RECYCLING PROCESS FOR CARBON/EPOXY COMPOSITES

Ronald E. Allred, Jan M. Gosau, and John M. Shoemaker

Adherent Technologies, Inc.
Albuquerque, NM 87123
(505) 346-1688
Rallred@adherent-tech.com

ABSTRACT
The depolymerization of thermoset carbon fiber-reinforced epoxy matrix composites was studied
to determine the significant reaction parameters and fiber quality produced by a catalytic
reclamation process. This process was designed to recover valuable carbon fiber and an organic
fraction from the depolymerization of carbon/epoxy composites. Design of experiments was
used to determine significant process parameters including effects of temperature, time, catalyst
concentration, heat transfer liquid to feedstock ratio, and agitation to estimate the purity of the
carbon fiber produced from the reaction. Significant feedstock parameters that will affect the
rate of reaction were the surface area available for reaction and the thickness of the composite.
The carbon fibers reclaimed from the reaction reached 99.8% carbon values, i.e., 0.2% residual
resin, which is sufficient to meet the market specifications for reuse in conductive molding
compounds. The fiber tensile strength showed an 8.6% reduction after reclamation indicating
that the process had little damaging effect on the fiber. Potential applications for the recycled
fibers include thermoplastic and thermoset molding compounds and nonwoven sheet
reinforcements. An economic analysis of a recycling business based on the catalytic
depolymerization process showed that it should be profitable provided that adequate scrap
composite feedstock can be obtained.

KEYWORDS: recycling, carbon/epoxy composites, depolymerization

1. INTRODUCTION
Large quantities of expensive, carbon fiber composites from sporting goods and government
aerospace and military applications are now being landfilled because there is not an economic
means of reclaiming the carbon fibers. It is expected that future land vehicles will also use
carbon fiber-reinforced composites to a large extent, which will greatly increase the need for an
effective recycling process. Average costs for virgin carbon fiber run from $4.00 to $18.00 per
pound based on the purity and type of carbon fiber.

The majority of work on composites recycling appearing in the literature is concerned with
grinding, shearing, chipping, or flaking the composite into suitable size to be used as filler in
new molded composite parts [1-7]. Pyrolysis (thermal decomposition of the polymer at
temperatures of 750-950C) has also been studied as a preparation method before grinding [8,9].
Most of that work has been on reclaiming automotive sheet molding compound (SMC)
composite parts, largely driven by German laws on recycling. Usually, the composite is ground
into a fine powder with this approach. While this approach may be satisfactory for automotive
SMCs, which contain large quantities of filler, it will not provide the full value from the
expensive fibers and resins used in aircraft and other high-performance applications that may be
achievable using other recycling processes.

Other processes such as acid digestion or incineration in the case of glass-reinforced composites
could be used to reclaim the fibers from some systems; however, those approaches generally
appear impractical from an environmental point of view. Acid digestion uses harsh chemicals
and conditions and creates a hydrocarbon/acid mixture that will require further processing.
Incineration (quaternary recycling) is an option for carbon- and aramid-reinforced composites,
but destroys what are valuable materials in the process and can be a source of pollution.

A new approach to composites reclamation is needed to improve the economics of and overcome
the technical barriers associated with current composites recycling methods. The most
promising approach is tertiary recycling [10-12]. This process breaks polymeric waste into
reusable hydrocarbon fractions for reincarnation as polymers, monomers, fuels, or chemicals,
thus promoting conservation of scarce petroleum resources. A tertiary recycling process
separates the polymer from the valuable fibers, fillers, and metals as low molecular weight
hydrocarbons. The fibers may then be reused in molding compounds, the metals resmelted, and
the pigments reused as fillers. Because of the valuable materials in high-performance
composites, reclaiming those materials should provide an economic benefit.

