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 recycling
Article
Washing Post-Consumer Flexible Polyethylene Packaging Waste
Ezgi Ceren Boz Noyan 1, * , Abhijit Venkatesh 2 and Antal Boldizar 1

1 Department of Industrial and Materials Science, Chalmers University of Technology, Rännvägen 2A,
412 96 Gothenburg, Sweden
2 RISE Research Institutes of Sweden, Argongatan 30, 431 22 Mölndal, Sweden
* Correspondence: [email protected]

Abstract: The mechanical and thermal properties of injection-molded recycled polyethylene were
studied, specifically with respect to the influence of large-scale washing and melt-compounding of
polyethylene from post-consumer packaging waste. Three types of materials were studied: those
taken after sorting, after sorting and washing, and after sorting, washing, and melt-compounding,
including melt-filtration, all from a large-scale material flow. The materials were further processed
on a laboratory scale and compared. The results showed that large-scale washing significantly re-
duced thermo-oxidative stability, as well as molar mass and melt viscosity. The degradation during
large-scale washing made the material susceptible to further degradation in the subsequent extrusion
compounding, as shown by the differences in compounding at 240 and 200 ◦ C using a high-shear
screw configuration. The compounding parameters, screw configuration, and compounding temper-
ature did not influence the stiffness and strength of the unwashed and large-scale-washed materials,
but the elongation-at-break varied, specifically, with the increased temperature. Washing had an
influence on the mechanical properties as well, and the unwashed material provided molded samples
with stiffness measurements of approximately 550 MPa, whereas the large-scale-washed material pro-
vided stiffness of approximately 400 MPa. The strength measurements were approximately 15 MPa
for samples made of both unwashed and large-scale-washed material, and the elongation-at-break
measurements were between 50 and 150%. The large-scale-washed and compounded materials
Citation: Boz Noyan, E.C.; Venkatesh, had very different mechanical properties, with stiffness measurements of approximately 320 MPa,
A.; Boldizar, A. Washing strength of approximately 20 MPA, and elongation-at-break of approximately 350%. The significantly
Post-Consumer Flexible Polyethylene different mechanical properties of the large-scale-washed and compounded materials were likely
Packaging Waste. Recycling 2022, 7, due to the melt-filtration included in the compounding through the removal of metal and rubber
90. https://doi.org/10.3390/ particles, and they may also have been due to the compatibilizing and stabilizing additive used in
recycling7060090
the compounding.
Academic Editor: Giovanni De Feo
Keywords: washing; melt-compounding; plastics recycling; polyethylene; degradation; mechanical
Received: 18 November 2022
properties
Accepted: 10 December 2022
Published: 14 December 2022

Publisher’s Note: MDPI stays neutral

with regard to jurisdictional claims in 1. Introduction
published maps and institutional affil-
Interest in plastics recycling has increased, primarily with an emphasis on an im-
iations.
proved waste management. There has been exponential growth in global annual plastics
production, which is expected in 2050 to reach four times the volume of that produced in
2014, which was 311 million tons [1]. Plastics packaging is the largest contributing factor,
Copyright: © 2022 by the authors.
creating short-lived products in the post-consumer plastics waste stream, and it has been so
Licensee MDPI, Basel, Switzerland. for many decades. An ambitious target has been set by Directive (EU) 2018/852 to increase
This article is an open access article the rate of recycling of post-consumer plastic packaging waste (pcppw) to 55% by 2030 [2].
distributed under the terms and The current recycling rates are low, and a study by Antonopoulos et al. suggested that the
conditions of the Creative Commons current rate of progress may be insufficient to fulfil the stated EU goal for the recycling of
Attribution (CC BY) license (https:// pcppw [3]. In this situation, it is interesting to increase our knowledge of the properties
creativecommons.org/licenses/by/ of materials made of real plastic waste and to better understand how recycling processes
4.0/). influence these properties.

Recycling 2022, 7, 90. https://doi.org/10.3390/recycling7060090 https://www.mdpi.com/journal/recycling

