Waste Management xxx (2014) xxxxxx

Contents lists available at ScienceDirect

Waste Management
journal homepage: www.elsevier.com/locate/wasman

Separation of polyethylene terephthalate from municipal waste plastics

by froth otation for recycling industry
Chong-Qing Wang, Hui Wang , You-Nian Liu
School of Chemistry and Chemical Engineering, Key Laboratory of Resources Chemistry of Nonferrous Metals, Ministry of Education, Central South University, Changsha,
410083 Hunan, China

a r t i c l e

i n f o

Article history:
Received 18 August 2014
Accepted 24 September 2014
Available online xxxx
Keywords:
Flotation
Municipal waste plastics
Polyethylene terephthalate
Recycling

a b s t r a c t
Recycling is an effective way to manage plastic wastes and receives considerable attention. Since plastic
mixtures are difcult to recycle because of their intrinsic characteristics, separation of mixed plastics is
the key problem for recycling. Separation of polyethylene terephthalate (PET) from municipal waste plastics (MWP) by froth otation combined with alkaline pretreatment was investigated for recycling industry. The effect of process variables was estimated by L9 (34) orthogonal array of experiments and single
factor experiments. The optimum conditions of alkaline pretreatment are 10 wt% sodium hydroxide,
20 min and 70 C. After alkaline pretreatment under optimum conditions, otation separation PET from
acrylonitrilebutadienestyrene, polystyrene, polycarbonate or polyvinyl chloride was achieved with
high purity and efciency. The purity of PET is up to 98.46% and the recovery is above 92.47%. A ow
sheet of separation PET from MWP by a combination of froth otation and sink oat separation was
designed. This study facilitates industrial application of plastics otation and provides technical insights
into recycling of waste plastics.
2014 Elsevier Ltd. All rights reserved.

1. Introduction
Plastics have been widely used owing to their advantages such
as cheapness, endurance, lightness, hygiene and design adaptability. The worlds total consumption of plastics has an average
growth rate of 56%, reaching 297.5 million tons by 2015
(Saisinchai, 2013). In 2010, China became the biggest production
region of plastics, accounting for 23.5% of the global production
265 million tons, and Europe, the second production region,
accounted for 21.5%. In the United States, 103.2 billion pounds of
plastics were produced in 2011 (Saisinchai, 2013). The sharp rise
and mass consumption of plastics produce a great quantity of
wastes, which poses a formidable challenge for waste
management.
At present, the disposal processes of plastic wastes are mainly
incineration and landll. The incineration and landll deposition
of municipal waste plastics (MWP) may cause environmental problems and is becoming more expensive. Due to increasing volume of
MWP and decreasing landll capacity for disposal, landll becomes
more challenging. In addition, landll can release hazardous substances and plastic wastes take long time to degrade. In terms of

Corresponding author. Tel.: +86 731 88879616.

E-mail address: huiwang1968@163.com (H. Wang).

incineration, it causes hazardous releases such as nitrous oxide,

sulphur oxides, dusts, dioxins and other toxins (Ali and Siddiqui,
2005). Especially, incineration of polyvinyl chloride (PVC) plastic
causes the environmental pollution and reduces the service life
of the incinerator by generating hazardous hydrogen chloride gas
and dioxins containing chlorine (Wey et al., 1998). In this regard,
the disposal of plastic wastes has become an important issue all
over the world, and recycling is an effective way to solve this problem. Recycling of plastic wastes shows numerous benets: reducing consumption of energy; reducing the amount of solid wastes
that go to incineration and landll and thus decreasing the environmental pollutions; displacing partially virgin plastics produced
from rened fossil fuels (Saisinchai, 2013; Siddique et al., 2008).
Different plastics, generally, cannot be recycled together due to
chemical incompatibility and difference in melt point and thermal
stabilities, which can limit the quality of the recycled plastic products (Carvalho et al., 2012; Kangal, 2010). Specically, PVC
decreases the recycling ratio of plastics by forming compounds
or deteriorating the nature of other materials even if a small quantity of PVC is present in the main plastics. In the case of energy
recycling, PVC-free plastics are more practicable because incineration of PVC generates gases that destroy the devices and pollute the
environment. Recycling of plastics encompasses four stages: collection, separation, processing/manufacturing and marketing, and
the key problem is separation at present (Ulrici et al., 2013;

http://dx.doi.org/10.1016/j.wasman.2014.09.025
0956-053X/ 2014 Elsevier Ltd. All rights reserved.

