Progress 10/01/08 to 09/30/13
Outputs
Target Audience: Farmers, ranchers, producers, processors, and other stakeholders interested in biomass, bioenergy, biofuels, and bioproducts. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided? 16 NDSU agriculture students learned about national and international implementation of bioenergy conversion processes. 6 graduate students were trained and involved in the research methods, data collection, writing, and prepared presentations. How have the results been disseminated to communities of interest? Results were presented at scientific conferences, seminars, trade shows, and in publications. What do you plan to do during the next reporting period to accomplish the goals?
Nothing Reported
Impacts
What was accomplished under these goals?
1. The "NDSU Biomass Testing Laboratory (BTL) at NGPRL" (Northern Great Plains Research Laboratory, USDA-ARS, Mandan, ND) was fully operational by June 2012. BTL specializes in physical, thermal, mechanical, and storage properties of biomass. The concept of standardization of biomass feedstocks by mixing different biomass for a desired gross calorific value (GCV) was researched. Three biomass feedstocks, switchgrass, wheat straw, and field pea stalk, were tested. Equations were derived for the designed proportions of biomass for a desired GCV of the biomass mixture. Results supported the concept of biomass feedstock standardization through simple mixing, as mixtures of actual and desired gross calorific values were statistically similar. Previously reported ΣVolume approach particle size and particle size distribution (PSD) analysis software was further improved for performance and utility. The performance improved from previously reported 2000/s to greater than 17,000/s. It would be helpful to determine the size reduction energy through the PSD parameters from a small sample. A correlation study collected the size reduction energy, determined using a power-meter that determines the size reduction energy through the electrical power drawn by the device, and PSD data from the machine vision (ΣVolume approach). Results indicate that screen size, and cumulative undersize particle lengths (e.g. D50, D60, D30) produced significant correlations (r > 0.85). New long-term storage techniques are necessary to preserve fermentable sugars from sugar beet (Beta vulgaris L.) varieties which may qualify as advanced biofuel feedstocks in the United States. The focus of this study was to evaluate the combined effect of pH and refractometric dissolved solids (RDS) content on fermentable sugar preservation in raw thick beet juice stored for 24 wk at 23±1°C. Combinations of pH≤3.5 or pH≥9.5 with RDS≥64.5 % were effective in preserving up to 99 % of fermentable sugars in stored raw thick juice. Following storage, yeast fermentation of acidic treatments achieved efficiencies of up to 82 % relative to raw juice, whereas yeast fermentation was hindered in alkaline treatments resulting in efficiencies of up to 54 %. Research activities were initiated on the front-end processing of energy beets for biofuel production. In the front-end processing, an industrial capacity hammer mill (20 hp) capable of processing wet material and a manual-hydraulic basket press were installed and tested. The weight of juice from the first press is approximately equal to 25% weight of pulverized beet. Sugar content on first press was 32% Brix and reduced to 12% and 4% Brix after water addition and subsequent presses. Process interactions between biomass densification and pretreatment and hydrolysis were tested using pelleted switchgrass and soaking in aqueous ammonia pretreatment followed by enzymatic hydrolysis. Pelleted switchgrass required lower pretreatment severity and lower enzyme loadings than non-pelleted switchgrass. Our previous work on the simulation of infield bale aggregation based on Euclidean distances resulted in the development of the infield bale aggregation logistics software (IBALS). In this study, the cost economics analysis will be performed on the various aggregation logistics scenarios already considered in IBALS. This work added an economics "layer" to the IBALS. Standard agricultural machine operation economics principles and cost and operation data were used in the economic analysis. The risk analysis software @RISK was used in the analysis. Economic analysis results ranked Direct3Min (tractor handling 3 bales, following a minimum path of collecting the "nearest" bale in sequence) and Direct3 (tractor with attachment following the baler path) as the top ranking strategies. 