Adherent Technologies is developing a family of low-temperature, catalytic conversion

processes for tertiary recycling of a variety of complex polymer-based wastestreams such as
scrap electronics, auto shredder residue, and aircraft composites [13-18]. Initial results show that
all types of plastics, thermosets as well as thermoplastics, can be converted in high yields to
valuable hydrocarbon products with these novel catalytic conversion processes. Conversion
times are rapid and the process is closed and, thus, nonpolluting. In addition to hydrocarbon
gases and liquids, valuable carbon fibers are recovered from composite materials that can be
reused in fabricating new composite parts.

The purpose of this study was to determine the operating conditions to support a pilot scale
operation of a process using a liquid heat transfer liquid, including reaction rate, activation
energy, and rate-limiting step, and to verify the carbon fiber product quality. The processing
conditions of interest include temperature, time, pressure, catalyst concentration, heat transfer
liquid to feedstock ratio, and agitation. Results show that high purity carbon fibers that have
near virgin properties can be reclaimed from carbon/epoxy composites using this tertiary
process. Economic analysis shows that a recycling facility processing scrap carbon/epoxy is an
attractive option to landfilling.
 2. EXPERIMENTAL
The experimental portion of this work included several individual tasks to ensure the integrity of
the results. Most importantly, the composites used in the study were made in-house as model
systems so that the chemistry of the system was well understood and the geometry of the
composites controlled. This control of the feedstock used in the experiment allowed assumptions
to be made concerning the mechanistic reaction model developed during this work. In addition,
commercial composites were used to verify the operating range for the temperature, pressure,
catalyst concentration, and residence time, as well as verify the effectiveness of the catalyst.

Based on similar research of

coal liquefaction and plastics
depolymerization, a batch
reactor system was constructed.
The reactor system used
included a Techne fluidized
sandbath for heating, 2.54-cm
stainless steel bomb reactors
with compression fitting caps
with a section of one-inch
stainless steel tubing in
between, a temperature
controller, and a Burrell wrist-
motion flask shaker for
agitation as shown in Figure 1.

Figure 1. Apparatus used for depolymerization studies

Some reactions were carried out

in bomb reactors fitted with
0.16-cm isolated K-type
thermocouples to evaluate the
reaction temperature profile.
The thermocouple can be seen
in Figure 2. This allowed a
temperature profile of the
reactants to be produced to
determine exactly how long the
reactants had been at
temperature.

A model composite laminate Figure 2. 2.54-cm compression fitting bomb reactors used
was made, using Hercules AS4 for depolymerization studies
carbon fiber woven fabric (5 x 1
weave)/EPON 826 (Bisphenol-A monomer)-EPI-Cure W (diethyltoluenediamine) epoxy matrix
(Shell Chemical). The laminate consisted of five plies of fabric 30 cm x 90 cm that were
weighed to determine the desired resin weight. After resin application, the composite was B-
staged at 60C for 2 hours to advance the resin before following the manufacturer's cure cycle to
a final 177C temperature. Resin content of the cured panel was determined to be 37% (by
volume) or 28% (by weight) with a standard deviation of 3% by the ASTM D3171-76 acid
digestion procedure [19]. Void content was less than one percent. The composite was cut into 1
cm x 6 cm strips that fit into the bomb reactors.

Trial Run design of experiments (DOE) software was used to develop experimental matrices
for parametric studies of the important reaction parameters. The parametric study was conducted
to evaluate the main effects from the reaction variables and to bound the reaction parameters that
produce quality product. DOE was used to maximize the information obtained from a minimum
number of experiments.

The reaction parameters and their ranges included:

(1) Temperature 275, 300, 325C

(2) Time 10, 15, 20 minutes
(3) Catalyst Concentration 0.25, 0.50, 1.0 M
(4) Heat Transfer Liquid:Feedstock Ratio 3:1 and 5:1
(5) Stir Angle (Agitation) 0, 2.5, 5.

A resolution III mixed level, fractional factorial test matrix was developed that had four 3 level
factors and one 2 level factor and required 18 runs.

