Progress 08/01/22 to 07/31/23
Outputs
Target Audience:Target audiences include the scientific community interested in understanding different sustainable compostable materials formulations involving polysaccharide polyelectrolyte complexes and barrier materials made from these useful for packaging and food handling applications; individuals associated with companies which can also include scientists and engineers, as well as individuals involved in business, marketing, and management, who wish to understand, and help guide the development of, practical sustainable packaging and food handling product solutions; and students of all ages and backgrounds participating in extension or resident education programs to learn about food packaging and handling technologies and products. Changes/Problems:We requested an extension to complete the work proposed, submit a patent on the new materials developed and publish several papers, some held back now until the patent can be submitted. We also are working with the extension team to develop and deliver quality educational modules in the packaging space. The main delay we experienced was in the development of a process to produce the modified celluloses. We wanted to start with a process that was the most sustainable so we explored more ecologically friendly solvent systems. These did not work well and we discovered that this was a project itself and had to move on to develop and demonstrate the material to determine if we had an improved barrier before optimizing every aspect of its sustainability. This caused a roughly 1.5 semester delay. What opportunities for training and professional development has the project provided?Throughout this project, various opportunities have emerged: The chance to work with different companies and gain a better understanding of the real needs on an industrial scale, troubleshooting the product applications based on the specific needs of each company. This project has also provided many entrepreneurial opportunities for us. Over the past three years, Parisa has successfully pursued a minor in Engineering Leadership and Innovation Management (ELIM) from Penn State. In addition to this, she has been able to participate in the national entrepreneurship programs of VentureWell (first and second stages) and win a total of $25,000 in awards. As a result of working on this project, we've been offered to collaborate with the Chesapeake Bay Foundation on their 10 million trees initiative to help them find sustainable materials for their grow tubes instead of plastic ones currently being used. Because this collaboration was very successful, our work was featured in Penn State's News articles and College of Agriculture at Penn State's News articles. How have the results been disseminated to communities of interest?Due to the interesting goal of this project, a lot of opportunities have come up for our research group lab and especially for the Ph.D. student, Parisa Nazemi who is directly working on this project. Every semester she has had the opportunity to train groups of undergraduate students about sustainability topics, their importance, and the potential applications of this specific project. A report was of our research lab and the efforts on replacing plastic were covered in the local CBS 21 NEWS highlighting two of our Ph.D. students' research topics. Parisa was also one of the speakers at the Global Sustainability Action: It Starts with Us conference held in November 2022 to talk about the new technologies developed for the production of sustainable materials. As a sustainability specialist, Parisa collaborated with the Chesapeake Bay Foundation (CBF) and a company, Plantra, to help use sustainable materials in the process of CBF's 10 million trees initiative during the summer of 2022. What do you plan to do during the next reporting period to accomplish the goals?Extension and outreach plans We are already working with several companies under Penn State NDA. In the near future, a recently optimized starch-based PPC will be ready to send to these companies for their testing, potentially followed by licensing the technology from Penn State. As part of the outreach program, the course modules are being prepared in transcript form, then they will be recorded in the Penn State recording studios with the Instructional Designers' support. Technical plans The next phase of the work will be about replicating the positive results we achieved so far, at a larger scale.We plan to complete and optimize the preparation of cationic and anionic celluloses; complete their characterization including NMR, FTIR, and Elemental analysis, and prepare films and paper coatings and characterize including barrier performance and mechanical properties. We will also continue to support existing and new industry interactions where we prepare formulations and test for specific product applications. We will also prepare formulations for the specific paper used in food handling in major restaurant chains as described herein. If grease barrier performance is acceptable, we will approach McDonald's and other chains with the aid of Doug Peck in an effort to eliminate PFAS paper products.
Impacts
What was accomplished under these goals?