2. Alternative soaking in aqueous ammonia pretreatment conditions were tested using pelleted switchgrass as a feedstock. Cellulase enzymes are being attached to polymer brushes grafted to silica or ferromagnetic core particles. Impact of immobilization and polymer brush enzyme density on cellulose and cellobiose hydrolysis is being explored. The combined hydrolysis and fermentation of whole, macerated sugarbeets was tested using E. coli KO11 and Saccharomyces cerevisiae. Ethanol yields, residual sugar concentrations, and effluent solids were modeled based on pectinase and cellulase loadings. Aqueous surfactant-assisted extraction (ASE) has been proposed as an alternative to n-hexane for extraction of vegetable oil; however, the use of inexpensive surfactants such as sodium dodecyl sulfate (SDS) and the effect of ASE on the quality of biodiesel from the oil are not well understood. The highest total oil extraction efficiency was 80 %, and was achieved using 0.02 M SDS at 20°C, solid–liquid ratio 1:10 (g:mL), 1,000 rpm stirring speed and 45 min contact time. The extracted oil from the scale-up of the ASE method passed the recommendation for biodiesel feedstock quality with respect to water content, acid value and phosphorous content. Water content, kinematic viscosity, acid value and oxidative stability index of ASE biodiesel were within the ASTM D6751 biodiesel standards. 3. Epoxidized vegetable oil (EVO) may be blended with petroleum-based epoxies for use in composite material applications; however, the use of high levels of EVO (30-40% of total matrix) results in a reduction of flexural strength and glass transition temperature. One solution is to replace the glycerol core with a sucrose core, thereby increasing the number of epoxy groups per molecule by up to 160%, resulting in significant improvements in mechanical performance in the cured resin. The main challenge faced by our group in the past year has been the scaled up production of epoxidized sucrose soyate (ESS). The yield and quality of the resin were comparable to resin produced at 300 g scale. 4. Students in several agricultural and engineering fields at NDSU enrolled in a European study abroad course to learn about European bioenergy crop production and conversion technologies including anaerobic digestion, biomass gasification, Fischer-Tropsch synthesis, and vegetable oil transesterification. Lecture materials used were modified from BEEMS materials developed with several S1041 participants.
Publications
- Type:
Conference Papers and Presentations
Status:
Accepted
Year Published:
2013
Citation:
Nahar, N., and S.W. Pryor 2013. Effects of Pretreatment Conditions for Enzymatic Hydrolysis of Pelleted Switchgrass, Paper No. 1619709. ASABE International Meeting. Kansas City, MO Jul 22-24, 2013.
- Type:
Conference Papers and Presentations
Status:
Accepted
Year Published:
2013
Citation:
Pryor, S.W., O. Kudina, A. Samaratunga, N. Nahar, S. Minko, and A. Voronov 2013. Kinetics and recovery of cellulases immobilized on pH-responsive polymer brushes grafted to nanosilica and ferromagnetic particles, Paper No. 23962. 35th Symposium on Biotechnology for Fuels and Chemicals. Portland, OR Apr 29-May 2, 2013.
- Type:
Conference Papers and Presentations
Status:
Accepted
Year Published:
2013
Citation:
Samaratunga, A., N.Nahar, O. Kudina, A. Voronov, S. Minko, and S. W. Pryor 2013. Impact of enzyme loading on activity and recovery of cellulases immobilized on polymer brushes, Paper No. 1620390. ASABE International Meeting. Kansas City, MO Jul 22-24, 2013.
- Type:
Conference Papers and Presentations
Status:
Accepted
Year Published:
2013
Citation:
Vargas-Ramirez, J.M., D.M. Haagenson and D.P. Wiesenborn. 2013. Evaluation of the effect of combined storage techniques on the preservation of industrial sugars from sugar beets for bioproducts, paper 1620707. ASABE Annual International Meeting, Kansas City, MO, July 21-24.
- Type:
Journal Articles
Status:
Accepted
Year Published:
2013
Citation:
Tuntiwiwattanapun, N., C. Tongcumpou, D. Haagenson, and D. Wiesenborn. 2013. Development and scale-up of aqueous surfactant-assisted extraction of canola oil for use as biodiesel feedstock, Journal of the American Oil Chemists Society,
90(7):10891099.
- Type:
Conference Papers and Presentations
Status:
Accepted
Year Published:
2013
Citation:
Igathinathane, C., H. Zerom, G. Bora, K. Nichols, M. Sanderson, J. Hendrickson, and W. Hoogmoed. 2013. Fruits and
Vegetables Volume Estimation by Machine Vision. Paper No: 131598833. 2013 ASABE Annual International Meeting, July
21 July 24, 2013, Kansas City, Missouri, US.
- Type:
Conference Papers and Presentations
Status:
Accepted
Year Published:
2013
Citation:
Monono, E., J. Perleberg, D. Haagenson, and D. Wiesenborn. 2013. Determining the temperature profile and heat transfer coefficient in an epoxidation process. ASABE Annual International Meeting, Kansas City, MO, July 21-24.
