Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?

id=14728088

Optimized extrusion techniques for ACM.

Title Annotation: polyacrylic rubber
Author: DeMarco, Robert D.
Date: Dec 1, 1993
Words: 2641
Publication: Rubber World
ISSN: 0035-9572

Over the past decide, the world wide automotive market has had to respond to governmental
regulations and public demand for vehicles with reduced environmental emissions as well as
improved fuel efficiency while maintaining vehicle performance. To meet these requirements
the automotive industry has made great strides with such innovations as catalytic exhaust
gas convertors, electronic fuel injection, front wheel drive-train systems, torque sensitive
automatic transmissions and turbo charged engine designs. In addition, an overall trend has
been the down-sizing of the vehicle itself. The sum result of these innovations is the
production of increasingly smaller automobile designs with more and more compact engine
compartments (ref. 1). This, in turn, has meant increased under-the-hood and service fluid
operating temperatures.

Under these conditions, traditional elastomers used in these applications are being replaced
by specialty elastomers with improved temperature and oil resistance (ref. 2). In the case of
engine and transmission oil cooling hose, nitrile rubber (NBR) has been used as the polymer
of choice for these applications, with good oil resistance (volume swell: ASTM #3 oil = 15 to
20%) but relatively poor high temperature resistance (110 [degrees]C) (ref. 3). This polymer
is now being replaced by polyacrylic rubber (ACM), which has superior heat (165
[degrees]C), and oil (volume swell: ASTM #3 oil = 10 to 25%) resistance to meet new
application requirements (refs. 4 and 5). ACM elastomers are polymers of acrylic acid esters,
which are inherently resistant to hot air, oil and ozone due to a highly saturated polymer
backbone (refs. 4 and 5)

Engine oil and transmission oil cooler hoses require the following properties (ref. 3):

* Low Compression set for good coupling retention ensuring leak free performance;

* good high temperature resistance for long term hose usage;

* good resistance to engine and transmission oil fluid;

* resistance to service fluid additive packages;

* low temperature flexibility.

Typical polyacrylic hose compounds are capable of providing what is shown in table 1. (ref.
6).
Table 1 -typical polyacrylic hose compounds
are capable of providing (ref. 6):

1. Compression set: 20/40% ASTM D395

(70 hr. @ 150 [degrees]C) Method B

1 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

2. Heat resistance 150 [degrees]C Continuous

200 [degrees]C Intermittent
3. Volume swell: +10/25% ASTM #3 oil
(70 hr. @ 150 [degrees]C) +2/10% Engine oil
0/+3% ATF
4. Low temperature -30/-40 [degrees]C ASTM D1053
flexibility: Gehman T100

To assist hose manufacturers in the processing of polyacrylic compounds, a design of

experiments was developed to statistically model the extrusion process. These models can
be useful in evaluating the complex interactions between ACM Compound, machine and
tooling parameters, as they relate to productivity and extrudate appearance. Once refined,
these models can yield extrusion settings required to achieve an optimum balance of output
rate and surface appearance. No attempt was made to relate the findings to fundamental
compound rheological characteristics.

Experimental

The polyacrylic compound formulation used in this experiment is shown in table 2. Mooney
viscosity, rheometer and physical property data for this compound are listed in table 3.
Extrusion evaluations of the ACM compound were performed on a cold feed extruder with
dimensions listed in table 4.
Table 2 -experimental

HyTemp ACM polymer: 100

(dual carboxyl/chlorine cure site)
Stearic acid 1
Octylated diphenylamine 2
Fatty acid ester 2
N326 HAF, carbon black 90
Ether/ester plasticizer 5
Sodium stearate 4
Diuron 2
206

[TABULAR DATA OMITTED]

Table 4

Screw type: Double wave: constant double

and single lead feed screw
Screw diameter: 38 mm
L/D ratio: 20:1
Compression ratio: 2:1
Tube die: 11 mm internal diameter
15 mm outer diameter
Tube die: Electrically heated
Die land length: 1x = 6mm
2x = 12mm