Recycling 2022, 7, 90 2 of 12

Flexible packaging, primarily consisting of single-use products, has been the fastest
growing and most challenging segment of the plastic packaging industry with regard to
recyclability [4]. In addition to monolayer products (one layer of the same type of polymer),
flexible packaging contains many multilayer films (several layers of different types of
polymers, and sometimes non-polymeric materials, as well) which are more complex and
difficult to recycle [5,6]. A variety of additives are included during their processing, e.g.,
antioxidants, photo-stabilizers, flame retardants, heat stabilizers, plasticizers, compatibi-
lizers, fillers, dyes, and pigments, and this increases their complexity even more [7]. In
the literature it is suggested that the commonly used additives in film products are fatty
acids, which are used as slip agents, and polyethylene glycol esters, which are used as anti-
static additives [8]. Even though low-density polyethylene (LDPE) and linear low-density
polyethylene (LLDPE) account for a significant amount of the polymers used in flexible
packaging, packaging is also made of medium-density and high-density polyethylene
(MDPE and HDPE), polypropylene (PP), polyethylene terephthalate (PET), polystyrene
(PS), expanded polystyrene (EPS), and polyvinylchloride (PVC), and it may also consist of
blends of polymers, which can lead to cross-contamination and miscibility problems [9–11].
Due to the comingled character of waste in collection schemes and the typically high levels
of contamination, increasing the recovery rate of flexible packaging is not a straight-forward
task [11–13].
There is also an interest in increasing quality of the packaging’s next application as a
new product, and this means that treatment of the waste fractions, such as the removal of
unwanted contaminants, is necessary [7,14]. In the mechanical recycling process, washing
is typically applied after the sorting step, where the mixed waste is separated with respect
to polymer type, e.g., an LDPE stream, an HDPE stream, a PP stream, etc. [15,16]. Several
studies have analyzed the effects of washing on plastic waste, and some of them have
assessed the possible degradation that occurs during the washing process [17–22]. It
has been shown that the temperature, time, and washing agent (type and amount) are
important for achieving effective cleaning, but their influence on the degradation of the
recycled material was not assessed. In one study, it was reported that the degradation of
recycled HDPE was accelerated by residues of NaOH [19].
Other factors that have been found to influence the properties of the recycled materials
include the impurity level [23], blending the recycled components with either virgin
material or material of a different grade, the type of polymer [24,25], and the source of
the waste (e.g., mixed municipal solid waste or source-separated household waste) [26,27].
Studies regarding the influence of melt-processing parameters on the properties of recycled
materials are, however, scarce. To the best of our knowledge, there are few publications that
have researched the mechanical properties of unwashed and non-treated post-consumer
flexible PE packaging waste and the effects of washing.
This work aims to describe the development of thermal and mechanical properties
during the recycling of post-consumer flexible PE waste originating from mixed munic-
ipal solid waste (MSW) sorted on a large scale in Norway. Specifically, the influences of
compounding temperature and screw design on sorted unwashed plastic waste were inves-
tigated, as was the influence of combined washing and melt-processing on the properties
of recycled material. The results were compared with those for industrially recycled pellets
of the same sorted fractions.

2. Materials and Methods

A bale of approximately 700 kg of sorted flexible PE (PE-2D) packaging waste origi-
nating from mixed municipal solid waste was received in March 2021 from a large-scale
recycling plant in Norway. A sample of approximately 60 kg of industrially washed flakes
and a sample of approximately 10 kg of washed, compounded, and melt-filtered pellets of
the same fractions were supplied by the same company, and they are hereinafter referred
to as “industrially washed” material and “industrially recycled” material, respectively. The
industrially washed material was prepared by shredding with a screen size of 60–80 mm
Recycling 2022, 7, x FOR PEER REVIEW 3 of 12

referred to as “industrially washed” material and “industrially recycled” material, respec-

Recycling 2022, 7, 90 tively. The industrially washed material was prepared by shredding with a screen size of
3 of 12
60–80 mm and magnetic separation. The industrial washing consisted of pre-washing at
room temperature, wet grinding, friction washing with NaOH and defoamer at 70–80 °C,
rinsing at room temperature,
and magnetic separation. The centrifuging, dewatering,
industrial washing consisted andofthermal drying,
pre-washing and the
at room tem-whole
perature,
washing wet grinding,
process took 30friction washing
min. The with flakes
washed NaOH were and defoamer at 70–80 ◦ C, rinsing at in-
then extrusion-compounded,
room temperature,
cluding filtration withcentrifuging,
a 120 μmdewatering,
mesh screen, and thermal drying, and
and pelletized. The theindustrially
whole washing washed
process took 30 min. The washed flakes were then extrusion-compounded,
sample was taken after the washing steps were completed and the industrially including
recycled
filtration with a 120 µm mesh screen, and pelletized. The industrially washed sample was
sample was taken after the extrusion-compounding with melt-filtration was completed.
taken after the washing steps were completed and the industrially recycled sample was
The unwashed
taken after thesorted plastic sample was
extrusion-compounding withtaken from a bale,
melt-filtration wasshredded
completed.using a Rapid Gran-
The unwashed
ulator
sorted300-45 with
plastic a screen
sample size offrom
was taken 17 mm, and
a bale, screened
shredded witha aRapid
using magnetic grid before
Granulator 300-45being
compounding on a laboratory scale.
with a screen size of 17 mm, and screened with a magnetic grid before being compounding
onThe unwashed
a laboratory and industrially washed samples were extrusion-compounded and
scale.
The unwashed and
then injection-molded, industrially
whereas washed samples
the industrially weresample
recycled extrusion-compounded
was injection-moldedand as
then injection-molded, whereas the industrially recycled sample was
it was received. A Werner & Pfleiderer ZSK 30 M9/2 co-rotating intermeshing twin-screwinjection-molded as it
was received.
extruder (TSE) wasA Werner & Pfleiderer
used for compounding,ZSK 30with
M9/2a co-rotating
screw length intermeshing
of 969 mmtwin-screw
and a diameter
extruder (TSE) was used for compounding, with a screw length of 969 mm and a diameter
of 30 mm. Two temperature profiles and two screw configurations were used: 100, 150,
of 30 mm. Two temperature profiles and two screw configurations were used: 100, 150, 200,
200, 200, 200, and 210 °C and 100, 150, 200, 240, 240, and 250 °C, and the first screw con-
200, 200, and 210 ◦ C and 100, 150, 200, 240, 240, and 250 ◦ C, and the first screw configuration
figuration
(SC1) had(SC1) had onlyelements,
only transport transport elements,
whereas whereas
the second the second(SC2)
configuration configuration (SC2) had
had four mixing
four mixingper
elements elements per as
screw shaft, screw
shownshaft,
in theasFigure
shown 1a.inThe
thefeeding
Figureof1a.
theThe feeding
fluffy of the
flakes into thefluffy
flakes into was
extruder the extruder
completedwas completed
manually. manually.was
The throughput The1.1throughput
± 0.3 kg/h at was 1.1 ± rotation
a screw 0.3 kg/h at a
rate rotation
screw of 80 rpm.rate of 80 rpm.

