Source: UNIVERSITY OF ARKANSAS submitted to NRP
ENHANCED SUPERCRITICAL CARBON DIOXIDE SYSTEM FOR THE GENERATION OF POROUS MATERIALS FROM AGRICULTURAL AND FOOD PROCESSING BYPRODUCTS
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
COMPLETE
Funding Source
Reporting Frequency
Annual
Accession No.
1030716
Grant No.
2023-67022-40164
Cumulative Award Amt.
$30,000.00
Proposal No.
2022-10857
Multistate No.
(N/A)
Project Start Date
May 15, 2023
Project End Date
May 14, 2024
Grant Year
2023
Program Code
[A1531]- Biorefining and Biomanufacturing
Recipient Organization
UNIVERSITY OF ARKANSAS
(N/A)
FAYETTEVILLE,AR 72703
Performing Department
(N/A)
Non Technical Summary
Agricultural and food processing byproducts are underutilized, creating major disposal problems and sustainability issues for the agriculture and food industries. The long-term goal is to generate advanced packaging materials from agricultural and food processing byproducts using a sustainable approach based on supercritical carbon dioxide (SC-CO2). The overall objective for this equipment grant application is to develop an innovative, custom-built SC-CO2 system that can be used for various applications. The specific objectives are: (1) Acquire high-pressure pumps for the delivery of CO2 and aerogel solutions, (2) Connect the acquired pumps with the high-pressure vessel and build the system, (3) Test the developed semi-continuous SC-CO2 system at different flow rates, pressures, and temperatures. The developed SC-CO2 system will enable innovative research to enhance the utilization of agricultural and food processing byproducts by generating alternative, high-value materials. This project will (i) enhance the capabilities of the Department of Food Science and Department of Biological and Agricultural Engineering, (ii) provide training opportunities to undergraduate and graduate students, and (iii) attract middle/high school students to STEM programs. This project supports Objective 2.3 Foster Agricultural Innovation in the USDA Strategic Goal 2, "Ensure America's Agricultural System is Equitable, Resilient, and Prosperous".
Animal Health Component
45%
Research Effort Categories
Basic
10%
Applied
45%
Developmental
45%
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
4025310202050%
5115310202050%
Goals / Objectives
The specific objectives are: (1) Acquire high-pressure pumps for the delivery of CO2 and aerogel solutions, (2) Connect the acquired pumps with the high-pressure vessel and build the system, (3) Test the developed semi-continuous SC-CO2 system at different flow rates, pressures, and temperatures.
Project Methods
Objective 1: High-pressure pumps for the delivery of CO2 and aerogel solutions will be acquired. Objective 2: The acquired pumps will be connected to a high-pressure vessel to build the system. Objective 3: The developed semi-continuous SC-CO2 system will be tested at different flow rates, pressures, and temperatures for various applications.

Progress 05/15/23 to 05/14/24

Outputs
Target Audience:During this reporting period, the target audiences reached include undergraduate and graduate students, postdoctoral researchers, food engineers/scientists, the food industry, and middle & high school students. Two graduate students and one postdoctoral researcher were directly involved in this project and trained on supercritical carbon dioxide technology. Two graduate students have used the newly developed system for their research on rice processing byproducts, sorghum flour, and wax fractionation. They were trained in sample characterization via scanning electron microscopy (SEM), gas chromatography (GC), thermal conductivity, rheology, texture, Fourier transform infrared spectroscopy (FTIR), and x-ray diffraction (XRD). Research findings were shared with peers at scientific conferences, including the Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, the American Oil Chemists' Society (AOCS) Annual Meeting & Expo, and the Rice Processing Program Industry Alliance Meeting. The technologies developed were discussed in two courses: Principles of Food Processing (~25 students) and Science of Chocolate (~170 students). We are planning to give a guest lecture in the BENG 4743 Food and Bio-Product Systems Engineering to introduce the technology. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?During this reporting period, the target audiences reached include undergraduate and graduate students, postdoctoral researchers, food engineers/scientists, the food industry, and middle & high school students. Two graduate students and one postdoctoral researcher were directly involved in this project and trained on supercritical carbon dioxide technology; specifically, they were trained in the development/engineering of new high-pressure systems for processing agricultural and food byproducts, and fundamentals of supercritical fluids. Two graduate students have used the newly developed system for their research on rice processing byproducts, sorghum flour, and wax fractionation. They were trained in sample characterization via scanning electron microscopy (SEM), gas chromatography (GC), thermal conductivity, rheology, texture, digestion, Fourier transform infrared spectroscopy (FTIR), and x-ray diffraction (XRD). How have the results been disseminated to communities of interest?We provided lab tours to middle and high school students and introduced the developed SC-CO2 system to attract their attention to Food Science and Engineering. We kept our lab website (foodeng4health.uark.edu) up to date, which helped us share the research being conducted in our lab with the public. Our lab, Food Engineering for Health, was featured in Arkansas News releases, and a video recording of Dr. Ubeyitogullari's research has been posted on the YouTube channel of the University of Arkansas Division of Agriculture. Two manuscripts were published in high-quality peer-reviewed journals, and one manuscript is currently under review. The findings were also disseminated via multiple conference presentations. Publications Kaur, S., & Ubeyitogullari, A. (2024). In vitro digestion of starch and protein aerogels generated from defatted rice bran via supercritical carbon dioxide drying. Food Chemistry, 139833. https://doi.org/10.1016/j.foodchem.2024.139833 Tuhanioglu, A., & Ubeyitogullari, A. (2024). Application of supercritical carbon dioxide to enhance the aroma of whole sorghum flour for use in 3D printing of sorghum cookies. Food Research International, 190, 114588. https://doi.org/10.1016/j.foodres.2024.114588 Ahmadzadeh, S., Sagardui, A., Huitink, D., Chen, J., & Ubeyitogullari, A. (2024). Cellulose-starch composite aerogels as thermal super-insulating materials. Under review. Presentations Kaur, S. & Ubeyitogullari, A. (2024). In vitro digestion of protein aerogels generated from defatted rice bran protein via supercritical carbon dioxide technology. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 14-17, Chicago, IL, USA. Tuhaniogulu, A. & Ubeyitogullari, A. (2024). Enhancing the aroma of whole sorghum flour using supercritical carbon dioxide: Application of the treated flour in 3D printing of sorghum cookies. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 14-17, Chicago, IL, USA. Kaur, S. & Ubeyitogullari, A. (2024). In vitro digestion of protein aerogels generated from defatted rice bran protein via supercritical carbon dioxide technology. The American Oil Chemists' Society (AOCS) Annual Meeting & Expo, April 28-May 1, Montreal, Quebec, Canada. Tuhanioglu, A. & Ubeyitogullari, A. (2024). Selective extraction of waxes from bioethanol production side-stream via supercritical carbon dioxide: Thermal characterization and modeling. The American Oil Chemists' Society (AOCS) Annual Meeting & Expo, April 28-May 1, Montreal, Quebec, Canada. Kaur, S. & Ubeyitogullari, A. (2023). Converting rice processing byproducts into high-value bioactive compounds and nanoporous materials using supercritical carbon dioxide. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 16-19, Chicago, IL, USA. Tuhaniogulu, A. & Ubeyitogullari, A. (2023). Enhancing the flavor of white whole sorghum flour using supercritical carbon dioxide. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 16-19, Chicago, IL, USA. Kaur, S. & Ubeyitogullari, A. (2024). In vitro digestion of starch and protein-based nanoporous aerogels generated from defatted rice bran protein via supercritical carbon dioxide technology. Rice Processing Program Industry Alliance Meeting, May 21, Fayetteville, AR, USA. What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? With this equipment grant, we have acquired a double-head high-pressure pump from Teledyne ISCO Inc. (NE, USA), which is composed of two 260x syringe pumps and a controller. The pump can operate up to 65.5 MPa with a flow rate of up to 107 mL/min. This dual-pump system can provide continuous flow to be used for various applications, including extraction of valuable components from agricultural and food processing byproducts as well as drying of biopolymer gels. In addition to the high-pressure dual-pump, a ReaXus LS Class pump was purchased for the delivery of co-solvents along with supercritical carbon dioxide (SC-CO2) to the system. Next, these pumps were used to develop a novel SC-CO2 system for the generation of aerogels, where high-pressure stainless-steel vessel, tubing, valves (i.e., check, needle, and micrometering valves), pressure gauges, heating elements, and flowmeter were connected. The operation of the system has been validated using the minimum/maximum working conditions, considering the flow rate, temperature, and pressure. The developed system is very flexible and can be customized for other SC-CO2 applications. We