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Reprocessing of polypropylene material through injection moulding:


investigation of part quality, physical properties, processing properties and
mechanical properties

Conference Paper · July 2010

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PPS 26, Banff, Canada, 2010. Paper No. R01-472.

Reprocessing of polypropylene material through injection moulding:


investigation of part quality, physical properties, processing properties and
mechanical properties
S. A. Elsheikhi1*, L.Mulvaney-Johnson1, I.F. Campean1, T.Gough1 and P.D Coates1
1
IRC in Polymer Engineering, School of Engineering, Design and Technology, University of Bradford,
Bradford, United Kingdom- salahelsheikhi@gmail.com; l.johnson@Bradford.ac.uk;
F.Campean@bradford.ac.uk ; t.gough@Bradford.ac.uk and p.d.coates@Bradford.ac.uk

Abstract

We investigate the effect of the multiple injection moulding reprocessing stages of copolymer polypropylene
upon physical material properties such as mechanical stiffness and strength, melt viscosity, degradation
response, colour , molecular weight along with trends observed in process related measurements. This work
demonstrates that reprocessing of the material over seven successful repetitive stages is possible, where tensile
test specimens are manufactured under identical moulding conditions. The reprocessing of this material has
some effect upon molecular weight (-10%), shear viscosity (-11% at injection moulding shear rate range and
-33% at lower shear rate) and a clear effect on melt flow rate (+43%). Mechanical properties in term of Young’s
modulus, elongation at yield and flexural strength have a decrease of 15%, 25% and 11% respectively.
However, degradation analysis indicated that no premature degradation was noted at any stage. Little relative
increase of crystallinity, density and mass over seven stages were noted, 4%, 0.48% and 0.2% respectively from
virgin as a reference. Shrinkage calculations showed no considerable change over eight stages. Aesthetic
“quality” was assessed through colour measurements, and insignificant change were observed up to 3
reprocessing stages, however a notable change was observed beyond this point.

Key words: Injection moulding; polypropylene; regrind; reprocessing stages; viscosity; crystallinity and
mechanical properties.