(a)

(b)
Figure 1. (a)
Figure TheThe
1. (a) extruder
extruder screw
screwconfigurations
configurations used
used for
for compounding:
compounding: (i) (i)screw
screw1,1,no
nomixing
mixing ele-
ments; (ii) screw
elements; 2, four
(ii) screw mixing
2, four mixingelements;
elements;and
and (b) thefilling
(b) the fillingpattern
pattern in the
in the moldmold
usedused for injection-
for injection-
molding, with an overall width of 64 mm, a length of 48 mm, and a thickness
molding, with an overall width of 64 mm, a length of 48 mm, and a thickness of 2 mm. of 2 mm.
Recycling 2022, 7, 90 4 of 12
Recycling 2022, 7, x FOR PEER REVIEW 4 of 12

The extruded pellets and the as-received industrially recycled PE pellets were injection-
molded The
in extruded
a frame, aspellets
shownand the as-received
in Figure industrially
1b, using an recycled PE
Arburg Allrounder pellets were
221M-250-5 injec-
machine.
tion-molded in a frame, as shown in Figure 1b, using an Arburg Allrounder
The frame had three sections with different molecular orientations: the gate region (G), 221M-250-5
machine.
with a mixedThemolecular
frame had three sections
orientation; with different
the simple molecular
flow region orientations:
(SF), with the gate
a unidirectional re-
flow;
gionthe
and (G),
weldwith a mixed
line regionmolecular
(WL), where orientation;
two flowthe simple
fronts met.flow
The region (SF), with
temperature a unidi-
profile was
rectional
120, flow;
170, 200, 220,and
andthe weld
220 ◦ C, line
andregion (WL), and
the injection where two flow
holding fronts were
pressures met. The
500 temperature
and 700 bar,
profile was The
respectively. 120,injection
170, 200,volume
220, andwas 220 °C, andfor
adjusted the injection
each and
material typeholding pressures
to achieve at leastwere
an
500 and 700 bar, respectively. The injection volume was adjusted for each
80% meeting of the weld line width before the holding pressure was applied. Table 1 showsmaterial type to
achieve
the codesat least anto80%
assigned the meeting
differentof the weld
samples, line
and width before
examples the and
of pellets holding pressure was
injection-molded
applied.are
samples Table
shown1 shows the codes
in Figure 2. assigned to the different samples, and examples of pel-
lets and injection-molded samples are shown in Figure 2.
Table 1. The samples’ codes and processing histories.
Table 1. The samples’ codes and processing histories.
Compounding Parameters
Treatment Compounding Parameters Sample Code
Treatment Screw Design Temperature Profile (◦ C) Sample Code
Screw Design Temperature Profile (°C)
Unwashed SC1 100-150-200-200-200-210 UW_SC1_200
Unwashed
Unwashed SC1 SC1 100-150-200-200-200-210
100-150-200-240-240-250 UW_SC1_200
UW_SC1_240
Unwashed
Unwashed SC2 SC1 100-150-200-240-240-250
100-150-200-200-200-210 UW_SC1_240
UW_SC2_200
Unwashed
Unwashed SC2 SC2 100-150-200-200-200-210
100-150-200-240-240-250 UW_SC2_200
UW_SC2_240
Unwashed
Industrially washed SC1 SC2 100-150-200-240-240-250
100-150-200-200-200-210 UW_SC2_240
IW_SC1_200
Industrially washed
Industrially washed SC1 SC1 100-150-200-240-240-250
100-150-200-200-200-210 IW_SC1_240
IW_SC1_200
Industrially washed
Industrially washed SC2 SC1 100-150-200-200-200-210
100-150-200-240-240-250 IW_SC2_200
IW_SC1_240
Industrially washed
Industrially washed SC2 SC2 100-150-200-240-240-250
100-150-200-200-200-210 IW_SC2_240
IW_SC2_200
Industrially recycled
Industrially washed SC2 100-150-200-240-240-250 IW_SC2_240
(washed and N/A N/A rLDPE
Industrially recycled
melt-filtered) N/A N/A rLDPE
(washed and melt-filtered)

Figure2.2.Examples
Figure Examplesofofpellets
pelletsand
andinjection-molded
injection-moldedsamples.
samples.