Previous work had shown a significant effect by using a liquid to act as a mass transfer and heat
transfer medium to reduce the reaction temperature and increase the reaction rate. Thus, the
effect of the Liquid:Feed Ratio was evaluated to understand if the amount of the liquid affected
the reaction rate or quality of products. Agitation was evaluated by varying the Stir Angle on the
Burrell wrist-motion shaker. This parameter was varied to understand the effect of film diffusion
of the catalyst to the composite surface. The metric used to evaluate the parameter effects was
the purity of the carbon fiber produced from the reaction.

The catalyst system was added proportionally to the bomb reactors based on the weight of
composite in each bomb to provide a constant ratio of catalyst to reactant mass. Groups of two
to three bomb reactors were processed at one time to ensure similar operating conditions and
repeatability. The sandbath was preheated to the desired temperature and the shaker was set to
the correct angle of deflection for each run. As the bombs were lowered into the sandbath, a
timer was started and the entire reaction time was used as the total processing time. After the
designated reaction time passed, the bomb reactors were withdrawn from the sandbath and
quenched in a room-temperature water bath. After reaction, the solids were washed with acetone
and water to remove any unbound material. Acetone and water were chosen as the wash liquids
because they have no effect on the epoxy matrix that remained bound to the fiber surface. In this
manner, an accurate estimate of the total amount of residual resin matrix could be obtained from
the acid digestion procedure. Once the solid products, fiber and residual resin, were washed, the
samples were placed in an oven overnight at 105C to dry.
Fiber reclaimed from the depolymerization experiments was analyzed for purity using acid
digestion to determine the amount of residual resin remaining on the fibers. This metric was
used to determine the extent of reaction and support the analysis of variance (ANOVA) study.

Reclaimed fibers were subjected to visual scrutiny via optical and scanning electron microscopy
(SEM) to determine the extent of residual surface contamination. Mechanical testing was also
performed on the reclaimed fiber in the form of single fiber tensile tests (ASTM D3379-75).

3. RESULTS AND DISCUSSION

3.1 Description of Products

The reaction products varied widely and certain conditions produced solid products that were
only slightly modified from the feed material. Incomplete reaction yielded solid products that
appeared swollen and distorted. Flakes of cracked epoxy, approximately 110 mm in diameter,
remained on the surface and throughout the composite. The composites retained the general
physical shape of the feed material, although they had no structural properties and were easily
flexed with the fingers. Individual fibers and tows, in the weave, were fixed in the remaining
matrix, and the wash time was significantly longer to wash residual liquids off the solid products.
Acid digestion results show that these materials increased in mass if the reaction was stopped
early enough. This indicates that the heat and mass transfer liquid diffused through the
composite and could not be washed from the matrix.

Solid products that were well processed with residual resin weights of less than 1% exited the
reaction bomb with no structure. The residual liquid product on the fibers after the reaction was
washed from the solids quickly and easily. The fibers were soft and flexible, atypical of fibers
with high concentrations of residual resin. No solid epoxy flakes were apparent, and it
appeared that the resin was completely removed from the carbon fibers.

3.1.1 Parametric Study Results

The goal of the parametric study was to evaluate the main effects from the reaction variables and
to bound the reaction parameters that produce quality product. DOE was used to maximize the
information obtained from a minimum number of experiments.

The use of 3k factorial experiments and mixed level factorial experiments are limited primarily to
evaluation of the main effects due the complex confounding tables that must be established to
generate the design [20]. With this type of experiment, the effect of low order generators masks
the effect of higher order interactions such as a factor square (temperature2, time2, [catalyst]2,
etc.) or combinations of factors (temperaturetime, temperature[catalyst], timeagitation, etc.).
This is purely a mathematical artifact from producing a fractional factorial experiment and
cannot be circumvented with this type of design. Since the goal of the experiment was to sample
a large number of variables and determine the main effect of those variables, this design was
considered sufficient.
The progress of the reaction was monitored by the purity of the fiber produced from the reaction
as determined by acid digestion. Thus, the lower the residual resin, or higher the purity, the
greater the extent of reaction. Fiber purity was chosen as the response variable to the DOE
because it is the primary product of the process and is an accepted measure of the quality of the
reclaimed fiber. In addition, other methods such gas chromatography/mass spectrometry
(GC/MS) and size exclusion or gel permeation chromatography (GPC) could not readily produce
the results sought.

