Progress 07/01/23 to 06/30/24
Outputs
Target Audience:The target audience of the research includes, but is not limited to, North Carolina State University Wilson College of Textiles, College of Education, and College of Natural Resources, the Sustainable Alternative Fibers Initiative (SAFI), the local community of Raleigh, NC, and rural North Carolina high school students and teachers in STEM. Target audience efforts have provided outreach and collaboration in part with industry partners in the program including Eastman Chemical company and other universities such as Aalto University in Finland. Changes/Problems:
Nothing Reported
What opportunities for training and professional development has the project provided?John Sanders has continued to serve as the responsible user for the gel permeation chromatograph (GPC). In this role, he has trained new users to operate the instrument and analyze their data. He has performed regular maintenance such as column changing and replacement of instrument components as needed. As the responsible user of the only functioning GPC on the NC State campus, he has coordinated with students from other departments to facilitate their research; this has expanded his professional network. Additionally, Sanders receives regular informal training on laboratory equipment and procedures from research group members as part of his research work. Autumn Reynolds led three hands-on training sessions in the Pulp and Paper Basics Short Course, reaching undergraduate students, professionals, and early-career researchers. She also facilitated workshops for high school students through a USDA-sponsored STEM outreach initiative in North Carolina. As a visiting researcher at Aalto University, Reynolds gained international research experience and received advanced training in dope rheology, fiber spinning, and dissolution analytics. She mentored early-stage Ph.D. and undergraduate students at NC State and advanced to Doctoral Candidate status after successfully completing her Preliminary Exam based on work supported by this grant. Multiple lab group discussions and interdisciplinary seminars further contributed to peer-to-peer knowledge exchange and research communication skills. Isabel Albelo completed a wide range of relevant coursework and laboratory safety and technical training. Coursework included TMS 763-Characterization of Structure of Fiber Forming Polymers, TC 589-Biobased Textile Materials and Processes, FPS 770-Advances in Polymer Science, TTM 508- Sustainability in the Textile and Apparel Industry, TMS 762-Physical Properties of Fiber Forming Polymers, and TC 704- Fiber Formation: Theory and Practice. Training included Laboratory Chemical Waste Management Training, Analytical X-ray Safety, NC State University, Wilson College of Textiles, Department of Textile Engineering, Chemistry, Microscopy Lab, Scanning Electron Microscope User Training, and NC State University, Department of Materials Science and Engineering, Dynamic Light Scattering User Training. How have the results been disseminated to communities of interest?Research and literature review findings were shared through peer-reviewed journal articles, conference and lab group presentations, hands-on training courses, and collaborative academic seminars. Specific dissemination channels included: Publication of a co-authored article on non-wood textile feedstocks in the Journal of Bioresources and Bioproducts. Presentations and lab tours at Aalto University and NC State, reaching international researchers, doctoral candidates, and industry representatives. Informal consultation and data-sharing with industry partners and research collaborators to discuss opportunities and limitations of recycled pulp in high-value fiber applications. What do you plan to do during the next reporting period to accomplish the goals?Goals will be accomplished during the next reporting period by creating and following a timeline of experimental research and publishing. The students will also collaborate/interact with the other Fellows from the NNF program as well as other institutions. Classes and informal research training will continue.
Impacts
What was accomplished under these goals?
John Sanders has worked on two major research projects. In the first project, Sanders measured the Kamlet-Taft solvatochromic parameters of several deep eutectic solvents before using them to perform biomass pulping experiments with aspen and pine wood. Compositional analysis of the untreated woods and the treated samples allowed for the determination of lignin and hemicellulose removal achieved by each solvent. Correlations were drawn between the Kamlet-Taft parameter values and the pulping performance metrics, building upon previous work in the literature. Solubilized lignin was recovered from the pulping filtrate for characterization via FTIR, 2D-HSQC NMR, and GPC. The second project focuses on the production of cellulose acetate from aspen wood chips. The wood chips are first pulped under pressurized conditions using 1 L Parr reactor, successfully pulping the chips at lower temperatures and residence times than what has been reported in the literature. Next, in a first of its kind strategy, the deep eutectic solvent pulp was upgraded to 90% cellulose content using a totally chlorine free bleaching sequence. The upgraded pulp was then used as a starting material to synthesize cellulose acetate, a high value bioplastic. Quality metrics of the upgrade pulp and the acetate such as brightness, degree of substitution, and acetone-insoluble gel particle content are being measured using a commercially obtained sample of dissolving pulp produced from aspen and maple wood chips. This work was presented as a poster at the 2024 Graduate/Undergraduate Research Symposium. Autumn Reynolds achieved major advancements in two separate