Theoxidation
The oxidationinduction
inductiontemperature
temperature(T(Toxox))according
accordingto toISO
ISO11357-6
11357-6and
andthe
thethermal
thermal
transitionsaccording
transitions accordingtotoISO11357-1
ISO11357-1ofofboth boththe
thepellets
pelletsand
andinjection-molded
injection-moldedsamples
sampleswere were
determinedusing
determined usingaaMettler-Toledo
Mettler-ToledoDSC DSC2 2instrument.
instrument.For ForthetheTT measurements,circular
oxoxmeasurements, circular
sectionswith
sections withthicknesses 0.65±±0.1
thicknessesofof0.65 0.1 mm
mmwerewereused,
used,and
andsamples
sampleswith withweights
weightsofofatatleast
least
55mg
mgwere
wereusedusedtotoassess
assessthe
thethermal
thermaltransitions.
transitions.The TheTToxoxmeasurements
measurementswere weremade
madeininair air
and
andthe
thethermal
thermaltransitions
transitionsininnitrogen,
nitrogen,both
bothatata aheating
heatingraterateofof1010◦ C/min.
°C/min.The
Thebaseline
baseline
was
wastaken
takenfromfrom60 132◦ C
60toto132 °Cfor
forthe
themeasurements
measurementsofofthe theheat
heatofoffusion
fusion(∆H).
(ΔH).The
Themeanmean
values
valuesofofthe
theduplicates
duplicateswere
werereported
reportedfor foreach
eachtype
typeofofmaterial.
material.
The
Theash ashcontent
content of
of the
the pellets
pellets was determined
determined usingusing 33 ±±1 1mg mgpowdered
powderedsamples.
samples. A
ATGA/DSC
TGA/DSC 3+ 3+
StarStar system
system fromfrom Mettler
Mettler Toledo
Toledo waswasused,used,
and and samples
samples werewere
heatedheated
from
from ◦ to 650 ◦ C at a rate of 10 ◦ C/min in air at a flow rate of 50 mL/min. Duplicate
25 °C25to C650 °C at a rate of 10 °C/min in air at a flow rate of 50 mL/min. Duplicate meas-
measurements
urements werewere made made
and and the mean
the mean values
values werewere calculated.
calculated.
Recycling 2022, 7, 90 5 of 12

The samples were sent to ITS Testing Services (UK) Limited (Redcar, UK) for evaluation
of their molecular weights by high temperature gel permeation chromatography (HT-GPC).
Approximately 40 mg of pellets were dissolved in 10 mL of TCB (1, 2, 4 trichlorobenzene
with 200 ppm BHT as antioxidant) and the analyses were made using a Polymer Labora-
tories GPC220 instrument. Three PlOlexis and PlOlexis guard columns were used with
lengths of 30 cm each, and 200 µL of polymer solution was injected with a flow rate of
0.8 mL/min at 160 ◦ C. The data were analyzed using Polymer Laboratories Cirrus soft-
ware. The mean values based on two independent measurements of the weight-average
molecular mass (Mw ) and polydispersity index (PDI) were reported.
A Ceast Modular Melt Flow (Instron) instrument was used to determine the melt flow
rate (MFR) of the pellets, using a standard weight of 2.16 kg at 190 ◦ C, in accordance with
ISO 1133-1:2011. The rheological behavior of the selected samples was determined with a
high-pressure capillary rheometer Rheograph 20 (Göttfert). The temperature was 220 ◦ C
during the analysis, and a constant piston speed was applied at each shear rate between
103 and 101 s−1 . To apply the Bagley correction as indicated in the ISO Standard 11443:2021,
three dies were used with diameters of 2 mm and aspect ratios (L/D) of 5, 10, and 15. A
Weissenberg–Rabinowitsch correction was made in accordance with ISO 11443:2021. The
.
viscosity (η) was reported as a function of shear rate (γ) for the die with an L/D ratio of 10.
A Zwick/Z2.5 instrument equipped with a 2 kN load cell was used to determine the
tensile properties. An Elastocon EP 04 ISO 37-2 cutting die, corresponding to specimen
type 5A in ISO 527-2, was used to cut test bars from three different regions of the molded
frames. The specimens were conditioned in a chamber at 23 ± 2 ◦ C and 50 ± 10% relative
humidity for at least 24 h prior to the tensile tests. The Young’s modulus, tensile strength,
and elongation-at-break were measured at a strain rate of 1 s−1 . The reported average
values and standard deviations were based on five independent measurements.

3. Results
Table 2 shows the thermal, structural, and rheological properties of the samples, and
Figure 3 shows the first heating curves of the pellets (P) and of the injection-molded
samples (IM).

Table 2. The thermal, structural, and rheological properties of the samples.

Tp1 (◦ C) Tp2 (◦ C) Tp3 (◦ C) ∆H (J/g) Tox (◦ C) Ash Content at

Sample Mw (g/mol) PDI MFR (g/10 min)
P IM P IM P IM P IM P IM 550 ◦ C (%)

UW_SC1_200 111 111 125 125 161 161 66 63 224 223 11.5 123,000 4.8 0.5
UW_SC2_200 111 112 125 126 162 161 68 66 232 231 11.3 124,500 5.2 0.5
UW_SC1_240 111 112 124 126 161 161 67 63 226 226 10.5 N/A N/A 0.6
UW_SC2_240 111 112 125 127 161 160 69 64 231 232 11.2 122,000 5.0 0.6
IW_SC1_200 113 111 125 122 161 161 76 71 192 195 5.2 N/A N/A 1.9
IW_SC2_200 113 111 126 123 161 161 76 71 195 194 5.3 87,000 4.1 2.4
IW_SC1_240 113 111 123 124 159 160 76 70 180 182 5.1 N/A N/A 4.8
IW_SC2_240 113 110 123 123 160 160 76 71 184 184 5.3 71,500 4.4 3.9
rLDPE 118 109 125 125 161 161 74 69 188 193 5.1 103,500 4.0 14.6
P: pellets after compounding; IM: injection-molded samples.

