Struktol Company of America

201 E. Steels Corners Road P.O. Box 1649

Stow, OH 44224-0649
(330) 928-5188 Fax (330) 928-8726

Compounding and Processing

Additives for Woodfiber-Plastic
Composites
Presented by Michael S. Fulmer

Presented at the 5th International Conference on

Woodfiber-Plastic Composites
Madison, WI

May 28, 1999

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ABSTRACT

The use of wood and other cellulosic fillers have been used extensively to fill both
thermoset and thermoplastic compounds for decades. Recent advances in
compounding technology and further research into this area have resulted in the
development of injection molding and profile extrusion grades of thermoplastic
compounds which provide many benefits to a wide variety of end-users. However the
use of these types of fillers, like other fillers, can cause a number of compounding and
processing problems associated with the dispersion of the filler and flow characteristics
of the resulting mixed composite. Common deficiencies include surface mottling and
fracture, poor flow characteristics and compounding problems due to low temperature
mixing requirements.

In this presentation we will discuss the use of chemical process additives, viscosity
modifiers and dispersion enhancers in wood flour-filled polypropylene composites. It is
our goal to show improvements in flow, surface appearance and physical properties at
specific levels of filler loading and further that the use of these types of additives may
allow for higher levels of filler loading without sacrificing processability, performance
properties or surface appearance.

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EFFECT MECHANISMS OF THE ADDITIVES:

u Tribological
l Adhesives

l Lubricants

l Surfactants

u Molecular

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EFFECT MECHANISMS OF THE ADDITIVES:

u Tribological
l Adhesives

Increased interfacial forces created by surface attachment

Increase energy required to break adhesive bonds causing increased
shear
l Lubricants

Function to minimize the frictional forces between moving surfaces

Can be divided into internal and external
Internal is polymer: polymer, polymer: filler interaction
External is polymer: hot metal, filler: hot metal interaction
l Surfactants

Create a surface active film via polar and non-polar ends

Polar end absorbs/bonds to a surface
Wetting of the filler allows for improved low energy dispersion
Similar to lubricants effect

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DIFFERENCES IN LUBRICANT TYPES:

Taken from PVC based terminology:

u External
Typically provide lubrication between the polymer and the metal surface of the
processing equipment.
Types
Polyethylene Homopolymers, Paraffins, Esters, Metallic Soaps,
Amides, Fatty Acids and Oxidized Polyethylenes

u Internal
Typically reduce bulk viscosity by being partially compatible with the PVC, thus
helping to open the polymer chain with the lubricants' soluble component, while
providing intermolecular lubrication with the less soluble portion of the lubricant
molecule.
Types
Fatty Alcohols, Esters, EVA Waxes

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SPECIFIC EFFECTS OF LUBRICANTS

n Internal Lubricants n External Lubricants

u Promote flow u Provide metal release
u Exhibit good clarity u Help reduce process temperature
u Promote good weld line strength u Can plate out
u Minimize sink marks u Slow fusion
u Improve die filling u Can cause delamination
u Reduce die swell u Can lower weld line strength
u Allow increased molding speed without u Can cause surging
shear burn
u Reduce head and back pressure
u Do not affect paintability
u Lower heat distortion

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EFFECT MECHANISMS OF THE ADDITIVES:

u Molecular
Chemical alteration of molecular weight average and number
In polypropylene, addition of peroxide results in chain scission
Lower molecular weight results in increased flow rates/low viscosity

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TYPICAL PROPERTIES OF HIGHLY FILLED COMPOUNDS:

u Increased:
3 Viscosity
3 Flexural modulus
3 Heat deflection temperature (HDT)
3 Dimensional stability

u Decreased:
3 Izod Impact
3 Mold shrinkage
3 Thermal expansion
3 Part cost

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MATERIALS USED IN THIS PROGRAM:

u Exxon Homopolymer Polypropylene PD3625 (38 MFI)

u American Wood Fibers 8010 Hardwood Flour (120 Mesh)
u Struktol TR016
l A unique blend of specialty amide and calcium stearate

l Specialty amide provides sites that can hydrogen bond to filler for improved

wetting and dispersion

l Also a very effective metal release agent

u Struktol TR251
l Blend of TR016 and ethylenebis-stearamide (EBS)

l EBS portion provides improved dispersion to complement the wetting

characteristics of TR016
l Also a very effective metal release agent

u Struktol TR060
l Highly branched blend of resinous materials acts as an adhesive

