Progress 10/01/09 to 09/30/14
Outputs Target Audience: Key target audiences such as the sustainable biomaterials industry including pellet and lumber. Future industries such as cellulose and lignin based composites were also investigated. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided? An NSF IGERT undergraduate summer student worked on this project to optimize the addition of cellulose to the adhesive prior to wood bonding. How have the results been disseminated to communities of interest? The results have been disseminated to various companies whom attended a meeting in the 4Q 2014. These results will be disseminated at our Auburn University School of Forestry and Wildlife Advisory Board meeting in the spring 2015. What do you plan to do during the next reporting period to accomplish the goals?
Nothing Reported
Impacts What was accomplished under these goals?
Bio-oil based feedstocks were reacted with epoxy to form a more environmentally friendly epoxy polymer. Up to 50% substitution of petroleum based components were replaced by bio-oil. This bio-oil to epoxy ratio was optimized to improve structural performance of wood based composites. Cellulose was also added to the epoxy composite but agglomeration was a problem. But a new slack wax encapsulation technique was developed in which the cellulose could be dispersed without agglomeration, yet there was enough cellulosic surface area available for linkage to the epoxy functional groups.
Publications
- Type:
Journal Articles
Status:
Accepted
Year Published:
2015
Citation:
Liu, Y., G. Jianmin, H. Guo, Y. Pan, C. Zhou, Q. Zheng, B.K. Via. 2014. Interfacial properties of loblolly pine bonded with epoxy/wood pyrolysis bio-oil blended system. Bioresources (In Press).
- Type:
Journal Articles
Status:
Published
Year Published:
2014
Citation:
Celikbag, Y., B.K. Via, S. Adhikari, Y. Wu. 2014. Effect of liquefaction temperature on hydroxyl groups of bio-oil from loblolly pine (Pinus taeda). Bioresource Technology 169 (10):808-811.
- Type:
Journal Articles
Status:
Published
Year Published:
2014
Citation:
Pan, Y., S. Sun, Q. Cheng, *Y. Celikbag, B.K. Via, X. Wang, R. Sun. 2014. Melt dispersion technique for preparing paraffin wax microspheres for cellulose encapsulation. Wood and Fiber Science 46(4):1-6.
- Type:
Journal Articles
Status:
Published
Year Published:
2014
Citation:
Wei, N., B.K. Via, Y. Wang, T. McDonald, and M.L. Auad. 2014. Liquefaction and substitution of switchgrass ( Panicum virgatum) based bio-oil into epoxy resins. Industrial Crops and Products 57:116-123.
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Progress 01/01/13 to 09/30/13
Outputs Target Audience: The Sustainable Biomaterials Industry, which includes conventional forest products, was targeted for this project by working toward more environmentally friendly biobased epoxy-bio-oil adhesives and polymers. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided? This project opened up the opportunity for sufficient graduate student training in the area of wood and phenol formaldehyde-cellulose based composites. How have the results been disseminated to communities of interest? Journal publications and conference based outlets were both accomplished. However, personal contacts with small businesses and large biomaterials corporations were made to promote (on a face to face basis) the results of this research. What do you plan to do during the next reporting period to accomplish the goals? The homogeneous dispersion of cellulose in PF was possible but difficult and in 2012 it was found that addition of cellulose to particleboard was even more difficult due to cellulose agglomeration during forming. Ways to restrict this agglomeration will be pursued during the next reporting period. Partial wax encapsulation and distribution of cellulose in solvents will be attempted to find cost effective ways to transport and distribute cellulose into an array of potential biomaterials and composites.
Impacts What was accomplished under these goals?