The melting curves for all the samples had main peaks at 125 ◦ C, with a shoulder
at 111 ◦ C and a small peak at 161 ◦ C. The main peaks (Tp2 ) were apparently associated
with the higher densities and linear grades, i.e., HDPE and MDPE, and the Tp1 peak was
associated with the LDPE and the Tp3 peak with the PP, as suggested in the literature [18,28].
The compounding temperature, screw configuration, and industrial washing had negligible
effects on the melting temperature, and the industrially recycled sample showed the
same behavior.
ling 2022, 7, x FOR PEER REVIEW
Recycling 2022, 7, 90 6 of 12

Figure 3. The first heating curves of the samples. The light colors show the unwashed samples
Figure 3. The first heating curves of the samples. The light colors show t
and the dark colors show the industrially washed and/or recycled samples, where the pellets (P)
the compounding
after dark colors are show thebyindustrially
represented washed
dashed curves and and/or recycled
the injection-molded samples (IM)samples,
by
solid curves.
compounding are represented by dashed curves and the injection-mol
curves.
The screw configuration and compounding temperature had negligible effects on the
oxidation temperature of the unwashed samples for both the pellets and IM samples. The
oxidation temperature of these samples was, however, slightly higher when they were
The with
compounded melting curves
the mixing for all
screw (SC2), thecompounding
but the samplestemperature
had main peaks
appeared to at 12
have ◦
111no°Ceffect.
andTheaindustrially
small peak washedatsamples
161 °C. had TThe
ox values
mainapproximately
peaks (T 30 p2C)lower
were app
when compounded at 200 ◦ C, but they were approximately 40 ◦ C lower after compounding
the
at 240higher densities
◦ C. The screw design hadand linear grades,
a negligible effect on thei.e., HDPE
Tox values andsamples.
of these MDPE, an
The industrially recycled sample showed a Tox value similar to that of the industrially
ciated with the LDPE and the Tp3 peak with the PP, as suggested
washed samples.
TheThe compounding
ash content of the temperature,
unwashed materials screw configuration,
was approximately 11%, as and industr
reported
in other studies on post-consumer plastic film collected from mixed MSW [7], and the
ble effects on the melting temperature, and the industrially recyc
ash content after industrial washing (~5%) was in the same range as that reported in
same behavior.
previous studies.
Table 2 shows that the screw design and compounding temperature had negligible
The screw configuration and compounding temperature had
effects on the weight-average molecular mass (Mw ) of the pellets made of unwashed
oxidation
material. After temperature
industrial washing ofthe the unwashed
Mw was lower than thatsamples for both
of the unwashed the pell
samples,
and it was even lower with increasing compounding temperature, in agreement with the
oxidation
T temperature of these samples was, however, slightly
ox results. The industrially recycled sample showed an intermediate Mw value.
compounded
The flow curveswith the mixing
of the unwashed screw (SC2),
and industrially washed but thecompounded
samples compounding
using SC2 and of the industrially recycled pellets are presented in Figure 4.
to have no effect. The industrially washed samples had Tox valu
lower when compounded at 200 °C, but they were approximately
pounding at 240 °C. The screw design had a negligible effect on
samples. The industrially recycled sample showed a Tox value sim
trially washed samples.
The ash content of the unwashed materials was approxima
other studies on post-consumer plastic film collected from mixe
 Recycling 2022, 7, x FOR PEER REVIEW 7 of 12
Recycling 2022,
Recycling 7, x90FOR PEER REVIEW
2022, 7, 7 7ofof 12
12

Figure 4. Viscosity as a function of shear rate for the unwashed, industrially washed, and recycled
pellets.
Figure
Figure 4.4. Viscosity asaafunction
Viscosity as functionofof shear
shear raterate
for for the unwashed,
the unwashed, industrially
industrially washed,
washed, and recycled
and recycled pellets.
pellets.
The viscosity curves for all the samples corresponded to the GPC results, as the melt
The viscosity curves for all the samples corresponded to the GPC results, as the melt
viscosity
viscosity tendedto
The viscosity
tended to decrease
curves
decrease with
for with
all thedecreasing molecularweights.
samples corresponded
decreasing molecular weights. Asshown
to the As
GPC shown inTable
results,
in Table
as 2,the
the
the2,melt
unwashed
viscosity
unwashed materials
tended compounded
to decrease
materials compounded at 200
with decreasing ◦°C with
at 200 C molecular both screw
weights.
with both screw designs had
As shown
designs MFR
in Table
had MFR values
2, the
values of
of
0.5 g/10
unwashed min,
0.5 g/10 min, while
materials those compounded
compounded
while those compounded at 200 at 240
at °C °C had
◦ C had
240with both values of 0.6
screwofdesigns
values g/10
0.6 g/10hadmin.
min.MFR In the case
values
In the case of of
of
theg/10
0.5
the industrially
min, while
industrially washed materials,
thosematerials,
washed compounded thecompounding
the compounding
at temperature
240 °C had values hadamin.
of 0.6 g/10
temperature had agreater
greater
In the influence
case of
influence
than
the the screw
thanindustrially design,
the screw washed with MFR
design, materials,
with MFRthevalues of approximately
compounding
values 2 g/10
temperature
of approximately min and
had amin
2 g/10 4 g/min,
greater respec-
and influence
4 g/min,
tively,
than for the
the screwfor
respectively, samples
design, compounded
with MFR
the samples at 200 and 240
values of approximately
compounded °C, respectively,
at 200 and 240 ◦
2 g/10C,min indicating
and 4 g/min,
respectively, a progres-
respec-
indicating
asive
tively, degradation.
progressive
for the samples Thecompounded
industrially
degradation. recycled
The industrially
at 200 andsample
recycledhadrespectively,
240 °C, the highest
sample values
had the at 15
highest
indicating g/10 min,
avalues
progres- at
indicating
15
siveg/10 min, further
degradation. degradation.
indicating
The further degradation.
industrially recycled sample had the highest values at 15 g/10 min,
Figure
Figure
indicating 55shows
shows
further thetheYoung’s
Young’s
degradation. modulus
modulus forfor
thethe different
different screw
screw designs
designs (SC1(SC1 and SC2)
and SC2) and
andFigure
different
different compounding
compounding temperatures
temperatures (200 (200
and and
240 ◦240
C) °C)
at at
three three positions
positions
5 shows the Young’s modulus for the different screw designs (SC1 and SC2) in in
the the injec-
injection-
tion-molded
molded
and samples.
different samples.
compounding temperatures (200 and 240 °C) at three positions in the injec-
tion-molded samples.