Fiber Purity and the standard deviation (Std Dev) for each sample are given for each run number
in Table I.

Table I. Results of the Reaction Experiment Matrix

Liquid-to- Temp Time [Catalyst] Stir Angle Fiber Purity Std Dev
Std Run Feed Ratio (C) (min) (Molar) (degrees) (%) (%)
16 1 3:1 275 20 0.50 2.5 69.410 3.116
3 2 5:1 300 15 0.50 5.0 71.880 2.340
7 3 5:1 275 20 0.50 2.5 68.500 1.046
2 4 5:1 300 10 1.00 2.5 71.392 1.170
5 5 5:1 325 10 0.50 0.0 95.110 0.572
6 6 5:1 325 15 0.25 2.5 99.788 0.436
15 7 3:1 325 15 0.25 2.5 99.726 0.221
11 8 3:1 300 10 1.00 2.5 69.895 0.561
17 9 3:1 275 10 0.25 5.0 65.673 3.658
14 10 3:1 325 10 0.50 0.0 90.830 1.489
12 11 3:1 300 15 0.50 5.0 70.510 1.290
4 12 5:1 325 20 1.00 5.0 99.780 0.206
18 13 3:1 275 15 1.00 0.0 67.802 0.858
9 14 5:1 275 15 1.00 0.0 64.831 0.999
13 15 3:1 325 20 1.00 5.0 99.810 0.132
8 16 5:1 275 10 0.25 5.0 63.481 1.251
1 17 5:1 300 20 0.25 0.0 68.040 1.095
10 18 3:1 300 20 0.25 0.0 70.469 2.746

The standard deviation represents the deviation between the solid products generated by each run
because three solid samples from each bomb run were acid digested as specified by ASTM
D3171-76. Sample standard deviations also show that the solids from each bomb were
homogeneous in extent of reaction and that the error introduced by acid digestion was
minimized. The fiber purity numbers are often less than that for the original composite formed
at 72% (by weight) fiber. Thus, at certain reaction conditions, the composites swelled and
gained weight by absorption of the contact liquid.

Based on the data generated from the reaction experiments and subsequent acid digestions,
ANOVA was used to determine the factors that had a significant effect, to 5% confidence
interval, on the extent of reaction (i.e., carbon fiber purity). Although this empirical model does
not have a mechanistic or physical basis, it provides a useful correlation to evaluate and control
the process.

The ANOVA analysis is based on evaluating the effect between treatments, such as temperature
or time, compared to the total error generated within each treatment. This type of analysis is
valid assuming the errors within each treatment are normally and independently distributed [20].
The initial ANOVA analysis (Table II) showed that the liquid/feed ratio and catalyst
concentration are not significant to the purity of the carbon fiber produced over the ranges
evaluated. The effects of time and agitation on the purity of the fibers are significant based on
the ANOVA; however, temperature has a much more significant effect.

Table II. Test Between Factors ANOVA Table for the Dependent Variable Fiber Purity or
Extent of Reaction

Type I Sum
Source of Squares df Mean Square F Sig. P
Corrected
Model 3495.407 9 388.3786 145.8479 6.6556E-08 1.00000
Intercept 109969.088 1 109969.0880 41296.7222 4.4409E-16 1.00000
WTRATIO 0.097 1 0.0972 0.0365 0.8532 0.14679
TEMP 3410.111 2 1705.0554 640.2999 1.4856E-09 1.00000
TIME 39.837 2 19.9185 7.4800 0.0147 0.98526
[CAT] 5.213 2 2.6066 0.9789 0.4166 0.58340
STIR 40.149 2 20.0745 7.5386 0.0144 0.98556
Error 21.303 8 2.6629
Total 113485.798 18
Corrected
Total 3516.710 17
1. Computed using Alpha = 0.05
2. R Squared = 0.831 (Adjusted R Squared = 0.760)
Surface plots of the predicted purity levels R esp onse Surface