Machine parameters

Part one of this experiment statistically models the effect of the following machine parameters
on the extrusion process (refs. 7-9).
Screw speed (R): RPM 10, 30,50
Screw temperature (S) ([degrees]C) 60, 70, 80

2 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

Barrel profile temps. (B) ([degrees]C) Constant-60; Constant-80;

Ramped (60, 70, 80)

A design of experiments worksheet was generated through the utilization of statistical

software program RS/Discover (ref. 10). The worksheet was based upon the following
statistical modeling criteria:
Objective: Response surface model
Design type: D-optimal
Model type: Quadratic
Total candidates: 27 runs
Design candidates: 14 runs
Design model: (9) terms
1 1
2 S
3 B
4 R
5 S*B
6 S*R
7 B*R
8 S**2
9 R**2

Machine parameter combinations according to the design worksheet were inputed into the
extruder where the process was allowed to come to steady state conditions over a period of
approximately 15 minutes prior to taking any response measurements on the resulting
extrudate (ref. 7).

Tooling parameters

Part two of this experiment statistically models the effect of the following tooling parameters
on the extrusion process (refs. 7 and 9):

Die temperature (D) [degrees]C 85, 95, 105

Land length (LL) 1X, 2X

A design of experiments worksheet was generated, as before. The worksheet was based
upon the following statistical modeling criteria:
Objective: Response surface model
Design type: D-optimal
Model type: Quadratic
Total candidates: 27 runs
Design candidates: 14 runs
Design model: (5) terms
1 1
2 D
3 LL
4 D**2
5 D*LL

The extrusion settings listed below were used for this portion of the experiment:

3 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

Screw speed (rpm): 35

Screw temperature ([degrees]C): 70

Barrel temp. profile ([degrees]C): ramped A list of measured design responses is in table 5.

[TABULAR DATA OMITTED]

Discussion of results

Response model analysis

Analyses of variance (ANOVA) (ref. 11) tables for each of the design response models were
generated and are available from the authors. These tables enable us to look at the ratio of
the output response signal to model variability in order to determine which machine/tooling
parameters have a statistically significant effect on our output response. The accuracy or
sensitivity of each model can be expressed as the percentage R-squared (R-SQ)(ref. 12).
This number is defined as the percent variability in each response factor which can be
explained by the correlation model. An R-SQ of 100% means all response variability can be
explained by our design model.

In the upcoming discussion of results we will refer to the terms "predicted main effects" and
"adjusted output responses." Predicted main effects can be defined as average effect or the
slope of each response ignoring interactive and quadratic effects (ref. 10). This information is
useful in determining which parameters have overall dominating effects on the output
response being modeled. Adjusted output response curves are plots of selected
machine/tooling parameters against the chosen response variable with all other
machine/tooling parameters set at their average value (ref. 10). Though useful in seeing how
a variation of a single setting might affect an output response, it should be noted that the
response plots will differ with changes away from the average process settings. This is
especially true where interactions between process parameters exist.

Extrusion response: based on machine parameter changes

Output temperature

This model shows that the only statistically significant machine parameter effect on output
temperature is screw speed. Predicted main effects and adjusted response curve for
extrudate output temperature are shown in figures 1 and 2. From these plots it is shown that
screw speed has an increasing quadratic effect on extrudate output temperature.

Linear output

In this model we can see that not only are screw speed, barrel profile and screw temperature,
to be statistically significant, but there also exists an interaction between screw and barrel
temperature profiles with screw speed. Figure 3 shows the predicted main and interactive
effects of screw temperature with screw speed. Figure 4 shows the predicted main and
interactive effects of barrel temperature profile with screw speed. In each case it shows that
we are capable of achieving a larger increase in linear output with higher screw and barrel
profile temperatures. Figure 5 shows the adjusted linear output response as affected by
screw temperature, barrel profile temperature and screw speed. From this figure we can
conclude that increase in screw speed is the dominant factor in controlling linear output.