A key objective of this projectwas to lower the density (make a lighter weight composite). Microcrystalline cellulose was found to successfully stiffen phenol formaldehyde adhesives whentested in shear. Nonlinear improvementin shear strength was made possible due to the contribution of the CH2 functional group (2925 cm-1) which through chemometric analysis was found to play arole in connecting cellulose with the PF matrix (Atta-Obeng et al. 2013). This finding was important because itqualified cellulose as more thanjust a filler but instead the cellulose exhibits sufficient functionality to interact with PF adhesives and provide additional shear strength. This could be important for wood based composites where shear forces are highest in the center resulting in concentrated load failures for products such as oriented strand board (OSB) which utilize PF adhesives (Via 2013). Another objective was to explore the conversion ofbiomass waste or low value biomaterial into bio-oil through pyrolysis or liquefaction procedures and then blend and modify epoxy polymers for acceptable crosslinkingresulting inimproved material and adhesive properties. Through the literature and in the laboratory it was found that the OH number of the bio-oil is important for crosslinking and needs to be appropriately balanced with the epoxy (proper stoichiometric ratio). However, characterization of the bio-oil found OH distributions to be complex, numerous, and highly sensitive to the liquefaction process utilized. This did allow for the ability to fine tune the liquefaction process to optimize epoxy polymer performance; however, more work is needed to lower the variation in the OH distribution such that a more repeatable manufacturing process is possible.
Publications
- Type:
Journal Articles
Status:
Published
Year Published:
2013
Citation:
Jiang, W., Via, B.K., Han, G., Wang, Q., Liu, S. 2013. Near Infrared monitoring of untreated and chemically delignified wood. Journal of Near Infrared Spectroscopy. 21: 485-493.
- Type:
Journal Articles
Status:
Published
Year Published:
2013
Citation:
Atta-Obeng, E., Via, B.K., Fasina, O., Auad, M., Jiang, W. 2013. Cellulose Reinforcement of Phenol Formaldehyde: Characterization and Chemometric Elucidation. International Journal of Composite Materials. 3(3): 39-47.
- Type:
Journal Articles
Status:
Published
Year Published:
2013
Citation:
Via, B.K. and *W. Jiang. 2013. Nonlinear multivariate modeling of strand mechanical properties with near infrared spectroscopy. The Forestry Chronicle 89(5):621-630
- Type:
Journal Articles
Status:
Published
Year Published:
2013
Citation:
Via, B.K. 2013. Characterization and evaluation of wood strand composite load capacity with near infrared spectroscopy. Materials and Structures 46(11):1801-1810.
- Type:
Conference Papers and Presentations
Status:
Published
Year Published:
2013
Citation:
Wei, N., Via, B.K., Auad, M.L., and Wang, Y. 2013. Synthesis and characterization of liquefied switchgrass-based epoxy resin. Abstracts of Papers of the American Chemical Society. Volume 245.
- Type:
Conference Papers and Presentations
Status:
Published
Year Published:
2013
Citation:
Via, B.K., Auad, M.L., Adhikari, S., Wang, S. 2013. Development of bio-based epoxy resin systems with bio-oil: polymers and wood composite binders. RESEARCH WEEK 2013, Auburn, Al.
- Type:
Conference Papers and Presentations
Status:
Published
Year Published:
2013
Citation:
Robinson, T.J. 2013. Physical properties of medium-density fiberboard utilizing an epoxy/wood pyrolysis oil resin system. Graduate Research Forum, Auburn University.
- Type:
Conference Papers and Presentations
Status:
Published
Year Published:
2013
Citation:
Jiang, W., Via, B.K., and Han, G. 2013. Near infrared monitoring of chemically delignified wood. SASEF Conference, Mobile, AL.
- Type:
Conference Papers and Presentations
Status:
Published
Year Published:
2013
Citation:
Celikbag, Y. and Via, B.K. 2013. Characterization of wood liquefaction oil for adhesive production. The International Conference on Wood Adhesives. Forest Products Society, Toronto, Ontario, Canada.
- Type:
Conference Papers and Presentations
Status:
Published
Year Published:
2013
Citation:
Via, B.K. 2013. Keynote Speaker: Chemometric modeling of biomass for chemistry and dependent properties prior to fiber manufacture. Taishan Academic Forum at Qingdao University, Qingdao, China.
