Lightweight, Compostable, And Biodegradable Fiberboard Jason Niedzwiecki, Jo Ann Ratto, Jeanne Lucciarini, Christopher Thellen, U.S. Army Natick Soldier Research, Development and Engineering Center, Natick, MA Xin Li, Xiuzhi Susan Sun, Bio-Materials and Technology Lab, Dept of Grain Science and Industry, Kansas State University Donghai Wang, Department of Bio & Agriculture Engineering, Kansas State University Richard Farrell University of Saskatchewan, Saskatoon, Canada Study of Soy Protein Adhesives for Biodegradable Fiberboard Research and Development of Fiberboard Containers Background Technical Approach Technical Objectives The development of biodegradable fiberboard is being researched by the Department of Defense’s Strategic Environment Research and Development Program with Kansas State University and U.S. Army as collaborators. The project will help to reduce the amount of solid waste for the military. Shipping containers fabricated from fiberboard are necessary to transport and store food and other military items. However, there are numerous disadvantages in producing fiberboard for the military: the process is costly, uses cellulose and hazardous chemicals, deletes natural resources in our environment, and creates hazardous waste. Effect of concentration of SPA on mechanical properties of LBF Problem Statement: In 2004, Army, Air Force, and Marine Corps consumed approximately 144 million operational rations generating 66,718 tons of ration related waste. The optimum concentration of SPA added in pulp is from 0.05% to 0.15%(Fig. 2). 6500 0 0.05 0.10 0.15 6000 a a MPa To develop light weight biodegradable fiberboard (LBF) that can be used for military ration packaging. 70 a 60 Materials and Methods 50 Soybean flour was the product of Cargill company; a Biodegradable Fiberboard (soy protein adhesive) Technical Objectives: Produce lightweight fiberboard materials, biodegradable polymer-coated fiberboard and paperboard that can be converted to a valuable byproduct, compost a a a Biodegradable Coatings (coated corrugated) Prepare and characterize coatings vs. different methods and substrates Prepare and optimize composite panels Produce and characterize coated fiberboard/paperboard Down select optimal materials through sample characterization Produce environmentally friendly materials that meet the operational and performance requirements of combat ration packaging b Composting trials are being conducted to assess the “environmental degradability” of these new coated paper and fiberboard formulations. These trials will ensure that, when used in combination with other waste materials (e.g. food waste, grass clippings, leaves, bark, etc.), the new paper and fiberboard products, do not interfere with the composting process and can generate a compost product that can ultimately be used as a soil conditioner that can be sold or given to local communities. Lightweight and Compostable Packaging b 5000 Introduction & Overview a 5500 Objective Compost Studies for Biodegradable Fiberboard Fabricate shipping containers and evaluate performance a Tier I & II Compost studies b 40 30 100% virgin pine pulp (made through an unbleached kraft process) was provided by Interstate Paper LLC; Tier III composting study 20 Transition Technology 0 TSH MOR MOE Properties Fig 2. Mechanical properties of LBF, Made at 66.7 KN forces, 160 ˚C for 3.5 min, with 1.0 g/cm2 of area density and 1.2 mm of thickness, prepared by different concentrations of SPA-I MRE Containers Fiberboard Manufacturing Process Glue station - single face / liner join Finished sheets Table 1 SPA Formula SPA-2 SPA-3 SPA-4 SPA-5 SDS-modified soy flour powder SDS-modified soy flour slurry Soy flour powder SDS-modified SPI slurry Soy protein isolates (SPI ) powder Weight – 1.22 lbs Compression Strength – 1327 lbs All of these LBFs showed highly strong tensile strength, MOR, wet-TSH and wet-MOR; Modified soy flour adhesives and SPI (with and without SDS modifications) adhesives provided significant higher mechanical properties than control; No apparent difference of mechanical properties were observed for LBFs with soy flour and control; mechanical properties after water soaking were improved by soy flour Heating Section Area density Pulp Mixing Paper sheet Pressing Thickness TSH MOR Weight – 1.42 lbs Compression Strength – 1827 lbs Tensile strength decreased with the replacement of 20% pulp with chicken feather fiber (Table 2). No apparent difference of tensile strength was observed for paper sheet with treated and untreated chicken feather fiber (Table 3). 