Advanced characterization techniques to evaluate the structure of nanofibrillated cellulose
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1 Advanced characterization techniques to evaluate the structure of nanofibrillated cellulose Final Conference Asko Sneck, Atsushi Tanaka, VTT Valerie Meyer, CTP Jens Kretzschmar, PTS
2 Aim Use advanced characterization methods to evaluate the properties of NFCs used in demonstrations 2
3 Characterization methods VTT Conductometric titration Zeta potential Viscosity Microscopy / SEM and OM Size profile by fractionation (fractionation trials) SEM Dissolved fraction analysis Total organic carbon (TOC) Carbohydrate by Ion chromatography (IC) Capillary electrophoresis (CE) PTS Fibre morpholoy / FibreLab DP/viscosity number / ISO Total Charge, carboxyl content / Tappi T237 om-88 revised version -93 Surface charge / Modified polyelectrolyte titration Length of the fibrils / FibreLab Structural and dimensional appearance / SEM CTP Length of the fibrils/morfi Visual appearance of nanocellulose / Optical microscopy Structural and dimensional appearance / SEM 3
4 Pilot NFCs to characterize NFC-CTP (2% solids) Enzymatically treated Homogenized at CTP NFC-TE/CTP (2% solids) TEMPO oxidized Homogenized at CTP NFC-TE/PTS (9% solids) TEMPO oxidized Homogenized at PTS 4
5 Characteristics of materials NFC-CTP NFC-TE/CTP NFC-TE/PTS Gel type opaque, viscous transparent, solid white, fluent Total acid group content 17 µmol/g 1073 µmol/g Zeta potential mv mv mv ph Conductivity 262 µs/cm 730 µs/cm 554 µs/cm Most stable well dispersed 5
6 Microscopy characterization Light microscopy NFC-CTP NFC-TE/CTP NFC-TE/PTS SEM TEM 6
7 Length in mm Length of the fibrils (FiberLab) 0,30 error bars: 1σ 30% 0,25 0,20 25% 20% Mean lengthweighted fibre length "L(l)c." in mm 0,15 15% Relative number of particles with L(l)c > 0,2mm in % 0,10 0,05 10% 5% Length-weighted content of particles with L(l)c > 0,2mm in % 0,00 NFC-CTP NFC-TE/CTP NFC-TE/PTS 0% 7
8 Fibre morphology and carboxyl content of NFCs Fibre = elements with a length > 80µm Fine = elements with a length < 80µm 8
9 Viscosity / mpa s NFC-CTP : Comparable with ARBOCEL NFC-TE/CTP : Highest viscosity due to fine fibrils NFC-TE/PTS : Viscosity (at 1.5% solids content) - fibrillation degree - aspect ratio Low viscosity due to low aspect ratio More information in a poster NFC-CTP/CTP NFC-TE/CTP NFC-TE/PTS Rotational speed / rpm 9
10 Fractionation trials More information in a poster 20µm 10µm 5µm Net 1µm Membrane 0.1 µm <0.1µm NFC (feed) >20µm 20-10µm 10-5µm 5-1µm 1-0.1µm Membrane filtrate Too diluted! (< 0.005% solids) reject Analyses for dissolved fraction - TOC - Carbohydrate composition - Capillary electrophoresis 10
11 Particle size profile Pilot NFCs NFC-TE/CTP Small portion at > 1µm (10%) Sharp peak at 1 0.1µm (85%) Dissolved fraction (<0.1µm) ~10% for enzyme treated NFC ~5% for TEMPO oxidized NFCs 11
12 SEM images (NFC-CTP) NFC (feed) 20µm 10µm 5µm Net 1µm Membrane 0.1 µm <0.1µm >20µm 20-10µm 10-5µm 5-1µm 1-0.1µm NFC4C-4 x3000 NFC5C-1 x3000 NFC5P-2 x
13 SEM images (NFC-TE/CTP) NFC (feed) 20µm 10µm 5µm Net 1µm Membrane 0.1 µm <0.1µm >20µm 20-10µm 10-5µm 5-1µm 1-0.1µm CTE4C-3 x3000 CTE5C-1 x3000 CTE5P-1 x
14 SEM images (NFC-TE/PTS) NFC (feed) 20µm 10µm 5µm Net 1µm Membrane 0.1 µm <0.1µm >20µm 20-10µm 10-5µm 5-1µm 1-0.1µm PTE4C-3 x2000 PTE5C-3 x3000 PTE5P-2 x
15 Analyses for dissolved fraction (membrane filtrate) Membrane NFC (feed) filtrate reject 15
16 Total organic carbon (TOC) for dissolved fraction (membrane filtrate) Total organic carbon (TOC) 2% NFC-CTP 640 mg/l 2% NFC-TE/CTP 470 mg/l 2% NFC-TE/PTS 270 mg/l * Why high TOC in NFC-CTP? NFC-CTP contained more monosaccharide due to enzyme? TEMPO oxidized NFCs lost dissolved materials due to washing away? * calculated from 9% NFC-TE/PTS 16
17 Carbohydrate composition of the starting spruce pulp and the dissolved fractions (< 0.1µm) Sample Arabinose Galactose Glucose Xylose Mannose Tot. Monosaccharides (rel %) (rel %) (rel %) (rel %) (rel %) mg/l Spruce pulp <0.05 < ,5 1,5 2 2% NFC-CTP filtrate < 0,05 < 0,05 96,4 1,7 1,6 830,0 2% NFC-TE/CTP filtrate < 0,05 < 0,05 71,4 15,0 12,1 140,0 2% NFC-TE/PTS filtrate < 0,05 < 0,05 68,8 14,4 18,1 36,0 Dissolved fraction of NFC-CTP carbohydrate composition similar as the carbohydrate composition of starting pulp Dissolved fraction of TEMPO treatment Decreased glucose Increased xylose and mannose 17
18 Summary Characterization methods are able to evaluate properties of NFC TEMPO oxidization increased carboxyl group significantly NFC-TE/CTP and NFC-CTP contain more fibrillar material compared to NFC-TE/PTS TEMPO treatment and Cavitron are cutting fibers to small fragments but material does not contain thin fibrillar material NFC-TE/CTP Rather short fibrils with least branching Only a slight sedimentation in fraction 0,1-1 µm Samples NFC-CTP and NFC-TE/PTS showed a significant sedimentation Manufacturing process affects the amount of dissolved compounds 18
19 THANK YOU FOR YOUR ATTENTION! Poster: Advanced characterization techniques to evaluate the structure of nanofibrillated cellulose / Asko Sneck and Atsushi Tanaka More detail information about fractionation and viscosity measurements 19
20 Acknowledgement The research leading to these results received funding from the European Community s Seventh Framework Programme under Grant Agreement No
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