Brief Summary of Minutes of Annual Meeting

S-1054 Multistate Cooperative Research Project Annual Meeting Minutes

Friday, October 30, 2015

Room 2115, College of Textiles, Centennial Campus

North Caroline State University, Raleigh, North Carolina.

Members Attending:

You-Lo Hsieh, Anil Netravali, Yiqi Yang, Majid Sarmadi, Suraj Sharma, Jonathan Chen, Karen Leonas, Sergiy Minko, Chunhui Xiang, and Yan Vivian Li.

1. The meeting began with a telephone call to the project's Administrative Advisor Dr. Robert Shulstad.

Dr. Shulstad commented that President's order to extend debt ceiling for 2 years would increase funds to Ag appropriation committee including funding for competitive research grants, in particular for multi-discipilinary and multi-institutional CAP projects in FY 2016 and FY2017, where priority in call for proposal may alter.

Dr. Shulstad asked if anyone received USDA grants this year and recommended the team to visit panel directors between now and Feb regarding relevant funding areas in FY 2017 budget. Dr. Shulstad also encouraged members to communicate to the private sector to contact their elective congressional members to generate support in the related areas. We were reminded that an annual report is due in 60 days from today's meeting. 

2. The meeting was called to order at 12:40 pm. Chair You-Lo Hsieh welcomed everyone and thanked Karen Leonas for taking care of room and lunch arrangement. All attending members self-introduced over box lunch and discussed the timing of annual report. The Chair and Secretary for 2016 was discussed and Suraj Sharma (UGA) and Yan Vivian Li (Colorado State) were voted in for the respectively positions. Individual reports will be submitted to Suraj Sharma by Thanksgiving to allow time for revision and edit by the group for submission by end of December.

3. Research station report: Station reports from committee members started at 1 pm and ended at 3:30 pm with brief Q&A and discussions at the end of each. Please see the consolidated annual report. 

4. Further discussions also included collaboration, capability and institution facility and funding for research. Interest to visit USDA NIFA panel directors were unanimous. Location for 2016 meeting was discussed. UGA and Cornell were viewed favorably for meeting team's Administrative Advisor Dr. Robert Shulstad and teaming again with Fall Fiber Society meeting, respectively.

 Respectfully submitted,

Suraj Sharma

(Secretary)

About the S-1054 Project

This multi-state research project addresses the nation’s research priority in bioenergy and biobased products by developing renewable fibrous materials and innovative technologies for eco-friendly and sustainable textile products that have an impact on improving the environment and quality of living. Four research objectives are defined: (1) to develop novel biobased polymeric materials; (2) to develop and evaluate biobased fibrous products for eco-friendly crop protection; (3) to develop and evaluate biobased products for health and safety applications; and (4) to develop and evaluate methods to remove dyes and finishing chemicals from textile waste water. The research progress is made through cooperation among the participants from nine universities in the states of CA, GA, MT, NE, NY, TN, TX, WA, and WI.

Progress

Objective 1

The University of Nebraska-Lincoln (NE) continued its development of biofibers from agricultural by-products, co-products and wastes for use in textiles, composites and medical applications. One focus was on the development of natural cellulosic fibers from corn husks with high aspect ratio for high quality applications in textiles and composite reinforcement. Another focus was on the continued development of nanofibers and nanoparticles from proteins for medical applications. Improving properties of polylactide from the molecular level was continued through the study of PLLA-PDLA interlocked structure for better textile applications for PLA. 

One major breakthrough included the development of a non-toxic crosslinking system, using polycarboxylic acids and oxidized sucrose for starch, proteins and other biomacromolecules. This non-toxic crosslinking system provides possibilities for food, food packaging, and biobased materials. It also provides opportunities to develop non-toxic systems for hair setting and perming.

Cornell University (NY) has developed a microcapsule based self-healing soy protein isolate (SPI) resin. SPI consists of over 90% polypeptide chains with reactive amino acid residues. It is an abundant and inexpensive renewable natural resource used in many applications in recent years including preparation of biodegradable materials, such as adhesives, plastics, binders, and resins. Pure SPI, in resin form, is very brittle and can crack easily under tension. This reduces its useful life significantly.  Poly(D,L-lactide-co-glycolide)(PLGA) microcapsules (average diameter 778 nm) containing SPI, as the healant, were prepared and characterized. The microcapsule preparation technique used in this study resulted in encapsulation efficiency of up to 89% and protein loading of up to 44%. Adding SPI-PLGA microcapsules to the green thermoset SPI resin containing glutaraldehyde was found to be successful in healing the microcracks created after tension loading. The SPI resin containing 15 wt% microcapsules and 12 wt% glutaraldehyde showed self-healing efficiency of approximately 50%. The results showed that the SPI released from SPI-PLGA microcapsules can easily react with the excess glutaraldehyde present in the resin as soon as they come in contact and bridge the two fracture surfaces. These results show that it is possible to extend the life of green, soy protein based thermoset resin by incorporating self-healing SPI-PLGA microcapsules.