were prepared for the significant variables

based on a regression model chosen for 100%

the process. Figure 3 is the surface plot of

90%
purity versus time versus temperature for a

Fiber Purity
range of 1020 minutes and 275325C. 80%
The minimum shown in the plot represents
the equilibrium point between the mass 70%

diffusion of the liquid and the depolymer-

ization reaction. At temperatures below 16
325
60%
315 320
this point, the composite is gaining weight T im e (m in) 10
285 290 295 300
305 310
275 280 T em perature (C)
from the adsorption of the liquid and
catalyst that was seen in the acid digestion 0.6-0.7 0.7-0.8 0.8-0.9 0.9-1
results.

Above the minimum, the depolymer- Figure 3. Surface plot for the predicted purity of
ization reaction speeds up and the the carbon fiber product varying temperature
composite begins to lose weight as the and time
resin is removed from the fiber surfaces
and the purity of the fiber increases. The time factor appears to have a weak effect on the fiber
purity although it shows increased purity with increasing time.

3.1.2 Carbon Fiber Characterization and Reinforcement Capabilities

SEM was used to evaluate the fiber surfaces and the bulk residual resin present on the
composites after the bomb reactions. Two samples were studied based on their varying extent of
reaction. The first sample (A, run 17) was processed at 300C for 20 minutes with a 0.25 M
catalyst concentration, 5:1 liquid-to-feed ratio, and no agitation. The residual resin content for
this sample was estimated at 32% by weight with a standard deviation of 1.1%. Large flakes of
residual resin appeared among loosened fibers and some fiber surfaces are spotted with bound
residual resin as seen in Figure 4. The white patches along the fibers are residual resin that has
not separated from the fiber surface.

The flaking action of the resin being removed from the composite in large chunks is evident in
Figure 5. Figure 5 shows the 7 diameter carbon fibers in the foreground with no indication of
residual resin on their surfaces unlike those seen in Figure 4. A flake of resin is seen in the
background with the impression of the carbon fibers molded in the surface. This suggests that
the depolymerization reaction is initially occurring along the fiber/resin boundary.
 20 m

Figure 4. SEM micrograph of residual Figure 5. SEM micrograph of residual resin

resin on the surface of sample A(700X) flake and released carbon fibers from sample
A(1200x)

The final SEM micrograph of sample A

is a single fiber with a sheath of resin
that is peeling off the fiber surface as
the reaction is proceeding (Figure 6).
Based on the micrographs, a shrinking
core kinetic model may be justified if
one considers the diffusion through the
ash layer analogous to diffusion
through the carbon fibers [21]. The
indication of the reaction proceeding
along the fiber/resin interface, i.e.,
flaking, creates a modification of the
shrinking core kinetic model based on
the geometry of the layer ash (carbon 20 m
fiber) and the reacting core (residual
resin). Therefore, with more agitation,
the carbon fibers would be removed
from the composite and diffusional Figure 6. Resin sheath being peeled from a
resistances would be minimized. single fiber of sample A as the reaction
proceeds (700x)

The next sample (B, run 12) evaluated with the SEM was processed at 325C (617F) for 20
minutes with 1.0 M catalyst concentration, 5:1 liquid-to-feed ratio, and maximum agitation (5).
The residual resin content for this sample was estimated at 0.22% by weight with a standard
deviation of 0.21%. SEM micrographs of the sample verified the acid digestion results of
99.78% pure fiber.
Figure 7 shows a low magnification view of
the carbon fibers reclaimed from the model
composite. Residual resin would show up on
the surface of the fiber as white specks. This
fiber was very soft and flexible, and visual
inspection of the entire sample yielded no
residual resin in the form of flakes. Small
particles of residual resin 1-2 in diameter
could be found on some fibers by high
magnification examination.