1. Introduction Many researchers have conducted studies in the


area of polymer reprocessing through the injection
It is clearly very important to produce and consume moulding technology. These studies concerned the
plastic materials in an environmentally friendly entirely recycled material in form of post consumer
way. Thermoplastics constitute 85% of consumed materials/ material reclaimed from scrap yards
plastics in the world (Meran et al., 2008). (Meran et al., 2008), entirely virgin material (Lewis
Therefore, the reprocessing of the thermoplastics and Buser, 1997), and/or entirely mixed materials
and the usability of the reprocessed materials are (Xu et al., 2002).
gaining significance. For many manufacturers it is common practice to
Rising raw material costs, linked to increasing oil introduce reground sprues, scrapped parts, and
prices, increased consumer demand and increased runner systems into the injection moulding process.
environmental awareness have led to the This is advantageous for economic and
development of plastic reprocessing programs environmental reasons (La Mantia, 2002) and easy
(La Mantia, 2002). to implement because it doesn’t require any
Polymer reprocessing can be performed with sorting, filtering or cleaning operations usually
many different technologies: this work concentrates required with material coming from landfill sites or
on injection moulding which is one of the most post consumer or rubbish yards. However, it is
versatile and important technology that widely used important to ensure that part quality is not affected;
to process and reprocess different type of polymers. i.e. the properties of the reprocessed material
remain the same with virgin material. Therefore,
the process set up products in forms of sprues,
runners and unused parts were regrind and used in
this work.
*
Corresponding author: Common industrial practice is to mix regrind
Tel: +44(0)1274 234529 material with virgin material in ratios from 0-50%
Fax: +44(0)1274 235925 or higher (Lewis and Buser, 1997) , depending on
Email address: salahelsheikhi@gmail.com the customer specifications. Lewis and Buster
(1997) have investigated the effect of processing a decrease in percentage of 30%, 45% and 25%
low density polyethylene “LDPE” on tensile respectively from virgin to cycle number eight.
properties by adding 25% of regrind to the virgin This implies that the material has been successful
material with differential melt histories within the in retaining many of its useful properties even after
same batch. Their result showed that LDPE with exposing it to repeated heating and shearing cycles
25% of regrind can be added to the process without (Charbonneau, 1997).
affecting either the processability or the tensile In spite of many researchers have conducted
properties. This allows manufacturers to save studies in the area of polymer reprocessing through
money producing parts with regrind without being injection moulding, however, some essential
concerned with the effects it may have on the information still needed especially those that
tensile properties. Another study (Dontula et al., linked to the part quality, physical properties,
1994) reported in, based on high density processing properties and mechanical properties.
polyethylene “HDPE” with different regrind ratios Therefore, the lack of comprehensive investigation
of 0%, 50% and 100% , found that the melt of these properties (for some materials such like
temperatures didn’t change between virgin to 100% co-polymer PP) over successive reprocessing
regrind, and the Young’s modulus was found to be stages make the examination of these properties is
the same between the three regrind ratios(virgin, interested and useful, especially, if connected to the
virgin +50% regrind and 100% regrind). industry. On other world, in industry, this could
Reprocessing of recycled materials or reclaimed help to know more accurate and varying
from post-consumer waste material feedstock is information for these properties, in order to satisfy
widely used in industry; however the product the customer who has a lot of requirements,
quality is an important challenge against the demands and specifications.
reprocessing operations. Therefore, the most In this work a comprehensive study on the
published studies of such recycling/reprocessing of current state of reprocessing polypropylene
such material have dealt with the effect of material for many times using 100% regrind
reprocessing on the physical and mechanical material (without considered the reprocessing of
properties of a range of polymers. The possibility post consumer wastes, but well controlled
of recycling and using recycled refuse LDPE, reprocessing of samples) under the same moulding
HDPE and polypropylene “PP” were investigated conditions, and a focus on the investigations of
(Meran et al., 2008), and it was found that the PP is varying properties and to find the possible links
the material which can be most successfully between these properties.
recycled based on the tensile strength of the The strategy of this study aims have some
processed part. advantages:
Reprocessing of filled polypropylene is important
given that it has many applications especially for  To reuse the process set up products in
injection moulding (Dave et al., 1997) , and hence form of sprues runners and none used
it is interest to study the behaviour under repetitive parts.
reprocessing stages. Studies were reported on glass  To reduce material consumption and