In another study at Cornell University, mango seed starch (MSS) was extracted from defatted mango seed kernels and crosslinked using a ‘green’ crosslinker/catalyst system, 1,2,3,4-butane tetracarboxylic acid (BTCA)/sodium propionate (NaP), to obtain the thermoset resin. Sodium hypophosphite (SHP) is a widely used catalyst for esterification using polycarboxylic acids and hydroxyl groups of starch or cellulose.  Effluents polluted with SHP, also containing phosphorous, are toxic to humans and can adversely affect the fauna in water. Results indicate that sodium propionate (NaP), used as a non-phosphorous green catalyst, is as effective and efficient as SHP. The crosslinking of starch was confirmed directly using ATR-FTIR spectra and the degree of substitution (DS) values obtained by chemical titrations as well as indirectly from the tensile properties. Higher modulus and strength, resulting from higher DS values and lower degree of swelling in water, confirmed that NaP acts as a better catalyst than the conventional SHP. Higher crosslinking also results in lower moisture absorption by the starch films increasing its potential application as biobased resin. The properties of the crosslinked MSS, strength of about 13 MPa and modulus of about 1.2 GPa, were found to be comparable to some petroleum based resins as well as edible starch based resins, e.g., potato, corn, or proteins such as soy.

The University of Georgia (GA) has continued work on developing a biodegradable bioplastic alternative to petroleum based plastics—microbial polyhydroxyalkanoates (PHAs).  PHAs are already being produced commercially via bacterial fermentation processes.  Because PHAs have to compete economically with petroleum-based polymers, the development of low-cost production strategies on the basis of diverse renewable materials is a crucial challenge.  Photoautotrophic cyanobacteria could provide a competitive alternative to bacteria for PHA synthesis. The cyanobacterial biosynthesis process may have an edge over the bacterial fermentation process, because cyanobacteria naturally produces PHAs, under stress conditions, by photosynthesis and requires fewer resources for growth and biomass production. As a result, the University of Georgia performed a pilot study to investigate the extraction and characterization of the biosynthesized polyhydroxybutyrate (PHB) from three oxygenic diazotrophic cyanobacterial species—Nostoc muscorum, Anabaena variabilis and Anabaena flos aquae. The average intracellular accumulation was 10% (dry cellular weight). A. flos aquae produced ~26% (dry cellular weight). The extracted PHB has comparable mechanical and chemical properties. Based on the cellular adherence and proliferation characteristics of the microalgal PHB, it can be used as a viable substrate in biomedical applications such as sutures and woven/knitted bandages for wound healing and scaffolds for tissue engineering.

The University of Texas at Austin (TX) studied a new approach for spinning micron-scale regenerated cellulose fiber.  Two types of ionic liquid, 1–butyl–3–methylimidazolium chloride (BMIMCl) and ionic liquid 1-ethyl-3-methylimidazolium acetate (EMIMAc), were used as new solvent systems for preparing the cellulose solutions. Comparison was carried out with respect to ionic liquid dissolubility, cellulose solution spinnability, and properties of regenerated cellulose micron-fiber produced with each ionic liquid solvent. The experimental fibers were characterized in terms of fiber diameter, strength, thermal property, crystallinity, and content of solvent residual by using tensile testing, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), X-ray diffraction (XRD), and mass spectrometry. The study concluded that there was a significant difference in the fiber tensile strength between the BMIMCl-generated fiber and the EMIMAc-regenerated fiber.  For the fiber crystal size, crystal orientation, and crystallinaty index, the BMIMCl-generated fiber had higher values than the EMIMAc-regenerated fiber. For the thermal property, the EMIMAc fiber was more stable at higher temperatures than the BMIMCl fiber. It was also revealed that the EMIMAc fiber had significantly less solvent residual content than the BMIMCl fiber.

Research progress was also made on the use of the ionic liquid for producing regenerated cellulose nanofiber nonwovens which could be used as a biocompatible and biodegradable biomaterial for tissue scaffolds. The cellulose was dissolved in the ionic liquid solvent BMIMCl. Then the nanofiber webs were spun and tested for tensile properties. A bioassay using HL-1 cells was conducted to determine cytotoxicity of the nanofiber webs produced from three different types of cellulose source. The study has shown that the cellulose nanofiber nonwovens featured a biocompatibility and non-toxicity desired for scaffold fabrication. The method of electrospinning was capable of making regenerated cellulose nanofiber nonwovens with dense structure and substantial tensile strength ensuring the biomaterial processability and durability. The fineness of nanofiber was identified in the range of 500-5000 nm.

At the University of California, Davis, (CA) scientists have derived highly crystalline nanocellulose from under-utilized agricultural by-products, including rice straw, cotton linters, grape skins and tomato peels. Pure cellulose isolated from tomato peels by either acidified sodium chlorite or chlorine-free alkaline peroxide routes was hydrolyzed (64% H2SO4, 8.75 mL/g, 45 °C, 30 min) into negatively charged (ζ=-52.4 mV, 0.48 at% S content) and flat spindle shaped (41:2:1 length:width:thickness) cellulose nanocrystals (CNCs). While CNCs could be facilely assembled into ultra-fine (f=260 nm) and highly crystalline (80.8%) fibers from dilute aqueous suspensions, narrower (f=42 nm) and mesoporous (0.4 m3/g) nanofibers could be assembled from CNCs in 1:1 v/v tert-butanol/water mixture. Minimizing inter-nanocellulose hydrogen bonding has been proven to be effective in controlling self-assembling of nanocellulose.