(mechanical) dispersion aid

u Elastochem EF(DBDB)-60 (60% Peroxide on Wax)

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FORMULATIONS:

40% Wood Flour Composites

Material Resin Cont. A B C D E F

PP Resin 100 60 60 60 60 60 60 60
Wood Flour 40 40 40 40 40 40 40
TR251 1 2
TR016 1 2 1 1
TR060 1
60% Peroxide 0.1
TOTAL 100 100 101 102 101 102 102 101.1

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FORMULATIONS:

60% Wood Flour Composites

Material H I J K L M N
PP Resin 40 40 40 40 40 40 40
Wood Flour 60 60 60 60 60 60 60
TR251 1 2
TR016 1 2 1 1
TR060 1
60% Peroxide 0.1
TOTAL 102 101 102 101 102 102 101.1

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LABORATORY EXPERIMENT RESULTS:

Data generated is based on compounding on a Brabender PL2000 torque rheometer

using the bowl mixer equipped with cam blades at 160C and 90 rpm. The total time
of the mixing cycle was 4 minutes.

Capillary rheometer testing was performed on a Shimadzu CFT-500C equipped with a

10 mm by 1 mm diameter die and set at 190C. A variety of shear rates were used to
give a complete viscosity picture.

Physical property data was generated using injection molded test specimens prepared
on a Cincinnati Milacron 33 ton lab molding machine. The temperature/pressure
profile was:
Barrel 355-365F
Nozzle 370F
Mold 100F
Pressure 1200 psi

The wood flour was dried overnight at 100C prior to processing.

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BRABENDER MIXING DATA:
40% Wood Flour Composites
Cont. A B C D E F
Peak Torque, Nm 90 68 57 67 62 65 55
Torque @ 2', Nm 11 13 10 12 12 11 9
Torque @ 3', Nm 9 11 8 11 11 10 6
Torque @ 4', Nm 9 11 7 11 10 10 5
Equilibrium Temp, C 174 172 171 175 172 173 169
Metal Release Rating + ++++ ++++ +++ +++ +++ ++

60% Wood Flour Composites

H I J K L M N
Peak Torque, Nm 100 68 57 59 58 65 64
Torque @ 2', Nm 16 15 15 16 14 14 9
Torque @ 3', Nm 13 13 13 14 13 13 7
Torque @ 4', Nm 11 13 12 13 12 12 6
Equilibrium Temp, C 184 181 180 181 180 179 171
Metal Release Rating + +++ ++++ +++ +++ +++ ++
Metal Release + = Poor ++ = Fair +++ = Good ++++ = Excellent

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PRELIMINARY CONCLUSIONS:

Review of the mixing data indicates that there is very little effect on the
viscosity/processability of the compounds even by adding relatively high levels
of lubricants (up to 2 phr). The only significant effect was on Peak Torque.
Based on the Peak Torque data we have established that the mixing procedure
is the primary cause of this drop in torque.

Our current mixing procedure includes dry blending the formulations in a

Waring blender (simulation of Henschel mixer) prior to melt compounding on
the Brabender. We established that the inclusion of an adhesive, lubricant
and/or surfactant significantly increases the bulk density of the resulting
powdered dry blend, allowing for easier incorporation of filler into the polymer
melt during mixing. Although this did not lead to a reduction in equilibrium
torque or the time to the peak torque, the overall energy used to mix was
significantly reduced.

The only other noted difference was metal release, which was improved
dramatically, although at varying degrees depending on the additive used.