Please cite this article in press as: Wang, C.-Q., et al. Separation of polyethylene terephthalate from municipal waste plastics by froth otation for recycling
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C.-Q. Wang et al. / Waste Management xxx (2014) xxxxxx

Serranti et al., 2012; Serranti et al., 2011; Serranti et al., 2012).

Therefore, the development of separation techniques that can
recycle plastic wastes is a growing necessity.
There are many kinds of plastics in MWP, including polyethylene (PE), polypropylene (PP), polyethylene terephthalate (PET),
acrylonitrilebutadienestyrene (ABS), polystyrene (PS), polycarbonate (PC) and PVC plastics. PET is the most common plastic
and currently the major recyclable plastic material, followed by
high density polyethylene (HDPE), PP and PVC (Saisinchai, 2013).
Numerous techniques are developed for plastics separation,
such as electrostatic separation (Inculet et al., 1998; Park et al.,
2007a; Park et al., 2007b; Cui and Forssberg, 2003), gravity separation (Pongstabodee et al., 2008; Pascoe, 2006), selective dissolution
(Achilias et al., 2007; Pappa et al., 2001), sorting based on infrared
analysis or laser scanning (Sommer and Rich, 2001; Ahmad, 2004).
Froth otation, an alternative method, receives increasing attention due to effective separation of plastics with similar properties
such as density, dielectric constant and surface hydrophobicity
(Fraunholcz, 2004; Alter, 2005; Wang et al., 2012, 2014, 2013).
Since most plastics possess low-energy surface, namely naturally
hydrophobic, selective wetting one or more components is necessary in otation process, which can be achieved by adsorption of
surfactants or surface modication. Surfactants, such as tannic
acid, lignosulfonates and methyl cellulose, were reported to be
effective to selectively change the hydrophobicity of plastics, and
otation separation of plastic mixtures were obtained at bench
scale (Saisinchai, 2013; Wang et al., 2012; Shen et al., 2002a,
2002b; Le Guern et al., 2000; Abbasi et al., 2010). Surface modications, such as alkaline treatment, plasma treatment, ame treatment, boiling treatment and ozonation, were developed to
facilitate plastics otation (Fraunholcz, 2004; Pascoe and
OConnell, 2003; Wang et al., 2014; Reddy et al., 2007). Alkaline
treatment can render PET surface more hydrophilic, which may
be a result of hydrolysis of ester bonds in PET chains. A combination of alkaline treatment and surfactants adsorption leaded to a
synergetic effect with improved separation and lower reagent
consumption.
This work aims at developing a reliable and relatively inexpensive technology for the effective separation of PET from ABS, PS,
PVC, and PC plastics by one stage otation process, based on alkaline pretreatment at optimum conditions. Particularly, our study is
focused on estimating process variables such as treatment time,
temperature, NaOH concentration, as well as particle size and pH
that affect the separation efciency. Flotation separation of binary
mixtures was conducted, and a ow sheet was designed to separate PET from MWP.
2. Materials and methods
2.1. Materials
Seven different kinds of plastics from MWP were selected as
research object. PP, HDPE, PET, PC, ABS and PS were achieved from

a waste plastics market (Miluo, Hunan Province, China), and PVC

was obtained from pharmaceutical blisters. Samples of plastics
were identied by Fourier Transform Infrared (FT-IR) spectrometer
(Nicolet Avatar 360, Nicolet Magua Corporation, USA). The samples
were crushed using a plastic cutting mill (SCP-180-2, Cixi Yinbo
Plastics Machinery Co., Ltd.), and the sieve size fraction used in this
study was 3.20.9 mm. The information of samples is shown in
Table 1. Plastic samples were of different colors or shapes, which
made analysis of purity of the plastics through manual sorting at
the end of each experiment easier. Terpineol was used as frother;
terpineol and sodium hydroxide were analytical purity and used
as received. Tap water was used throughout the otation tests.

2.2. Alkaline pretreatment

The samples were soaked in sodium hydroxide solutions in
1000 mL beaker for 045 min, and the fraction of plastic particles
was approximate 15 wt%. The alkaline pretreatment were conducted in a thermostat-controlled (DF-101S, Shanghai Bilon Instruments Co., LTD., China) water bath. After alkaline pretreatment, the
particles were taken out from alkaline solutions, rinsed with tap
water, soaked in tap water for 5 min, and used to conduct otation
experiment.