fiber reinforced PP, paying particular attention to hence to improve the material
two important aspects of injection process: firstly productivity.
the heat history to which the material is subjected,  To reduce material cost.
and secondly, the number of times the material is
subjected to the shear of the screw (Guimond, The key properties under investigations are:
1997). The effect of four recycle histories on the
properties of 30% glass fiber reinforced  Part quality (mass, in-plane shrinkage and
polypropylene was investigated (Guimond, 1997). colour).
He found the tensile modulus, percentage of  Physical properties (density, crystallinity,
elongation at yield and impact strength do decrease thermal stability and molecular weight).
with each reprocessing cycle, but not at an  Processing properties (viscosity index,
alarming rate. It was found that the glass fibre do melt flow index, and melt viscosity at high
seem to shred when exposed to excess shred and and low shear rate).
grinding, but there was no sign of a major loss in  Mechanical properties (Young’s modulus,
mechanical properties, and hence it can be percentage of elongation at yield and
concluded that the glass fiber reinforced PP can be flexural strength).
effectively reprocessed and retain most of its
properties (Guimond, 1997). Charbonneau (1997) The material used through this study was high
examined the effect of eight reprocessing cycles impact copolymer polypropylene injection
using 40% long glass fiber on the mechanical moulding grade. Impact copolymer PP is widely
properties. It was found that the tensile strength, used in variety of applications for instant; in the in
tensile modulus and impact strength have the automotive it is used to produce battery cases;
in medical it is used for disposable syringes , also it that the tensile sample thickness is 4 mm , but the
is used for appliances and hand tools as well as the runner is 8 mm and will solidify after the tensile
rigid packaging containers and housewares sample. The processing settings are summerized in
( Karian, 2003). The reprocessing operations (see Table 1
Figure 1) were done under the same moulding
conditions by using 100% of regrind material in 2.3 Reprocessing sequence
form of product set up, runners and sprues without The reprocessing operations started by introducing
using any type of additive materials. 4.5Kg of virgin material. The first processing
cycle was named virgin as an output from virgin
2. Procedure material; and subsequent reprocessing cycles were
labelled stage 1, stage 2 and so on up to seven.
2.1 Material and sample preparation After each reprocessing stage, a number of
Injection moulding high impact copolymer specimens were extracted for testing and the
polypropylene (H814) supplied from ExxonMobil remainder (including runners and sprues)
chemical with melt flow rate of 14 grams/10 min granulated in a ‘Cumberland granulator’ with three
based on the technical data sheet of this material, tangential knives. A small portion of regrind
solid density , average molecular weight and shear material (about 300 grams) from every stage was
viscosity(at shear rate = 6000 sec-1) based on the kept for the related tests.
laboratory measurements, were 0.8918 grams/cm³,
206,000 g/mol and 14.24 Ps.sec , respectively. 2.4 Part quality
2.4.1 Specimen mass
The injection moulding machine used in this The mass of a product is commonly used as a “part
study was a 100 tonne clamp force FANUC quality” indicator and changes of specimen mass
(Roboshot S-2000i-100A) all-electric drive with can often be linked to changes in dimensions, and
screw diameter Ø = 32 mm and L/D = 22:1. The hence the stability in the specimen mass could
injected test part was a ASTM D638 tensile bar indicate to the stability of the part dimension. The
specimen with gage length of 90 mm, width of 10 specimen mass is obtained by measuring the test
mm and thickness 4mm. The moulding machine sample including the runner and sprue on
was fitted with a special nozzle adaptor that houses a standing mass balance for every reprocessing
a melt pressure with a Kistler melt pressure sensor stage then the average specimen mass was
type 6190A08 and a FOS melt infra-red (IR) calculated.
temperature sensor type MTS408-HT. These
sensors are computer monitored along with the 2.4.2 In-plane shrinkage
screw position and pressure from a transducer Shrinkage behaviour of a moulded plastic part
mounted at the back of the screw. The computer plays a principle role in determining final
monitoring system is a National Instruments (NI) dimensions of the part. Shrinkage occurs due to the
LabVIEW based software application. The signal thermal contraction of the molten material during
conditioning and interface system is through cooling and the relaxation of stretched polymer
a NI SCXI unit connected to a 12-bit PCI 6024E chains (Fathi and Behravesh, 2007). This
data acquisition card. phenomenon is affected by many factors including
Sample collection for subsequent testing on process parameters at filling, packing and cooling
viscosity index results will be discussed in more phases, cooling system design, and material
details in section 2.7.1. properties (Fathi and Behravesh, 2007).
In-plane shrinkage was measured in several
2.2 Injection moulding conditions locations on the specimen.
The melt processing temperature was set to 225 °C,
based on the material technical data sheet. The Five samples were selected for each