4 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

Mass output

Here our model indicates that not only screw temperature, barrel profile temperature and
screw speed affect mass output, but there also exists an interaction between screw
temperature and screw speed. Figures 6 and 7 show the predicted main and interactive
effects of screw temperature and barrel profile temperature with screw speed. Here we see
that screw speed is the overriding factor in controlling mass output. Adjusted weight output
response for each of the machine parameters is illustrated in figure 8.

Head pressure

This model shows that the only machine parameter which has an effect on head pressure is
screw speed. Figure 9 shows die predicted main effects of screw speed on head pressure.
Figure 10 illustrates the quadratic effect of screw speed.

Appearance

In this model both barrel temperature profile and screw speed are shown to have statistically
significant effects on surface appearance of the extrudate. Extrudate appearance is improved
with decreases in screw speed and with a constant 60 [degrees]C barrel temperature profile.

Overall machine parameter effects

Screw speed

Screw speed has an overriding effect on all measured extrusion process responses. Here we
can conclude that increased screw speed causes quadratic increases output temperature,
mass output and bead pressure, as well as linear increases in linear output. Decreased
screw speed causes improvements in surface appearance.

Screw temperature

Screw temperature has no statistically significant effect on output temperature, head

pressure and surface appearance. Screw temperature does, however, have an interactive
effect with screw speed for both linear and mass output. Increases in screw temperature
cause significantly larger increases in linear and mass output at higher screw speed settings.

Barrel temperature profile

Barrel temperature profile has no statistically significant effect on output temperature and
head pressure. A low, constant 60 [degrees]C barrel profile temperature will provide an
extrudate with the best surface appearance, though, a higher constant 80 [degrees]C profile
will yield the greatest mass output. There also exists an interaction between barrel
temperature profile and screw speed on the linear output response. Here an increased barrel
temperature profile of a constant 80 [degrees]C causes significantly greater linear output at
higher screw speeds than al lower screw speeds.

Extrusion response: based upon tooling parameter changes

Output temperature

This model shows both die temperature and land length to have a statistically significant
effect on output temperature. Increases in both die temperature and land length cause
increases in output temperature.

5 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

Linear output

This model shows that both the temperature and land length have a statistically significant
effect on linear output. Increases in both the temperature and land length cause increased
linear output.

Mass output

This model indicates that both die temperature and land length have a statistically significant
effect on mass output and an interaction exists between die temperature and land length. At
low die temperatures, mass output actually decreases with an increase in land length. At
higher die temperatures, this does not seem to be the case. Increases in both die
temperature and land length cause increased mass output with die temperature being the
dominating factor.

Head pressure

Here our model indicates both die temperature and land length have statistically significant
effects on head pressure, and an interaction exists between die temperature and land length.
It was found that with low die temperatures larger head pressure increases can be expected
with increased land length. Increased die temperature causes decreased head pressure and
increased land length causes increased head pressures.

Appearance

This model shows that both die temperature and land length have statistically significant
effects on the surface appearance of the extrudate. Land length is the dominant factor in
controlling surface appearance. Extrudate appearance is improved with increased die
temperature and decreased land length.

Overall tooling parameter effects

Die temperature

Increases in die temperature cause significant quadratic increases in output temperature and
linear increases in mass output when compared with the effect of longer land lengths. There
is also an interactive effect between die temperature and land length on mass output.
Increases in die temperatures cause a greater effect of increased mass output at longer land
lengths than with shorter land lengths. It is also noted that increases in die temperatures
have more significant effect on mass output than do increased land lengths. Of particular
significance is the drastic improvement of extrudate surface appearance seen with increases
in die temperature.

Land length

Increases in land length are found to have significant effects on increasing linear output but
only marginal effects on increases in mass output. There also exists an interactive effect
between land length and die temperature on head pressure. Head pressure increases
associated with increased land length can be minimized with increased die temperatures.
While increased land length is shown to have only marginal effects on increasing output
temperature it has greatly negative effects on surface appearance.