0.77 80% pulp/20% CFF 0.73 80% pulp/20% CFF/0.1% SPA-1 0.85 SPA-1 SPA-2 SPA-3 SPA-4 SPA-5 Control (no adhesive) Medium Glue Roll Double Face Liner Weight – 1.64 lbs Compression Strength – 2568 lbs Cutting/Scoring Wheels Wet TSH Wet MOR 55# liner / 30# WAM medium / 55# liner 69# liner / 30# WAM medium / 69# liner 72# liner / 30# WAM medium / 72# liner Roll Station for Liner Weight – 2.36 lbs Compression Strength – 1665 lbs 80% pulp/20% CFF/0.2% SPA-1 1.15 g/cm2 mm MPa MPa Mpa MPa 0.090 0.090 0.088 0.094 0.089 1.10 1.18 1.15 1.13 1.13 61.0a 51.7b 39.9c 54.2b 51.9b 46.7a 45.2a 37.9b 47.5a 48.0a 4.12a 3.73a 4.14a 3.81a 4.23a 3.53a 3.28a 3.17a 3.34a 3.30a 0.090 1.21 42.8c 36.7b 2.60b 2.10b Compare to commercial solid fiberboard (SF), the light weight biodegradable fiberboards had significantly higher tensile strength, similar burst index(Fig.3); higher or similar tensile strength after water soaking; similar linear extension and thickness swell (table 5). 8 A B SF(Parallel) SF(perpendicular) 6 V3C <1 129 11 1.05 27 The specific goal of the first phase of this research is to demonstrate the “environmental degradability” of packaging materials incorporating biodegradable polymer coatings and adhesives with natural fibers and pulp under composting conditions. This effort will determine how fast the fiberboard degrades in compost and if, when combined with other waste materials (e.g., food waste, grass clippings, leaves, bark, etc.), these packaging materials produce a valuable compost product. V2S solid board V2S <1 123 20 1.00 29 30# Uncoated Kraft E <1 101 10 0.82 41 30# Kraft coated w/MBX CS06082205 F 1 95 1 0.77 41 Metabolix MBX 1507-20A J 2 100 20 0.81 39 MRE box MRE-bx 2 86 11 0.70 47 This research is a collaboration between the U.S. Army (Natick Soldier Research, Development and Engineering Center, Natick, MA) and the University of Saskatchewan (Dep. of Soil Science, Saskatoon, SK, Canada). MRE liner MRE-ln 2 87 19 0.71 41 90# Liner 12 1 113 12 0.92 37 Fiberboard KSU-Q 2 68 13 0.55 85 Raw wood fiber KSU-R 4 79 1 0.64 62 Materials & Methods Cheese cloth KSU-S 3 109 14 0.89 35 Standard (ASTM or ISO equivalent) laboratory test methods were used to assess the degradation/disintegration (measured as weight loss; Tier I test) and mineralization (conversion of organic-C into CO2; Tier II test) of the test materials. Compost quality was assessed in accordance with U.S. Composting Council standards (Leege & Thompson, 1997). Modified soy protein KSU-T 1 122 29 0.99 39 Chicken Feather KSU-U 2 71 27 0.58 94 – “compostable” material demonstrates satisfactory disintegration if ≤ 10% of original material is recovered on a 2-mm sieve after a 12 week test exposure. • Weight, Waste & Cube Bioreactors maintained in a controlled environment chamber at 52 ± 2°C. – Transport/Storage – Material Handling/Use – Disposal Weight – 1.36 lbs Compression Strength – 2174 lbs Each reactor is maintained under aerobic conditions and at a moisture content of 55 ± 5% water-holding capacity by flushing with humidified air. Roll Station for Medium A poisoned control reactor is maintained in order to assess the contribution of abiotic degradation. Package Testing and Characterization Compression Testing of Fiberboard Containers Objective: To perform compression test of MRE / UGR fiberboard containers Background: Compression strength is the containers resistance to uniform