Accomplishments pertaining to extension and education goals The extension program was expanded in the number of companies we work with and reshaped the format of our educational goals. Over the past 6 - 9 months, we found new companies to work with, some to provide us with their anionic and cationic starches to test and characterize for specific applications of polysaccharide polyelectrolyte complexes (PPCs) and some to provide us with their paper samples of pristine paper and PFAS coated paper to do a comparison between PPC coating and PFAS coating while keeping the paper specs constant. This way, we have become the bridge between the starch companies and paper companies by first, providing science-proved technologies to replace their current non-sustainable practices, and second, introducing new applications of their products (starches) which will open up a new horizon in the sustainable product developments. Concerning the education goals and accomplishments, our collaboration with Dr. Cutter and Mr. Doug Peck (packaging expert) led to planning for creating an online course on the department of Food Science's Extension website. The audience for this course is set to be food industry professionals and/or food industry employees with food packaging responsibilities. Mr. Peck is working on modules (approximately 60 min in length) to address glass, paper, plastic, and flexible packaging. Our Ph.D. student, Parisa Nazemi is working on two modules covering the topic of active packaging (including antimicrobial, smart, intelligent, gas scavenging, moisture control, anti-oxidation, and temperature control), and the future of packaging (what's new and innovative). Next, our instructional designer (ID) for Extension recommends breaking up the modules into 4, 15 min sections per topic with 3-5 questions after each section to assess learning knowledge. The content will be first delivered in a written transcript to the instructional designer, and with their input, the content will be recorded and the videos will be captured to create the course and to maximize engagement. Accomplishments pertaining to the formulation and product development During this part of our experimental work, the goal is to synthesize anionic and cationic celluloses with an optimized degree of substitutions from cellulose fibers. To accomplish this goal, we used cellulose powder and produced Carboxymethylcellulose (CMC) and Quaternized cellulose (QC) with different degrees of substitution by changing parameters including the solvent system, cellulose form (pulp, powder), and cellulose concentration. Later, FTIR and NMR methods were used to analyze the products and verify the modifications. The next step is to optimize the mixing ratio of CMC and QC and measure the quality of the obtained polysaccharide polyelectrolyte complex films. Although different samples showed different results, promising results were obtained by mixing concentrated CMC and QC, forming a transparent film. However, the challenge was to make the materials in a larger quantity so that the films could be tested for various analyses including mechanical tests, water vapor permeation tests, grease resistance tests, hydrophobicity tests, etc. To do so, an experiment with cellulose concentration of 6% w/w, instead of 1%w/w, took place and showed a lower degree of a substitute and thus made the products insoluble in water meaning a film could not be formed in the end. To fix this issue, a lower cellulose concentration is going to be tested for successful film formation and subsequent analyses. This optimization will be finished over the next semester. Here are a few of the sample results when characterizing the synthesized products. 1H NMR spectrum of quaternized cellulose (QC) dissolved in Deuterium (D2O) ? 1C NMR spectrum of carboxymethylcellulose (CMC)dissolved in Deuterium (D2O)
Publications
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Progress 08/01/21 to 07/31/22
Outputs
Target Audience:Target audiences include the scientific community interested in understanding different sustainable compostable materials formulations involving polysaccharide polyelectrolyte complexes and barrier materials made from these useful for packaging and food handling applications; individuals associated with companies which can also include scientists and engineers, as well as individuals involved in business, marketing, and management, who wish to understand, and help guide the development of, practical sustainable packaging and food handling product solutions; and students, scientists, engineers, people from industry and the pubic participating in extension or resident education programs to learn about food packaging and handling technologies and products. Changes/Problems:There have been no major changes beyond what was reported in the past. The most significant challenge we faced in this project to date was an initial effort to produce anionic and cationic celluloses using a modified process that employed fewer chemicals with the aim of increasing the sustainability of the manufacturing process from the start. This delayed progress up front, but has helped the work overall. We believe that researchers need to consiuder the entire life-cycle of the technologes and products they are developingfrom the start of the program, even in the concepotualization stage. What opportunities for training and professional development has the project provided?Due to the interesting goal of this project, a lot of opportunities have come up for our research group lab and especially for the Ph.D. student, Parisa