Optimized extrusion settings

6 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

Table 6 shows optimized extrusion settings for linear output and appearance based upon the
statistical models for machine parameters as generated by the RS-1 software program. It is
noted that increased linear output is inversely related to surface appearance. Table 7 shows
optimized extrusion settings for output and surface appearance based upon the statistical
models for tooling parameters. It is noted here that high outputs and good surface
appearance can be achieved through increased die temperatures.

[TABULAR DATA OMITTED]

Table 7 -optimized tooling parameter settings

Factor/response Range Optimized settings

Factor: for: Appearance
Die temp. 95 to 106 105
Land length Ramp/constant 80 1x
Response:
Output temp. 96.2
Linear output 121.5
Mass output 309.1
Head pressure 14.1
Appearance (4.4)

Based upon the design models and optimization presented in this article we can make some
general recommendations in the setting of machine and tooling parameters for the extrusion
of polyacrylic tube profiles with the best surface appearance. Linear outputs would be
maximized by increasing screw speeds to a level providing a stock temperature below that of
its scorch temperature.
Screw temperature: 80 [degrees]C
Barrel temp. profile: Constant 60 [degrees]C
Land length: Short (1x)
Die temperature: 105 [degrees]

Conclusions

A statistical model was developed to evaluate the performance of a typical extrusion grade
polyacrylic rubber compound. The model developed was capable of predicting key output
responses of the extrusion process: extrudate output, temperature, surface appearance and
head pressure. Complex interactive relationships between key extrusion parameters: screw
speed, screw temperature, barrel temperature profile, die temperature and land length were
identified. The statistical model, based upon relatively few experiments, was used to generate
optimized extruder/tooling settings. The importance of optimizing extrusion parameter and
tool settings to achieve high output rates and excellent surface appearance was determined.

References

[1.] Nakamura, Motoyama, Kiyota, "Passenger car engines for the 21st century,"
SAE Technical Paper Series #911908, (1989). [2.] J.R. Dunn, Elastomerics, Vol 11, No.3,
"Elastomeric materials for demanding automotive applications," 18 (1992). [3.] Hosoya,
Nakagawa, Yagishita, A new polyacrylic elastomer cure system for automatic transmission
fluid (ATF) hose, " SAE Technical Paper Series: #880028, (1988). [4.] P. Starmer,
"Acrylic elastomers: 1947 to 1987" Zeon Chemicals Technical Bulletin: PA 0900.0. [5.] R.
DeMarco, R. Flecksteiner, "Polyacrylic elastomers" Zeon Chemicals Technical Bulletin: PA
901.0. [6.] "Acrylic elastomers for automotive hose applications, Zeon Chemicals Technical

7 -> 8 05.05.2010 22:18

Optimized extrusion techniques for ACM. http://www.thefreelibrary.com/_/print/PrintArticle.aspx?id=14728088

Bulletin: PA 0740.1. [7.] McCormick, Christy, Lue, "Coldfeed vented extruders for hose
manufacture" ACS Rubber Div. Paper 51, October 1982. [8.] P. Johnson, "Developments in
extrusion science and Technology" ACS Rubber Div. Paper #72, October 1982 [9.] J. White,
"Flow visualization and flow mechanisms of rubber compounds in the screw and die regions
of an extruder" ACS Rubber Div. Paper #6, October 1985. [10.] BBN Software, "RS/Discover
Release 3.0 Software: Reference Manual" Cambridge, MA, (1992). [11.] T.B. Barker "Quality
by experimental design" ASQC Quality Press, (1985). [12.] D.J. Wheeler "Understanding
industrial experimentation" SPC Press Inc. (1988).

COPYRIGHT 1993 Lippincott & Peto, Inc.

Copyright 1993, Gale Group. All rights reserved. Gale Group is a Thomson Corporation Company.

8 -> 8 05.05.2010 22:18