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CAPILLARY RHEOMETER DATA:
40% Wood Flour Composites

Resin Cont. A B C D E F
30 kgf/cm @ 190C
Flow, g/sec 0.07 0.01 0.02 0.02 0.02 0.02 0.02 0.08
Viscosity, Pa s 102 564 423 305 382 350 387 89
Shear, sec-1 718 130 173 240 192 209 190 822
50 kgf/cm @ 190C
Flow, g/sec 0.16 0.04 0.05 0.08 0.05 0.06 0.06 0.31
Viscosity, Pa s 68 274 216 139 382 183 199 39
Shear, sec-1 1792 446 567 879 192 668 615 3126
80 kgf/cm @ 190C
Flow, g/sec 0.24 0.13 0.21 0.31 0.22 0.26 0.24 1.16
Viscosity, Pa s 79 152 90 62 89 74 82 17
Shear, sec-1 2482 1283 2167 3146 2209 2637 2394 11770

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 40% WOOD FLOUR COMPOSITE RHEOLOGY
LOG FLOW VS. PRESSURE

10

RESIN CONTROL A B C D E F

1
FLOW, g/sec

0.1

0.01
30 50 80
PRESSURE, kgf/cm2

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 40% WOOD FLOUR COMPOSITE RHEOLOGY
LOG VISCOSITY VS. SHEAR RATE

1000

RESIN CONTROL A B C D E F
VISCOSITY, Pa s

100

10
100 1000 10000 100000
SHEAR RATE, sec-1

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CAPILLARY RHEOMETER DATA:
60% Wood Flour Composites

H I J K L M N
30 kgf/cm @ 190C
Flow, g/sec * * * * * * *
Viscosity, Pa s * * * * * * *
Shear, sec-1 * * * * * * *
50 kgf/cm @ 190C
Flow, g/sec 0.01 0.01 0.01 0.01 0.01 0.01 0.04
Viscosity, Pa s 2226 3142 1561 3280 1200 1497 332
Shear, sec-1 55 39 78 37 102 81 368
80 kgf/cm @ 190C
Flow, g/sec 0.02 0.03 0.03 0.03 0.04 0.03 0.12
Viscosity, Pa s 1247 758 925 682 464 636 157
Shear, sec-1 157 258 211 287 422 308 1248

* Data too low to record

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 60% WOOD FLOUR COMPOSITE RHEOLOGY
LOG VISCOSITY VS. PRESSURE

10000
H I J K L M N
VISCOSITY, Pa s

1000

100
50 80
PRESSURE, kgf/cm2

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NEW CONCLUSIONS:

The capillary rheometer data tells us that the torque data generated during the
Brabender mixing phase is not directly correlative with the viscosity of the
composites over a range of pressures. As we expected, the presence of the
additives caused significant improvements in flow (reductions in viscosity), with
the greatest difference shown in the higher pressure profiles.

The most dramatic viscosity change occurred in compounds "F" and "N".
These formulations both contained 0.1 phr of a 60% peroxide on wax
concentrate. As shown in the data, this very small amount of peroxide
decreased the compounds' viscosity to levels near or lower than the neat
polypropylene resin.

At this point we have shown we can formulate a compound with high filler
loading that processes with the same viscosity as the neat resin.

But do we get improved physical properties??

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PHYSICAL PROPERTY DATA (BEST FLOWING COMPOUNDS):
40% Wood Flour Composites
Cont. A D E F
Izod Impact, ft lbs./in.
Notched 1.3 1.3 1.3 1.4 1.4
Unnotched 2.3 3.0 2.7 2.7 2.5
Flexural Properties, MPa
Strength 49.3 46.1 39.6
Modulus 3390 3300 2810
60% Wood Flour Composites
H L N
Izod Impact, ft lbs./in.
Notched 1.3 1.3 1.4
Unnotched 2.3 2.3 2.3
Flexural Properties, MPa
Strength 42.1 37.8 38.6
Modulus
5050 4790 4550
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FINAL CONCLUSIONS:

u The use of process adhesives, lubricants and surfactants can significantly

improve the processability of woodfiber composites. In addition to improved
processability we see:
Significant improvements in mold release
Improved surface appearance
Maintained or improved physical properties

u The addition of a very small amount of peroxide into the compound allows for
an extremely high flow material (higher than the base resin) combined with the
physical properties of a highly filled compound. This is important for thin part or
high surface area injection molding.

u Compounds with high levels of filler can be processed the same as compounds
with lower level of fillers using the right additive package.

u The slightly lower flexural modulus values indicate more continuity of the
polypropylene phase resulting from better dispersion of the wood flour.

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The presenter would like to thank the following for their assistance in preparing this
presentation:

u S. Neal Kendall, Research Associate

u E.K. Koss, Research Engineer
u Dr. John VanderKooi, Manager of Research and Development
u ARDL - Plastics Testing Division

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