applied external forces. The ability to carry a top load is affected by the structure of the container and the environment it encounters, and the ability of the inner packages/dunnage to help support the compressive load. Results: Studies under standard lab conditions (50%RH and 23C) have shown that CAD samples have higher compression strength when compared to existing solid fiberboard containers. New studies will be conducted to analyze the affect of compression strength of production samples. Unit Load Testing of Fiberboard Containers Objective: To perform transportation test of MRE / UGR fiberboard containers Background: Unit load performance plays a major role in protecting ration components and defines the logistic requirements needed to transport, handle and store combat rations. Optimizing performance under dynamic/static compression, shock and vibration can help absorb or divert energy away from the product and ultimately improve product performance and quality. Results: Studies have shown that the prototype corrugated containers perform similarly to existing MRE rations under unit load compression and random vibration testing which simulates transportation activities. Environmental Testing - Cold Weather Test of Fiberboard Containers Objective: To subject fiberboard containers to cold weather climates Background: The prototype corrugated and solid fiberboard containers were exposed to environmental conditions which included: high winds, snow and some rain/freezing conditions with an average low of 18F and an average high of 34F over the 27 test days. Several container designs and industrial adhesives were tested/inspected during the cold weather study. Results: Studies from the cold weather test have shown that the corrugated containers and industrial adhesives maintain their performance under cold weather conditions. Since the cold weather study, the water resistant coatings have been optimized to better perform under wet environments. Environmental Testing – Spray Test of Fiberboard Containers Objective: To determine the water resistance of MRE / UGR containers Background: The water spray test is used to establish the water resistance of shipping containers, by determining the ability of the container to protect the contents from water and high humidity. Performance in these environments must be achieved in order to maintain the compression strength required for combat ration storage and use. Results: Results have shown that the coated corrugated containers actively repel water from the container. Studies are ongoing to determine the overall impact on compression strength at high humidity/wet conditions. Weight Analysis of Fiberboard Containers Objective: To conduct weight analysis of fiberboard containers Background: The weight and volume of MRE rations has a major influence on the packaging supply chain and can impact logistic operations within the military distribution system. Weight reduction can improve operations within the supply chain and can dramatically reduce material consumption while at the same time lower costs incurred during procurement, manufacture, shipment and disposal. Results: By optimizing the overall size and structure of the corrugated containers, studies have shown that weight reduction can be reduced by as much as 40% (1 lb) of the original packaging weight. This weight reduction can add up to over 3.6 million lbs per year based on average procurement. Results 0 Compression Testing of Fiberboard Containers 3000 Tensile strength (10MPa) Weight Reduction of Fiberboard Containers Burst Index(KPa m2/g) Fig.3 Comparison of mechanical properties of LBF with SF: A) LBF with 0.09 of area density and 1.1 mm of thickness; B) LBF with 0.05 g/cm2 of area density and 0.6 mm of thickness Table 5 Comparison of water soaking properties of LBF with SF Area density g/cm2 LBF A 0.09 Thickness mm 1.1 Wet-TSH MPa 3.1 LE % 0.6 TS % 60.0 LBF B SF (Parallel ) 0.05 1.24 Treatment* Area density (g/cm2) Tensile