particle size Binder et al., 1980 O3 Conc: mg/l Particle size: 0.2 mm

11 11 OBJECTIVES To simulate large scale compacted material treatment by: 1.Using industrially feasible O3 concentration. 2.Bale like particle size(1-200 mm) 3.Treatment of compacted material.

12 12 OUTLINE Introduction Previous Work Methods Results & Discussion Conclusion

13 13 EXPERIMENTAL DESIGN Full factorial Design; Dependent variable: Digestibility (g/g) Independent Variable Each trial a random combination of the following; Levels Treatment time (h) Ozone concentration (mg/l) Flow rate (L/min) Location inside reactor Top Mid. Bot.

14 14 EXPERIMENTAL DESIGN Shawnee Switchgrass Purdue TPAC research farm Harvested November Fix bed Reactor size: L=30 cm D=10 cm 40% Moisture content (constant) g dry solids in each reactor (130 kg/m3)

15 15 OUTLINE Introduction Previous Work Methods Results & Discussion Conclusion

16 16 RESULTS OBSERVATIONS Bleaching Moisture relocation Strong smell of treated material Zero ozone in the outlet for 8 hrs at 3 slpm 15% MC 33% MC 44.5% MC

17 17 RESULTS EXTRACTIVES Water Extractives (g/g) 12.00% 10.00% 8.00% 6.00% 4.00% 2.00% 0.00% Water Extractive Free Sugars Glucose g/g Xylose g/g Arabinose g/g 95.0 g Total O3 input (g) (Control) - Hemicellulose Solubilized, up to 50% - Up to 20% of the initial mass extracted with water

18 RESULTS COMPOSITIONAL CHANGES 18 Amount/initial mass (g/g) 90% 80% 70% 60% 50% 40% 30% 20% 10% 12% 14% 16% 18% 20% 22% 24% 27% 42% 40% 39% 34% Acid Soluble Lignin Acid Insoluble Residue Arabinan Xylan Glucan 0% 95 g 47.5 g 11.8 g (Untreated) Treatment level (Amount O3 Applied)

19 19 RESULTS ENZYME HYDROLYSIS NREL Standard Enzymatic Hydrolysis Assay 0.25 g glucan in each reactor 50 ºC, ph 5.25, 72 hours 10 FPU/g glucan Novozymes Cellic CTec2 250 ml reactors Sugar quantified on HPLC Cellulose conversion calculated by NREL method

20 20 RESULTS ENZYME HYDROLYSIS All water extractives removed before hydrolysis. Treated but unwashed samples were ~ 60% less digestible.

21 21 RESULTS ENZYME HYDROLYSIS Digestibility (g/g) 70% 60% 50% 40% 30% 20% Digestibility increase in different parts of reactor, 72 hr, 1FPU/g cellulose 24hr, 3SLPM, 22 mg/l O 3 3hr, 1.5SLPM, 10 mg/l O 3 Top Middle Bottom 10% 0% Treatment level (1:most severe, 12: least)

22 22 RESULTS CONCENTRATION PROFILE 10 cm

23 23 RESULTS CONSUMPTION VSDIG. - Ozone Gas Transport in the reactor: [ ] = +.( 1 ) :bed porosity : Overall mass transfer coef. : Dist. From gas entrance : interstitial velocity & : O 3 concentration at biomass surface & gas phase Digestibility, TOP (g/g) 80% 70% 60% 50% 40% 30% 20% 10% 0% Maximum Consumption (g) Digestibility, TOP (g/g) 80% 70% 60% 50% 40% 30% 20% 10% 0% Ozone consumed/mass biomass (g/g)

24 24 OUTLINE Introduction Previous Work Methods Results & Discussion Conclusion & Future Work

25 25 CONCLUSION 1. Low ozone concentrations applied to compacted biomass can add value in terms of digestibility. 2. Solubilization of the hemicellulose after ozone treatment. 3. Ozonolysis can effectively delignify energy grasses with negligible sugar losses. 4. Washing solids prior to hydrolysis significantly enhanced sugar yields. 5. Average sugar yields of 450 mg/g achieved with 0.15 g ozone/g biomass. 6. ~ 24.75$ / USD to treat a 1000kg switchgrass bale with ozone gas 0.40$/gallon of etoh.

26 26 FUTURE WORK 1. Mass transfer analysis of O3 diffusivity inside the reactor. 2. Complete mechanistic models for reaction of O3 with the biomass in different parts of the reactor. 3. Statistical model proves basic positive effect on digestibility, lacks actual reaction kinetics of ozone with biomass.

27 27 RESULTS CONCENTRATION PROFILE +!"#+ $%&'(%). "+).#',.+ "+).$%&'(%).+ [ ] = "+).#', - $%&'(%)).. 0 /

28 Laboratory of Renewable Resources Engineering

29 ACKNOWLEDGEMENT Dr. Mosier, my advisor. Dr. Michael Ladisch and other LORRE members and staff. Department of Agricultural and Biological Resources Engineering.

30 Thank you!

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