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Progress 01/01/12 to 12/31/12
Outputs OUTPUTS: The sub objectives of the project for 2012 (in support of the broader 5 year project) was: 1) Use liquefaction (part of an integrated biorefinery process) to convert juvenile and mature wood to liquefied phenolics. 2) Substitute (20, 30, 40 percent) liquefied wood (juvenile and mature) into Phenol Formaldehyde and characterize the thermal and mechanical properties. The activities completed during this period included the completion of a significant portion of laboratory work around the liquefaction of juvenile pine and switchgrass into bio-oil through liquefaction at 200 to 300 degree C with Diethylene Glycol as a solvent. The bio-oil was then blended in with PF adhesive at up to 40 percent with 10 percent acetone as a solvent for viscosity reduction and wood composite particleboard using sweetgum hardwood particles were manufactured. It was found that lower temperatures yielded optimal values for adhesive product due to higher available OH groups for reaction. We also found that addition of cellulose to the PF adhesive could be used to counter strength losses that might occur during substitution of bio-oil for PF in wood composites. Liquefaction was also compared with pyrolysis oil and both were found to work similarly for wood composite manufacture. For events, the student attended a conference joint sponsored by the Center for Bioenergy and Bioproducts and National Science Foundation and won 3rd place in the competition. The products from this research (besides papers and posters as listed in the publication section) included new collaborations with faculty in the Department of Biosystems Engineering and the Department of Polymer and Fiber Engineering at Auburn University. PARTICIPANTS: Dr. Maria Auad - Collaborator Dr. Steve Taylor - Collaborator Dr. Oladiran Fasina - Collaborator Dr. Sushil Adhikari - Collaborator Dr. Emily Carter - Collaborator Dr. Yifen Wang - Collaborator Sam Linhart - Undergraduate Nan Wei - Graduate (MS) T.J. Robinson - Graduate (PhD) Emmanuel Atta-Obeng - Graduate (MS) TARGET AUDIENCES: Phenol formaldehyde and cellulose manufacturers were targeted with one study. Oriented strand board (OSB), bio-oil woody composite (co-product) manufacturers, and pyrolysis oil based manufacturers were also targeted. PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts Pine and switchgrass was liquefied using the same processing conditions and suggests that multiple feedstocks could be utilized with minimal changes in the manufacturing process. The upgrading of low value biomass into higher value bio-oil could thus be substituted into a wood-sweetgum particleboard composite process resulting in both higher value for low value pine and lower costs for the wood composite manufacturer. An MS student attended a conference joint sponsored by the Center for Bioenergy and Bioproducts and National Science Foundation and won 3rd place in the competition. Successful application of bio/pyrolysis oil into wood composites could help lower the cost of creating moisture resistant wood if bio-oil could be used as a replacement to more conventional/petroleum based materials. This parameter/impact/benefit will be validated in 2013.
Publications
- Atta-Obeng, E., Via, B.K., Fasina, O.O. 2012. Effect of microcrystalline cellulose, species, and particle size on mechanical and physical properties of particleboard. Wood and Fiber Science. 44(2):227-235
- Robinson, T.J., Via, B.K., Auad, M.L., and Adhikari, S. 2012. Optimization of pine derived pyrolysis oil to epoxy ratio in bio-based epoxy resins. Forest Products Society 66th International Convention, Washington, D.C.
- Robinson, T.J., Auad, M.L., Via, B.K., and Adhikari, S. 2012. Stoichiometric determination of chemical components in pyrolysis oil-epoxy resin systems. Lignocellulosic Biofuels Conference, Auburn, Alabama.
- Wei, Nan, *Celikbag, Y., Via, B.K., and Wang, Y. 2012. Synthesis and Characterization of Liquefied Switchgrass-Based Epoxy Resin. Lignocellulosic Biofuels Conference, Auburn, Alabama.
