Wastewater Treatment Facilities: A Source of Oil for Producing Biodiesel Rafael Hernandez and Todd French Mississippi State University Dave C.

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1 Wastewater Treatment Facilities: A Source of Oil for Producing Biodiesel Rafael Hernandez and Todd French Mississippi State University Dave C. Swalm School of Chemical Engineering

2 Biodiesel Industry: Present & Future Challenges Total US BD usage is ~80 Mgal/yr US uses ~75 Bgal/yr of Petro-Diesel Total oleochemical production capacity is ~500 Mgal/yr More than 70% of current biodiesel production cost is the feedstock There is a glut of crude glycerine in the market Current price of crude glycerine is ~ $0.01/lb compared to $0.60/lb in Many biodiesel producers are storing crude glycerine

3 DOE SERC Biofuels Research & Development at MSU Lipid Source Production Lipid Extraction Biofuel Production Biofuel Market Development Plant Sciences Biochemistry Chemical Engineering Chemical Engineering Chemistry Plant Sciences Biochemistry Agricultural and Biological Engineering Chemical Engineering Food Sciences Chemical Engineering Agricultural Economics Mechanical Engineering

4 Technical Accomplishments/ Biodiesel from Sewage Sludge (~1 Bgallons oil) Municipal Wastewater Treatment Influent S-102 P-1 / GB-101 Grit Chamber S-103 S-104 S-106 S-109 S-110 S-111 S-112 Liquid Effluent S-114 S-105 P-3 / AB-101 Aerobic BioOxidation S-107 P-4 / AB-102 Aerobic BioOxidation P-5 / CL-101 Clarification S-108 P-6 / FSP-101 Flow Splitting S-101 S-120 S-123 Sludge Effluent S-113 P-9 / TH-101 Thickening S-126 P-11 / BF-101 Belt Filtration S-127

5 Biosolids Generated for Use or Disposal in the United States M dry tons M dry tons M dry tons M dry tons Biosolids Generation, Use, and Disposal in the United States, EPA530-R , September

6 Extraction and Transesterification Yield of Waste Activated 100% Hexane b Sludge a f % of Oil Extraction Medium % Oil Yield Saponifiable g % Overall Yield h % Methanol b 19.39± ± ± % Hexane c Extraction % Methanol Extraction ± ± % Acetone Extraction ± % Methanol d Extraction ± ± ± % Hexane Extraction SC-CO SC-CO 2 w/ 1.96 wt% MeOH SC-CO 2 w/ wt% MeOH In Situ Transesterification e ±0.11 a All extractions carried out at 100 C for 1 hour, solvent to solids ratio 40:1 b Sample extracted once c Solvent mixture extracted three times d Sequential extraction using Methanol followed by Hexane e Dried to 95 weight percent solids. Solvent was Methanol with 1% Sulfuric Acid f Gravimetric yield of oil in grams of oil per gram of dry sludge g Percent of extracted oil saponifiable on a mass basis. h Grams of FAME produced per 100 grams of dry sludge g,h Values on left indicate individual extraction yields. Values on the right indicate total yield. Production Cost Estimate for Sludge Biodiesel a Centrifuge O&M Drying O&M Extraction O&M Biodiesel Processing O&M Labor Insurance Tax Depreciation Capital P&I Service Total Cost $0.30/lb a Assuming 7.0% overall transesterification yield $0.43 /gal $1.29 /gal $0.34 /gal $0.60 /gal $0.10 /gal $0.03 /gal $0.02 /gal $0.12 /gal $0.18 /gal $3.11 /gal üprimary and secondary sludge from the Tuscaloosa Wastewater Treatment Facility has been extracted and converted into fatty acid methyl esters (biodiesel) üexamination of the various transesterification methods shows that in situ conversion of lipids to FAMEs provides the highest overall yield of biodiesel. üassuming at 7.0% overall yield of FAMEs from dry sewage sludge on a weight basis the cost per gallon of biodiesel would be $3.11. üas transesterification efficiency increases the cost per gallon drops quickly, 6 hitting $2.01 at 15.0% overall yield.

