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Haake Mixer
Haake Mixer
Polymer Testing
journal homepage: www.elsevier.com/locate/polytest
Test method
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 25 October 2013
Accepted 2 December 2013
HAAKE MiniLab is an apparatus specially designed for compounding polymer material and
on-line testing of rheological properties. For the rst time, it was used to establish a dynamic speed test method for the rapid determination of steady-state torque of polymer
melts. The choices of sample feed quantity and screw rotation speed, as well as calibration
for real torque, were carefully studied before torque measurements. The repeatability and
reliability of torque data were also evaluated. Results showed that the torque could be
calibrated by subtracting the torque without samples. Also, a feed quantity of ca. 6 g with a
dynamic speed test range of 10105 r/min was suitable for the determination of steadystate torque of polyolen samples. The new method was quick, effective and reliable to
correlate the steady-state torque with rotation speed. Therefore, MiniLab would be a very
useful tool in exploring and characterizing polymer ow behavior through its torque
measurements.
2013 Elsevier Ltd. All rights reserved.
Keywords:
HAAKE MiniLab
Steady-state torque
Dynamic speed test method
Repeatability
Reliability
1. Introduction
In the polymer eld, torque refers to the hindering force
met when polymer resins or compounds are plasticized
and mixed with rotation of screws or rotors. It has been
used as an engineering indicator to learn the polymer
melting process for determining suitable processing conditions, as well as to monitor industrial extrusion production for process quality control. Steady-state torque is the
measurement of the torque at equilibrium as the plasticized material is in a stable and homogeneous melt state.
For a pure polymer in a given process, the steady-state
torque is a characteristic of the polymer, which can be
used as a rheological parameter to characterize the polymer ow behavior [14].
The torque-rheometer is the most commonly used tool
in polymer processing laboratory for torque measurements.
It can simulate a mixer and the extrusion process in nearly
* Corresponding author. Tel.: 86 028 85460817; fax: 86 028
85402465.
E-mail address: wgli2007@126.com (W. Li).
0142-9418/$ see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.polymertesting.2013.12.001
139
Table 1
Characteristics of materials used.
Material Grade
HDPE
HDPE
LDPE
iPP
Melt ow index
(g/10 min)
Supplier
unit (2), extruder housing (3) and feeding device (5). The
control system includes the manual operating panel (4) and
the application software (1). Both the dynamic speed
measurement and the experimental data documentation
can only be performed through the software. The drive unit
offers motor motion and precisely controls experimental
conditions, such as testing temperature and rotation speed.
It also measures the motor torque from a mixer sensor. The
structure of the extruder housing with co-rotation twin
screws is displayed in Fig. 2 (the co-rotation mode was used
in this study). The lled-in sample can be extruded in a
circulation via an integrated backow channel. The backow channel is constructed as a rheological slit capillary
with two pressure sensors. While the sample is extruding
through the backow channel, the rheological information
about the viscosity of the sample can be obtained from the
two pressure sensors. Lastly, the feeding device enables
periodic sample feeding by the piston of a pneumatic
cylinder.
2.3. Dynamic speed test method
There are two stages in the dynamic speed test method.
In the rst stage, samples were dynamically plasticized and
melted under a rotation speed range predetermined according to the requirement of the experiment and the nature of the material. The number of speed points was set to
520 with equal distance logarithmic intervals (rpm)
within the speed range. At each speed, the software program measured the torque of the material, and then
2. Experimental
2.1. Materials
All the samples in this study were carefully selected
from commercial resins. These were high-density polyethylene (HDPE), low-density polyethylene (LDPE) and
isotactic polypropylene (iPP). The characteristics of the
materials were shown in Table 1.
2.2. Instrumental details
The HAAKE MiniLab, as illustrated in Fig. 1, is made up of
ve functional elements: control system (1 and 4), drive
Fig. 1. The constitution of HAAKE MiniLab: (1) and (4) control system, (2)
drive unit, (3) extruder housing, (5) feeding device.
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Fig. 5. The steady-state torque of 6070 EA plasticized under different rotation speed.
plasticized at a xed speed of 100 r/min, the torquerotation speed curve dramatically declined with
increasing speed as compared to that of other two samples.
This trend indicates that polymer chains had been greatly
degraded under that plasticizing condition.
Thus, from the above results, a dynamic speed range of
10105 r/min was chosen for torque measurements. This
speed range was appropriate enough for the preparation of
samples with identical melt states. Therefore, the true
torque values can be obtained within a relatively wide
speed range.
3.4. Evaluating the repeatability of torque data
Repeatability of measured data must be a primary criterion of how well an instrument works. Fig. 6 shows the
torque-rotation speed curves of 6070 EA measured at
different times (on March 23, May 17 and June 6 of 2012,
respectively). It can be seen that, although there was a
small deviation of data at the speeds of above 80 r/min, the
highest standard deviation was only 2.15% (at a speed of
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