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Progress 01/01/11 to 12/31/11
Outputs OUTPUTS: Objectives: 2, 3, and 4 were achieved in 2011. These three objectives were to 2) Substitute lignin and/or hemicelluloses waste streams into petroleum based resins and/or bio-oil and determine their cure and thermal degradation characteristics through near infrared spectroscopy (NIR), mid infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and/or thermal gravimetric analysis (TGA); 3) Optimize resin placement, pressure, temperature, and press time of the wood composite based on design of experiment (DOE) methods, multivariate modeling from NIR and FTIR spectroscopy, and/or response surface methodologies. 4) Lower the density of the composite based on the three optimization methods such that mechanical and physical properties are at least equal their original performance. Objective 2 was partially achieved by substituting phenolic rich bio-oil for petroleum based phenols and the epoxy resins were manufactured. NIR, FTIR, DSC, TGA, and dynamic mechanical analysis (DMA) was run to characterize the mechanical, cure, and thermal properties of the polymer. A paper/manuscript is currently near completion (90%) and will be submitted to the Journal of Applied Polymer Science in early 2012. Objective 3 was achieved by testing different levels of Phenol Formaldehyde reinforced with microcrystalline cellulose into the wood particleboard composite. It was found that higher levels of cellulose resulted in higher required adhesive (PF) loadings due to the increased surface area of the cellulose. Objective 4 was achieved by substituting microcrystalline cellulose and larger wood particle lengths within the particleboard composite to maintain strength while achieving lower densities. Substitution of cellulose into the particleboard composite was not successful due to springback issues of the panel after pressing; however, inclusion of larger particles was successful at increasing the strength, resulting in significant reductions in particleboard density. Finally, while not exactly meeting objective 1 (which required a low cost hardwood from an ethanol stream), we were able to partially satisfy objective 1 by including sweetgum as a substitute for pine in the particleboard based bio-composite. It was found that sweetgum yielded equivalent performance in mechanical and physical properties resulting in an alternative resource for making lightweight particleboard panels. Information has been disseminated at Forest Products Society International Convention. PARTICIPANTS: Dr. Maria Auad, Dr. Fasina, Dr. Taylor, graduate students (Neil Kohan, Emmanuel Atta-Obeng, and TJ Robinson) assisted or provided input to the PI on this project during 2011. The epoxy development portion in 2011 was leveraged from initial funding for the U.S. Forest Service in which bio-oil was manufactured from small diameter trees; however, the funding in 2011 was from Hatch funds. TARGET AUDIENCES: Not relevant to this project. PROJECT MODIFICATIONS: Initally the project called for (Objective 1) the development of a method for utilzing low cost hardwood from an ethanol waste stream. The project was modified to still use a low cost harddwood (sweetgum) but from a pyrolysis process and not an ethanol waste stream.
Impacts Successful engineering of the particleboard panel with longer particles was more effective and cheaper than the addition of cellulose for particleboard manufacture. Furthermore, it was found that southern pine could be replaced by a low cost hardwood (sweetgum) which is important as we strive to find new resources to support existing products and bioenergy manufacturing demands. This work was presented at the 21st Annual Graduate Scholars Forum and was submitted and accepted by the Journal of Wood and Fiber Science (see publication record below). Additionally, southern pine wood strands were tested for mechanical properties based on manufacturing conditions such that higher quality strands could be placed on the surface to improve composite quality and lower the density.
Publications
- Kohan, N.* and Via, B.K.*. 2011. Nondestructive evaluation of wood strand mechanical properties using near-infrared spectroscopy. 21st Annual Graduate Scholars Forum, Auburn, Alabama.
- Atta-Obeng, E.* Via, B.K.*, Auad L. M., and Fasina O. 2011. Characterization of phenol formaldehyde resin and resin-MCC composites. 21st Annual Graduate Scholars Forum, Auburn, Alabama.
- Atta-Obeng, E.*, Via, B.K., Fasina, O.O. 2011. Effect of microcrystalline cellulose, species, and particle size on mechanical and physical properties of particleboard. Wood and Fiber Science (Published Online).
- Kohan, N.*, B.K. Via, and S. Taylor. 2011. A comparison of geometry effect on tensile testing of wood strands. Forest Products Journal (In Press).
