Production and Application of Cellulose Nanomaterials. Michael Bilodeau Director, Process Development Center University of Maine

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1 Production and Application of Cellulose Nanomaterials Michael Bilodeau Director, Process Development Center University of Maine

2 Outline UMaine Process Development Center Introduction to Cellulose Nanomaterials Partnerships Applications Commercialization Activities May 19, 2015 E2 Tech Meeting - BioBased Maine 2

3 UMaine Process Development Center Serving the Needs of Industry Since 1987 Department of Chemical and Biological Engineering Not-for-Profit Contract Research Group Self Supporting Professional Staff Fee-for-Service Basis May 19, 2015 E2 Tech Meeting - BioBased Maine 3

4 Innovation Continuum R,D,& C Its Cyclical not Linear Production/ Public Access Basic Research Applied Research Development Demonstration Commercialization +$$ $ Fed Grants DoD,DOE,USDA. $$ VC --Equity-- Debt $ Fed Grants NIH,NSF, etc. $$ -Regional & State Seed Grants, Development Awards, Fed SBIR -$$ Science & Technology Drives Univ and Non-profit R&D $ Company Funds Family, Fools and Friends Valley of Death Business & Markets Drive Commercial R&D May 19, 2015 E2 Tech Meeting - BioBased Maine 4

5 Operating Model Partner with Industry Collaborate with other Institutions & Agencies Coordinate Project Activities Public Academia Private May 19, 2015 E2 Tech Meeting - BioBased Maine 5

6 Pilot Capabilities Pilot paper machine Web coater / laminator May 19, 2015 E2 Tech Meeting - BioBased Maine 6

7 Example of Private-Public Partnership High Speed Pilot Coater - Client Owned and Operated May 19, 2015 E2 Tech Meeting - BioBased Maine 7

8 Example of Private-Public Partnership Specialty Paper Machine - Client Owned and Operated May 19, 2015 E2 Tech Meeting - BioBased Maine 8

9 Introduction to Cellulose Nanomaterials May 19, 2015 E2 Tech Meeting - BioBased Maine 9

10 Cellulose Based Materials Cellulose Derivatives Cellulose Acetate Hydroxyethyl Cellulose Methyl cellulose Carboxymethyl Cellulose Functionalize -OH Cellulose based nanoparticles Microcrystalline Cellulose Fiber Lumber May 19, 2015 E2 Tech Meeting - BioBased Maine Courtesy Dr. Robert Moon USFS 10

11 Cellulose Nanofibrils May 19, 2015 E2 Tech Meeting - BioBased Maine 11

12 What are Cellulose Nanomaterials (CNs)? Nano-sized particles isolated from: trees, plants, algae Highly ordered cellulose chains: parallel stacking of chains ordered & disordered domains Nano Effect : Fewer defects Aligned chains Properties: Length Aspect ratio Crystallinity May 19, 2015 E2 Tech Meeting - BioBased Maine Courtesy Dr. Robert Moon USFS 12

13 Several Flavors of CNs All Biomass Mechanical Acid Hydrolysis Chem/Mech Cellulose Nanocrystals (CNC) Rod-like D=3-20 nm L= nm Low branching Cellulose Nanofibrils (CNF) Fibril-like: D=3-40 nm L=100s nm - >1µm Branching Particles: Source Method Properties: Length Aspect Ratio Branching Crystallinity Dufresne et al., J. App. Poly. Sci., 1997 May 19, 2015 E2 Tech Meeting - BioBased Maine Courtesy Dr. Robert Moon USFS 13

14 Cellulose Nanofibrils Fibril width nm Lengths up to 10 s of microns High aspect ratio ( ) Large specific surface area ( g/m 2 ) x 100k 200 nm SEM image of isolated Cellulose Nanofibrils May 19, 2015 E2 Tech Meeting - BioBased Maine 14

15 History of Nanocellulose Reduced to practice by ITT Rayonier, 1977 Patented in 1983 Turbak, et. al. May 19, 2015 E2 Tech Meeting - BioBased Maine 15

16 CNF Related Patents May 19, 2015 E2 Tech Meeting - BioBased Maine 16

17 CNF Related Publications May 19, 2015 E2 Tech Meeting - BioBased Maine 17

18 Why CNF Again? Three Major Driving Forces Breakthrough lower cost manufacturing methods New, novel application technology National priorities driving federal funding May 19, 2015 E2 Tech Meeting - BioBased Maine 18

19 Overcoming Commercial Barriers Scalable Low Capital Low Energy Applications

20 Partnerships May 19, 2015 E2 Tech Meeting - BioBased Maine 20

21 May 19, 2015 E2 Tech Meeting - BioBased Maine 21

22 US Forest Service #1 Priority Forest Fire Suppression >$1 MM/hr spent fighting forest fires More than ½ of USFS annual Budget Millions of acres need Restoration Only 200,000 acres/yr restored. May 19, 2015 E2 Tech Meeting - BioBased Maine 22

23 May 19, 2015 E2 Tech Meeting - BioBased Maine 23

24 Capability UMaine CNF Pilot Facility Refiner CNF Pre-treatment Mass Colloider Grinder Capacity 1 ton/day Slurry form (3% solids) May 19, 2015E2 Tech Meeting - BioBased Maine 24

25 Availability UMaine CNF Pilot Facility Fee-for-service basis Samples available Kg to tonne quantities CNF & CNC Slurry or dry May 19, 2015E2 Tech Meeting - BioBased Maine 25

26 Spray Dryer UMaine CNF Pilot Facility Several kg/day capacity May 19, 2015E2 Tech Meeting - BioBased Maine 26

27 Cellulose Nanomaterials Distributed between April 2013 February 2015 Samples provided to 167 private companies 119 academic institutions 25 research centers In 35 different countries May 19, 2015 E2 Tech Meeting - BioBased Maine 27

