Highlighting parietal modifications through imaging techniques

Transcription

1 Lignocellulosic biomass subjected to hydrothermal pretreatment: Highlighting parietal modifications through imaging techniques Julia PARLATORE LANCHA, Pin LU, Julien COLIN, Giana ALMEIDA, Patrick PERRÉ ELB2018 Reims, June Julia Parlatore Lancha

2 General context : production of second generation biofuels Lignocellulosic biomass Pretreatment Enzymatic treatment Fermentation 2G Biofuels Hydrothermal pretreatment Dilute acid Temperature : ~ 200 Pressure : ~ 20 bar Duration : 2 30 min Explosive phase Brutal decompression Instant pressure drop ~ 1 ms Importance of cell wall s mechanical properties 2

3 General context : production of second generation biofuels Lignocellulosic biomass Pretreatment Enzymatic treatment Fermentation 2G Biofuels Hydrothermal pretreatment Dilute acid Temperature : ~ 200 Pressure : ~ 20 bar Duration : 2 30 min Explosive phase Brutal decompression Instant pressure drop ~ 1 ms Importance of cell wall s mechanical properties 3

4 Hydrothermal process Chemical modifications Anatomical modifications Perspectives 4Julia Parlatore Lancha

5 Hydrothermal pretreatment: experimental protocol Distilled water Biomass : Koster Poplar (Populus euro-americana Koster ) Temperature : 180 Pressure : 15 bar Duration : up to 40 minutes 5Julia Parlatore Lancha

6 Hydrothermal pretreatment: experimental protocol Pre saturation Air (RH = 100 %) Saturation H 2 O and vacuum cycles Hydrothermal pretreatment 180 C / saturated steam Temperature ( C) min 20 min 10 min 0 min Pre drying Air (RH = 75 %) Drying Ambient air Time (min) 6Julia Parlatore Lancha

7 Hydrothermal pretreatment: experimental protocol Pre saturation Air (RH = 100 %) Saturation H 2 O and vacuum cycles Hydrothermal pretreatment 180 C / saturated steam Temperature ( C) min 20 min 10 min 0 min Pre drying Air (RH = 75 %) Drying Ambient air Time (min) 7Julia Parlatore Lancha

8 Hydrothermal pretreatment: experimental protocol Pre saturation Air (RH = 100 %) Saturation H 2 O and vacuum cycles Hydrothermal pretreatment 180 C / saturated steam Temperature ( C) min 20 min 10 min 0 min Pre drying Air (RH = 75 %) Drying Ambient air Time (min) 8Julia Parlatore Lancha

9 Qualitative observations at macro-scale 40 min 20 min 10 min 0 min Native Saturated pretreated samples Shrinkage Air dried pretreated samples T L R 9Julia Parlatore Lancha

10 Reactor T = 190 C RH = 100 % Julia Parlatore Lancha Instrumentation T = 20 C RH = 50 % Hydrothermal pretreatment: Rheological compression tests under severe conditions Kinetics of thermal degradation assessed by the evolution of storage modulus of saturated poplar in the radial direction (MOKDAD et al., 2018) (MOKDAD et al., 2018) Mokdad S. et al. Assessment of biomass alterations during hydrothermal pretreatment by in-situ dynamic mechanical analysis Biomass Bioenergy, 2018, 108,

11 Hydrothermal process Chemical modifications Anatomical modifications Perspectives 11

12 Raman Microspectrometry : a powerful tool for chemical-mapping Quantum Energy Transitions for Rayleigh and Raman Scattering (B&W Tek, 2018) CABROLIER, 2012 B&W Tek, Introduction to Raman Spectroscopy Cabrolier, P. (2012). Caractérisation des propriétés structurales et mécaniques des composantes pariétales du bois à l échelle du tissu. AgroParisTech ENGREF/INRA. 12

13 CABROLIER, 2012 Pretreated wood: a challenging sample preparation Sample s burning by the laser Weak cohesion of cells and cell wall layers Quality of cut Slice s thickness Cabrolier, P. (2012). Caractérisation des propriétés structurales et mécaniques des composantes pariétales du bois à l échelle du tissu. AgroParisTech ENGREF/INRA. 13

14 CCD cts (relative) Julia Parlatore Lancha CCD cts (relative) Cell wall (Panshin et De Zeeuw 1980, Siau 1995, Cloutier 2005). Increasing in sample s fluorescence Secondary cell wall Cell corner min 10 min 20 min 40 min Native wood min 10 min 20 min 40 min Native wood rel. 1/cm rel. 1/cm 14

15 Fluorescence reduction by successive measurements 0 min 5000 Cell wall (Panshin et De Zeeuw 1980, Siau 1995, Cloutier 2005) min 1st measurement 2nd measurement 3rd measurement CCD cts Average spectra for secondary cell wall region rel. 1/cm 10 min 20 min min 20 min 1st measurement 2nd measurement 3rd measurement CCD cts CCD cts rel. 1/cm st measurement 2nd measurement 3rd measurement rel. 1/cm 15

16 CCD cts Julia Parlatore Lancha Cell wall (Panshin et De Zeeuw 1980, Siau 1995, Cloutier 2005). Fluorescence reduction by successive measurements (zoom) 0 min 0 min Average spectra for secondary cell wall region 1st measurement 2nd measurement 3rd measurement rel. 1/cm 10 min 20 min min 20 min CCD cts 1500 CCD cts st measurement 2nd measurement 3rd measurement rel. 1/cm st measurement 2nd measurement 3rd measurement rel. 1/cm 16

17 Raman spectral mapping Fluorescence 2894 cm cm -1 Native wood Saturation 40 min 17

18 Hydrothermal process Chemical modifications Anatomical modifications Perspectives 18

19 Nano-tomography X-ray source θ Sample θ = 0 θ = 90 θ = 180 θ = 360 2D Projections of the sample Cross-sectional slices 3D volume rendering RX Solutions EasyTom XL Ultra D-BioMat Project 19

20 Anatomical modifications Hydrothermally pretreated wood 180 C / 40 min Cell wall collapse Shrinkage through tangential direction 50 µm 20

21 Hydrothermal process Chemical modifications Anatomical modifications Perspectives 21

22 Perspectives Other laser wavelengths for Raman micro-spectrometry Chemical analysis Coupling with mechanical results Evaluation of hydrothermal pretreatment s influence on enzymatic hydrolysis 22

23 For a period of three years (from 01/05/2016 to 30/04/2019), the 3D-BioMat project is hosted by the European Center for Biotechnology and Bioeconomy (CEBB Pomacle, France). With a total budget of 965,000, 3D-BioMat is co-financed by Grand Reims for 31% and by the European Union for 48.7% (ie 50% of eligible expenses). Europe is committed to the Grand Est region with the European Regional Development Fund. Poplar obtained thanks to the National Council of Poplar and kindly donated by Scierie Huberlant. Thank you for your attention 23