mould temperature was set to 25 °C which was also stage to measure the shrinkage; Equation 1
the minimum controlable setting for the mould (Mamat et al., 1994) was used to determine the in
temperature controllers (Regloplas type 90s). Melt plane shrinkage in as a percentage of the cavity
plastication condition was set to 150 rpm for screw dimension.
speed and 80 bars for back pressure based on the
technical data sheet. Injection velocity and cooling R= (1-L/L0).............................................Equation 1
time set to 80mm.sec-1, 20 sec respectivily. Gate
frozen time was determined from a range of Where L0 is a dimension measured on the mould
holding times against part weight at 100 bar cavity and L is the same dimension measured on
holding pressure, as shown in Figure 2. The part at the specimen. The mould cavity shape and the
which specimen mass no longer increases with selected measurement positions are shown in
applied pressure is the gate freeze. In this case the Figure 3.
hold time is taken to be 40 sec. It should be noted
2.4.3 Colour measurement Thermogravimetric Analysis “TGA” is used to
The colour of the samples is an important quality determine the thermal stability of a material by
issue where the change of the product colour measuring mass loss (material evaporation) over
could indicate to the degradation phenomena. In a range of temperature.
this work the colour of the reprocessing samples TGA model Q5000 was used here, and all samples
are gradually changed from “white” to were gently prepared by cutting into round shape
“yellow/light brown” and digital photo was taken (samples weight range is 2 - 4mg) then the samples
by using Canon digital camera model EOS 350D. were subjected under nitrogen atmosphere using
Photo taken in cloudy conditions (no flash), and the temperature range of 35-600ºC and heating rate
all samples (from virgin to stage 7) included of 10ºC.min-1. Universal TA Instruments software
within the same frame. This avoided the need to was used to determine the initial degradation
build a light controlled environment, but allows temperature for each stage based on the onset point.
for a reasonable comparison of colour change.
Adobe Photoshop CS 2 version 9 was used to 2.5.4 Molecular weight (Mw)
analyse the yellow colour for the selected images Molecular weight is important because it influences
(for every stage). However, image mode CYMK with many properties such as stiffness, strength,
(C: cyan, Y: yellow, M: magenta and K: black) viscoelasticitic response, toughness, melt & glass
and yellow channel were selected in order to transition temperatures and viscosity. As molecular
determine the yellow colour percentage. weight increases, melt and transition temperatures
along with the mechanical properties will generally
2.5 Physical properties increase. Low Mw materials are typically not useful
2.5.1 Density in structural applications Gowariker et al., 1986.
Density is one of the important physical features In this study gel permeation chromatography model
for the polymer as it linked to the volume “GPC” was used, and two runs for each sample
and crystallinity. It has been measured using were analysed to determine the average molecular
AccuPycTM 1330 Pycnometer. The regrind weight for each reprocessing stage.
materials for each stage in form of pallets were
used, and then the apparatus calculated the best five 2.6 Processing properties
readings of the density and provided the average 2.6.1 Viscosity index
values. Viscosity index “VI” is a process measurement that
has been shown to indicate process variation
2.5.2 Crystallinity through material viscosity change and/or process
Crystallinity is indication of amount of crystalline control (R.G.Speight, 1993). It has been used here
region in polymer with respect to amorphous to obtain an indication of material viscosity
content. Crystallinity influences many of the changes directly from the process and to identify
polymer properties such like hardness, tensile, regions of process stability within a reprocessing
stiffness, crease and melting point (Gowariker et stage. VI is of absolute metric and well change
al., 1986). with injection velocity, temperature...etc. However,
Differential scanning calorimetry “DSC” is where the process settings are constant it can be
a thermo-analytical technique in which the used to indicate process variations, may be through
difference in the amount of heat required to statistical process control.
increase the temperature of a sample and reference VI was obtained from the available nozzle
are measured as a function of temperature. It’s used pressure signals recorded from FANUC machine
to study what happens to polymers when they're by integrating the area under the nozzle pressure -
heated and give useful information such like actual time curve, where only the portion from 60% to
melt temperature; crystallinity and glass transition 80% of the velocity controlled phase is considered.
temperature. In this work it’s used to determine the Figure 4 shows the selected area under the nozzle
degree of crystallinity for each reprocessing stage pressure curve which is integrated to calculate the
using DSC model Q2000. Universal TA software viscosity index. A stable value of VI across cycles
was used to analyse the data and the experiment indicates consistent sample manufacture. Sample
was done under standard setting using temperature here, therefore, selected for stable regions if VI as
range of 0 ºC - 220oC and liquid nitrogen was used shown in Figure 5.