Figure5.5.Young’s
Figure Young’smodulus
modulusofofthe
thesamples
samplesatatdifferent
differentregions
regionsininthe
theIM
IMframe.
frame.
Figure 5. Young’s modulus of the samples at different regions in the IM frame.
There
Therewaswasno nogreat
greatvariation
variationin inthe
themoduli
moduliof ofthe
theunwashed
unwashedsamples,
samples,as asindicated
indicatedbyby
light colors
lightThere in
inFigure
colorswas Figure 5,
5,either
either between
between the
the different
different compounding
compounding parameters
parameters
no great variation in the moduli of the unwashed samples, as indicated by or
orbetween
between
the
thedifferent
light colors inregions
different regions5,
Figure of the
themolded
ofeither molded
between samples.
samples. The
The average
the different average values
compounding of
of the
theYoung’s
valuesparameters Young’s moduli
moduli
or between
were
were 570,
570, 541,
541, and
and 571
571 MPa
MPa for
for the
the weld
weld lines, gates, and simple flow regions, respectively.
respectively.
the different regions of the molded samples. The average values of the Young’s moduli
There
There was
was a significant lower
lowermodulus
modulusafter after the industrial washing, with the average
were 570, 541,significant
and 571 MPa for the weld lines, the industrial
gates, and simplewashing, with
flow regions, therespectively.
average val-
values
ues of of Young’smoduli
Young’s modulibeing
being419,419,395,
395,andand403403MPa
MPa forfor the
the weld
weld lines,
lines, gates,
gates, and
and simple
simple
There was a significant lower modulus after the industrial washing, with the average val-
flow
flow regions, respectively. In case ofofthe industrially washed samples, the
thecompounding
ues ofregions,
Young’srespectively.
moduli beingIn419, case395, the
andindustrially
403 MPa for washed
the weldsamples,
lines, gates,compounding
and simple
temperature
temperature had
had a small
a small influence
influence on the
on modulus,
the modulus,but the
but screw
the design
screw and
design structure
and had
structure
flow regions, respectively. In case of the industrially washed samples, the compounding
no great effects.
had no greathad The
effects. industrially
The influence recycled
industrially sample showed the lowest Young’s moduli of
temperature a small onrecycled samplebut
the modulus, showed the lowest
the screw designYoung’s moduli
and structure
350, 331,
of 350, and
331, and324 MPa
324 Thefor the weld
MPaindustrially
for the weldlines, gates,
lines, gates,and simple
andshowed flow
simplethe regions,
flow respectively.
regions, respectively.
had no great effects. recycled sample lowest Young’s moduli
of 350, 331, and 324 MPa for the weld lines, gates, and simple flow regions, respectively.
 Recycling 2022, 7, x FOR PEER REVIEW 8 of 12
Recycling 2022, 7, x FOR PEER REVIEW 8 of 12
Recycling 2022, 7, 90 8 of 12

Figure 6 shows the tensile strengths of the molded samples made with different
Figure
screw
Figure 66shows
designs shows
(SC1the the
and tensile
SC2)
tensile andstrengths
different
strengths of the molded
compounding
of the molded samples
mademade
temperatures
samples with
with(200 anddifferent
different240 °C),
screw
screw
which designs
were (SC1
taken and
from SC2)
the and different
different regionscompounding
of the temperatures
injection-molded (200 and
samples.
designs (SC1 and SC2) and different compounding temperatures (200 and 240 C), which ◦ 240 °C),
which
were werefrom
taken takenthefrom the different
different regions regions of the injection-molded
of the injection-molded samples.samples.

