Microfibrillated Cellulose Reinforcement in Phenol Formaldehyde Wood Adhesive

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1 Microfibrillated Cellulose Reinforcement in Phenol Formaldehyde Wood Adhesive Will Hand Department of Chemical Engineering Auburn University Sun Grant Initiative 2015 Sun Grant Regional Conference

2 Microfibrillated cellulose (MFC) 3-30 nm diameter Wide range of lengths Crystalline and amorphous regions

3 Why MFC? Advantages Sustainable, renewable resource High strength and stiffness Transparent and translucent High surface area and aspect ratio High reactivity, barrier properties

4 Microfluidics Hydraulic pump Interaction chamber (87 µm) 500 m/s, ,000 psi High shear and impact forces

6 Why MFC? Disadvantages High energy consumption to process Large water content (1-30% solids content) Hornification Hydrophilic character compatibility with hydrophobic materials

7 Methods to improve processing TEMPO-mediated oxidation Carboxymethylation Acetylation

8 Phenol Formaldehyde Used as adhesive in production of Oriented Strand Board (OSB) Disadvantage Formaldehyde off gassing Expensive Soy waste Cheap Improves strength MFC Past studies show strength improves Synergistic effect

9 Method Microfibrillated cellulose (MFC) was mixed with Soy MFC/Soy mixture was mixed with Phenol Formaldehyde (PF) adhesive All pulp and soy mixed with PF was heated or hydrated until original consistency matched PF (52%) DIN EN 205 (shear stress) modified to include MOE

10 Results Soy - strength 11 Soy addition to PF T % 20 30

11 Preparation of samples 150 mm Wood samples were cut according to standard DIN EN 205 from species Pinus taeda 2x4 s into 80 mm x 20 mm x 5 mm pieces Adhesive was applied to a 20 mm x 10 mm overlap area Samples were pressed Samples were put into oven for 4 hours at 105 C to cure 10 mm 20 mm 5 mm 5 mm

12 Equipment Zwick/Roell Z010 Static Material Testing Machine was used to measure strength and MOE 9 x9 press was used at 200 psi at different times and temperatures

13 Procedure A lap shear test was conducted on the Zwick Roell Z010 using the European standard DIN EN 205 for wood adhesives to determine the tensile shear strength of the lap joints The testxpert II software was used to control the machine and analyze the data

14 Box-Behnken Design Experimental Design for Response Surface Methodology Great for costly or timely experiments Great for not operating at unsafe operating limits

15 Experimental Design Response: Strength (N/mm 2 ) and MOE (Gpa) Factors: MFC/Soy (%) (Low: 0%, Mid: 1%, High: 2%) Press Temperature ( C) (Low: 125 C, Mid: 150 C, High: 175 C) Press Time (minutes) (Low: 7, Mid: 11, High: 15) Loading (g/m 2 ) (Low: 90, Mid: 110, High: 130) Optimal conditions for best Strength and MOE while using MFC/soy in PF?

16 Strength Contour plots with temperature and MFC/soy factors Temperature ( C) Lower Temperatures are better Strength (N/mm2) < > Hold Values Time (min) 11 Loading (g/m2) % 0.50% 1.00% MFC/Soy 1.50% 2.00%

17 Time (min) Strength Contour plots with time and MFC/soy factors Lower 12 press times are better Strength (N/mm2) < > Hold Values Temperature ( C) 150 Loading (g/m2) % 0.50% 1.00% MFC/Soy 1.50% 2.00%

18 Loading (g/m2) Strength Contour plots with loading and MFC/soy factors 130 Strength (N/mm2) < % MFC/Soy performs > 7.8 Hold Values 110 Temperature ( C) 150 Best at lower loadings Time (min) % 0.50% 1.00% MFC/Soy 1.50% 2.00%

19 Time (min) Strength Contour plots with temperature and time factors Lower 12 Temperatures 11 and Times are better 10 Strength (N/mm2) < > Hold Values MFC/Soy 0.01 Loading (g/m2) Temperature ( C) 170

20 Strength Contour plots with temperature and loading factors Loading (g/m2) Lower Temperatures 110 at lower loadings Strength (N/mm2) < > Hold Values MFC/Soy 0.01 Time (min) are better Temperature ( C) 170

21 Loading (g/m2) Strength Contour plots with loading and time factors Lower Times At lower loadings Strength (N/mm2) < > Hold Values MFC/Soy 0.01 Temperature ( C) are better Time (min)

22 Conclusions for Strength When using MFC/Soy/PF or PF Lower temperatures and press times are optimal 1% MFC/Soy maintained strength at lower loadings Less adhesive needed with MFC and soy in PF When using lower loadings Lower temperatures and press times are optimal Optimum settings are: Low Temperature, press time, and loading

23 MOE Contour plots with temperature and MFC/soy factors Temperature ( C) Lower Temperatures are better MOE (GPa) < > Hold Values Time (min) 11 Loading (g/m2) % 0.50% 1.00% MFC/Soy 1.50% 2.00%

24 Time (min) Long 12 press time for MOE Contour plots with time and MFC/soy factors more MFC/Soy MOE (GPa) < > Hold Values Temperature ( C) 150 Loading (g/m2) % 0.50% 1.00% MFC/Soy 1.50% 2.00%

25 Loading (g/m2) MOE Contour plots with loading and MFC/soy factors Lower loadings For more MFC/Soy MOE (GPa) < > Hold Values Temperature ( C) 150 Time (min) % 0.50% 1.00% MFC/Soy 1.50% 2.00%

26 Time (min) MOE Contour plots with temperature and time factors Lower 12 Temperatures 11 And times are better 10 MOE (GPa) < > Hold Values MFC/Soy 0.01 Loading (g/m2) Temperature ( C) 170

27 Loading (g/m2) MOE Contour plots with temperature and loading factors Lower Temperatures 110 are better MOE (GPa) < > Hold Values MFC/Soy 0.01 Time (min) Temperature ( C) 170

Loading (g/m2) 130 120 110 MOE Contour plots with loading and time factors Lower Times are better MOE (GPa) < 3.3 3.3 3.4 3.

28 Loading (g/m2) MOE Contour plots with loading and time factors Lower Times are better MOE (GPa) < > Hold Values MFC/Soy 0.01 Temperature ( C) Time (min)

29 Conclusions for Modulus of Elasticity When using MFC/Soy/PF or PF Lower temperatures are optimal When using MFC/PF Longer press times are optimal Lower loadings are optimal Optimum settings are: Low Temperature, press time Loading optimum 118 g/m 2

30 Thank you Dr. Brian K. Via Dr. W. Robert Ashurst Dr. Virginia Davis Dr. Marko Hakovirta Dr. Sujit Banerjee Dr. Qingzheng Cheng Tiffany Ulep

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