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Progress 10/01/11 to 09/30/12
Outputs
OUTPUTS: Objective 1. Task: Quantify and characterize biological feedstocks. The "NDSU Biomass Testing Laboratory (BTL) at NGPRL," Mandan, ND was established and fully operational from June 2012. BTL specializes in physical, thermal, mechanical, and storage properties of biomass in order to evaluate their quality and develop a database for utilization of wider audience. (a) Thermal characteristics (TGA/DSC) of various biomass, such as big bluestem, bromegrass, corn stalk, switchgrass, wheat straw, alfalfa stem, bromegrass, and miscanthus were analyzed. Calorific values of these biomass varied from 16284 to 17095 J/g. (b) Tensile, shear and cutting (modified Warner-Bratzler) UTM attachments were designed and fabricated. These attachments were used to measure the mechanical strength of the above selected biomass. (c) Moisture hydration characteristics of switchgrass, bromegrass, and big bluestem biomass were determined at 20, 40, and 60 deg C at a fixed 95% RH and modeled using various hydration kinetics models. Peleg model in combination with the Arrhenius equation is recommended for moisture sorption prediction. Task: Develop and evaluate harvest, process and handling methods. * An improved Sigma-Volume machine vision particle size distribution (PSD) approach was developed and used to evaluate PSD of particulate materials. * Machine vision ImageJ plugin for determining the volume of fruits and vegetables that can be directly applied to biomass feedstocks was developed. * Research activities were initiated on the front end processing of the "Energy Beet Research - Phase II" project. Task: Model and analyze integrated feedstock supply and process systems. * Infield aggregation of bales is influenced by several field variables and their effects were evaluated statistically. Several infield aggregation strategies were ranked using the developed simulation program. Objective 2: Task: Develop an understanding of fuel quality and performance issues. * The effect of reaction scale up on properties of epoxidized canola oil was determined. Reaction scaled-up beyond 300 g, in turn, requires increased understanding of exothermic reaction phenomena. * Near infrared spectroscopy (NIRS) is widely used for quantitative analysis of oilseeds in a non-destructive manner. NIR spectra from 100 canola samples (3 g portions) were collected and calibration models accurately analyzing canola constituents were developed. * Optimization of vegetable oil detachment efficiency by reducing interfacial tension was determined. Objective 3. Task: Discover and characterize biochemicals, biocatalysts, and biomaterials in biomass. * High-yielding sugar beets are becoming an attractive feedstock for the production of ethanol in the Red River Valley region of the US. Anaerobic storage of sugar beets was evaluated as an alternative to conventional pile storage. Improving the storage life of raw beet juice for ethanol production studies are in progress. * Near infrared analysis of sugar beet raw thick juice for ethanol production was performed. A PLS calibration model with mean centered preprocessing and multiplicative signal correction provided the best models for thick juice evaluation. PARTICIPANTS: Nothing significant to report during this reporting period. TARGET AUDIENCES: Nothing significant to report during this reporting period. PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts
* Results on the physical, mechanical, and thermal properties of several species from the "NDSU Biomass Testing Laboratory at NGPRL" will help the farmers and ranchers of ND to assess the value of their biomass. A database of this nature benefits the producers, industry personnel, and researchers of the state as well as the nation. * The economical machine vision method of PSD determination of particulate biomass generated a lot of interest among personnel involved with biomass handing. * A new ASABE standard creation (ASABE Committee FPE-709 and PM-23/7/2) on application of machine vision applied to forage and biomass is being lead by NDSU. * The infield biomass bales transport study results serve as an excellent extension tool to inform producers/farmers of the state and the nation of the best method of colleting the bales and thus realizing time, energy, and cost saving. * The cold soak filtration, fatty acid composition, cloud point, and oil stability index test results help evaluate canola biodiesel quality traits of canola breeding program. * The application of bio-based epoxy resins in the production of composites materials helps decrease the dependence on petroleum-based resins, and may lead to a high added-value product from vegetable oils. * Developed combined calibration model, using NIR spectra from 100 canola samples, was able to accurately analyze canola constituents. Such calibration models are often preferred in plant breeding programs. * Research efforts initiated on the energy beet processing will lead to the better understanding of the front end processing and the storage of whole and extracted juice as well as biofuel fermentation.
Publications
- * Vargas-Ramirez, J.M., Haagenson, D.M., Rahman, S., and Wiesenborn, D.P. 2012. Change in fermentable sugars in sugar beets stored anaerobically. ASABE Paper No. RRV12100, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
- * Rijal, B., Igathinathane, C., Karki, B., Yu, M., and Pryor, S.W. 2012. Combined effect of pelleting and pretreatment on enzymatic hydrolysis of switchgrass. Bioresource Technology, 116: 36-41.
- * Igathinathane, C., Ulusoy, U., and Pordesimo, L.O. 2012. Comparison of particle size distribution of celestite minerals by machine vision Sigma-Volume approach and mechanical sieving. Powder Technology, 215-216: 137-146.
