July 7, 2010DS Sustainable Fuels1 Insight into Commercial Biodiesel Production CONASTA David Schaller

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Biodiesel quality standards Test results of Tallow biodiesel after water wash

Palm oil Rape seed oil, Soyabean oil, Sunflower oil, Canola oil, Coconut oil, Jatropha nut oil, Used Cooking Oil, Animal fats Conversion High viscosity Poor combustion properties Low viscosity Excellent combustion properties Raw oil sources of biodiesel Bio- Diesel July 7, 2010DS Sustainable Fuels8

Triglycerides Fatty-Acids: Micelles, phospholipids, proteins, mineral saltsOthers: > 95% % Raw oils chemical composition O O O O O O OH O < 1% July 7, 2010DS Sustainable Fuels9

Triglyceride transesterification Purified Triglycerides > 95% O O O O O O OCH 3 O OH HO OH Biodiesel Glycerine NaOCH 3 CH 3 OH July 7, 2010DS Sustainable Fuels10

Soap formation Free fatty acid (FFA) < 5% OH O Methanol NaOCH 3 CH 3 OH The FFA content of the triglycerides should be maintained below 0.5% to minimize soap formation and maximize BD selectivity ONa O Soap + + July 7, 2010DS Sustainable Fuels11

Biodiesel production with Lewatit® K2567 Bio- Diesel July 7, 2010DS Sustainable Fuels12

Conventional Biodiesel Production Process Glycerine + Salts Transesterification Low-acid Triglycerides MeOH MeONa HCl Separation MeOH + Gly. + salts Water + Glycerine + Salts Methyl ester Glycerine Water Water strip Pure ethyl esters (Biodiesel) Antioxidant Water wash Water strip MeOH Strip Glycerine purification Raw oils with free fatty acids Esterification July 7, 2010DS Sustainable Fuels13

Pure ethyl esters (Biodiesel) Transesterification Glycerine + Salts MeOH MeONa Separation MeOH + Glycerine Glyc. Adsorption Desorption Methyl ester Glycerine Antioxidant MeOH Strip Lewatit K 2567 Glycerine purification Esterification Raw oils with free fatty acids Biodiesel production with Lewatit K2567 Low-acid Triglycerides July 7, 2010DS Sustainable Fuels14

Lewatit K2567 has specifically been developed for biodiesel purification and is used to remove glycerine, monoglycerides, soaps and salts. Biodiesel purified with K 2567 fulfills the stringent specification requirements of the European and American fuel industries. K2567 is a macroporous cation exchange resin with monodisperse bead sizing, to optimize break-through and pressure drop performance in packed beds. One liter of K2567 will purify tons biodiesel / year It can be reused many times, thus minimizing resin disposal costs. Resin lifetimes up to 7 years have been obtained. Therefore only relatively small beds are necessary for cycle times of 7–10 days It can be retrofitted into existing plants. All biodiesel qualities irrespective of the triglyceride source can be treated. It is currently used in plants ranging widely in size, from 10,000  350,000 to/a. And it is the most cost-effective ion exchange resin based purification system in the market. Lewatit K2567 has been used for biodiesel production in Europe since Advantages of using Lewatit K2567 July 7, 2010DS Sustainable Fuels15

K 2567 “sponge-structure“ Resin packing & structure of Lewatit K2567 Monodisperse bead sizing, hexagonal closest packing July 7, 2010DS Sustainable Fuels16

Mechanism of glycerine removal Solvation of glycerine with K 2567 SO 3 - OH HO OH Na + OH HO OH HO OH K 2567 July 7, 2010DS Sustainable Fuels17

Application mode of Lewatit K2567 Alternate loading and washing 1. Biodiesel + glycerine 2. Washing with MeOH 1. Purified biodiesel 2. MeOH + glycerine B. MeOH tank or MeOH strip A. Transesterification tank Lewatit K 2567 July 7, 2010DS Sustainable Fuels18

Biodiesel from phase separation glycerine: 600…2000 ppm soap:10 – 200 ppm refined biodiesel glycerine: <10 ppm soap: < 5 ppm Operating Conditions: Temperature:30°C – 40°C LHSV: 1.5 – 2 BV*biodiesel/hr Bed height:1 – 2 m Op. Capacity:250 g glycerine/liter Regeneration: 20-35°C Reg. volume:2-4 BV to transesterification 5-10 BV to MeOH storage Resin life:4-5 years (average) *BV = bed volumes Removal of glycerine and soap with Lewatit K 2567 Fresh K2567 is first preconditioned by drying with 3-4 bed volumes MeOH at 2BV/h. The MeOH is then drained and the biodiesel passed into the reactor. Before the MeOH wash, the biodiesel is also drained. After preconditioning, K2567 is only subjected to alternate MeOH / biodiesel treatments and never washed with water. Preconditioning Lewatit K 2567 July 7, 2010DS Sustainable Fuels19

Reduced investment Biodiesel production with Lewatit Lower operating costs Ease of operation Advantages of water wash elimination July 7, 2010DS Sustainable Fuels20

Basic design and resin cost Capacity100,000to/a Annual operation8,000h Throughput12.5to/h 15,600l/h 69gal./min. LHSV2bed vols/h Bed volume7,800liter K2567 Bed height2meter Pressure drop0.4bar Glycerine capacity250g/liter resin Glycerine conc800ppm Cycle time156h Resin lifetime5years Resin cost / l biodiesel € / l $ / gal This basic design can be scaled linearly for plant sizing ranging from 1,000  300,000 to/a. Bed depth should be kept in the range 1.5 m (1,000 to/a) to 3 m (300,000 to/a) July 7, 2010DS Sustainable Fuels21

Additional Information Fox Design: Poppy oil and meal: IX resins: www. lewatit.de, July 7, 2010DS Sustainable Fuels22