Exploitation of Inulin-type Fructans (ItF) from Chicory Roots for the Production of Platform Chemicals
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1 Exploitation of Inulin-type Fructans (ItF) from Chicory Roots for the Production of Platform Chemicals Dominik Wüst, Markus Götz, Andrea Kruse & Judit Pfenning Chair of Conversion Technology and LCA of Renewable Resources (440f) & Agronomy (340a)
2 Introduction
3 Introduction HMF can be synthesized from hexoses: - Fructose - Glucose - Inulin (polyfructose) - Cellulose (polyglucose)
![20 tons of HMF per year purity: up to 99,9 % [1] extraction unit for HMF purification](/docs-images/93/114045501/images/4-3.jpg "[1] HMF [1] http://www.ava-biochem.")
4 First industrial production - HMF from fructose syrup ( 85%) uses the worldwide first industrial plant for HMF production from biomass in Switzerland plant capacity: max. 20 tons of HMF per year purity: up to 99,9 % [1] extraction unit for HMF purification [1] HMF [1] used October 2014 HMF produced by AVA Biochem [1]
5 Pathways from biomass to HMF Lignocellulose Chicory Roots pretreatment extraction Cellulose Inulin depolymerization hydrolysis depolymerization hydrolysis isomerization -3 H 2 O D-glucose D-fructose HMF
6 Chicory - Potential in Numbers Germany: 4,7 % = 13,000 t 8,220 t 46,580 t 32,880 t 41,100 t 142,480 t
![Chicory - Potential in Numbers Chicory roots: forceable: 130 160 190 thousand Roots ha * year-1 [1] Up to 50 %](/docs-images/93/114045501/images/7-2.jpg "non-forceable roots remain on the field or being sorted out Inulin content: 15 20 % fresh weight [2] Fresh weight")
![potential in Europe, status of the 16 th of October 2015 [3] France 2014 (Brittany) [4] 7.](/docs-images/93/114045501/images/7-4.jpg "504 ha = 211,291 t The Netherlands 2014 (Westland) [5] 3.555 ha * 28 t ha -1 99,540 t Belgium 2013 (Flanders) [6] 2.")
7 Chicory - Potential in Numbers Chicory roots: forceable: thousand Roots ha * year-1 [1] Up to 50 % non-forceable roots remain on the field or being sorted out Inulin content: % fresh weight [2] Fresh weight potential in Europe, status of the 16 th of October 2015 [3] France 2014 (Brittany) [4] ha = 211,291 t The Netherlands 2014 (Westland) [5] ha * 28 t ha -1 99,540 t Belgium 2013 (Flanders) [6] ha * 28 t ha -1 64,400 t Germany ha * 28 t ha -1 7,896 t Total Total inulin content in roots size 383,127 t 76,625 t Import of Chicory roots from main cultivating countries [7] for forcing in Germany Bio-economical approach: Production Waste recycling
8 Chicory (Chicorium inybus L.) - Root & Salad production Inulin: - storage/ reserve carbohydrate - polyfructose (DP 35) with or without terminal glucose-residue - chain length is a function of sort, degree of maturity and storage 1. Cultivation of Chicory Roots 2. Chicory Roots during/ after forcing Chemical structure of inulin: left figure: GF n with terminal glucose residue (DP = n + 2); right figure: F m without glucose residue (DP = m + 2) [8]
9 Biosynthesis and degradation of ItF (1) SST-reaction: GF + GF GFF + G (2a) FFT-reaction: GFF + GFF GFFF + GF (2b) FFT-reaction: GF n + GF m GF n+1 +GF m-1 (3) FEH-reaction: GF n GF n-1 + F Legend: F: Fructose; G: Glucose; GF: Saccharose; GFF: 1-Kestose; GFFF: Nystose; SST: Sucrose- 1-fructosyltransferase, FFT: Fructan-fructosyltransferase, FEH: Fructanexohydrolase [8] During Cultivation Before Storage After Forcing
10 Carbohydrate metabolism - Forcing
11 Carbohydrate metabolism - Forcing
12 Carbohydrate metabolism - Forcing
13 Carbohydrate metabolism - Forcing Topscore Dry matter [%] Ash [%] before 23.42± ±0.09 during 23.01± ±0.01 after 15.24± ±0.04