- * Dhillon, B., Wiesenborn, D.P., Sidhu, H., and Wolf-Hall, C. 2012. Improved microbial quality of buckwheat using antimicrobial solutions in a fluidized bed. Journal of Food Science, 77(4):E98-E103.
- * Wooten, J.R., Filip To, S.D., Igathinathane, C., and Pordesimo, L.O. 2011. Discrimination of bark from wood chips though optical texture analysis. Computers and Electronics in Agriculture, 79(1): 13-19.
- * Naimi, L.J., Sokhansanj, S., Womac, A.R., Bi, X.T., Lim, C.J., Igathinathane, C., Lau, A.K., Sowlati, T., Melin, S., Emami, M., and Afzal. M. 2011. Development of a population balance model to simulate fractionation of ground switchgrass. Transactions of the ASABE, 54(1): 219-227.
- * Igathinathane, C., Gustafson, C., Archer, D., Hendrickson, J., and Kronberg, S. 2012. Effects of field variables on infield biomass bales aggregation strategies. ASABE Paper No. 121337357, ASABE Annual International Meeting, July 29-August 1, 2012, Dallas, Texas, US.
- * Yu, M., Igathinathane, C., Gustafson, C., Hendrickson, J., and Sanderson, M. 2012. Mechanical shear and tensile characteristics of selected biomass stems. ASABE Paper No. 121337358, ASABE Annual International Meeting, July 29-August 1, 2012, Dallas, Texas, US.
- * Rijal, B., Karki, B., Yu, M., Igathinathane, C., and Pryor, S.W. 2012. Interaction of densification and pretreatment for the enzymatic hydrolysis and fermentation of biomass. ASABE Annual International Meeting, July 29-August 1, 2012, Dallas, Texas, US.
- * Igathinathane, C., and Backer, L.F. 2012. Simplified no-code machine vision method of accurate dimension measurement of granular materials. ASABE Paper No. RRV12124, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
- * Igathinathane, C., and Ulusoy, U. 2012. Particle size distribution analysis of ground coal by machine vision Sigma-Volume approach. Paper Number 924. XXVI International Mineral Processing Congress (IMPC) 2012 Proceedings-Peer-reviewed, September 24-28, New Delhi, India.
- * Igathinathane, C., and Ulusoy, U. 2012. Particle size distribution of particulate materials by Sigma-Number, Sigma-Length, Sigma-Area, and Sigma-Volume machine vision methods. ASABE Paper No. RRV12123, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
- * Yu, M., Igathinathane, C., Gustafson, C., Hendrickson, J., and Sanderson, M. 2012. Hydration characteristics of switchgrass, big bluestem, and bromegrass. ASABE Paper No. RRV12121, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
- * Rijal, B., Igathinathane, C., Karki, B., Yu, M., and Pryor, S.W. 2012. Interaction effect of pelleting and pretreatment on the sugar yields of switchgrass. ASABE Paper No. RRV12102, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
- * Sidhu, H.K., Haagenson, D.M., and Wiesenborn, D.P. 2012. Validation of NIRS Calibration models for single plant canola (Brassica Napus) Seeds. ASABE Paper No. RRV12125, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
- * Tuntiwiwattanapun, N., Wiesenborn, D.P., and Tongcumpou, C. 2012. Optimization of vegetable oil detachment efficiency by reducing interfacial tension. ASABE Paper No. RRV12113, ASABE/CSBE North Central Intersectional Conference, March 30-31, 2012, Fargo, North Dakota, US.