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29 Applications May 19, 2015 E2 Tech Meeting - BioBased Maine 29

30 Production Yields Process Costs Commercial Application Areas Acoustic Structural Thermal Foams Paakko et al., Soft Matter, 2008 Continuous Fibers Reinforcement Textiles Woven Dong et al., 2012 Tissue Engineering Scaffolds Bandages Ligament Blood Vessels Drug Delivery Deng et al. Flexible Electronics Self Powered Display Solar LED Yano et al. Separators/Barrier Filtration Batteries Pumps Rheology Modifier Paints Cosmetics Food Adhesives May 19, 2015 Specialty Packaging Herrera et al. Vartiainen et al. E2 Tech Meeting - BioBased Maine Courtesy Dr. Robert Moon USFS Specialty Cements Foamed Panel Siding Cao et al. 30

31 Commercial Scale-up Release Base Paper Surface Control 208 X CN X 5% CNF added May 19, 2015 E2 Tech Meeting - BioBased Maine 31

32 Stain Results Silicone Coated Release Base A. Control Base B. CN 200 Base Pilot paper machine samples 5% CNF May 19, 2015 E2 Tech Meeting - BioBased Maine 32

33 Paper Coated with CNF X µm 1.5 g/m2 coating X µm 0.5 g/m 2 coating 3.0 g/m2 coating X µm May 19, 2015 E2 Tech Meeting - BioBased Maine 33

34 Ink density of Ink Jet Printed Samples EKA Chemicals Inc. CNF improves ink jet print quality May 19, 2015 E2 Tech Meeting - BioBased Maine 34

35 Polymer Composites Conventional Bleached CNC & CNF Very poor dispersion BioPlus L-CNC Very uniform dispersion 1% CNC in PLA 1% TEMPO CNF in PLA Neat PE 1% L-CNC in PE Agglomerates Neat PHB 1% L-CNC in PHB Neat Silicone 1% L-CNC 2% L-CNC 0.3% L-CNC in PLA Neat PS 1% L-CNC in PS May 19, 2015 E2 Tech Meeting - BioBased Maine 35

36 BioPlus Compostable Bags Strong Renewable Compostable PLA + BioPlus L-CNC May 19, 2015 E2 Tech Meeting - BioBased Maine 36

37 Vehicle Light Weighting Project Objective: Development of a sprayable binder resin system containing nanocellulose as a reinforcing phase to replace steel in seating assemblies Opportunity to achieve commercial application on electric vehicles Results: Clark ATL has successfully dispersed L-CNC in the hydrophobic resin system of choice Impact: Reducing a vehicle s weight by just 10 percent can improve fuel economy by 6-8 percent U.S. DOE s target vehicle weight reduction is 50% by According to the DOE the limiting factor in use of lightweight materials in vehicles is availability of sufficient quantities at affordable cost 1 ReinforcingMaterial Density (g/cm 3 ) Calcium carbonate 2.71 Talc 2.69 E-glass fiber 2.5 Carbon fiber 1.8 Nanocellulose 1.5 May 19, 2015 E2 Tech Meeting - BioBased Maine 37

38 3D Printing Project Objective: Reinforce 3D printing feedstock with high temperature stability, highly dispersable BioPlus-L to obtain desired mechanical properties for load-bearing parts Impact: Replace high cost, peutroleum based carbon fiber as reinforcing agent for high temperature polymers like ABS, PLA, Nylon 6,6, and PC with renewable, biobased nanocellulose. Phase II Goal: Print a golf cart from nanocellulose reinforced polymer using Oak Ridge s Big Area Manufacturing (BAAM) facility. May 19, 2015 E2 Tech Meeting - BioBased Maine 38

39 CNF Films May 19, 2015 E2 Tech Meeting - BioBased Maine 39

40 Industrial Epoxy Coatings Link Link Link May 19, 2015 Link E2 Tech Meeting - BioBased Maine 40

41 May 19, 2015 E2 Tech Meeting - BioBased Maine 41

42 Commercialization Activities May 19, 2015 E2 Tech Meeting - BioBased Maine 42

43 Ref: Shatkins, J Tappi Nano Conference Vancouver, BC May 19, 2015 E2 Tech Meeting - BioBased Maine 43

44 Commercial Start-ups American Process Inc. Thomaston, GA BioPlus Pre-commercial plant tpd capacity CNF and CNC capacity Started-up April 2015 May 19, 2015 E2 Tech Meeting - BioBased Maine 44

45 API s Thomaston Biorefinery Biomass Fractionation and Cellulose Separation Cellulose products Regenerated Solvent, SO 2 Chemical Regeneration Liquor (hemicelluloses solvent, SO 2, lignin) Washed Lignin to energy and chemical applications Hemicelluloses Auto Hydrolysis Enzymatic Hydrolysis Hemicelluloses Sugars to Ethanol / Butanol Glucose to chemicals conversion May 19, 2015 E2 Tech Meeting - BioBased Maine 45

46 BioPlus Demonstration Line ½ ton per day Start-up in April 2015 Located at Thomaston Biorefinery Screening & Cleaning Bleach Plant Mechanical Treatment Product Cooling & Storage May 19, 2015 E2 Tech Meeting - BioBased Maine 46

47 Commercial Start-ups Paperlogic Paper Turners Falls, MA Commercial CNF plant - 2 tpd capacity Internal and merchant sales Started-up May 14, 2015 May 19, 2015 E2 Tech Meeting - BioBased Maine 47

48 Contacts Michael Bilodeau, Director Phone: Pros Bennett, Managing Director Phone: May 19, 2015 E2 Tech Meeting - BioBased Maine 48