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Progress 01/01/10 to 12/31/10
Outputs OUTPUTS: Objectives number 2, 3, and 4 were approached in 2010. These three objectives were to a) To substitute lignin and/or hemicelluloses waste streams into petroleum based resins and/or bio-oil and determine their cure and thermal degradation characteristics through near infrared spectroscopy (NIR), mid infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and/or thermal gravimetric analysis (TGA); b) To optimize resin placement, pressure, temperature, and time of pressing of the wood composite based on design of experiment (DOE) methods, multivariate modeling from NIR and FTIR spectroscopy, and/or response surface methodologies. c) To lower the density of the composite based on the three optimization methods such that mechanical and physical properties at least equal their original performance. Objective 1 was partially met by obtaining a grant from the U.S. Forest Service (2009-2010) in which we converted underutilized/small diameter southern pine into pyrolysis/bio-oil. We then impregnated that pyrolysis oil into solid wood to make a moisture resistant product. We found that only a 10% loading is necessary to make wood resistant to high humidity environments. However, higher loadings may be necessary for liquid water exposure. Leaching of the pyrolysis oil out of the wood was found to be a major hurdle. So in 2011, we plan to try to find a way to polymerize bio-oil so that it will not leach from the product. Objective 2 and 3 was partially carried out by obtaining internal funds from the AAES Hatch/Multistate Grant Award. This proposal was to a) use near infrared spectroscopy to stress rate wood and b) utilize stress rated flakes in wood composites to lower the density while maintaining mechanical properties. We found that modulus of elasticity (stiffness) could be better measured /predicted with NIR than modulus of rupture (strength) for thin flakes that are prone to internal fracture. We tested industrial and laboratory made flakes. Objective 2 and 3 was additionally carried out by investigating the addition of cellulose into phenol formaldehyde resin. The resin cure temperature was optimized through DSC characterization and the degradation temperature of PF-cellulosic resins was determined through TGA. FTIR was utilized to identify the compatibility of PF to cellulose. It was found that the shear strength of the PF-cellulose composite increased non-linearly from 0 to 10%. The optimal loading was found to occur at 6% loading. Information has been disseminated at Forest Products Society 64th International Convention, Society of Wood Science and Technology International Convention, and the Alabama Composites Conference. PARTICIPANTS: Dr. Brian Via - PI Dr. Steve Taylor - Collaborator Dr. Tim McDonald- Collaborator Dr. John Fulton - Collaborator Dr. Oladiran Fasina - Collaborator Dr. Sushil Adhikari Dr. Bob Rummer - Collaborator Dr. Emily Carter - Collaborator Training (student): Amber Clark - Undergraduate Neil Kohan - Graduate (MS) T.J. Robinson - Graduate (PhD) Emmanuel Atta-Obeng - Graduate (MS) Cole Chappel - Graduate (MS) Partner Organizations: Auburn University - Center for Bioenergy and Bioproducts Auburn University - Department of Biosystems Engineering U.S. Forest Service - Southeastern Unit TARGET AUDIENCES: Phenol formaldehyde and cellulose manufacturers were targeted with one study. Oriented strand board (OSB), bio-oil woody composite (co-product) manufacturers, and pyrolysis oil based manufacturers were also targeted. PROJECT MODIFICATIONS: None
Impacts Successful characterization of the wood flakes prior to composite manufacture may help a manufacturer to better adjust resin volumes resulting in lower density and light weight OSB. The master student (Neil Kohan) who performed this study presented an International poster (below in publications) in Geneva and won first place in the student competition. Successful application of bio/pyrolysis oil into wood composites could help lower the cost of creating moisture resistant wood if bio-oil could be used as a replacement to more conventional/petroleum based materials.
Publications
- Via, B.K. 2010. Prediction of oriented strand board wood strand density by near infrared and Fourier transform infrared reflectance spectroscopy. Journal of Near Infrared Spectroscopy. 18(6): 491- 498.
- Kohan, N. and B.K. Via. 2010. Nondestructive evaluation of wood strand mechanical properties using near-infrared spectroscopy. Society of Wood Science and Technology (SWST) International Convention, Geneva, Switzerland.
- Via, B.K.. 2010. A comparison in using FTIR to NIR spectra when predicting strand density prior to composite manufacture. Forest Products Society 64th International Convention, Madison, Wisconsin.
- Via, B.K. and T.J. Robinson. 2010. Multivariate modeling of composite strand density from FTIR spectra. Forest Products Society 64th International Convention, Madison, Wisconsin.
- Kohan, N., B.K. Via, H. Carino, and S. Taylor. 2010. NIR as a tool to predict mechanical properties of OSB flakes. Forest Products Society 64th International Convention, Madison, Wisconsin.
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