Progress 05/12/04 to 06/06/05
Outputs
1. What major problem or issue is being resolved and how are you resolving it (summarize project aims and objectives)? How serious is the problem? What does it matter? Over the past twenty years, exports of US wheat have been both unpredictable and declining. A potentially huge market for wheat is the biorefining and bioconversion of wheat into biobased products, including fine chemicals and fuel-grade ethanol. A key biorefining step is the fractionation of the wheat into starch and protein concentrates. Current separation technologies, which produce concentrates of starch and gluten, are costly and have difficulty competing with foreign imports. Contributing to the expense of the commercial methods are: (1) outdated, nonstandard mill technologies; (2) the inefficient use of energy; and (3) the generation of copious amounts of wastewater. This project researches new and relevant separation technologies and systems. One of these is the cold-ethanol process invented at
WRRC, in which ethanol serves as a process fluid to largely replace the use of water and reduce energy use. The cold-ethanol method of separation has the potential to reduce energy and water usage, leading to optimal use of all co-product streams. Another important technology is the separation of ethanol and water, which is important to the cold ethanol method, as well as to the eventual production of fuel-grade ethanol from surplus starch. The overall project goal is to improve wheat refining, increase wheat usage in bioproducts and biofuels (ethanol), and improve grain-to-ethanol processing efficiency. The total value of US wheat exports is 2/3 of its 1987 value, yet the total production has remained constant. The amount of wheat available for domestic non-food use is roughly 30 billion pounds and growing. Of this amount, the US gluten industry currently separates a little more than 2 billion lbs of wheat into starch and protein for food and non-food uses. This represents 58% of the
total domestic gluten market; the rest of which is mostly imported from Europe due to their relative cost advantage. The potential of improving separation processes to improve starch and gluten separation would lead to increased domestic production of gluten, reduced imports, and improved attractiveness of all fractionated wheat components including starch for fuel-grade ethanol. Wheat starch as a fermentation feedstock could significantly expand grain-to-ethanol production in the US, help to reduce dependence on imported fuels and toxic oxygenates, and improve the nation's ability to produce ethanol in a wider range of diverse regional locations. Improved energy-efficiency through improved ethanol-water separations is crucial to the future of the wheat biorefinery. This is a bridging project from 5325-41000-037-00D to 5325-41000-047-00D. 2. List the milestones (indicators of progress) from your Project Plan. This project is being terminated and replaced by 5325-41000-047-00D. Please
see the report for 5325-41000-047-00D for milestones. 3a List the milestones that were scheduled to be addressed in FY 2005. For each milestone, indicate the status: fully met, substantially met, or not met. If not met, why. 1. This project is being terminated and replaced by 5325-41000-047-00D. Please see the report for 5325-41000-047-00D for milestones. Milestone Substantially Met 3b List the milestones that you expect to address over the next 3 years (FY 2006, 2007, and 2008). What do you expect to accomplish, year by year, over the next 3 years under each milestone? This project is being terminated and replaced by 5325-41000-047-00D. Please see the report for 5325-41000-047-00D for milestones. 4a What was the single most significant accomplishment this past year? Recovery of ethanol from water solutions is critical for fuel ethanol production and use of ethanol as a biorefining solvent in wheat fractionation. The energy balance for ethanol production using standard technology,
distillation, is energy-intensive. Solvent extraction and membrane permeation are two low-energy alternatives. Researchers at WRRC, Albany have screened a large number of solvents for performance in extracting ethanol, including a variety of biobased solvents, and have developed structure/performance correlations useful for prediction. This has led to discovery of several solvents with significantly better extraction performance than those typically considered for this application. 4b List other significant accomplishments, if any. The use of wheat as a platform to produce new biobased products and biofuels can be advanced with the ability to produce stable and enriched wheat gluten protein subfractions with non-varying compositions and properties. These could be used as platform chemicals. WRRC scientists have conducted extraction studies to assess the separation of wheat gluten components using ethanol and reduced temperatures that lower the risk of protein denaturation; hence,
both food and non-food markets may be met. The data obtained by capillary electrophoresis of flour extracts provide composition maps useful to the design of separation processes. 4d Progress report. Wheat Fractionation: Wheat protein and protein fraction solubility at low temperatures has not been previously reported except for very broad classes of protein. This information was acquired to develop strategies for fractionation of narrow classes of protein that can potentially be recombined without loss of functionality. The adoption of the technologies being developed here are partially dependent on valuation of the fractions produced. This is especially true for wheat gluten intended for bread flour fortification. We have elicited collaboration from a domestic producer, importer, and supplier of wheat gluten and have processed about 75 kilo of flour to produce both water-based and cold-ethanol based gluten from two commercial sources of flour (the collaborator and a local