Figure 7 shows two distinct features of the

carbon fiber surface that are critical to the
quality of the recycled fiber produced. First,
the surface shows little residual resin.
Second, the carbon fiber surfaces are very
smooth. Since the tensile strength of carbon
fibers is a strong function of surface structure,
pitting on the surface from the depolymer-
ization reaction would result in degradation
of the fiber tensile strength from the recycling
process.

Single fibers from the starting materials, i.e.,

carbon fiber fabric used for the model 20 m
composites, and fibers reclaimed from the
reaction were tested for tensile strength. The
results of the single fiber tensile tests showed
an 8.6% reduction in the average tensile Figure 7. Sample B reclaimed carbon fiber
strength of the reclaimed fiber compared to with 0.22% (wt/wt) residual resin (500x)
the control fiber (13.21 g to 14.45 g). This
result shows that the process does not harm the fiber surface to the point where it could not be
used for future applications.

3.2 Liquid Reaction Products

Analysis of the epoxy depolymerization products using GC/MS techniques showed that they
largely consist of isomers of substituted phenolic compounds. Those compounds have potential
value in the production of phenolic-based adhesives for wood products such as plywood, chip
board, and particle board. The compatibility of the phenolic recycling products with wood
adhesives is being explored and will be reported at a later date.

3.3 Markets and Process Economics

The market demand for chopped and milled carbon fiber and nickel coated carbon fiber in the
US is at an all time high and is being driven by the electronics industry need for conductive
thermoplastic materials for shielding. Markets in Europe and the Pacific Rim continue to grow,
but at slightly lesser rates than in the US. The global demand for these materials in 1998 was 8.1
million pounds with a market value of $64.5 million. By the year 2007, the demand is projected
to grow to 25.5 million pounds, with a market value of $205.4 million.

A single-site model has been developed that provides an economic analysis for placing a
recycling plant at any location in the US and includes costs for all necessary equipment, labor,
collecting, transporting, size reducing, recycling, separation of products, post processing (if any)
packaging, and transporting the products to market. The model calculates a rate of return on
investment. Initial results for a commercial 2-ton/day processing plant to be located in
Albuquerque, NM, have been developed.

A forecast of the first year business performance of a tertiary recycling operation based upon a
conservative estimate of recovering 435,000 pounds of high purity fiber from 660,000 pounds of
carbon composite scrap has been conducted. This volume would utilize about 40% of the plant
capacity. All of the recovered product would be milled and sold to thermoplastic molding
compounders for $5.15 per pound. A combination recycling and milling operation is projected
to have a 68 percent internal rate of return and generate a profit of $2 million per year.

4. CONCLUSIONS
Evaluation of the depolymerization of thermoset carbon/epoxy composites was performed in an
attempt to determine significant reaction parameters (e.g., temperature, time, agitation, catalyst
concentration) for the production of high purity carbon fiber by minimizing the amount of
residual resin left on the surface after depolymerization.

DOE and an ANOVA analysis were used to determine the significant reaction parameters and
ranges of those parameters and to develop a regression model for the purity of the carbon fiber
produced. The data generated for this analysis were produced from a resolution III (18 runs)
DOE. From these experiments, the reaction conditions that produced very pure fiber (i.e., 99.8%
carbon fiber) were 325C, 20 minutes, and 5 of stir angle on the wrist motion shaker. The
catalyst concentration and the heat transfer liquid to feedstock ratio did not have a significant
effect over the range studied; however, previous experimentation showed these parameters
significantly affect fiber quality and reaction rate and temperature. Specification of the pilot-
scale process equipment should include these reaction parameters to ensure the equipment can
meet the operating conditions that will produce acceptable product from the scaled-up process.