The less pristine rice straw holocllulose could be defibrillated into either holocellulose nanocrytals (holoCNCs) via acid hydrolysis or holocellulose nanofibrils (holoCNFs) by TEMPO-oxidization. While both holoCNCs and holoCNFs were amphiphilic similar to their pure nanocellulose counterparts, their greater hydrophobicities prevent self-assembling to produce finer nanofibers as well as distinct surface active behaviors. HoloCNCs lowered equilibrium surface tension to 49.2 mN/m at above 0.57 % critical aggregation concentration, stabilized 30 % more oil-in-water (O/W) emulsion to double the droplet sizes and self-assemble into highly mesoporous structures with up to 3 times higher specific surface (111 m2/g) and total pore volume (0.40 cm3/g), than that from CNCs upon freeze-drying. The unique surface active, amphiphilic and less self-assembling properties of holoCNCs offer additional desirable characteristics without needing surface modification of CNCs. This streamlined isolation process has proven to be a win-win green approach to generate new arrays of nanocellulose.

Objective 2

University of Tennessee (TN) has advanced the development of robust biodegradable agricultural mulches (BDMs) to alleviate concerns about the long-term environmental impact of debris formed during weathering of conventional polyethylene-based mulches. Developing a better understanding of the underlying processes and mechanisms for soil degradation of the BDMs is equally as important as developing BDMs. ASTM is developing a new standard for soil degradation, ASTM WK29802, which requires 90% degradation of plastics in 2 years when buried in soil under ambient conditions, as measured by a standardized laboratory test, ASTM D5988. Through a major USDA Specialty Crop Research Initiative (SCRI) grant received by (Project Director) Hayes, Wadsworth, Belasco, and collaborators at the University of Tennessee (UT), Washington State University (WA), and Montana State University (MT), the long-term impact of using BDMs was investigated by examining soil quality, the soil microbial community, specialty crop production, pests and diseases.  Consumers are also being educated on BDMs (http://biodebradablemulch.org). One investigation looked at the effect of field weathering and simulated weathering of commercially available and experimentally derived biodegradable plastic mulch films. The physicochemical analysis of the mulches is currently being completed.  Data was further analyzed (and additionally collected) for a soil burial study of nonwoven fully biobased mulches that provided the change of physicochemical parameters during the time course of biodegradation, a 40 week period.

Objective 3

Wisconsin (WI) worked on Energy-efficient Recycling of plastic waste. At the beginning of the project WI started with blending of virgin plastic materials as a basis for a comprehensive study to be able to evaluate the results with recycled material from oil-based vs bio-based plastics. In parallel, WI developed a plastic collection and sorting strategy as well as a marketing campaign to get participation from students, faculty and staff of UW-Madison. A lot of plastic waste was collected from three different buildings at UW-Madison. The polymer blends were prepared in a Leitritz ZSE18HPe laboratory, modular intermeshing, co-rotating twin-screw extruder and subsequently pelletized with the appropriate downstream equipment (a water-through, blown-air drier and a rotary cutter). All blends are extruded using a barrel-temperature profiles of 170-200 °C and screw speed of 50 rpm, 100 rpm and 200 rpm, respectively. Blends of virgin plastic materials, LDPE, HDPE and PP were prepared in various ratios. The properties of the virgin blends will be compared with those of recycled in our University. Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), and  Rheological Behaviors were used to study the properties of virgin vs blends . Preliminarily results are encouraging and work will continue in 2016.

Research conducted at the University of California, Davis, (CA) proved lignin to be a highly effective “green” multi-functional binding, complexing and reducing agent for silver cations as well as capping agent for the synthesis of silver nanoparticles on ultra-fine cellulose fibrous membranes. Silver nanoparticles could be synthesized in 10 min to be densely distributed and stably bound on the cellulose fiber surfaces at up to 2.9 % mass. The silver nanoparticle sizes may be synthesized from 5 to 100 nm in diameters by controlling the reaction time. Cellulose fiber bound silver nanoparticles did not agglomerate under elevated temperatures and showed improved thermal stability. The lignin bound silver nanoparticles on cellulose fibers exhibited moderate UV absorbing ability in both UV-B and UV-C regions and excellent antibacterial activities toward Escherichia coli.

Objective 4

The University of Nebraska-Lincolon (NE) was developing an environmentally responsible sizing/slashing agent to substitute PVA, which is a major problem for high chemical oxygen demand (COD) in textile effluent and on the development solvent dyeing systems for cotton, polyester and PLA that could eliminate dyeing effluents.  The large scale industrial demonstration on feasibility of soy proteins as effective slashing agent for textile weaving to substitute PVA proved to be a breakthrough this year. The industry high speed weaving tests showed, first time in the world, that soy protein is the first possible substitution of PVA for polyester and poly/cotton high speed weaving. Such a substitution could substantially decrease COD from textile effluent, since PVA is the largest contributor to textile COD.

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