ingredient supplier). Samples will be provided to the collaborator and others expressing interest. Ethanol-Extraction Solvents: The reasons why isomers of the higher alcohol solvents show differences in ethanol extraction performance are unknown. Molecular simulation is being used to determine if intermolecular associations between solvent molecules, and between solvent, water, and ethanol molecules, can explain these observations. Preliminary indications are very positive, and will be a significant improvement in understanding the fundamentals of solvent performance. Membrane Permeation: Membrane processes for recovery of ethanol from water solutions are attractive due to their low energy requirements, compared to distillation. Currently available ethanol-selective membranes cannot economically compete with distillation because of their low throughput, requiring large membrane area. Supported liquid membranes, and mixed matrix membranes incorporating fine particles into the
polymer, can have enhanced properties compared to standard polymer membranes. We have built an apparatus for measuring the permeation performance of membranes, and have instituted preparation of new membranes for evaluation. A patent application, Spiral-Wound Liquid Membrane Module for Separation of Fluids and Gases" has been filed. 5. Describe the major accomplishments over the life of the project, including their predicted or actual impact. This is a bridging project. Prior reports for the parent project may be found in annual reports for project 5325-41000-037-00D and the continuation is found in 5325-41000-047-00D. The parent project developed the fundamental basis of separability of wheat components in non-aqueous ethanol systems and established significant new knowledge about the material and chemical properties of sensitive proteins and natural protein combinations following exposure to ethanol. This information is crucial to the development of the novel cold-ethanol method
patented by WRRC. Specific accomplishments include: (1) discovery that the cold ethanol extraction method improves wheat gluten quality as determined in farinograph, mixograph, and baking evaluations, and maintains quality through severe drying conditions, and (2) definition of the use of novel "dough-ball" and "dispersed-batter" methods for the production of wheat gluten concentrates, and (3) development of new fundamental knowledge about selective protein solubility and the composition of proteins in processing fluids applied to developed wet-dough. As a whole, these findings provide critical support for adoption of the cold-ethanol method as a processing technology that can produce improved quality. This should lead to market advantages for domestically-produced wheat components. Further, the body of information developed by us has recently stimulated interest by both process development and grain processing companies for further investigation. Advancement of this technology will
require preliminary costing, further process definition and small pilot-scale evaluations. In addition, these findings help to improve the fundamental understanding of the chemical and functional properties of native and processed wheat fractions. The accomplishments were reported in 10 peer reviewed publications and one patent with additional manuscripts in preparation. Oral presentations and individual meetings with company representatives have been included in the ongoing effort to effect technology transfer. Substantially all scientific milestones have been, or will be addressed in these publications. This project was consistent with two components of the National Program 306 Action Plan: (a) "New knowledge derived from improved understandings of the structure, properties, metabolism, and function of crop and animal components, particularly carbohydrates, proteins, and lipids, will generate development of a variety of new food, feed, and industrial products." and (b) "New
technologies to convert commodities and processing byproducts into important value-added products such as fat substitutes, high-quality animal feeds, improved textiles, pharmaceutical ingredients, enzymes, and cosmetics will fill demonstrated needs." This project was consistent with two components of the National Program 307 Action Plan: (a) "New technologies that integrate feedstock pretreatment, biological conversion and product recovery processes, as well as fundamental knowledge regarding fermentation, milling and membrane separations. The information gained will result in a reduction in capital and processing costs associated with biofuel production." and (b) "Higher value coproducts generated from current low-value production byproducts. Envisioned coproducts include specialty oils, novel polysaccharides that will compete with imported gums, sugar alcohol food additives that are currently imported, enzymes, and inexpensive aquaculture feeds." 6. What science and/or technologies
have been transferred and to whom? When is the science and/or technology likely to become available to the end- user (industry, farmer, other scientists)? What are the constraints, if known, to the adoption and durability of the technology products? The technology is currently available through patent and publications. Information has been conveyed to a number of interested companies through reference to web summaries, printed brochures and personal discussions at meetings such as the Fuel Ethanol Workshop (June 2005) and the 4th Starch Utilization Technology Conference (June 2005). Scientists on the staff have been invited to make oral reports for staff of a principal firm involved with ethanol plants. Particular targets have been grain processing companies and design firms. Constraints: the separation technology affects many parameters of the overall process system and would require retirement of complex existing facilities and installation of new processing operations. Therefore,
reliable data on product quality, drying properties, etc. and larger scale evaluations are essential to implementation. The technology may become available for small-pilot evaluation (outside WRRC) within the next 2-3 years as scale-up experiments proceed.