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Progress 10/01/10 to 09/30/11
Outputs
OUTPUTS: Comparison of curing agents for epoxidized vegetable oils (EVO) applied to composites. Interest in polymers from renewable sources, as alternatives to petroleum-based polymers, remains strong; however, their performance must be acceptable. To improve performance of EVO in composite matrices, 5 amine curing agents were compared with an anhydride used previously. Agents were tested in matrices containing petro-based epoxy plus 0% or 30% epoxidized oil from canola (ECO) and soybean (ESO). The two amines with the highest glass transition temperature, determined by DSC, were characterized by dynamic mechanical analysis; bis (p-aminocyclohexyl) methane (PACM) showed the highest performance. Amine: epoxy ratios 0.6 to 1.6 were then evaluated; ratios of 0.8 and 1.0 showed superior performance. E-glass fiber reinforced composites with PACM/EVO showed thermal and mechanical performance slightly lower than the composites with 0% EVO and comparable with those of the anhydride curing agent. Therefore, PACM is recommended for E-glass composites containing ECO and ESO. Effect of trace contaminants on cold soak filterability (CSF) of canola biodiesel. A CSF test (ASTM D 7501-09b) was included in B100 specifications, bringing new challenges to biodiesel producers and researchers. For a canola breeding program concerned with biodiesel use, rapid assessment of biodiesel quality is important. Typically, a limited amount of seed from new canola lines is available; therefore, obtaining the 300 mL of biodiesel for evaluating CSF is not possible. Thus a scaled down CSF test is needed. The primary objective of this study was to evaluate the impact of saturated monoglycerides, glycerin, and soap on CSF. Biodiesel filtration time rapidly escalated when the SMG concentration was above 0.28%. The influence of saturated monoglycerides (0.04% to 0.46% w/w) on biodiesel precipitate formation was also evaluated. A regression model predicted biodiesel CSF based on levels of trace contaminants, and will be instrumental to scaling down the CSF test. Impact of growing location on canola biodiesel quality. Canola biodiesel has superior cold flow properties due but quality may be significantly related to location, year and seed variety. Thus we determined the effect of ND location and production year on canola biodiesel fatty acid composition, cloud point (CP) and oil stability index (OSI). First, bulked varieties from 7 seasons were analyzed, and then two locations were analyzed for a single variety. Biodiesel was produced directly from seed via in situ alkaline transesterification. CP ranged from -0.1 to -2.4 deg C and was significantly impacted by year and location. The ASTM B100 specification for OSI (3 h) was met, but increased seed storage decreased stability. No significant differences were detected in FAME composition, and iodine value ranged from 108 to 123 g I2/100 g. Variation in fatty acid composition was small; thus, the significant variability in CP and OSI suggests these resulted from either differences in minor constituents or environmental seed stress. This supports examining biodiesel quality in a canola breeding program. PARTICIPANTS: NDSU Personnel and students: Judith Espinoza-Perez, Postdoctoral Scientist, Agricultural & Biosystems Engineering; Zhigang Chen, Assistant Professor, Center for Nanoscale Science and Engineering; Cole Gustafson, Professor, Agribusiness & Applied Economics; Darrin Haagenson, Research Specialist, Agricultural & Biosystems Engineering; Chad Ulven, Assistant Professor, Mechanical Engineering; Bhavnita Dhillon, Postdoctoral Scientist, Agricultural & Biosystems Engineering; Hongjian Lin, Graduate Research Assistant, Agricultural & Biosystems Engineering; Mukhlesur Rahman, Canola Breeder, Plant Sciences. Partner organizations and businesses: North Dakota Agricultural Experiment Station, Northern Canola Growers Association, North Dakota Soybean Council, Tecton Products LLC (Fargo, ND). TARGET AUDIENCES: Not relevant to this project. PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts
The application of bio-based epoxy resins in the production of composites materials helps decrease the dependence on petroleum-based resins, and may lead to a high added-value product from vegetable oils. However, future studies are needed to increase the thermal and mechanical performance of the bio-based resin relative to synthetic resins, which will in turn improve the performance of the composites. Results were shared at the Association for the Advancement of Industrial Crops annual meeting and the Northern Canola Growers Association annual meeting in 2011. The experience and knowledge base gained through this project has been instrumental in developing a broader partnership involving academia and industry. Canola has already come into widespread use as a biodiesel feedstock; however, improved productivity of commercial seed varieties and improved winter performance of the biodiesel are essential for the continued viability of this industry. The in situ technique for transesterification was shown to be a useful technique for characterizing and differentiating biodiesel produced from canola seed from different sources. Improved understanding of cold temperature filterability of biodiesel will improve the reliability of this young biofuel.
Publications
- Espinoza-Perez, J.D., B. A. Nerenz, D.M. Haagenson, Z. Chen, C.A. Ulven, and D.P. Wiesenborn. 2011. Comparison of curing agents for epoxidized vegetable oils applied to composites, Polymer Chemistry, 32(11):1806-1811.
- Lin, H., D.M. Haagenson, D.P. Wiesenborn, S.W. Pryor. 2011. Effect of trace contaminants on cold soak filterability of canola biodiesel. Fuel, 90(2011):1771-1777.
- Haagenson, DM, and D.P. Wiesenborn. 2011. Impact of North Dakota growing location on canola biodiesel quality. Journal of the American Oil Chemists Society, 88:1439-1445.
- Espinoza-Perez, J.D., B. A. Nerenz, D.M. Haagenson, Z. Chen, C.A. Ulven, and D.P. Wiesenborn. 2011. Renewable oils for use in composite materials. Published abstract. Oilseeds session III, The Association for the Advancement of Industrial Crops Annual Meeting, Sept 11-14, Fargo, ND.
