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Melt Shear Viscosity of Original and Recycled PET PDF

This paper examines the melt shear viscosity of original and recycled polyethylene terephthalate (PET) using rotational and capillary rheometry over a wide range of shear rates and temperatures. Flow curves were measured for pure original and recycled PET materials at 270, 280, and 290°C. The original PET showed decreasing viscosity with increasing temperature, while recycled PET exhibited similar temperature-dependent behavior with potentially higher degradation due to recycling and grinding processes. The rheological analysis provides insight into the molecular structure changes that occur during recycling.
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0% found this document useful (0 votes)
64 views7 pages

Melt Shear Viscosity of Original and Recycled PET PDF

This paper examines the melt shear viscosity of original and recycled polyethylene terephthalate (PET) using rotational and capillary rheometry over a wide range of shear rates and temperatures. Flow curves were measured for pure original and recycled PET materials at 270, 280, and 290°C. The original PET showed decreasing viscosity with increasing temperature, while recycled PET exhibited similar temperature-dependent behavior with potentially higher degradation due to recycling and grinding processes. The rheological analysis provides insight into the molecular structure changes that occur during recycling.
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© © All Rights Reserved
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Journal of Physics: Conference Series

PAPER • OPEN ACCESS

Melt shear viscosity of original and recycled PET in wide range shear
rate
To cite this article: Attila Bata et al 2018 J. Phys.: Conf. Ser. 1045 012007

View the article online for updates and enhancements.

This content was downloaded from IP address 139.81.155.14 on 17/07/2018 at 15:09


3rd Internatiomal Conference on Rheology and Modeling of Materials (ic-rmm3) IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1045 (2018)
1234567890 ‘’“” 012007 doi:10.1088/1742-6596/1045/1/012007

Melt shear viscosity of original and recycled PET in wide


range shear rate

Attila Bata, Gergely Toth, Dorottya Nagy, Karoly Belina


Department of Materials Technology, Faculty of Mechanical Engineering and
Automation,
John von Neumann University, Hungary

E-mail: bata.attila@gamf.uni-neumann.hu

Abstract. Among the plastic materials, the PET is the most often used one. The collecting of
the material to be recycled is partially solved. This way we have great quantity of reground
PET. During the regrinding the structure of molecules changes and these properties can be
measured by rheology methods. Polymer melts are -Newtonian fluids and the flow curves of
the materials can be used to characterize the molecular weight and the molecular weight
distribution. This research is focused on the characterization of original and ground PET
materials. Inherent viscosities were determined to characterize the materials. Flow curves of
pure and blended materials were measured at different temperatures.

1. Introduction
Nowadays polyethylene terephthalate (PET) is one of the most common plastics, also because of its
wide spread use. For the PET bottles there are certain places where recycled PET is already used and
produced. In this case, about 10-25 % of the recycled PET is used. Our goal is to increase the quantity
of the recycled PET. From the recycled materials the new bottles, products can be made. This requires
a development path and a more sophisticated technology since it is not easy to determine for once used
bottle what was stored in it, how it was used previously [1]. PET is a hygroscopic thermoplastic
polymer, therefore drying process is very important, since it affects the rheological properties of the
material, the subsequent processing, and the product characteristics [2].
The rheological analysis mentioned in this paper is of polyethylene terephthalate (PET) base
material, in which a specific raw material - a melt viscosity of structural, elastic and viscoelastic
behavior was investigated. The study was carried out by ARES-G2 type oscillational rheometer, and
capillary rheometer with which the material was examined at the low and the high shear rate. The
Goettfert Rheograph 25 original granulate was analyzed between 270-290 °C. Then, the original raw
material was processed with injection molding machine and then it was granulated again. There was a
full investigation at the same temperatures. The measuring values are presented on diagrams and from
these the conclusions were drawn.

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution
of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.
Published under licence by IOP Publishing Ltd 1
3rd Internatiomal Conference on Rheology and Modeling of Materials (ic-rmm3) IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1045 (2018)
1234567890 ‘’“” 012007 doi:10.1088/1742-6596/1045/1/012007

2. Experimental
2.1 Material
RAMAPET N180 is a general purpose, non-reheat PET resin for bottles, film, thermoformed
containers and other transparent applications. It has good optical properties, the mechanical properties
are representative for a PET resin.
The PET is hygroscopic, and since moisture adversely affects the IV during the melt processing of
the polymer, it must be dried prior to molding. Undried PET pellets can contain up to 0.2 % (2000
ppm) of moisture. After drying, the moisture content is typically below 50 ppm [3].
The PET has good surface hardness, stiffness, and dimensional stability that absorbs low volume of
moisture. The PET material is heat-resistant until 180 °C, it does not decrease in strength, its melting
temperature is around 260 °C. Above 250 °C the crystallite section is continuously disappearing, so
the melting process of the material could be observed. Usually, the material is processed in the molten
state, so it is worth to study the rheological properties only above this temperature point [4]. The
measurements were performed at 270 °C, 280 °C and 290 °C.