Nazemi who is directly working on this project. Every semester she has had the opportunity to train groups of undergraduate students about sustainability topics, their importance, and the potential applications of this specific project. A report of our research lab and the efforts on replacing plastic were covered in the local CBS 21 NEWS highlighting two of our Ph.D. students' research topics. Parisa was also one of the speakers at the Global Sustainability Action: It Starts with Us conference held in November 2022 to talk about the new technologies developed for the production of sustainable materials. As a sustainability specialist, Parisa collaborated with the Chesapeake Bay Foundation (CBF) and a company, Plantra, to help use sustainable materials in the process of CBF's 10 million trees initiative during the summer of 2022. How have the results been disseminated to communities of interest?Results have not been dissemainted beyondwhat was mentioned above. What do you plan to do during the next reporting period to accomplish the goals?Extension and outreach plans We are already working with several companies under Penn State NDA. In the near future, a recently optimized starch-based PPC will be ready to send to these companies for their testing, potentially followed by licensing the technology from Penn State. Once a final cellulose PPC production process has been established, we will work with our existing and new industrial partners to begin translating this technology to the market. As part of the extension education program, the course modules are being prepared in transcript form, then they will be recorded in the Penn State recording studios with the Instructional Designers' support and disseminated using the Penn State on-line extension site. Technical plans We plan to complete and optimize the preparation of cationic and anionic celluloses, complete their characterization using NMR, FTIR, and elemental analysis, and prepare films and paper coatings and characterize their barrier performance and mechanical strength. We will also continue to support existing and new industry interactions where we prepare formulations and test for specific product applications. We will also prepare formulations for the specific paper used in food handling as described herein and will approach several of the major global restaurant chains with the aid of Doug Peck in an effort to eliminate PFAS paper products.
Impacts
What was accomplished under these goals?
Accomplishments pertaining to extension and education goals The extension program was expanded in the number of companies we work with and reshaped the format of our educational goals. Over the past 6 - 9 months, we found new companies to work with, some to provide us with their anionic and cationic starches to test and characterize for specific applications of polysaccharide polyelectrolyte complexes (PPCs) and some to provide us with their paper samples of pristine paper and PFAS coated paper to do a comparison between PPC coating and PFAS coating while keeping the paper specs constant. We have become a bridge between starch companies and paper companies by providing scientifically proven materials and coating technologies to replace their current non-sustainable barrier coatings. Concerning our educational goals, our collaboration with Dr. Cutter and Mr. Doug Peck (packaging expert) led to planning an online course to be delivered via the department of Food Science's Extension website. The audience for this course is set to be food industry professionals and/or food industry employees with food packaging responsibilities. Mr. Peck is working on modules (approximately 60 min in length) to address glass, paper, plastic, and flexible packaging. Our Ph.D. student, Parisa Nazemi, is working on two modules covering the topic of active packaging (including antimicrobial, smart, intelligent, gas scavenging, moisture control, anti-oxidation, and temperature control), and the future of packaging (what's new and innovative, including this work). We continue to work with PSU's Instructional Designer (ID) for Extension who has provided guidance on the format for these modules. We are working on a written transcript, and with their input, the content will be recorded and videos will be captured to create the course. Accomplishments pertaining to the formulation and product development The goal of this phase of our experimental work is to synthesize anionic and cationic celluloses with an optimized degree of substitutions from cellulose fibers. To accomplish this goal, we used cellulose powder and produced Carboxymethylcellulose (CMC) and Quaternized cellulose (QC) with different degrees of substitution by changing parameters including the solvent system, cellulose form (pulp, powder), and cellulose concentration. Later, FTIR and NMR methods were used to analyze the products and verify the modifications. The next step is to optimize the mixing ratio of CMC and QC and measure the quality of the obtained polysaccharide polyelectrolyte complex films. Although different samples showed different results, promising results were obtained by mixing concentrated CMC and QC, forming a transparent film. However, the challenge was to make the materials in a larger quantity so that the films could be tested for various analyses including mechanical tests, water vapor permeation tests, grease resistance tests, hydrophobicity tests, etc. To do so, an experiment with cellulose concentration of 6% w/w, instead of 1%w/w, took place and showed a lower degree of a substitution and thus made the products insoluble in water meaning a film could not be formed in the end. To fix this issue, a lower cellulose concentration is being tested for successful film formation and subsequent analyses. This optimization will be finished over the next semester. Here are a few of the sample results when characterizing the synthesized products. 1H NMR spectrum of quaternized cellulose (QC) dissolved in Deuterium (D2O) 1C NMR spectrum of carboxymethylcellulose (CMC)dissolved in Deuterium (D2O)