Figure 6. The tensile strengths of samples taken from different regions of the IM frame.
Figure 6.6. The
Figure Thetensile
tensilestrengths
strengthsof
ofsamples
samplestaken
takenfrom
fromdifferent
differentregions
regionsofofthe
theIM
IMframe.
frame.
The strengths were lowest in the weld line regions, at approximately 9, 11, and 10
MPaTheThe strengths
forstrengths
the unwashed, werelowest
were lowest in in
industriallythethe weld
lineline
washed,
weld and regions,
regions, at approximately
industrially 11,9,and
recycled9,samples,
at approximately 11,10and 10
respec-
MPa
MPa
for thefor
tively. Thetheindustrially
unwashed, unwashed, industrially
recycled
industrially sample
washed, washed,
showed
and andthe industrially
industriallyhighest recycled
strength
recycled in samples,
samples, other respec-
the respectively.
two re-
tively.
gions,
The The
withindustrially
industrially averages
recycledofrecycledand 20sample
22sample MPa for
showed showed
the gates theand
highest highest
simple
strength strength
flow in the other
in theregions,
other two re-
respectively.
two regions,
gions,
with with
Theaverages
unwashed averages
and
of 22 and of 22 and
industrially 20
20 MPa forwashed MPa for the gates
the gatesmaterials
and simple and simple
hadflowsimilar flow regions,
average
regions, respectively.
strengthThe
respectively. values,
un-
The
washed unwashed
especially
andin and
the gate
industrially industrially
region,
washedwith washed materials
15 MPa,
materials hadwhereas
similarhad thesimilar
average
average average
strength
strength strength
values, thevalues,
in especially
simple
especially
in the gate
flow region in the
wasgate
region, with
16 MPa region,
15 MPa, forwith 15 MPa,
whereas
the unwashedthewhereas
average
samples the average
strength
and 13inMPa strength
the simple
for the inflow
the region
simple
industrially
flow
was 16region
washed MPa was
for
samples. the16 MPa for samples
unwashed the unwashed
and 13 MPa samples andindustrially
for the 13 MPa for the industrially
washed samples.
washedFigure 77shows
samples.
Figure showsthe theelongation-at-break
elongation-at-breakofofthe themolded
moldedsamples.
samples.As Asexpected,
expected,the theweld
weld
line regions
Figure showed
7 shows the
the lowest average
elongation-at-break elongations,
of the with
molded 6, 18, and
samples.
line regions showed the lowest average elongations, with 6, 18, and 24% for the unwashed, 24%
As for the
expected, unwashed,
the weld
industrially
line
industrially washed,
regions showed
washed,the and
and industrial
lowest average recycled samples,
elongations,
recycled samples, withrespectively.
6, 18, and 24%
respectively. InIn the
for
the gate
the
gate regions,
unwashed,
regions, the
the unwashed
industrially
unwashed samples
washed,
samples andshowed
showed thethe
industrial lowest
recycled
lowest average
averagesamples, elongation-at-break
respectively. Invalues,
elongation-at-break thevalues,
gatewith with
regions,
67%. 67%.
the
The
The industrial
unwashed
industrial washing
samples
washing provided
showed
provided an
theanlowest average
averageaverage value
value of 164%,
elongation-at-break
of 164%, and andthethe melt-filtration
values, of of
with 67%.
melt-filtration the
theThe
in-
industrially
industrial recycledprovided
dustrially washing
recycled samplesprovided
samples provided
an average anan average
value
averageof 164%,value
value ofof315%.
and 315%.
the In In
thethe
melt-filtration simple
simple offlowflow
the in-
re-
regions,
dustrially
gions, thetherecycled
industrially
industrially recycled
samples
recycled samplean
provided
sample had
had the
the highest
average valueaverage
highest of 315%.
average elongation-at-break,
In the simple flow
elongation-at-break, with
re-
with
367%,
gions, followed
367%, the by
industrially
followed the industrially
by therecycled
industriallysample washed samples,
had the
washed with
highest with
samples, average128%,
128%, and the lowest
elongation-at-break,
and the lowest values values
with
belonged
367%,
belonged totothe
followed theunwashed
by samples,
samples,with
the industrially
unwashed with96%.
washed 96%.samples, with 128%, and the lowest values
belonged to the unwashed samples, with 96%.

Figure7.7.The
Figure Theelongation-at-break
elongation-at-break values
values of of
thethe samples,
samples, taken
taken from
from different
different regions
regions of IM
of the the frame.
IM
frame. 7. The elongation-at-break values of the samples, taken from different regions of the IM
Figure
frame.
Recycling 2022, 7, 90 9 of 12