Impacts
(N/A)
Publications
- Wong, D., Batt, S.B., Lee, C.C., Robertson, G.H. Rapid selection of alpha- amylase mutants in yeast libraries for raw starch activity. 2003. Society of Biomolecular Screening Annual Conference, Portland, Oregon.
- Wong, D., Batt, S.B., Lee, C.C., Robertson, G.H. Engineering apha-amylase for enhanced activity by molecular evolution. American Society of Biochemistry and Molecular Biology Annual Meeting, June 12-16, 2004, Boston, Massachusetts. Abstract No. B38.
- Wong, D., Batt, S.B., Lee, C.C., Robertson, G.H. 2004. Direct screening of libraries of yeast clones for alpha-amylase activity on raw starch. Journal of Biomolecular Screening. 10:459-468.
- Robertson, G.H., Cao, T. 2004. Proteins extracted by water or aqueous ethanol during refining of developed wheat dough to vital wheat gluten and crude starch as determined by capillary-zone electrophoresis (cze). Cereal Chemistry. 81(5):673-680.
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Progress 10/01/03 to 09/30/04
Outputs
1. What major problem or issue is being resolved and how are you resolving it (summarize project aims and objectives)? How serious is the problem? What does it matter? Over the past twenty years, exports of US wheat have been both unpredictable and declining. A potentially huge market for wheat is the biorefining and bioconversion of wheat into biobased products, including fuel-grade ethanol and fine chemicals. A key biorefining step is the fractionation of the wheat into starch and protein concentrates. Current separation technologies, which produce concentrates of starch and gluten, are costly and have difficulty competing with foreign imports. Contributing to the expense of the commercial methods are: (1) outdated, nonstandard mill technologies; (2) the inefficient use of energy; and (3) the generation of copious amounts of wastewater. This project researches new and relevant separation technologies and systems. One of these is the cold-ethanol process invented at
WRRC, in which ethanol serves as a process fluid to largely replace the use of water and reduce energy use. The cold-ethanol method of separation has the potential to reduce energy and water usage, leading to optimal use of all co-product streams. Another important technology is the separation of ethanol and water, which is important to the cold ethanol method, as well as to the eventual production of fuel-grade ethanol from surplus starch. The overall project goal is to improve wheat refining, increase wheat usage in bioproducts and biofuels (ethanol), and improve grain-to-ethanol processing efficiency. The total value of US wheat exports is 2/3 of its 1987 value, yet the total production has remained constant. The amount of wheat available for domestic non-food use is roughly 30 billion pounds and growing. Of this amount, the US gluten industry currently separates a little more than 2 billion lbs of wheat into starch and protein for food and non-food uses. This represents 58% of the
total domestic gluten market; the rest of which is mostly imported from Europe due to their relative cost advantage. The potential of improving separation processes to improve starch and gluten separation would lead to increased domestic production of gluten, reduced imports, and improved attractiveness of all fractionated wheat components including starch for fuel-grade ethanol. Wheat starch as a fermentation feedstock could significantly expand grain-to-ethanol production in the US, help to reduce dependence on imported fuels and toxic oxygenates, and improve the nation's ability to produce ethanol in a wider range of diverse regional locations. Improved energy-efficiency through improved ethanol-water separations is crucial to the future of the wheat biorefinery. 2. List the milestones (indicators of progress) from your Project Plan. 2. List the milestones (indicators of progress) from your Project Plan. FY ( 2002) a. Complete evaluation of lab scale separation using a
screening/drying system to model full-scale operation in an analog of the conventional batter process. b. Complete evaluation of the influence of drying conditions (particularly temperature) on changes to gluten vitality. FY (2003) a. Complete development of new project component for using biopolymer membranes to separate ethanol from water during fermentation to fuel- grade ethanol. b. Complete countercurrent extraction experiments on wheat separation. Evaluate opportunity for pentosan recovery. FY (2004) a. Establish new project: biopolymer-based barriers to separate ethanol from water from ethanol fermentation fluids and from cold-ethanol separation of wheat gluten and starch. b. Establish collaborative research through MU or CRADA for additional evaluation and engineering assessment. c. Assess current project and develop project plan for next 5 years subject to peer review by OSQR. 3. Milestones: FY (2003) a. Completed countercurrent extraction experiments on wheat separation.