Publications
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Progress 08/01/20 to 07/31/21
Outputs
Target Audience:Target audiences include the scientific community interested in understanding different sustainable compostable materials formulations involving polysaccharide polyelectrolyte complexes and barrier materials made from these useful for packaging and food handling applications; individuals associated with companies which can also include scientists and engineers, as well as individuals involved in business, marketing and management, who wish to understand, and help guide the development of, practical sustainable packaging and food handling product solutions; and students of all ages and backgrounds participating in extension or resident education programs to learn about food packaging and handling technologies and products. Changes/Problems:The only change in the program involves the extension outreach component where we have shifted to a remote delivery approach. Also, rather than having a remote workshop that brings many companies together at one time, we have been pursuing a one-on-one approach. In the event that the COVID-19 pandemic eases, we may change again to in-person group events. What opportunities for training and professional development has the project provided?A Ph.D. student Parisa Nazemi has been hired to work on this program and has taken a semester of classes in Fall 2020. She is being actively mentored and has expanded her Ph.D. program to include the PSU Engineering Leadership and Innovation Minor. Parisa is a very enthusiastic student who is interested in a career in developing and commercializing sustainable materials. This graduate minor will aid her in achieving those goals. Parisa has also expressed an interest in ethics and ethical leadership and her program of study is being shaped to provide her with relevant experience. How have the results been disseminated to communities of interest?Results achieved prior to this grant have been the starting point as we develop new formulations as proposed. These results have been disseminated to individual companies under a PSU NDA. What do you plan to do during the next reporting period to accomplish the goals?Extension and outreach plans We plan to continue interacting with new companies on a one-on-one basis to help them commercialize sustainable packaging and food handling products. We also plan to continue our work with Doug Peck on the new extension course offering for industry professionals. Technical plans We plan to complete and optimize the preparation of cationic and anionic celluloses; complete their characterization; and prepare films and paper coatings and characterize. We will also continue to support existing and new industry interactions where we prepare formulations and test for specific product applications. We will also prepare formulations for the specific paper used in food handling in major restaurant chains as described herein. If grease barrier performance is acceptable, we will approach McDonald's and other chains with the aid of Doug Peck in an effort to eliminate PFAS paper products. Changes The only change in the program involves the extension outreach component where we have shifted to a remote delivery approach. Also, rather than having a remote workshop that brings many companies together at one time, we have been pursuing a one-on-one approach. In the event that the COVID-19 pandemic eases, we may change again to in-person group events.
Impacts
What was accomplished under these goals?
Accomplishments pertaining to extension and education goals The extension program is still undergoing substantial changes because of the COVID-19 pandemic. It is transitioning to a fully remote delivery platform and is no longer providing in-person educational programs. Even with the decline in COVID cases, remote delivery is still expected to continue to be the predominant program delivery mode. Extension educators continue to modify or remake programs to accommodate remote delivery. Rather than wait for this transition, the extension based outreach and education activities have been adjusted. The company workshop has been replaced with one-on-one interactions. Several companies have been engaged under NDA agreements. In addition, a food packaging industry expert Doug Peck has been engaged. Mr. Peck has been working in the food packaging industry since 1987 (ConAgra Foods and Silgan Containers). Recently Mr. Peck has made an important contribution to this program. Mr. Peck identified an important product application for our technology that the PIs were unaware of: the replacement ofper- and polyfluoroalkyl substances (PFAS) that are used extensively on paper food handling products (paper wrappings and paperboard containers for French fries, burgers, etc.) in all major food chains. The removal of these surface coatings is one of the highest priorities for this industry. We added this to our program and under his guidance are working to prototype a coating for these applications. Mr. Peck has worked with McDonalds, Wendy's, Burger King