- Haagenson, DM, and D.P. Wiesenborn. 2011. Screening oilseed feedstocks for improved biodiesel quality. Published abstract. Oilseeds session III, The Association for the Advancement of Industrial Crops Annual Meeting, Sept 11-14, Fargo, ND.
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Progress 10/01/09 to 09/30/10
Outputs
OUTPUTS: Epoxidized High-Oleic Vegetable Oils Applied to Composites. Vegetable oils are a renewable source for the production of oleochemicals. Oils with high-oleic and low saturate content may be an excellent source for producing epoxy resins, because of the uniform distribution of cross-linking sites. Bio-based epoxy resins can be used as matrix components for composite materials. Vegetable oils with oleic acid content varying from 22 to 86% were epoxidized in situ with peracetic acid and a heterogeneous catalyst. Contents of 30, 35, and 40% (% wt of total matrix) of bio-based epoxy resins were blended with a synthetic epoxy resin, and an anhydride curing agent to be applied as the matrix in the preparation of composites using E-glass as the structural fiber. A control was also prepared with a 100% synthetic epoxy resin. Mechanical properties (flexural properties, interlaminar shear strength, and dynamic mechanical analysis) of the produced composite materials were evaluated. More flexible but less resistant composites were obtained as the content of oleic acid in the initial vegetable oil and the content of bio-based resin increased. Toughness increased at lower levels of oleic acid content. Interlaminar shear strength showed low adhesion of the matrix-fiber at a bio-based epoxy resin content of 40%. High homogeneity and slightly reduced glass transition temperatures were shown in composites with high-oleic bio-based resins when compared with the control. Implementing an in situ alkaline transesterification method for canola biodiesel quality screening. Increasing demand for canola (Brassica napus) as an edible oil crop and biodiesel (B100) feedstock has encouraged genetic development for increased oil yields and expanded acreage in the US Northern Plains. Crop production environment and plant genetics influence metabolism and fatty acid composition, but the influence of this interaction on the resulting fatty acid methyl esters (FAME) is not clearly understood. The objective of this study was to develop a canola in situ transesterification (TE) method for facilitating the identification of genetic, abiotic or biotic factors impacting B100 quality, and to evaluate FAME quality properties from conventional TE (degummed oil) and in situ TE methods. In situ reactions containing 40 g canola flour conducted for 6 h at 60 deg C with a 275:1:1.05 molar ratio of methanol:TAG:KOH provided 80% conversion of seed lipid to FAME. Replicated reactions provided sufficient FAME volume for measuring several ASTM D6751-09 standards including cloud point, kinematic viscosity, acid value, moisture content, oxidative stability, and total glycerin, but adjustments are necessary to provide sufficient volumes for routine analysis of cold soak filtration test. PARTICIPANTS: NDSU Personnel and students: Judith Espinoza-Perez, Postdoctoral Scientist, Agricultural & Biosystems Engineering; Zhigang Chen, Assistant Professor, Center for Nanoscale Science and Engineering; Cole Gustafson, Professor, Agribusiness & Applied Economics; Darrin Haagenson, Research Specialist, Agricultural & Biosystems Engineering; Chad Ulven, Assistant Professor, Mechanical Engineering; Katherine McKinnon, Undergraduate Research Assistant, Agricultural & Biosystems Engineering; Bhavnita Dhillon, Postdoctoral Scientist, Agricultural & Biosystems Engineering; Hongjian Lin, Graduate Research Assistant, Agricultural & Biosystems Engineering; Rachel Brudvik, Research Specialist, Agricultural & Biosystems Engineering; Mukhlesur Rahman, Canola Breeder, Plant Sciences; Phil McClean, Professor, Plant Sciences; Bill Wilson, Professor, Agribusiness & Applied Economics. Partner organizations and businesses: North Dakota Agricultural Experiment Station, Northern Canola Growers Association, North Dakota Soybean Council, Tecton Products LLC (Fargo, ND). TARGET AUDIENCES: Nothing significant to report during this reporting period. PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
The application of bio-based epoxy resins in the production of composites materials helps decrease the dependence on petroleum-based resins, and may lead to a high added-value product from vegetable oils. However, future studies are needed to increase the adhesion of matrices containing bio-based resin with synthetic and natural fibers, which will improve the mechanical performance of the composites. Results were shared at the US Canola Association Research Conference and the Northern Canola Growers Association annual meeting in 2010. The experience and knowledge base gained through this project has been instrumental in developing a broader partnership including an additional discipline and commodity group, and an industry partner to pursue a commercial application of a biopolymer. The in situ transesterification (TE) protocol established over this research period would permit weekly analysis of 40 canola samples. Thus, the in situ TE method provides an opportunity to evaluate the impact of genetic or environmental factors on B100 quality, and such an application was under investigation in 2010 and will be reported on in 2011. The in situ TE method will be instrumental in assisting the development of new canola varieties.