strength (MPa) 80% pulp/20% U-CFF(control) 1.44 6.61 Tested after 24 h water soaking 80% pulp/20% SBH-CFF 1.40 6.98 Conclusion 80% pulp/20% M-CFF 1.46 6.12 80% pulp/20% F-CFF 1.42 6.43 SF (perpendicular ) 0.6 5.5 0.4 69.3 3.5 0.1 56.3 2.5 2.5 55.6 bench-scale test under controlled aerobic conditions (Farrell et al. 2001) – a test material is considered “biodegradable” if it achieves 60% ThCO2 relative to the positive control during a 180-day test exposure. Bioreactors maintained in a controlled environment chamber at 52 ± 2°C. Each reactor is maintained under aerobic conditions and at a moisture content of 55 ± 5% water-holding capacity. Headspace gas samples collected at 12 to 120 h intervals and analyzed for CO2 and O2 content using GC-TCD. Daily and cumulative CO2 production (total and net) are calculated relative to a control reactor (unamended compost). Figure 1. Net mineralization of the positive control (cellulose) and test materials. All test runs performed with the compost kept at 52 ± 1°C and 55 ± 5% water-holding capacity. Figure 2. Disintegration of the EVCO sample during a 42-d, bench-scale composting test. The compost was kept at 52 ± 1°C and 55 ± 5% water-holding capacity. Discussion Standardized (ASTM equivalent) tests were conducted to assess the bio-environmental degradability of light weight packaging materials under controlled aerobic composting conditions. Of the 28 test materials evaluated during test exposures of 140–198 days, all but two [KSU-Q (fiberboard) and KSU-U (chicken feather)] achieved the relative net mineralization threshold (RBI ≥0.60) required for designation as a readily biodegradable/compostable material. In general, the test materials and positive control (microcrystalline cellulose powder) included in the first test run produced relatively low net CO2-C yields, which are believed to reflect matrix effects related to the amount of readily available C-substrate present in the compost. These effects were not observed in the second test run, which employed the compost from the same source but which had been aged for an additional seven months. All 15 materials included in the first test run were characterized by RBIs >0.60, indicating that they could be considered biodegradable/compostable. However, because of the low CO2 yields, these test results should be considered ‘conservative’. A sub-set of the samples is being retested to confirm these results. Weight-loss (Tier I) tests demonstrated that the new packaging materials were compostable (e.g., EVCO, Fig. 2), though the intact materials degraded at a significantly slower rate than the powdered materials. Results 40 2000 35 1500 2527 2485 2223 2355 1000 1898 500 32 31 Acknowledgements - - - - - Weight Loss (%) - - - - - 30 25 21 Time (d) V2S V3C MRE-liner MRE-box EVCO SF 7 0.76 0.64 1.11 1.72 1.06 2.40 This research was funded through the USDOD Strategic Environmental Research and Development Program. All test materials were supplied by the Natick Soldier Research Development and Engineering Center (Natick, MA). All composting tests were carried out at the Dept. of Soil Science, University of Saskatchewan (Saskatoon, SK, Canada). RF & DR gratefully acknowledge the assistance of Mark Cooke and Luke Pennock in monitoring the compost tests. 14 4.84 3.39 1.50 8.57 7.56 8.83 References 21 8.59 6.48 9.03 11.17 10.92 11.59 28 12.11 9.38 10.09 12.91 18.43 17.04 35 17.81 12.84 14.07 20.71 18.43 15.35 42 18.91 14.13 16.45 24.03 17.71 15.30 20 15 10 0 55# RSC/Insert 55# WD 72# RSC/Insert 72# WD MRE SF 5 0 55# RSC/Insert Random Vibration testing of MRE corrugated containers 1.7 Cold weather testing of fiberboard containers 4 hr rain test – corrugated fiberboard containers This research suggests that the light weight biodegradable fiberboards with soy protein adhesives prepared from either modified soy flour or soy protein isolate have great potential as alternatives to current commercial fiberboard. These soy protein adhesives would be easier for re-pulping, which is under evaluation. Acknowledgement: This research was supported by the US Department of Defense Strategic Environmental Research and Development Program. – Tier I Composting 42 45 g/cm2 Tier II Composting - targets mineralization as a measure of a material’s ultimate biodegradability Test materials were ground to a powder, dried to a constant weight in a convection oven (50°C for 12 to 18 h) and stored in glass vials until needed. All samples were analyzed for their carbon (C) content using a LECO CNS analyzer. 