research areas. The first focused on fractionating and purifying various pulps--including US OCC, repulped boxes from the US and South Korea, and unbleached kraft and semichemical hardwood pulps--into dissolving-grade feedstocks. Key outcomes included a validated classification strategy, improved bleaching protocols, and a clearer understanding of how fiber properties like viscosity and particle size can be controlled through fractionation. The second project evaluated the suitability of OCC pulp for use in the Ioncell® process. Rheological assessments, compositional analysis, and dope filtration data demonstrated that selectively purified OCC could yield dopes with promising spinnability, laying the foundation for continuous filament production from recycled fiber sources. Altogether, this work contributed to a peer-reviewed publication, informed a doctoral Preliminary Exam, and established a reproducible experimental pathway for scaling OCC-to-Ioncell processing. Collaborative research across North Carolina State University and Aalto University supported method development and data interpretation, while industry engagement helped contextualize the findings within the broader biobased fiber economy. Isabel Albelo investigated the characteristics of cotton fiber fragments produced by enzymatic degradation of textile waste and the effect of degradation protocols on their potential recycle use. Albelo gained competency in performing enzymatic textile degradation (and instructed graduate and undergraduate students in the process). She performed enzyme assays to enable accurate tracking of enzyme activity over time and incorporate activity measurements into meaningful dosing protocols. Additionally, she performed degradation condition studies (enzyme dosage and experiment time) using commercially available cellulase enzymes to determine the effect on degradation product distribution and fiber fragment properties, especially with respect to incorporation in 3D printing feedstocks. Finally, she utilized gravimetric analysis, Fiber Quality Analysis, and electron/optical microscopy to characterize the fiber fragments produced during enzymatic degradation. Isabel Albelo published a literature review article focusing on the current research and demonstration of all-cellulose 3D printing feedstocks (including types of cellulose used and feedstock formulations, printing methods, post-print solidification and processing techniques, and print properties/applications). She also submitted a research proposal to the Oak Ridge National Laboratory (ORNL) Center for Nanophase Materials Sciences in collaboration with NCSU staff/student (Dr. Sonja Salmon, Dr. Jialong Shen, and Youngwoo Hwang) and ORNL staff scientist (Dr. Yue Yuan).
Publications
- Type:
Peer Reviewed Journal Articles
Status:
Published
Year Published:
2024
Citation:
Sanders, J. H., Cunniffe, J., Carrejo, E., Burke, C., Reynolds, A. M., Dey, S. C., Islam, M. N., Wagner, O., Argyropoulos, D. S. Biobased Polyethylene Furanoate: Production Processes, Sustainability, and Techno?Economics. Advanced Sustainable Systems, 2024
- Type:
Peer Reviewed Journal Articles
Status:
Published
Year Published:
2024
Citation:
Frazier, R. M., Lendewig, M., Vera, R. E., Vivas, K. A., Forfora, N., Azuaje, I., Reynolds, A., Venditti, R., Pawlak, J. J., Ford, E., Gonzalez, R. (2024). Textiles from non-wood feedstocks: Challenges and opportunities of current and emerging fiber spinning technologies. Journal of Bioresources and Bioproducts, Published July 2024
- Type:
Peer Reviewed Journal Articles
Status:
Published
Year Published:
2024
Citation:
Albelo I, Raineri R, Salmon S. Materials and Methods for All-Cellulose 3D Printing in Sustainable Additive Manufacturing. Sustainable Chemistry. 2024
|
Progress 07/01/22 to 06/30/23
Outputs
Target Audience:The target audience of the research includes, but is not limited to, North Carolina State University Wilson College of Textiles, College of Education, and College of Natural Resources, the Sustainable Alternative Fibers Initiative (SAFI), the local community of Raleigh, NC, and rural North Carolina high school students and teachers in STEM. Target audience efforts have provided outreach and collaboration in part with industry partners in the program including Eastman Chemical company and other universities such as Aalto University in Finland. Changes/Problems:The recruitment and onboarding of the two remaining PhD students to the Department of Forest Biomaterials and the Wilson College of Textiles was the only major change that took place during this reporting period. There were no significant problems regarding the recruitment process nor the continuation of research for either of the three students. Obstacles are not anticipated to arise in the following reporting periods. What opportunities for training and professional development has the project provided?The students engaged in several training and professional development opportunities during this period. John Sanders participated in multiple departmental training programs regarding laboratory safety and the proper handling of chemical waste as part of the onboarding process. He has also received informal training in the use of equipment and instruments in the department as well as laboratory procedures such as the NREL biomass compositional analysis method. He has also been given the position of Instrument Lead for the Gel Permeation Chromatograph in which he trains new users and performs regular maintenance on the instrument. Rachel Raineri has also completed training in laboratory safety to the satisfaction of the university and department, as well as in the use of optical microscopy and a laboratory procedure for dry ice making with Arc3 gases in April 2023. Additionally, she has participated in a number of workshops offered by the Graduate School