14 Hot water extraction of saccharides (ORAFTI Process) Extraction Filtration Centrifugation Extract Storage: 7 days (harvest delivery date) T = 10 C atmosphere: ~250 L CO 2 d -1 t -1 Chicory roots Processing: 1. washing, 2. slicing, 3. chipping Extraction: Solubility of ItF (90 %) with DP = 10-12: 120 g L -1 at C 350 g L -1 at 90 C 600 g fresh weight L -1 water (85 C) Counter-current diffusing Alternative Processing: purification by liming and carbonation (CaCO 3 ) Demineralization (Ion-Exchange Resin)
15 Batch experiments - yields Input: m = 1 g inulin V = 10 ml mineral acid (0.2 N) 14 ml micro-batch reactors T = 160 C t = 3 min
16 Batch experiments Carbon balance in aqueous product
17 Batch experiments structural analysis of solid product
18 Half-continuous experiments Experimental studies Target: Currently: Experimental and modeling studies on the hydrolysis and dehydration of ItF in diluted mineral acid 1. Physical and chemical characterisation of commercial ItF and Chicory root samples ( analytical problems) 2. Pretests to examine the stability of feed solution (ItF with 0.2 N H 2 SO 4 ) T = 80 (±2) C t 30 min T = C t 15 min c Acid = 0.2 N Preheated water Sugar Extract Product Solution
![Half-continuous plant Modelling studies + Humins 2,5-Dioxo-6-hydroxyhexanal [10] Patil, K. R. S.; Heltztel, J.; Lund, C. R. F.](/docs-images/93/114045501/images/19-4.jpg "Comparison of Structural Features of Humins Formed Catalytically from Glucose, Fructose, and 5-Hydroxymethylfurfuraldehyde. Energy Fuels (2012), 26 26, 5281-5293. [9] Fachri, B. A.; Abdilla, R. M.")
19 Half-continuous plant Modelling studies + Humins 2,5-Dioxo-6-hydroxyhexanal [10] Patil, K. R. S.; Heltztel, J.; Lund, C. R. F. Comparison of Structural Features of Humins Formed Catalytically from Glucose, Fructose, and 5-Hydroxymethylfurfuraldehyde. Energy Fuels (2012), 26 26, [9] Fachri, B. A.; Abdilla, R. M.; Rasrendrac, C. B.; Heeres, H. J. Experimental and modeling studies on theacidcatalyzed conversion of inulin to 5-hydroxymethylfurfural in water. Chemical engineering research and design 109 (2016)
![12-15 % [3] Behr, H.-C.](/docs-images/93/114045501/images/20-4.jpg "(2014) Oral report.")
20 Vision Potential of Inulin-containing crops Example: German Producer Market 3-10 % % [3] Behr, H.-C. (2014) Oral report. Agrarmarkt Informations-Gesellschaft mbh %
21 Thank you very much for your attention!
22 References [1] Konrad, P.; Schneidiger, M. (2013) Kulturblatt Chicorée-Wurzelanbau. Bildungs- und Beratungszentrum Arenenberg Fachstelle Gemüse- und Beerenbau TG/SH. [2] Stolzenberg, K. (2009) Tobinambur Steckbrief. Landwirtschaftliches Technologiezentrum Augustenberg, Außenstelle Rheinstetten-Forchcheim. [3] Behr, H.-C. (2014) Oral report. Agrarmarkt Informations-Gesellschaft mbh. [4] Wikipedia (2014) Bretagne. URL: de.m.wikipedia.org/wiki/bretagne. [5] Foodfreak (2013) Besuch im Westland: Alles Tomate. URL: foodfreak.de/2013/07/besuch-im-westland-alles-tomate/ [6] Hortipendium (2012) Gemüsebau in Belgien. URL: hortipendium.de/gemüsebau_in_belgien [7] Fritsche, B.; Ertel, U. (2009) Gemüsebauerhebung Statistisches Landesamt des Freistaates Sachsen, Statistik in Sachsen 3/2009. [8] Meyer, D.; De Wolf, J.; Olivier, P. Handbuch Süßungsmittel: 4. Neue Zucker, S , 2. Auflage 2007, Hrsg.: Rosenplenter, K.; Nöhle, U.; ISBN: [9] Fachri, B. A.; Abdilla, R. M.; Rasrendrac, C. B.; Heeres, H. J. Experimental and modeling studies on theacid-catalyzed conversion of inulin to 5-hydroxymethylfurfural in water. Chemical engineering research and design 109 (2016) [10] Patil, K. R. S.; Heltztel, J.; Lund, C. R. F. Comparison of Structural Features of Humins Formed Catalytically from Glucose, Fructose, and 5-Hydroxymethylfurfuraldehyde. Energy Fuels (2012), 26 26,
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