4. Discussion
There was no great variation in the melting temperatures between the unwashed,
industrially washed, and industrially recycled samples, and they were affected neither
by the process temperature nor by the screw configuration. However, the heat of fusion
(∆H) values of the industrially washed and recycled samples were slightly higher, which
indicates a small increase in crystallinity, likely due to lower content of impurities after
washing [29].
The screw configuration had an impact on the Tox values of the unwashed samples,
but the temperature had a greater influence on the industrially washed samples. The
industrial washing reduced the thermo-oxidative stability of the samples. In one study, the
Tox of un-stabilized virgin PE was 180 ± 5 ◦ C. This suggests that the unwashed samples still
retained some active stabilizers, having a Tox of at least 223 ◦ C, whereas a possible depletion
of stabilizers in the industrial washing and recycling processes reduced the Tox values
to 180–195 ◦ C [30]. These decreases in Tox values increases the samples’ susceptibility to
further degradation at further processing after industrial washing, possibly caused by the
washing agents [19].
The ash content was significantly reduced by industrial washing, with the high ash
content in the untreated samples presumably due to unwanted materials, such as paper,
PET, abrasives, etc. [7].
The slight variations in the Mw and PDI values of the unwashed samples may be
insignificant, but the lower values of both the Mw and the PDI values of the industrially
washed samples compared to those of the unwashed samples implies that chain scission
dominated the degradation [31,32]. The influence of washing agent residues also suggests
that chain scission is preferred in the case of HDPE [19]. Industrial washing reduced the
Mw values, but the industrially recycled sample had an intermediate Mw value, indicating
that additives were used in the industrial recycling process [32,33].
The viscosity curves supported the Mw data. Compounding at a higher temperature
resulted in a slightly lower viscosity for both the unwashed and washed materials, presum-
ably because degradation leads to a lower Mw value [34]. However, the balance between
the chain scission and chain branching during degradation made the rheological behavior
of the samples more complicated [35–37]. This may be one of the reasons why the MFR
values did not show the same order, since the industrially recycled material had the highest
MFR, but it did not have the lowest viscosity curve. Another possibility may be that the
MFR represented a single, not-well-defined point on the viscosity curve in terms of shear
rate and viscosity. The MFR values for the unwashed and washed materials indicated
that they could be useful for extrusion-based processes such as film-blowing and profile
extrusion, but they may be less suitable for injection-molding. The MFR value suggests
that industrially recycled materials would likely be suitable for injection-molding, e.g., for
caps, toys, and housewares [38,39].
The Young’s modulus of the unwashed samples was not affected by the compounding
parameters, but there was a significant reduction in the modulus after industrial washing,
with a further decrease after industrial compounding with melt-filtration. The industri-
ally washed samples showed a slightly higher stiffness when compounded at a higher
temperature. The differences in Young’s moduli between the different regions of the IM
samples were negligible in all cases, but this was not the case for the tensile strength and
elongation-at-break measurements. As expected, the weld line regions showed the lowest
strength values, between 9 and 11 MPa, but these values were unexpectedly high and close
to the reported value (13 MPa) for the virgin PE-LLD [40]. The industrially recycled sample
had the highest strength in both the gate and simple flow regions, whereas the unwashed
and industrially washed samples showed similar strength values in the gate region and the
latter had a slightly lower strength value than the former in the simple flow region. This
slight decrease in the better-oriented region may be due to the lower Mw after washing [41].
Neither the temperature nor the screw design during compounding had a great influence
on the tensile strength of the unwashed and industrially washed materials.
Recycling 2022, 7, 90 10 of 12

The weld line region had the lowest elongation-at-break values in all cases. Both a
higher temperature and the mixing screw in the compounding process resulted in increased
values of elongation-at-break for the unwashed samples, possibly due to a better melting
and better mixing of polymer contaminants, which might otherwise act as stress concen-
trators [18,42]. However, in the case of the industrially washed samples, compounding
at a lower temperature resulted in a higher elongation-at-break, while the screw design
had a negligible effect, possibly because washing reduced the amount of impurities, but
also because the degradation increased with the increasing processing temperature [43].
The effect of industrial washing was significant in the weld line and gate regions, resulting
in a higher elongation-at-break measurement. In the simple flow region, there was an
increase in elongation-at-break at a lower compounding temperature after washing and a
slight decrease at a higher compounding temperature, implying that the effect of reduced
contaminants might dominate at lower processing temperatures, while the degradation
increased at higher temperatures.

5. Conclusions
The melt-processing parameters had a small influence on the properties of molded
samples, and the influence of the compounding temperature was greater than that of
the screw configuration for both the unwashed and industrially washed samples. No
differences in the degradation of the unwashed samples as a result of different melt-
processing parameters were observed. Washing led to a significant degradation, leading
to further degradation in the subsequent melt-compounding. The mechanical properties
implied that the material would be useful for suitable applications. The results also
indicated a need for upgrading components.

Author Contributions: Conceptualization, E.C.B.N., A.V. and A.B.; methodology, E.C.B.N., A.V.
and A.B.; validation, E.C.B.N. and A.V.; formal analysis, E.C.B.N.; investigation, E.C.B.N. and A.V.;
resources, A.B.; data curation, E.C.B.N. and A.V.; writing—original draft preparation, E.C.B.N.;
writing—review and editing, E.C.B.N., A.V. and A.B.; visualization, E.C.B.N.; supervision, A.B.;
project administration, A.B.; funding acquisition, A.B. All authors have read and agreed to the
published version of the manuscript.
Funding: This work was funded by the Norwegian Retailers’ Environment Fund, grant number
ID11297, Plastkretsen AB: s Stiftelse för Forskning and Chalmers University of Technology.
Data Availability Statement: The data presented in this study are available on request from the
corresponding author.
Acknowledgments: The authors thank the Norwegian Retailers’ Environment Fund, Plastkretsen
AB: s Stiftelse för Forskning and Chalmers University of Technology for the financial support. The
Swedish Plastic Recycling AB and the Research Institutes of Sweden (RISE) are acknowledged for
their support in sampling and in the melt mass-flow rate measurements, respectively. J. A. Bristow is
gratefully acknowledged for his linguistic revision of the manuscript.
Conflicts of Interest: The authors declare no conflict of interest.

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