The quality of the fiber product reclaimed was characterized in terms of residual resin content,
surface appearance, and tensile strength. Under the optimum conditions for generating high fiber
purity, the fiber surface texture showed no signs of pitting, which can cause a significant
reduction in the tensile strength of the fiber. The results of the single fiber tensile tests showed
an 8.6% reduction in the average tensile strength of the reclaimed fiber compared to the control
fiber (13.21 g to 14.45 g). This result shows that the process does not harm the fiber surface to
the point where it could not be used for future applications.
Products from depolymerization of the epoxy matrix material are largely isomers of substituted
phenolics. Those phenolic compounds are being investigated for use in phenolic-based
adhesives for the wood industry. An economic analysis for a recycling plant in combination with
a milling operation shows a projected $2 million in pretax income per year for a 68% internal
rate of return.

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ACKNOWLEGMENTS
The authors gratefully acknowledge funding for this work by the Naval Air Systems Command
under contract N00421-98-C-1032. Mr. L. D. Busselle conducted the design of experiments
studies for catalyst parameter development as part of his MS thesis in chemical engineering at
the University of New Mexico.

BIOGRAPHIES

Dr. Ronald E. Allred

Dr. Allred earned his Sc.D. in the Polymerics Panel of the Department of Materials
Science and Engineering at MIT under a Doctoral Study Fellowship from Sandia
National Laboratories. He has a B.S. in Chemistry and an M.S. in Nuclear
Engineering Materials, both from the University of New Mexico.

Dr. Allred is president and owner/founder of Adherent Technologies, Inc. that

provides contract research and development services to government and industry.
He has previous research experience at Sandia National Laboratories, MIT, and
PDA Engineering.

Dr. Allred's research has included radiation curing materials, plasma surface
chemical modification of materials, plasma and surface spectroscopy, environmental
effects on polymers and composite materials, composites and adhesives test
development, materials for electronic packaging, acoustic wave and fiber optic
microsensors, tertiary recycling of complex polymer-based mixtures, and the
development of specialty polymers, adhesives, coatings, and foams. Dr. Allred has
published over 90 papers in technical journals and conference proceedings and has
20 patent disclosures and over 70 company reports. The vast majority of those
publications are in the fields of composites, polymers, recycling, and sensors.

Dr. Jan-Michael Gosau

Dr. Jan-Michael Gosau received his Dr. rer. nat. from the Freie Univeristt Berlin
in 1993. He has a Diploma in Chemistry from the Univeristt Mainz. The work for
both thesis and dissertation was performed at the Max-Planck Institute for Polymer
Science.

Dr. Gosau holds the position of Polymer Research Scientist at Adherent

Technologies. Before joining Adherent Technologies he was engaged as a
postdoctoral research associate at the University of Arizona and as research
assistant at the University of New Mexico while completing the course work for a
M.S. in chemical engineering. His research focused on self-assembled monolayers
for sensor applications, composite recycling, and thermal control coatings for
spacecraft.

In addition to research on self-assembled monolayers for sensors at UNM, Dr.

Gosau has done research in opiod mimetics at the University of Arizona, where he
gained an extensive background in biochemistry. His current research focuses on
the development of novel polysilylenes for waveshifter applications.

Mr. John M. Shoemaker, Marketing Director

Mr. Shoemaker has a BA in Economics from San Diego State College. He is the
Director of Marketing at Adherent Technologies, Inc.

For two years before joining the company, Mr. Shoemaker had been retained as an
independent contractor by Fiberite, Inc. in a business development role for
Composite Recycling Technologies. His responsibilities included: the assessment of
global composite scrap feedstock locations, quantities and method for its acquisition;
validation of the composite recycling technology; identification of markets for the
recycled products; and determination of the economic viability of a commercial
composite materials recycling business.

Mr. Shoemaker has more than thirty years in the materials industry, 20 years
serving as the senior executive officer of a number of industry leading companies
engaged in the research, development and manufacturing of advanced composite
materials and processes with applications in commercial and military airframes,
aerospace, turbine engines, sporting goods, and electronics.