3. Method
3.1 The rotational viscometry
Our measurements were performed by a shear viscosity investigation method; that means a low range
of shear rate and temperature steps near the processing temperature. This was the reason why the
rotational viscometry was measured in the low shear rate range (0.05 – 20 1/s). With the rotational
viscometry we could measure torsion flow in a polymer melt between parallel plates. The measuring
technique conceptual layout is shown in Fig. 1. The CMT means combined motor and transducer
concept [5].

Figure 1.Rotation viscometry CMT conceptual layout and


marking system [5]
From the marking system the stress, deformation and deformation rate components can be calculated
with the equations described below:

(1)

(2)

(3)

2
3rd Internatiomal Conference on Rheology and Modeling of Materials (ic-rmm3) IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1045 (2018)
1234567890 ‘’“” 012007 doi:10.1088/1742-6596/1045/1/012007

where r is the circle plate radius; h is the gap between the plates; is the driving engine rotation (rad); is
the driving engine angular speed (rad/s) and M is the torque (Nm) [5].
The stress and deformation rate can be calculated from expressions (1) to (3) and the shear viscosity
can be defined. It is a frequent measuring technique to determine shear viscosity for small molecular
liquids, or oils and thermoplasts at low shear rate. With this method we can measure at higher
temperature (to 600 °C) and monitor the degradation process. For our testing we used the SMT
(Separate motor and transducer) conceptual TA Ares G2 type rotation viscometer with 25 mm parallel
circle plates and 0.4 mm gap. In this type of rotation viscometer the drive engine and the transductor
are separated [6].
3.2 The capillary rheometer
The capillary rheometer is a measuring device in which we are able to measure the shear viscosity of
thermoplastics. The shear rate ranges between 100 and 10 000 1/s near to the processing temperature
[7].
The GoettfertRheograph 25 capillary rheometer was used. The measuring method is based on
continuous melt flow in known geometry capillary(ies), while the pressure drops is measured between
the capillary inlet side and the atmospheric pressure (Fig. 2.).

Figure 2.Capillary rheometer conceptual layout [7]

The variable parameters are the barrel temperature and the piston speed (parallel to the deformation
rate). In this case, the shear viscosity depend on temperature and deformation (shear) rate. In our tests,
the shear rate changed between 100-10.000 1/s and the barrel temperatures changed in three steps
around the material supplier recommended process temperature.
The measuring method uses two other geometry capillaries because of the entrance and exit effects
(pressure drop). With this equipment in one step we can do the Bagley correction (correct the pressure
drop) which gives the real shear viscosity [8].

4. Results
4.1 The capillary rheometer
The viscosity curves were determined as functions of the shear rate. The measurements were
performed with original material and with recycled material. The viscosity of the original material is
shown in Fig. 3.

3
3rd Internatiomal Conference on Rheology and Modeling of Materials (ic-rmm3) IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1045 (2018)
1234567890 ‘’“” 012007 doi:10.1088/1742-6596/1045/1/012007

Figure 3.Original PET shear viscosity curves

The curves at different temperatures are not the same. It can be observed that the viscosity is the
highest at 270 °C. The higher is the temperature, the lower is the viscosity. From the differences of the
curves, the transformation of the molecular structure can be determined. The viscosity of the recycled
materials is shown in Fig. 4.

Figure 4. Recycled PET shear viscosity curves

The recycled material shows the same tendency (Fig. 4). Increasing the temperature the viscosity
decreases. During the recycling and grinding processes, the molecules in the materials can easily
degrade. This is caused by the rising thermal and mechanical strain during the processes. The
degradation makes the molecular weight lower, so the molecular density dispersion widens. The
polymer with shorter chains can move easier.Above the glass transition temperature the segments of
the polymer move increasingly.The viscosities of the original and recycled materials are shown in Fig.
5.