for cooling the system at 100 µL min−1, with
heating rate10oC.min-1. 2.6.2 Melt flow index “MFI”
MFI is popular method for comparing and quality
2.5.3 Thermal stability control of materials. MFI is an indicator of
Thermal degradation of polymeric materials is a flow ability of a material (in the melt phase). The
an importance issue for industrial viewpoint, MFI test is often used commercially to monitor
especially in polymer processing and higher melt batch and discriminate between polymers. The
temperature applications. MFI result is not complete as a full rheological
awe, but has been used here to compliment the an L: D ratio of 16 (long die) and the other bore
other rheological data. This test is based upon a set was fitted with zero length die. The melt
driving pressure that results in a measured mass temperature was 230°C on all cases. The material
flow rate. This test method has been included due was subjected to precompression pressures of 1.0
to its popularity and results with be compared with and 0.5 MPa for the long and short dies
more extensive viscosity testing. respectively, and subjected to a total preheating
In the current work, MFI was performed using time of 540 sec. Rosand flowmaster control
Kayeness melt flow indexer model 7050 using die software was used to analyse this data.
diameter of 2.01 mm at the temperature of 230ºC
and the constant weight of 2.16 kg according to 2.6.4 Mechanical properties
ASTM D1238. Five samples were cut off at 2 Tensile test samples were analysed to determine the
minutes interval and then weighted to determine tensile properties (Young's modulus and percentage
the flow rate in grams per minutes. This test is of elongation at yield) along flexural strength.
repeated three times and the average of the melt ‘Instron testing machine’ model 5564 using
flow index was reported as grams.10 min-1. An ‘Instron Bluehill software’ was utilised for testing
approximate value for MFI can be calculated using and data analysis.
Poiseulle law as shown in Equation 2 Kelly et al., The tests were carried out at room temperature (20-
2009 below: 22ºC) and relative humidity of 50 %. For tensile
test, three crosshead speeds (200mm.min-1, 250
γº = 4Q/πR3 .............................................Equation 2 mm.min-1 and 300mm.min-1) were selected
according to the ASTM test properties for this
Where, Q is a volumetric flow rate (m3 /sec) and material. On other hand, 300mm.min-1 was selected
R is a radius of the capillary (m). for 3 points bending test. It should be noted that the
specimens were selected for each speed category
2.6.3 Shear viscosity based on viscosity index as explained in section
Rheologically, viscosity is the resistance of a fluid 2.6.1.
to flow, caused by its internal friction, which
makes it resist flowing past a solid surface and 3- Results and Discussion
makes layers of the fluid resist flowing past other
layers (Johannaber, 1983). Viscosity is very 3.1 Part quality
important to the injection moulding process and it’s 3.1.1 Specimen mass
affected by the temperature of the material. The In this study, the specimen mass is consistent at
effect of shear rate on viscosity is very important as any given reprocessing stage, but mass slightly
the viscosity can reduce several orders of increases over the seven reprocessing stages. This
magnitude when the shear rate is increased is shown in Figure 6 , where the mass increase
(pseudo-plastic shear thinning). This is a very from virgin to stage 7 is around 0.2 %. The process
important in injection moulding as very high local parameter settings are consistent for all of the
shear rates can be present within the flow path, in reprocessing stages. An increase in specimen mass
particular at the gate region, where the channel is may be linked to reductions in melt viscosity, (as
very small and the flow velocity is relatively high. described in sections 3.3.1 and 3.3.3) along with
In this work, viscosity measured off line over the increase in crystallinity and density entitled in
seven reprocessing stages. Two methods were section 3.2.1.
employed to determine low (rotational rheometer)
and high shear rate viscosity (capillary rheometer). 3.1.2 In-plane shrinkage
Low strain rate measurements (0.1-100 sec-1, for It can be noted from Figure 7 that the shrinkage
all reprocessing stages) were made on an Anton- through thickness (D1, D2 and D3) reduces along
Paar MCR501 rotational rheometer using a 25 mm the flow path. Similarly, the shrinkage through
diameter parallel plate geometry with a gap size of width (W1, W2 and W3) reduces along the flow
1 mm and a strain of 5%. This strain value is within path. Oppositely, the shrinkage increases along the
the linear viscoelastic regime for all melts tested as length of the specimen (L), which is along the flow
confirmed by amplitude sweep measurements on direction. This is due to the fact that the crystalline
the rheometer. Melt viscosity at higher shear rate materials tend to have high shrinkage and the
(500-6000 sec-1) was studied using twin bore shrinkage is grater in the direction of flow than
Rosand RH10 capillary rheometer, Dual pistons of across the direction of flow (Bryce, 1996). The
diameter 15 mm were used to drive melt flow shrinkage at “L” position has a relative increase of
through capillary dies at speeds up to 20 mm.s-1 27% from virgin to stage 7. Regarding to the
and the a maximum crosshead force of 100 kN . thickness, the higher percentage of shrinkage is