including the Engineering Café's: How to Organize Your Journal Article workshop in August 2022, the Engineering Café's: How to Synthesize Lit Reviews workshop in September 2022, the Engineering Café's Concise Sentences workshop also in September 2022, and the Fall 2022 Virtual Writing Retreat in December 2022. Autumn Reynolds led multiple laboratory demonstrations on paper packaging recycling and property testing with local (North Carolina) middle and high school students interested in the NCSU Paper Science and Engineering B.S. program in collaboration with Eastman Chemical and the Sustaining STEM Career Clubs in Rural North Carolina (USDA) with NCSU's College of Education. She also assisted leading laboratory training in the Hands-On Workshop for Pulp and Paper Basics Short Course sponsored by TAPPI at NCSU in October of 2022. Reynolds received training on hazardous unwanted material disposal following the NCSU EHSA standard procedures and began managing two laboratories material disposal. She also mentored three NCSU undergraduate work-study need-based students (B.S. Biology, B.S. Sustainable Materials and Technology, B.S. Paper Science and Engineering/ Chemical Engineering) for roles as undergraduate research assistants she created with support of her primary advisor. How have the results been disseminated to communities of interest?Research results have been disseminated to communities of interest through formal and informal verbal conversations, presentations, and training, both in-person and remotely. Multiple discussions and informal presentations to the target audience were given by students about the research topics of the processing various raw materials into dissolving-grade pulp, processing biomass using dep eutectic solvents, and producing textile grade fibers from soy cellulose. John Sanders presented research findings and reviews of relevant literature in one-on-one meetings with his advisor and to the rest of his research group. Sanders also presented a poster describing his experimental proposal for the study of deep eutectic solvents at the NC State College of Natural Resources Research Symposium in March 2023 and prepared a research-based proposal which was presented to the satisfaction of second Qualifying Exam of the Department of Forest Biomaterials in May 2023. Rachel Raineri gave informal weekly presentations to her industry partner, R5 Labs as well as a presentation to members of the Department of Chemistry at North Carolina State University to introduce a collaborative project. Autumn Reynolds attended the 2023 Sustainable and Alternative Fibers Initiative ConsortiumBoard Meeting in January 2023. She also presented research at the NCSU College of Natural Resources Graduate Student Research Symposium, remotely to members of the Sustainable Biomaterials and Packaging Society of Auburn University, and to graduate students of the Bioproducts and Biosystems Department in the College of Chemical Engineering at Aalto University. What do you plan to do during the next reporting period to accomplish the goals?Goals will be accomplished during the next reporting period by creating and following a timeline of experimental research and publishing. The students will also collaborate/interact with the other Fellows from the NNF program as well as other institutions. Classes and informal research training will continue.
Impacts
What was accomplished under these goals?
The remaining two PhD positions were filled during this period. John Sanders was recruited to the Department of Forest Biomaterials in August 2022 to work under the advisement of Dr. Sunkyu Park and Dr. Richard Venditti. Rachel Raineri was recruited to the Wilson College of Textiles in August 2022 as a dual-enrolled masters and PhD student in the Textile Engineering and Fiber and Polymer Science programs, respectively, under the advisement of Dr. Sonja Salmon. John Sanders successfully performed preliminary experiments for a proposal submitted to the US Department of Energy in January 2022 with the goal of reducing carbon emissions from the pulp and paper industry. Sanders optimized reaction conditions for the preparation of dissolving pulp from lignocellulosic biomass using deep eutectic solvents (DES). He has since continued to study the fundamental properties of DES and how they translate to reactivity in biomass pretreatment applications while completing coursework with a 4.00 GPA. Rachel Raineri's research focus is the development of cellulose carbamate as an alternative to cellulose xanthate in the textile industry. She is investigating the use of DES as a reaction medium for the carbamation of soy cellulose to produce textile-grade cellulose carbamate fibers. To this end, she has investigated the thermal properties of DES and has characterized reaction products resulting from the carbamation reaction using various analytical methods. Raineri has also completed her MS in Textile Engineering as of May 2023. The goals of Autumn Reynolds's research are focused on the upgrading of waste and recycled fibers in value-added bioproducts for packaging and textile applications that traditionally utilize petroleum-derived materials. A manuscript draft is nearing completion on using fiber physical and chemical fractionation as a means of pre-treatment of formic acid pulping to upgrade US and Korean sourced old, corrugated containerboard (OCC) fibers into low-grade high yield dissolving pulp. Reynolds also joined a collaboration project with Eastman Chemical company on a project assessing various treatment methods of OCC to upgrade into high quality (acetate grade) dissolving pulp. A research collaboration began with Aalto University (June 5 - September 2, 2023) to convert OCC pulp into precursor filaments via Ioncell®-F technology, then carbon fibers on a continuous biomass pyrolysis line.