12.01 *U-CFF, untreated chicken feather fiber; SBH-CFF, 6g/L sodium bisulfate solution with pH=10 treated chicken feather fiber; M-CFF, 40mmol/L 2-mercaptoethanol solution treated chicken feather fiber; F-CFF, 88wb% formic acid treated chicken feather fiber. V3C corrugated board • Rough Handling 2 2.41 Table 3 Spell out of paper sheet prepared with pulp and chemically treated CFF with 0.1% SPA-1 31 • System Performance Regular Slotted Container with Width Divider Corrugated Structures Comparison of properties of LBF with commercial fiberboard 8.92 5.67 --- bench-scale test under controlled composting conditions Percent Reduction (%) 100% pulp (control) Tensile strength (MPa) 123 14 • Water/Moisture resistance Regular Slotted Container with Insert Single Face Liner Compressive Load (lbs) Area density (g/cm2) Treatment 1 – 2500 Table 2 Spell out of paper sheet prepared with mixture of pulp and CFF Cell • Bursting Strength Paper sheet prepared with mixture of pulp and chicken feather fiber (CFF) Cellulose powder (positive control) Solid Fiberboard Container 4 Results and Discussion Finished Sheets Heating Section Fig 1. Preparation of the light weight biodegradable fiberboards Fiberboard evaluation Burst index test: TAPPI T 810 om-06 (Technical Association for the Pulp, Paper, and converting Industry ) Mechanical and water soaking properties - ASTM D1037-99 (American Society for Testing and Materials) Tensile strength (TSH); Modulus of rupture (MOR) and modulus of elasticity (MOE); TSH after 24 h water soaking; Thickness swell (TS); Linear expansion (LE) t60 (days) Note: Compression data and weights based on 55# corrugated structure Light weight biodegradable fiberboard (LBF) preparation Molding in Special Mold RBI c Tier I Composting - targets material disintegration (ASTM D6003) Cooling Section Glue Roll Formula SPA solution ThCO2 (%) - - - Test Material - - Description • Compression Strength Regular Slotted Container with Length Divider Cutting Section Table 4 Properties of LBF with SPAs All SPAs were prepared at 5% solid content, and stirred prior to applications R & D Efforts Regular Slotted Container Properties of LBF with five SPAs (Table 4) SPA-1 I.D. Laga (days) 10 Five soy protein-based adhesives (SPA) was prepared (Table 1) Tier II Composting Compression equipment for MRE / UGR analysis Unit load compression of MRE corrugated containers. Test duration 27 days with an average high of 34F 4 hr rain test – 4 column stack of fiberboard containers 55# WD 72# RSC/Insert 72# WD Benefits Weight Reduction – 3.6 million lbs of packaging per year! Material Reduction – 20%-40% fiber reduction vs. MRE container Compostable – Coatings and fiberboard containers maintain compostability Repulpable – New coatings allow fiberboard to be reprocessed at the paper mill Recyclable – Move packaging out of land filling and into the recycling waste stream American Society for Testing and Materials. 2003b. Annual Book of ASTM Standards. ASTM: West Conshoshocken, PA; Vol. 08-03; Standard D 6002. Farrell, R.E., T.J. Adamczyk, D.C. Broe, J.S. Lee, B.L. Briggs, R.A. Gross, S.P. McCarthy, and S. Goodwin 2000. Biodegradable bags comparative performance study: A multi-tiered approach to evaluating the compostability of plastic materials. Pp. 337-375 In R.A. Gross and C. Scholz (eds.) Biopolymers from Polysacharides and Agroproteins, ACS Symposium Series 786. American Chemical Society Washington, DC. UNCLASSIFIED