Evaluated opportunity for pentosan recovery. Substantial progress. Reevaluation of this milestone suggested a more critical need for compositional studies including the assessment of soluble and insoluble protein removed during the washing of dough with cold ethanol. These studies were completed. Collaboration has been formed with WRRC scientist to assist in the pentosan assessment. FY (2004) a. Established new project: biopolymer-based barriers to separate ethanol from water from ethanol fermentation fluids and from cold-ethanol separation of wheat gluten and starch. Successfully met. New support position filled and analytical instrumentation installed and tested. Literature analysis of ethanol- selective membranes substantially completed and experimentation initiated. b. Established collaborative research using Memorandum of Understanding or CRADA for additional evaluation and engineering assessment. Successfully met. Three companies with interest in barrier separations, plant
design, and grain refining have indicated the desire in writing to collaborate with us in the evaluation and development of this research. c. Assess current project and develop project plan for next 5 years subject to peer review by OSQR. Successfully met. New project plan formulated and in final evaluation received the highest scoring level by peer panel. B. Refer to the annual report for new CRIS project, pending OSQR process completion. 4. What were the most significant accomplishments this past year? A. Single Most Significant Accomplishments With unpredictable and declining exports of US wheat over the past 20 years, creation of new markets for US wheat hinges on efficiently separating or biorefining this grain into its constituents to optimize its value as a feedstock for bioproducts, fine chemicals and ethanol. Researchers at Western Regional Research Center (WRRC) developed and scaled-up cold-ethanol based methods for separating and refining wheat into its major constituents.
During this year WRRC researchers developed and implemented technology that resulted in the ability to track each protein constituent and to identify how ethanol composition and temperature affected the removal, quality and end-use value of each protein. This new knowledge is being used to predict the full-scale capability of this process, define the separation equipment required, and to facilitate industrial adoption of improved wheat bio-refining. B. Other Significant Accomplishments Barrier-based separation of ethanol and water is critical in all ethanol fermentation processes, and thus has widespread implications. It is particularly pertinent in the present research because of the need to manage ethanol concentrations in the cold ethanol starch/gluten separation with the requirement to eliminate added processing water. Researchers at WRRC, Albany invented a "New Filtering Device Utilizing a Combination of Membrane Materials which Allows for Selective Isolation of Target Compounds
from a Production Stream" which can be used for separating ethanol from fermentation broths. This invention, which has been approved by the Area-wide Patent Committee and will be filed shortly, is based on experimental evaluation of ethanol-selective extractants as components of a novel hybrid barrier system employing both selective barriers and solvent extraction. C. Significant Accomplishments/Activities that Support Special Target Populations None. D. Progress Report Barrier-based separation of ethanol and water: This effort is critical in all ethanol fermentation procesess, and thus has widespread implications. A complete overview and analysis of the existing barrier literature is substantially complete. We initiated experimental evaluation of ethanol- selective extractants as components of a novel hybrid barrier system employing both selective barriers and solvent extraction. Wheat separation: Kilogram-scale wheat separation methods are now regularly employed to disperse and
separate wheat fractions using enclosed vibratory screening. In addition to producing high quality vital gluten, this process has the added benefit of creating separate phases in the chilled ethanol starch "wash-off" that contain pentosans and soluble and insoluble protein. An improved understanding of the composition of the wash-off is important in the identification of co-product and process equipment and was sought during this period. Recovery of these components could have important implications to the overall attractiveness of the cold-ethanol method eg. the pentosans have specific food-ingredient and potential health benefits. Differences in both starch and protein functionality/composition between cold-ethanol-produced and water- produced vital products continue to be studied. Using the cold-ethanol process, gluten properties are generally better, and starch is more specifically fractionated into its morphological components, such as A- type starch, B-type starch. New
processing capabilities have been acquired, installed, and tested by the team, including a solvent ready basket centrifuge, a solvent-ready decanter centrifuge, and capillary electrophoresis. Substantial progress was made in the development of thermoformed gluten polymers. A variety of crosslinking and formulation strategies were assessed for their impact on elastic properties of these pliable polymers. 5. Describe the major accomplishments over the life of the project, including their predicted or actual impact. This project developed the fundamental basis for optimalling separating wheat components in non-aqueous ethanol systems. It established significant new knowledge about the material and chemical properties of sensitive proteins and natural protein combinations following exposure to ethanol. This information is crucial to the development of the novel cold-ethanol method patented by WRRC. Specific accomplishments include: (1) discovery that the cold ethanol extraction method
