72 - SERDP-ESTCP - Strategic Environmental Research and

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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
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