IMPROVED GLYCERIN QUALITY VIA SOLID CATALYST TRANSESTERIFICATION TECHNOLOGY: THE ESTERFIP-H PROCESS

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1 IMPROVED GLYCERIN QUALITY VIA SOLID CATALYST TRANSESTERIFICATION TECHNOLOGY: THE ESTERFIP-H PROCESS Michel Bloch - Axens Bio-Oil International Conference, Vigo, February

2 Agenda A few words about us The Esterfip-H new heterogeneous catalyst process Principles Process Scheme Comparison with homogeneous catalysis Commercial status Conclusions 2

3 Institut Français du Pétrole from the Well to the Wheel Independent Industrial R&D center E&P, Refining & Petrochemicals, Engines & Energy 1730 peoples on 2 main locations (Paris Lyon) 3

4 IFP-Lyon in a few figures 630 employees (81% of them in R&D) 50% of IFP's R&D staff > 170 pilot units, mock-ups & test benches 4

5 Institut Français du Pétrole from the Well to the Wheel Refining & Petrochemicals Develop clean and economical processes & products for the production of current & future fuels (and petrochemicals bases) from Oil, Gas, Coal & Biomass. Commercialisation through subsidiaries such as AXENS 5

6 Axens Benchmark technology and service provider to the hydrocarbon industries Axens enhances customer performance through innovative technical solutions Innovative processes, catalysts, adsorbents, equipment and services, backed by nearly fifty years of commercial success Axens is a fully owned subsidiary of IFP ISO 9001 (2000) Certified since

7 Global Network Calvert City Princeton Savannah Houston Moscow Beijing Tokyo Caracas Offices Manufacturing Sites Agencies Tech Service Rueil-Malmaison (Headquarters) Lyons, Solaize Salindres 7

8 Catalyst Manufacturing Facility Salindres, France 8

9 IFP/Axens: a Pioneer in Biofuels Technologies 1992: 1993: 1996: 2006: First biodiesel plant started-up First MTBE converted to ETBE First ETBE plant started-up First solid catalyst biodiesel plant 9

10 Esterfip Process Milestones 1984 Lab research initiated : Pilot operations for homogeneous process Esterfip Preliminary trials and operating conditions screening Process validation Methyl ester production for captive fleet tests 1992 Start-up of first Esterfip industrial plant for Sofiproteol at Compiègne (France) - Initial capacity = t/y 1997 Debottlenecking of Compiègne unit (Present capacity = t/y) 2002 Development of heterogeneous process Esterfip-H 2004 Selection of Esterfip-H by Sofiproteol for its new plant in Sète (France) with a capacity of 160,000 t/y 10

11 Trans-Esterification Reaction A Three-Step, Catalytic, Reversible Reaction Vegetable Oil Methanol Methyl-Esters (Biodiesel) Glycerin CH 2 OCOR 1 R 1 COOCH 3 CH 2 OH CH OCOR CH 3 OH Catalyst R 2 COOCH 3 + CH OH CH 2 OCOR 3 R 3 COOCH 3 CH 2 OH 11

12 Esterfip-H Reaction R-COO-CH 2 R-COO-CH R-COO-CH 2 + CH 3 -OH NaOH or NaOMe Heterogeneous Homogeneous Catalyst Glycerin Glycerin CH 3 -OH R-COO-CH 3 Biodiesel HO-CH 2 HO-CH HO-CH 2 NaO-CH 2 +CH 3 ONa HO-CH + R-COONa HO-CH 2 Neutralization Aqueous Step HCl HO-CH 2 MeOH HO-CH + R-COOH + H 2 O HO-CH 2 Fatty Acids NaCl 12

13 Heterogeneous Esterfip-H Methanol Partially Refined Vegetable Oil Reactor Solid Catalyst Reactor Settler Mineral Acid Neutralization Washing Evaporation Biodiesel (Diester) Catalyst Mineral Acid Glycerin Purification Glycerin Fatty Acids 13

14 Esterfip-H Simplified Process Flow Diagram Partial Evap. R1 Partial Evap. R2 Full Evap. Methyl Esters Methanol Vegetable Oil > 98% Glycerin 15

15 Glycerin quality (wt %) Glycerol Water Organic compound Methanol Salts Homogeneous 80 balance Esterfip - H

16 Homogeneous vs. Heterogeneous Homogeneous Maximum yield, 99.5% Glycerin quality Complex separation & purification steps Salt and aqueous wastes Consumption of chemicals Mild conditions T & P Low MeOH/oil ratio Heterogeneous Yield above 100% Glycerin quality Simple separation & purification steps No waste stream No Consumption of chemicals Lower Catalytic cost T & P conditions more severe Higher MeOH/oil ratio 17

17 Esterfip-H - 1 st Commercial Reference New plant in Sète, France Capacity: 160,000 tons per year To be commissioned in the Q Sète Selected by Diester Industrie (Europe s largest producer) 19

18 Conclusions Axens / IFP Over 10 years of experience in biodiesel production technologies Ongoing research and development in the field of vegetable oil esterification 21

19 Conclusions Esterfip-H is IFP/Axens answer to the growing biodiesel demand High biodiesel yield High glycerol quality Green process (no waste) Simplified operations (no chemicals handling) 22

20 Thank you! 23

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