Publications
- Espinoza-Perez, J.D., C.A. Ulven, and D.P. Wiesenborn. 2010. Epoxidized high-oleic vegetable oils applied to composites, Transactions of the ASABE, 53(4):1167-1174.
- Espinoza-Perez, J. 2010. Production, Characterization and Raw Material Cost Analysis of a Canola Oil-Epoxy Resin Applied to Composites. ABEN doctoral dissertation, North Dakota State University, Fargo, ND.
- Haagenson, D.M., R.L. Brudvik, H. Lin, and D.P. Wiesenborn. 2010. Implementing an in situ alkaline transesterification method for canola biodiesel quality screening, Journal of the American Oil Chemists Society, 87(11):1351-1358.
- Espinoza-Perez, J.D., D. Wiesenborn, C.A. Ulven, C.R. Gustafson. 2010. Canola-based epoxy resins for bio-based plastic composites, paper 143-3, Symposium-Canola End Uses-Biofuels/Bio-Based Products, U.S. Canola Association Research Conference in conjunction with ASA-CSSA-SSSA Annual Meetings, Long Beach, CA, Nov. 2-3. (electronic abstract, ASA-CSSA-SSSA)
- Haagenson, D.M. and D. Wiesenborn. 2010. Impact of North Dakota growing location on canola biodiesel quality, paper 141-18, U.S. Canola Association Research Conference in conjunction with ASA-CSSA-SSSA Annual Meetings, Long Beach, CA, Nov. 2-3. (electronic abstract, ASA-CSSA-SSSA)
- Lin, H., D. Haagenson, D.P. Wiesenborn, S.W. Pryor, and R. Brudvik. 2010. Effect of trace contaminants on cold soak filterability of canola biodiesel, paper 1009049, Session FPE-21 Biodiesel Production Distribution and Engine Performance, ASABE Annual International Meeting, Pittsburgh, PA, Jun 20-23. (electronic abstract, ASABE Technical Library).
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Progress 10/01/08 to 09/30/09
Outputs
OUTPUTS: Canola oil-based epoxy resin (epoxidized canola oil, ECO) was produced and characterized for use in composite materials. Process conditions have been identified that achieve >98% conversion with 90% yield of ECO, by adapting processes reported for other epoxy resins. The process uses a heterogeneous catalyst that is readily recovered and reused, unlike the liquid acid catalysts traditionally used. The solvent t-butyl alcohol was shown to be an effective substitute for toluene solvent, thereby eliminating a significant workplace and environmental hazard. An additional alternative was found, when using the heterogeneous catalyst, which is that the solvent can actually be omitted without loss of product quality; yield decreased 10%, but this loss was largely eliminated with catalyst reuse. This ECO process has thus far been scaled up to 300 g batches, and a new reactor recently underwent its first test to produce a 1-kg batch of ECO. This scaled-up reactor will enable future demonstrations of the practical applications of canola epoxy resin. The ECO was blended with a synthetic epoxy system at 30, 35 and 40% of the total resin weight, combined with E-glass and cured. The resulting composite specimens had lower flexure strength and glass transition temperature than the zero-ECO control; however, the flexure modulus and toughness were similar to the control. Thus, composites prepared using high-ECO-blends should perform well in applications requiring flexibility and toughness. Models for fractionation of field peas to supplement corn ethanol were developed to help determine the economic feasibility of peas. Feedstocks such as field peas are being considered, in order to meet new ethanol production capacity. Recent studies have shown that pea starch can directly supplement the corn ethanol process. Engineering computer models for four progressively complex pea processing scenarios to supplement a corn ethanol plant were developed to help evaluate commercial feasibility of field peas. The complexity of the processes modeled ranges from basic cleaning and destoning to cleaning, destoning, dehulling, drying, and double-pass milling and air classification. Flow rates and compositions were quantified throughout the steps of the processes. One specific modeled scenario was 10% supplementation (final ethanol product contributed from peas) of a 380 x106 L/y (100 MGY) corn ethanol facility, but the models can be readily adapted to other user inputs. Results from the models at default settings return required pea feedstock rates of 16,700 to 17,800 kg/h (36,800 to 39,200 lb/h). Co-product stream flows are also quantified. This information enables the user to evaluate the extent of pea processing that might be a feasible means for ethanol production supplementation and aid in capital investment and operating cost estimates. PARTICIPANTS: Graduate students who received training through this project include Andrew Wilhelmi, who