Publications
|
Progress 07/01/21 to 06/30/22
Outputs
Target Audience:The target audience of the research includes, but is not limited to, North Carolina State University Wilson College of Textiles, College of Education, and College of Natural Resources, the Sustainable Alternative Fibers Initiative (SAFI), the local community of Raleigh, NC, and rural North Carolina high school students and teachers in STEM. Target audience efforts have provided outreach and collaboration in part with industry partners in the program including Westrock from Roanoke, VA, and Greif from Amherst, VA. Changes/Problems:A major challenge with this research is the lack of reported literature on successful purification processes specific to old, corrugated containerboard (OCC) for dissolving-grade pulp products and applications. Moreover, dissolving-grade pulp has strict products requirements, and old corrugated containerboard is a material latent with contaminants and variable chemistries. Thus, much of this time was focused on learning to properly characterize relevant properties of the starting and end product. A change in the upcoming reporting period is that the student will move from primarily reviewing literature and planning to actively experimenting and reporting data from laboratory studies over this reporting period. Less emphasis will be on network development and more on major and minor products/outputs from manuscripts to posters, as well as conference presentations of research results. What opportunities for training and professional development has the project provided?Professional development opportunities that the student was able to achieve not listed elsewhere in this document include a visit to a pulp mill to see process of lignocellulosic biomass pulping (International Paper in New Bern, North Carolina), and attendance at the following conferences and/or events: 2021 Hands On Workshop for Pulp and Paper Basics by NCSU and TAPPI, 2022 TAPPI Convention, Young Professional Workshop, and Women in Industry Summit, and Evolving Textiles Conference 2022. The student worked with faculty in the Forest Biomaterials department to initiate the creation of a work-study need-based lab position. The student now advises an employed work study undergraduate student from the Sustainable Materials & Technology program at NCSU in effort to practice mentorship to need-based students. How have the results been disseminated to communities of interest?Research results have been disseminated to communities of interest through formal and informal verbal conversations, presentations, and trainings, both in-person and remotely. What do you plan to do during the next reporting period to accomplish the goals?Goals will be accomplished during next reporting period by creating and following a timeline of experimental research and publishing. The student will also collaborate/interact with the other Fellows from the NNF program. Classes and informal research training will continue. The two remaining PhD positions will be filled, and those students will begin the process of research and experimentation as well as completing relevant course work within their respective programs.
Impacts
What was accomplished under these goals?
Student achieved high success in relevant graded courses related to research area (GPA = 3.88) and developed a professional network of resources based on the target audiences. For further training, student attended the 2021 Pulp and Paper TAPPI Short Course, USDA High School Teachers Training for STEM labs, and learned how to operate and report data from multiple standardized procedures and lab equipment (analytic and process). Student also learned the full NREL procedure on the compositional analysis of biomass. Student took leadership on performing repulpability and recyclability testing in collaboration with industrial partners. For community outreach, and in promotion of scientific communications to underrepresented communities, student spoke with multiple high school teachers and their classes for 60 minutes via Zoom (remotely) about her journey entering a career path in the sustainable bioeconomy, and about the processes and implications of current research topic joined by NCSU College of Education post-doc scholar and USDA fellow Katie McCance. Recruitment efforts were made to fill the two remaining PhD positions. As a follow-up to a topical presentation via Zoom at the September 2021 Fast Fashion FrenZy event hosted by the UNC-Charlotte chapter of the Zeta Phi Beta Sorority, Inc. (https://zphib1920.org/), a historically African American sorority, Dr. Salmon promoted the open PhD student positions for the NC State USDA NNF program to the chapter secretary in February 2022. The information was disseminated but no applicants arose at that time. Dr. Park and Dr. Venditti reached out to prospective candidates via email in March 2022 and held interviews via ZOOM.
Publications
- Type:
Journal Articles
Status:
Accepted
Year Published:
2022
Citation:
Szlek, D. B., Reynolds, A. M., & Hubbe, M. A. (2022). Hydrophobic Molecular Treatments of Cellulose-based or Other Polysaccharide Barrier Layers for Sustainable Food Packaging: A Review. BioResources, 17(2).
- Type:
Journal Articles
Status:
Submitted
Year Published:
2022
Citation:
Van Schoiubroeck, S., Chacon, L., Reynolds, A., Lavoine, N., Hakovirta, M. Gonzalez, R., Van Passel, S., Venditti, R. A. (2022) Environmental sustainability perception toward obvious recovered waste content in paper-based packaging: an online and in-person survey best-worst scaling experiment, submitted Resources, conservation and recycling journal.
|