have used the system to generate aerogels from defatted rice bran using SC-CO2 drying, where aerogels were produced using 15% (w/w) concentration of starch, crude starch, and protein fractions from defatted rice bran. The developed aerogels showed high surface areas of 36-47 m2/g with porosities higher than 84%. In addition, the in vitro digestion of the aerogels was determined using a sequential oral, gastric, and intestinal simulated digestion. The hydrolyses of starch and proteins were improved after aerogel formation. In another application, the aroma of sorghum flour was improved using SC-CO2, where flour samples were treated under different temperatures (40-60 °C) and pressures (8-15 MPa). The SC-CO2 treatment effectively removed undesired aroma from the flour. Finally, the cellulose-starch composite aerogels were generated as thermal super-insulating materials. In this study, we investigated the aerogel formation from different mass ratios of microcrystalline cellulose and starch (1:0, 2:1, 1:1, 2:1, and 0:1, respectively). The 1:2 microcrystalline cellulose:starch aerogel exhibited the highest porosity (97%), the lowest density (0.058 g/cm3), and the lowest thermal conductivity (0.012 W/m?K) along with a high specific surface area (258 m2/g). Overall, the developed system has been used for various SC-CO2 processing applications in the first year of its installation. We plan to continue employing the newly installed system for various SC-CO2 applications to increase the sustainability of agricultural and food systems. We are developing a standard grant proposal, that utilizes the acquired equipment, to be submitted to USDA-NIFA AFRI this year.

Publications

  • Type: Journal Articles Status: Published Year Published: 2024 Citation: Kaur, S., & Ubeyitogullari, A. (2024). In vitro digestion of starch and protein aerogels generated from defatted rice bran via supercritical carbon dioxide drying. Food Chemistry, 139833. https://doi.org/10.1016/j.foodchem.2024.139833
  • Type: Journal Articles Status: Published Year Published: 2024 Citation: Tuhanioglu, A., & Ubeyitogullari, A. (2024). Application of supercritical carbon dioxide to enhance the aroma of whole sorghum flour for use in 3D printing of sorghum cookies. Food Research International, 190, 114588. https://doi.org/10.1016/j.foodres.2024.114588
  • Type: Journal Articles Status: Under Review Year Published: 2024 Citation: Ahmadzadeh, S., Sagardui, A., Huitink, D., Chen, J., & Ubeyitogullari, A. (2024). Cellulose-starch composite aerogels as thermal super-insulating materials. Under review.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Tuhaniogulu, A. & Ubeyitogullari, A. (2023). Enhancing the flavor of white whole sorghum flour using supercritical carbon dioxide. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 16-19, Chicago, IL, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Kaur, S. & Ubeyitogullari, A. (2024). In vitro digestion of protein aerogels generated from defatted rice bran protein via supercritical carbon dioxide technology. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 14-17, Chicago, IL, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2024 Citation: Tuhaniogulu, A. & Ubeyitogullari, A. (2024). Enhancing the aroma of whole sorghum flour using supercritical carbon dioxide: Application of the treated flour in 3D printing of sorghum cookies. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 14-17, Chicago, IL, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2024 Citation: Kaur, S. & Ubeyitogullari, A. (2024). In vitro digestion of protein aerogels generated from defatted rice bran protein via supercritical carbon dioxide technology. The American Oil Chemists' Society (AOCS) Annual Meeting & Expo, April 28-May 1, Montreal, Quebec, Canada.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2024 Citation: Tuhanioglu, A. & Ubeyitogullari, A. (2024). Selective extraction of waxes from bioethanol production side-stream via supercritical carbon dioxide: Thermal characterization and modeling. The American Oil Chemists' Society (AOCS) Annual Meeting & Expo, April 28-May 1, Montreal, Quebec, Canada.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2024 Citation: Kaur, S. & Ubeyitogullari, A. (2024). In vitro digestion of starch and protein-based nanoporous aerogels generated from defatted rice bran protein via supercritical carbon dioxide technology. Rice Processing Program Industry Alliance Meeting, May 21, Fayetteville, AR, USA.
  • Type: Conference Papers and Presentations Status: Published Year Published: 2023 Citation: Kaur, S. & Ubeyitogullari, A. (2023). Converting rice processing byproducts into high-value bioactive compounds and nanoporous materials using supercritical carbon dioxide. Institute of Food Technologists (IFT) FIRST Annual Meeting & Food Expo, July 16-19, Chicago, IL, USA.