completed his MS degree in December 2008, Judith Espinoza-Perez, who will complete her doctoral degree in January 2010, and Hongjian Lin, who will complete his MS degree in summer 2010. All three degrees are in Agricultural & Biosystems Engineering. Other key individuals include NDSU faculty members Chad Ulven, Mechanical Engineering; Cole Gustafson and William Wilson, Agribusiness & Applied Economics; Mukhles Rahman, Plant Sciences; and NDSU research specialists Darrin Haagenson and Rachel Brudvik, both in Agricultural & Biosystems Engineering. Other partners include the North Dakota Center of Excellence in Oilseeds Development, the Northern Canola Growers, Monsanto, and the North Dakota Agricultural Products Utilization Commission. A number of additional NDSU projects address the objectives of the multistate project, but are described in other CRIS reports. TARGET AUDIENCES: Target audiences include the following industries and researchers: agricultural machinery manufacturing, composites manufacturing, oilseed and oleochemicals processing, bioethanol processing, and pea and oilseeds production. PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
Epoxies are already a well-established type of resin used in composites, and thus the current focus is on blends of canola oil-based epoxy and synthetic epoxy resins. Composites may be used to create strong, light-weight exterior shields for machinery. A demonstration of the practical application of composites containing ECO was undertaken by a group of senior-level students in the capstone design course for Agricultural & Biosystems Engineering at NDSU. A number of students in this department voluntarily participate in the national ASABE quarter-scale tractor competition, and because of competition weight restrictions, the low weight of ECO-composite shields relative to steel shields provides a competitive advantage. Fenders and an instrument panel were successfully molded with 10% ECO in the matrix, by using the methods developed in this project. Thus, we are demonstrating that canola oil-based resins are suitable for high-value applications, thereby helping to create a new market for canola, fostering new business opportunities in the North Central U.S., and lessening our nation's dependence on imported petroleum. Access to the field pea fractionation models is available at www.ageng.ndsu.nodak.edu/fieldpea/. Field pea fractionation will be most attractive in cool, dry locations, where field peas are more competitive with corn. This research was showcased during tours of the NDSU Pilot Plant, which recently included tours for Undersecretary of Agriculture Gail Buchanan, the NATURE program, ND Department of Commerce, and NDSU Harvest Bowl honorees. Other visitors to the Pilot Plant in recent years included Governor Hoeven, Senator Conrad, North Dakota Empower, and various government staff and news media personnel who accompanied these visits. This research was also presented via posters or talks in 2008-2009 to ND Research & Technology Conference, Fargodome; BioOpportunities Conference, Ramada Plaza Suites, Fargo; and Northern Canola Growers Association, NDSU Alumni Center. This research was also cited in the November 2008 issue of Biomass Magazine (J. Kram, "Plastics from the Prairies").
Publications
- Espinoza-Perez, J.D., D.P. Wiesenborn, D. Haagenson, C.A. Ulven, S. Pryor. 2009. Production and characterization of epoxidized canola oil. Trans ASABE 52(4):1289-1297.
- Wilhelmi, A.J., D. P. Wiesenborn, C. R. Gustafson, S. W. Pryor. 2009. Models for fractionation of field peas to supplement corn ethanol, Applied Engineering in Agriculture, 25(5):709-717.
- Espinoza-Perez, J.D., D. Haagenson, R. Brudvik, C.A. Ulven. D.P. Wiesenborn. 2009. Epoxy resin from high-oleic oils applied to composites, paper 090001. ASABE Annual International Meeting, Reno, NV, Jun 21-24. (electronic abstract, ASABE Technical Library).
- Haagenson, D., R. Brudvik, H. Lin, and D. Wiesenborn. 2009. Development of high-throughput measurement of canola biodiesel cold flow properties, IOP-P. 100th AOCS Annual Meeting & Expo Abstracts, Orlando, FL, May 3-6.
- Lin, H., D. Haagenson, R. Brudvik, D.P. Wiesenborn. 2009. Influence of seeds moisture on in situ alkaline transesterification of canola seeds for biodiesel production, paper 096339. ASABE Annual International Meeting, Reno, NV, Jun 21-24 (electronic abstract, ASABE Technical Library).
- Wilhelmi, A.J. 2008. Field Peas to Supplement Corn Ethanol: Engineering Process Models, Capital Investment, and Annual Operating Costs, M.S. Thesis, Agricultural & Biosystems Engineering, NDSU.
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