and other chains and is willing to help us work with them when we have needed performance data. Mr. Peck, along with Dr. Cutter, is working on a new course tentatively entitled "Introduction to Food Packaging", which will be an online extension course for food industry professionals. It will also be offered as a part of the Food Science Certificate Program. Dr. Catchmark and the graduate student involved in the program will participate in this course and provide content on emerging sustainable packaging materials including the work being done in this program. Accomplishments pertaining to formulation and product development A new Ph.D. engineering student, Parisa Nazemi, stared in this program in Fall 2020. She has B.S. and M.S. degrees in chemical engineering. During the fall semester, Parisa received all essential training to begin her work in the lab and began producing standard formulations and coating samples. The bulk of the work in the Fall semester was focused conducting a literature search focused on all known processes for imparting cationic and anionic functional groups onto cellulose. Based on this search, a preliminary process was developed for producing a cationic cellulose and an anionic cellulose to be used in new barrier coating formulations. The anionic group is an acid group and the cationic group is aquaternary ammonium salt. In Spring and Summer 2021, this process was demonstrated experimentally and is still under optimization. See details below. Coatings based on starches, carboxymethyl cellulose and chitosan were prepared for 2 companies (NDA in place). One was very successful and the company is negotiating a license to commercialize the material. The first full volume production run is expected as early as September. This was a final goal of this program and is happening 2 years ahead of schedule. We have also obtained paper substrates used in food handling containing PFAS coatings. We have generated preliminary data suggesting that our polysaccharide barrier coating is superior to PFAS coatings and are looking for company partners to develop new food packaging and handling products in this space. Current process for making cationic and anionic celluloses Cellulose pulp preparation Part of the cellulose processing in making the cellulose paper into the form of pulp sheets. To do so, cellulose filter papers were cut into 5 mm x 5 mm sizes and dispersed into DI water to make 1% w/v dispersions. The dispersion was stirred over the hot plate at room temperature for 7 days. After cellulose fibers were uniformly dispersed into water, the dispersion was then transferred into aluminum trays and kept at - 80°C overnight. The frozen dispersions were then freeze-dried over a week and sealed in packages for further use. Cellulose Mercerization (Alkali cellulose) Cellulose is naturally in the form of Cellulose I, which is highly crystalline and thus it has a low rate of reactivity. In order to increase the cellulose reactivity, it is mercerized to decrystalize. A solution of 18% w/v sodium hydroxide was made from sodium hydroxide pellets. Cellulose and NaOH solution were mixed in 0.5% solids loading. The mixture was blended via ultrasonication at 100 Watts power for 30 minutes. The mercerized cellulose was then filtered using a centrifuge at 6000 rpm for 10 minutes at room temperature. Three samples were taken from the pulp for further XRD analysis and to measure the crystallinity of the mercerized cellulose. 3. Cellulose Carboxylation Cellulose carboxylation is done to make anionic cellulose, a negatively charged polyelectrolyte for further reactions. The purpose here is to make carboxylated cellulose with a DS of higher than 0.5. Monochloroacetic acid (MCA) (98%) and isopropyl alcohol (IPA) (99%) were used in the following process. The alkali cellulose was added to IPA in the 1:20 ratio in a round flask connected to a condenser. The temperature was raised to 60°C and 2 g MCA/ g cellulose was then added, and the mixture was kept stirring for 5 hours. After the reaction was completed, the flask was cooled down to room temperature the mixture was neutralized with 10% glacial acetic acid, then centrifuged to separate the solid and liquid. Both parts were mixed with an excess amount of methanol (~200 ml) to precipitate the carboxylated cellulose. The mixtures were transferred to the dialysis tubes for 3 days and freeze-dried to get the dried product. The dried sample was dissolved in the water later to test the water solubility. 4. Cellulose Quaternization Quaternization of alkali cellulose is done for the purpose of producing positively charged polyelectrolytes. This process could be done by different paths and reagents, however, the use of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHPTAC) is one of the most common methods. The alkalized cellulose was taken from the mercerization step and mixed in a flask with CHPTAC and IPA in a 1:8:8 ratio (cellulose: CHPTAC: IPA). The flask was connected to a condenser and was stirred at 70°C for 5 hours. After the reaction time, the mixture was cooled down to room temperature and neutralized with 10% glacial acetic acid. The product was then centrifuged at 6000 rpm for 10 minutes at 25°C. The solid was then dissolved in DI water and transferred into dialysis tubes for 7 days. The samples were then freeze-dried and kept for further use. XRD, FTIR and NMR analyses are underway, and films/coatings using these functionalized celluloses will be created shortly and tested for solubility and barrier performance.
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