7 Biodiesel produced from primary sludge üthe experimental data indicated that the production of biodiesel by in-situ transesterification of primary sludge is second order, when the methanol:lipid molar ratio employed is in great excess compared to the stoichiometric requirement. ($) Centrifuge O&M 0.22 Drying O&M 0.64 Extraction O&M 0.17 Biodiesel processing O&M 0.60 Labor 0.10 Insurance 0.03 Tax 0.02 Depreciation 0.12 Capital P&I service 0.18 Total cost 2.08 Cost per gallon $0.15/lb üthe biodiesel compositions derived from primary and secondary sludge are indicative of the source of acylglycerides and fatty acids. üthe cost per gallon of biodiesel from dry primary sludge would be $2.08. üthis is more cost effective compared to biodiesel from dry secondary sludge.

8 Saturated vs. Unsaturated Distribution in Sludge Sources Fatty Acid Saturation vs. Feedstock Polyunsaturated FAMEs Monounsaturated FAMEs Saturated FAMEs 100% 90% 10.83% 7.01% 12.60% 16.03% 80% 22.84% 31.28% 70% 42.00% 39.80% 60% Percent of Total 50% 40% 70.13% 30% 57.89% 20% 45.40% 44.17% 10% 0% Lafayette Lafayette Primary Lafayette Starkville Biosolids 1 Primary Solids 1 Secondary Solids 1 Secondary Solids 2

9 The Yeast Rhodotorula glutinis Means red glutton Aerobic, oleaginous (oil-producing) yeast High methyl ester yield 1,2 Breaks down carbon oxygen demand (COD) in waste streams 2,3 1. Granger, L-M; et al. Biotech. & Bioengineering, 1993, 42, Zheng, S; et al. Bioresource Tech., 2005, 96, Xue, F; et al. Process Biochem., 2006, 41,

10 Oleaginous Microorganisms Grown on Wastewater Oleaginous Yeast Grown on Wastewater with 0.1g/L of Dextrose Oleaginous Yeast Grown on Wastewater with 1g/L of Dextrose Optical Density (600nm) R. glutinis C. curvatus Pos. Control: R. glutinis Pos. Control: C. curvatus Negative control: wastewater optical density (600nm) R. glutinis C. curvatus Pos. control: R. glutinis Pos. control: C. curvatus Negative control: wastewater Time (hr) time (hr)

11 Conversion of Lignocellulosic Biomass to Microbial Oil

12 Envisioned Process: The New Biorefineries Influent S-102 S-104 S-109 S-112 P-1 / GB-101 Grit Chamber S-118 P-7 / CL-102 Clarification S-105 P-3 / V-101 Oxidation Unit S-106 S-110 P-2 / MX-101 S-107 Mixing P-4 / AB-102 Aerobic BioOxidation S-111 P-5 / CL-101 Clarification Liquid Effluent S-114 S-108 Sugars Lignocellulose S-101 P-6 / FSP-101 Flow Splitting P-10 / MX-102 S-113 Mixing S-120 S-123 S-116 Oily Sludge S-117 S-119 S-115 P-8 / AB-101 Lipid Accumulation Chamber P-9 / TH-101 Clarification S-121 P-11 / BF-101 Belt Filtration S-122

13 Environmentally Sustainable Fuel Production

14

15 Benefits üprovides a profitable aspect to sewerage treatment üapproximately 30% reduction in biosolids generation (note that biosolids management has become a big problem for cities disposal costs >$50/dton) ügreatly improved pathogen stabilization (Produces Class A Sludge) üminimal impact to on-site treatment operations üminimal additional footprint requirements üprovides cheap diesel source to city fleets üadds a fuel production incentive to third world countries to treat sewage

16 Summary The MSU Biodiesel Project integrates three key research areas associated with biodiesel production: feedstocks, oil extraction, and biodiesel processing technologies. Although the process for biodiesel production is relatively simple, specific feedstocks may require unique extraction and processing techniques to assure quality. The Sugar Platform, and current wastewater treatment, biodiesel, and fuel distribution infrastructure could be integrated to potentially generate 10 billion gallons of biodiesel (~10% diesel displacement).

17 Acknowledgements US Department of Energy USEPA-RARE PERC LS9 Mississippi Technology Alliance MSDEQ Hilliard Fletcher Wastewater Treatment Plant, Tuscaloosa AL

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