4
3rd Internatiomal Conference on Rheology and Modeling of Materials (ic-rmm3) IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1045 (2018)
1234567890 ‘’“” 012007 doi:10.1088/1742-6596/1045/1/012007

Figure 5. Original and recycled PET shear viscosity curves

In each diagram the viscosity curves show a typical form (Fig. 5). In the curves of newtonian fluids it
could be recognised that the curves are almost linear and not dependent on the shear rate. In our
measurements, the viscosity curves approach the horizontal line, but they do decrease within a small
range. It was confirmed that these materials behave like non newtonian fluid. At a constant
temperature, the difference between the original and the recycled materials approaches 150 Pa*s. The
impact of the recycling is the continuously decreasing molecular weight. The lower molecular weight
means easier molecular movement.
4.2The capillary rheometer
The measurements were performed with original material and with recycled material. The viscosities
of the original and recycled materials are shown in Fig. 6.

Figure 6. Original and recycled PET shear viscosity curves

5
3rd Internatiomal Conference on Rheology and Modeling of Materials (ic-rmm3) IOP Publishing
IOP Conf. Series: Journal of Physics: Conf. Series 1045 (2018)
1234567890 ‘’“” 012007 doi:10.1088/1742-6596/1045/1/012007

Comparing the data to the 270 °C viscosity curve in the lower shear range: There is a ~30 – 35 %
reduction at 280 °C, and at 290 °C we can see a 40 – 50 % reduction. As we approach the larger shear
ranges (10000 - 18000 1 / s) the differences are reduced: at 280 °C ~15 – 18 %, while at 290 °C ~7 –
13 %. In the initial shear speed range, the recycled material shows a 70 % reduction at 270 °C, while
in the higher shear range this value shows a 15 % - 30 % reduction. We could observe the following
viscosity reductions in the results: at 280 °C, ~ 65 % and at 290 °C ~ 50 %. Although the initial
viscosity values at 290 °C show a different tendency compared to the curve we measured at the
previous two temperatures, this can be attributed to a measurement error with a great certainty. From
these values we can conclude that we have to consider the viscosity change of the material during the
recycling, because with such a degree of deviation we could assume that the material will not be able
to withstand the requirements, which are set by design.

5. Conclusion
In our investigation we measured one type of material, but the temperature of the process was
different. An original and a recycled material were examined. The measurements were performed by
an ARES G2 rotational rheometer and Goettfert Rheograph 25 capillary rheometer at 270 °C, 280 °C
and 290 °C. The shear rate was changed from 0.05 to 20 1/s and 100-10 000 1/s. It was determined
that the viscosity of the recycled material is lower than the value of the original material at each
temperature. The molecules of the recycled material were supposed to shorten during the grinding
process. If the temperature increases, the shear viscosity decreases, but there was no linear correlation
between these two variables. The structure viscous behavior of the polymer melt was revealed. This
area offers lot of possibilities for future research, so we hope to continue with further investigations.

6. Acknowledgement
This research is supported by the EFOP-3.6.1-16-2016-00014 project. The Project is supported by the
Hungarian Government and co-financed by the European Social Fund.
References
[1] Ronay F 2006 Physical Recycling of the Material of PET Bottles (in Hungarian) PhD Thesis,
Budapest University of Technology and Economics
[2] Czvikovszky T, Nagy P, Gaal J 2000 The basics of polymer technology (in Hungarian)
University publisher Budapest. http://www.tankonyvtar.hu/hu/tartalom/tkt/polimertechnika-
alapjai/adatok.html
[3] http://plasticker.de/recybase/docs/27055_1463559873.pdf
[4] Ronkay F, Czigany T 2004 Properties Modifying of Recycled PET with Additives. Proceedings
of the Fourth Conference on Mechanical Engineering Hungary, 170-174
[5] General Rheo Training_2015_v1 with Questions
https://www.scribd.com/document/340563607/General-Rheo-Training-2015-v1
[6] TA Instruments Factory Ares G2 Rotational Viscometer Equipment Education Material – Study
of Rheology Theory and Applications http://www.tainstruments.com
[7] Szucs A 2010 Investigation Polimer Melt Properties High Shear Rate (in Hungarian) PhD Thesis,
University of Miskolc www.kerpely.uni-miskolc.hu/downloads/docs/cikkek/szucsandras-
ertekezes.pdf
[8] Toth G, Bata A, Belina K 2017 IOP Conf. Ser.: Mater. Sci. Eng. 175 012056
https://doi.org/10.1088/1757-899X/175/1/012056

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