One pair of long and short capillary dies with entry 1.46, located at D1 (stage 7). Similarly, the width
angle of 180º and Ø=1 mm. One barrel of the has a percentage of shrinkage of 1.33, located at
rheometer was fitted with a capillary die with W1 (stage 7) .This is might be as a result of the
moulded part has more tendency toward the It can be noted from Figure 11, the initial
shrinkage in the posions that more closes to the degradation temperatures of the virgin and stage 7
direction of flow (ie.D1,W1) , because the other are 400.6 ºC and 399.78 ºC, respectively.
positions of the part (ie.D3,W3) are already filled Therefore, these results indicate to there is no
and started to solidify earlier than others. significant change, in practical processing terms of
According to ASTM D955, the shrinkage range of the degradation temperature for these stages.
polypropylene material related to injection
moulding is between 0.254-0.762 mm/mm (Bryce, 3.2.3 Molecular weight
1996), this could lead to say the calculated The importance to study the Mw behaviour here,
shrinkage in this work is slightly low and hence due to it has influenced with processing and
the moulded parts produced in every reprocessing mechanical properties over 8 reprocessing stages.
stages have tendency toward dimensional stability. Figure 12 shows the average molecular weight over
seven reprocessing stages. As can be seen in this
3.1.3 Colour measurement graph, the data has some fluctuations across the
The aesthetics of a polymeric material may be an stages, but the general trend is for Mw result to
important quality feature, depending upon the end reduce the average Mw on 10% from virgin to
use of the product. The colour change has been stage7. A reduction in molecular weight with
assessed by the percentage of yellow within the increasing the number of reprocessing stages could
colour spectrum. The colour analysis indicated to be linked to the reduction of the amount of the
the yellowness started to be appeared gradually material chain branching and the changing in
from stage 4 as shown in Figure 8. This is, chemical bonds as a result of material degradation.
probably, as a result from repetitive heat The behaviour of Mw over 8 reprocessing stages
reprocessing stages and might be caused by has clear correlated with shear viscosity as
oxidative degradation that taken place during mentioned in the section 3.3.3. In spite of seven
reprocessing operations, but it could be said that reprocessing stages, this reduction in Mw could be
percentage of yellow up to stage 3 has little change considered as a little and reasonable.
from the virgin as a reference. The behaviour of molecular weight has clear effect
In industry, to accept or refuse the relative and has linked with mechanical properties as
change in the product’s colour is absolutely represented in section 3.4.
depended on the type of application, and the
customer’s specifications/requirements. However, 3.3 Processing properties
this problem can be solved, if no severe or sharp 3.3.1 Viscosity index
drop in the mechanical properties, by adding In-line process measurement is comparative
pigments or artificial colours. technique was used at process where the
measurement was taken directly in real time as
3.2 Physical properties mentioned before. However, it can be seen from
3.2.1 Density & crystallinity Figure 13, a little reduction in viscosity index.
Polypropylene is a semi-crystalline material Stage 7, for example, is reducing 14% from the
consisting of amorphous and crystalline regions virgin. This reduction in viscosity index as a result
(Gowariker et al., 1986). The density of the bulk from reducing of the nozzle pressure due to the
material is dependent upon the relative volume material is easier to flow as explained in section
fractions of the amorphous (low density) and 3.3.2, and this cause to the cavity has filled more.
crystalline (high density)phases (Gowariker et al., Therefore, this probably causes to increase the
1986). As shown in Figure 9, the density increases specimen mass.
slightly (by 0.48%) with reprocessing stages from
virgin to stage 7 reprocessed material. This 3.3.2 MFI
correlates well with the 4% increases in In this work, MFI result is not complete as a full
crystallinity observed over 8 stages as shown in rheological awe, but has been used here to
Figure 10. compliment the other rheological data. However,
from Figure 14, it can be noted that the MFI
3.2.2 Thermal stability increases with relative percentage of 43% from
Thermal degradation is an irreversible effect due to virgin to stage 7. The shear rate presented in Figure
the breaking of chemical bonds. Results are 14 is generated using Poiseulle law (equation 2).
reported as percentage of mass loss as a function of The shear rate of the melt also increases along the
temperature, and the results of virgin and stage 7 reprocessing stages. However, when the material
are shown in Figure 11. The typical processing become easier to flow, the cavity will be filled
temperature based on the material data sheet is more and hence the specimen mass will be
located between 199 ºC to 226 ºC and the increased, this may explain the behaviour of
experimental set point is 225 ºC (based on the specimen mass which was increasing over 8
actual setting temperature in the Fanuc machine). reprocessing stages .
MFI is an indirect indicate to the molecular
weight, high melt flow rate corresponding to low
molecular weight (La Mantia, 2002) as presented in
section 3.3.