improves wheat gluten quality as determined in farinograph, mixograph, and baking evaluations. It maintains quality through severe drying conditions, (2) definition of the use of novel "dough-ball" and "dispersed-batter" methods for the production of wheat gluten concentrates, and (3) development of new fundamental knowledge about selective protein solubility and the composition of proteins in processing fluids applied to developed wet-dough. As a whole, these findings provide critical support for adoption of the cold-ethanol method as a processing technology that can produce improved wheat quality. This should lead to market advantages for domestically- produced wheat components. Further, the body of information developed within this project has recently stimulated interest by grain processing companies for further investigation. Advancement of this technology will require preliminary costing, further process definition and small pilot- scale evaluations. In addition, these
findings help to improve the fundamental understanding of the chemical and functional properties of native and processed wheat fractions. The accomplishments were reported in 7 publications and one patent with additional manuscripts in preparation. Oral presentations and individual meetings with company representatives have been included in the ongoing effort to effect technology transfer. Substantially all scientific milestones have been, or will be addressed in these publications. This project was consistent with two components of the National Program 306 Action Plan (a) "New knowledge derived from improved understandings of the structure, properties, metabolism, and function of crop and animal components, particularly carbohydrates, proteins, and lipids, will generate development of a variety of new food, feed, and industrial products." (b) "New technologies to convert commodities and processing byproducts into important value-added products such as fat substitutes, high-quality
animal feeds, improved textiles, pharmaceutical ingredients, enzymes, and cosmetics will fill demonstrated needs." This project was consistent with two components of the National Program 307 Action Plan (a) "New technologies that integrate feedstock pretreatment, biological conversion and product recovery processes, as well as fundamental knowledge regarding fermentation, milling and membrane separations. The information gained will result in a reduction in capital and processing costs associated with biofuel production." (b) "Higher value coproducts generated from current low-value production byproducts. Envisioned coproducts include specialty oils, novel polysaccharides that will compete with imported gums, sugar alcohol food additives that are currently imported, enzymes, and inexpensive aquaculture feeds." 6. What science and/or technologies have been transferred and to whom? When is the science and/or technology likely to become available to the end- user (industry, farmer,
other scientists)? What are the constraints, if known, to the adoption and durability of the technology products? The technology is currently available through patent and publications. Information has been conveyed to a number of interested companies through reference to web summaries, printed brochures and personal discussions at trade related meetings such as the Fuel Ethanol Workshop and the Corn Utilization and Technology Conference held this year. Particular targets have been grain-processing companies and design firms. Constraints: the separation technology affects many parameters of the overall process system and would require retirement of complex existing facilities and installation of new processing operations. Therefore, reliable data on product quality, drying properties, etc. and larger scale evaluations are essential to implementation. The technology may become available for small-pilot evaluation (outside WRRC) within the next 1-2 years as scale- up experiments
proceed. 7. List your most important publications in the popular press and presentations to organizations and articles written about your work. "Creating and capturing total value of agricultural resources for biofuels and biobased products." 8pp. Posted at http://www.pw.usda.gov. Also distributed as brochure at trade meetings.
Impacts
(N/A)
Publications
- Wong, D., Batt, S.B., Lee, C.C., Robertson, G.H. Rapid selection of alpha- amylase mutants in yeast libraries for raw starch activity. 2003. Society of Biomolecular Screening Annual Conference, Portland, Oregon.
- Wong, D., Batt, S.B., Lee, C.C., Robertson, G.H. Engineering apha-amylase for enhanced activity by molecular evolution. American Society of Biochemistry and Molecular Biology Annual Meeting, June 12-16, 2004, Boston, Massachusetts. Abstract No. B38.
- Wong, D., Batt, S.B., Lee, C.C., Robertson, G.H. 2004. Direct screening of libraries of yeast clones for alpha-amylase activity on raw starch. Journal of Biomolecular Screening. 10:459-468.
- Robertson, G.H., Cao, T. 2004. Proteins extracted by water or aqueous ethanol during refining of developed wheat dough to vital wheat gluten and crude starch as determined by capillary-zone electrophoresis (cze). Cereal Chemistry. 81(5):673-680.
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