3.3.3 Viscosity
Shear viscosity has been determined using both the
Anton Paar rotational viscometer (low shear) and
the Rosand RH10 two bore capillary rheometer
(intermediate to high shear). The data for virgin
and all reprocessing stages has not been presented
on a single axis since discrimination between the
data is difficult. Instead, the viscosity of each stage
is presented at specific shear rates. These are 0.1,
100, 500, 6000 sec-1 shown in Figure 15(a, b) and
Figure 16 (a&b), respectively. Figures 15&16 show
the change in shear viscosity over 8 reprocessing
stages (-33% at 0.1 sec-1 , -20% at 100 sec-1, -13%
at 500 sec-1 and -11% at 6000 sec-1) . Figure 17
shows the rheologized behaviour of the virgin
material and that after 7 reprocessing stages over
the full range of shear rates studied.
A reduction in viscosity could be related to the
reduction of the amount of the material chain
branching as well as overall molecular weight as
explained in section 3.2.3.

3.4 Mechanical properties


Mechanical properties have been assessed through
tensile (modulus of elasticity, % of EL at yield) and
flexural (flexural strength) tests. In the former case,
the strain is determined through crosshead
displacement. Figure 18 shows the modulus of
elasticity at all crosshead speeds of 200, 250 and
300 mm.min-1. From Figure 18, it can be noted that
the modulus decreased with increasing crosshead
speed. This is might be related to the crystallinity
that cause to the material become more brittle, and
hence the elasticity is reduced by increasing the
crosshead speed. However, the modulus is reduced
with relative percentage of 16%. Similarly the
percentage of elongation at yield is reduced 25%
(see Figure 19). Flexural strength, on other hand
has less reduction with percentage of 11% from
virgin as a reference as shown in Figure 20. These
reductions due to the repetitive shearing stages
(that may cause to reduce the viscosity and lead to
decrease the molecular weight) and also this
material has a tendency to become more brittle, and
less ductility.
Some investigators presented the same behaviour
of the modulus and the elongation of polypropylene
material for multiple reprocessing stages
(La Mantia, 2002;Dintcheva and La Mantia, 2003;
Meran et al., 2008 ).
Table 1 Moulding settings 15.5
Parameter Setting 15.4
Barrel temperature 225 C° 15.3

Specimen mass (grams)


Nozzle temperature 225 C° 15.2
Back pressure 80 bar 15.1
Holding pressure 100 bar 15
14.9
Cooling time 20 sec
Holding time 45 sec 14.8
14.7 a
Shot Size 33 mm
14.6
Screw rotation speed 150 rpm
14.5 Holding pressure: 100bars
Injection velocity 80 mm/sec
14.4
0 5 10 15 20 25 30 35 40 45 50 55
Holding time (sec)

Figure 2 Specimen mass vs. holding time


(a: specimen with runner)

Positions (in mm)


L =110.49 D1=4.11 W1=20.18
D2=4.1 W2=10.05
D3=4.06 W3=20.18

Figure 1 Reprocessing procedure Figure 3 Mould cavity shape and measurement


locations
15.48

15.47

Specimen mass (grams)


15.46

15.45

15.44

15.43
Virgin 1 2 3 4 5 6 7
Stage no.

Figure 4 Viscosity index is calculated from a portion Figure 6 Specimen mass for all stages
of the primary injection pressure-time date

14
Stage7
Stage6
12 Stage5
Stage4
Stage3
Shrinkage (%)

10 Stage2
Stage1
8 Virgin

0
W1 W2 W3 D1 D2 D3 L
Shrinkage Positions

Figure 5 Viscosity index for all stages Figure 7 Shrinkage effects over 7 reprocessing
stages
25.8
7

6 25.6

% of Crystallinity
7
5 25.4
6

Increasing of yellowness
Stage no.

4 5
25.2
3 4
3
2 25
2
1 1 24.8

Virgin Virgin
24.6
0 5 10 15 20 25 30 35 40 45 Virgin 1 2 3 4 5 6 7
% of Yellow Stage no.

Figure 8 Colour measurements (Yellowness Figure 10 Percentage of crystallinity


produced in moulded parts by each one of the 7
stages of injection)

0.897 120

0.896
100
0.895
Density (grams/cm³)

Weight (%)

80 Virgin
0.894
Stage 7
0.893 60

0.892
40
0.891
20
0.890

0.889 0
Virgin 1 2 3 4 5 6 7 270 310 350 390 430 470

Stage no. Temperature (C°)

Figure 9 Density for all stages Figure 11 TGA result: mass vs. temperature
195000
Average molecular weight (gm/mol)

190000

185000

180000

175000
21
43
170000 20 MFI
virgin 1 2 3 4 5 6 7 41
Stage no. 19
γ°(sec¯¹ ) 39

MFI (g.10 min¯¹)


18
37

γ°(sec¯¹)
17
Figure 12 Average molecular weight for all stages 35
16 33
15 31

14 29

13 27
Virgin 1 2 3 4 5 6 7
Stage no.

30
29.5 Figure 14 MFI and shear rate for all stages
29
Viscosity Index

28.5
28
27.5
27
26.5
26
25.5
Virgin 1 2 3 4 5 6 7
Stage no.

Figure 13 Viscosity index for all stages


1300 76.0
1250
γº =0.1 sec¯¹ 74.0 γº =500 sec¯¹
1200
1150 72.0

ɳ (Pa.sec)
ɳ (Pa.sec)

1100
70.0
1050
1000 68.0

950 66.0
900
64.0
850
800 62.0
Virgin 1 2 3 4 5 6 7 Virgin 1 2 3 4 5 6 7

Stage no. Stage no.


(a) (a)

340 15.5

320 γº =100 sec¯¹ 15.0 γº =6000 sec¯¹


300
14.5
ɳ (Pa.sec)

ɳ (Pa.sec)

280
14.0
260
13.5
240
13.0
220

200 12.5
Virgin 1 2 3 4 5 6 7 Virgin 1 2 3 4 5 6 7
Stage no. Stage no.
(b) (b)

Figure 15 Melt viscosity at low shear rate Figure 16 Melt viscosity at high shear rate
(a: γº =0.1 sec¯¹ and b: γº =100 sec¯¹) (a: γº =500 sec¯¹ and b: γº =6000 sec¯¹)
10000 7.50
Virgin Stage 7 % of El. at 200 mm.min¯¹
7.00 % of El. at 250 mm.min¯¹

% of Elongation at yield
1000 % of El. at 300 mm.min¯¹
ɳ (Pa.sec)-log scale

6.50

100 6.00
Anton Paar MCR
501 rotational 5.50
rheometer
10
Rosand RH10 5.00
capillary rheometer
1 4.50
0.1 1 10 100 1000 10000 Virgin 1 2 3 4 5 6 7
γº (sec¯¹)- log scale Stage No.

Figure 17 Shear viscosity data from Anton Parr Figure 19 Percentage of elongation at yield
rotational rheometer (low shear) and Rosand
capillary rheometer (high shear) for virgin and
stage 7

680 27
200 mm.min¯¹
660 26.5
250 mm.min¯¹
Flexural strentgh (MPa)
Modolus of Elasticity (MPa)

640 300 mm.min¯¹ 26


620
25.5
600
25
580
24.5
560
24
540
520 23.5

500 23
Virgin 1 2 3 4 5 6 7 Virgin 1 2 3 4 5 6 7
Stage No. Stage no.

Figure 18 Modulus of elasticity Figure 20 Flexural Strength


4- Conclusions it could be said that the modulus of
elasticity (at all crosshead speeds), flexural
This study has investigated the effects of strength have reasonable change, where
reprocessing a polypropylene material. Effects Young’s modulus and flexural strength have
have been investigated in terms of: percentage of reduction of 5% for from the
 Part quality (mass, in-plane shrinkage and virgin as a reference.
colour).
 Physical properties (density, crystallinity, Acknowledgement
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 Processing properties (viscosity index, The authors would like to thank the technical staff
melt flow index, and melt viscosity at high in IRC polymer engineering at the University of
and low shear rate). Bradford for their help and support.
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