2.3. Flotation experiments

The otation experiments were conducted using a self-designed
otation column (shown in the Supplementary Material) with a
height of 170 mm and a diameter of 30 mm. Air was passed
through the sand core to produce gas bubbles, and an adjustable
air-pump (Guangdong Hailea Group Co., Ltd) with maximum airow rate of 7.2 ml/min was employed. Terpineol (52.7 ml/g or
70.3 ml/g) serving as frother was added into the otation column
during the otation experiments. At the end of the otation test,
the oat and non-oated plastic particles were collected, rinsed
with tap water, dried in atmosphere, and weighed.
The alkaline pretreatment of PET was studied rstly by orthogonal array of experiments with respect to temperatures (30 C,
50 C and 70 C), NaOH concentrations (5 wt%, 10 wt% and
15 wt%) and treatment time (5 min, 20 min and 35 min). Then, single factor experiments involving NaOH concentrations (020 wt%),
treatment time (045 min), temperatures (3075 C), particle sizes
(0.94.0 mm) and pH (2.512.2) were conducted to investigate the
otation behavior of PET. The otation behavior of ABS, PS, PVC and
PC was tested and was shown insensitive to alkaline pretreatment
(not presented in this work). Based on the otation of PET, otation
separation of binary plastic mixtures (5050 wt%), namely PET/
ABS, PET/PS, PET/PVC and PET/PC, was conducted combined with
alkaline pretreatment. The separated products were manually
sorted based on the difference in color or shape, and the otation
recovery and purity of each plastic in the oat and non-oated
products were calculated based on mass balance.

Table 1
The information of samples.

Plastics

Abbreviation

Source

Density (g/cm3)

Appearance

High density polyethylene

Polypropylene
Polyethylene terephthalate
Polyvinyl Chloridea
Acrylonitrilebutadienestyrene
Polystyrene
Polycarbonate

HDPE
PP
PET
PVC
ABS
PS
PC

Shampoo bottles
Shampoo bottles
Beverage bottles
Pharmaceutical blisters
Electrical shells
Packing boxes
Drinking machine buckets

0.951
0.911
1.452
1.318
1.068
1.075
1.197

White particle
Transparent plate
Transparent ake
Beige ake
Titanium white particle
Transparent particle
Blue particle

PVC from pharmaceutical blister was leached by NaOH solutions to removing non-plastic materials.

Please cite this article in press as: Wang, C.-Q., et al. Separation of polyethylene terephthalate from municipal waste plastics by froth otation for recycling
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C.-Q. Wang et al. / Waste Management xxx (2014) xxxxxx

3. Results and discussion

3.1. L9 (34) orthogonal array of experiments
The factors of temperatures (A), NaOH concentrations (B) and
treatment time (C) were investigated by orthogonal array of experiments of three factors and three levels (Yang and Tarng, 1998;
Taguchi, 1990). The liquid/solid ratio was 100:1 ml/g when alkaline pretreatment was conducted; based on preliminary tests, the
otation experiments were carried out under conditions of pH
7.0 0.2, otation time 4 min and frother concentration 52.7 ml/
g. The variable assignment and the level settings are shown in
Table 2. The results of L9 (34) orthogonal array of experiments
are presented in Table 3. It should be noted that otation recovery
is dened as the percentage of oat particles. K1, K2 and K3 represent the sum of otation recovery of level 1, level 2 and level 3 of a
factor, respectively. K1/3, K2/3 and K3/3 denote the average of K1, K2
and K3, respectively. R represents the maximum difference value
among K1, K2 and K3.

O
H O C

O
O
NaOH
C O CH2 CH2 O H + H2O
HO C

Table 2
Experimental factors and levels.
Level

Factor

1
2
3

A (C)

B (wt%)

C (min)

30
50
70

5
10
15

5
20
35

Table 3
The results of L9 (34) orthogonal array of experiments.
Number

Factor
Treatment
time (min)

NaOH
concentration
(wt%)
B

30
30
30
50
50
50
70
70
70
155.96
128.67
15.54
51.99
42.89
5.18
46.81

5
10
15
5
10
15
5
10
15
158.55
74.57
67.05
52.85
24.86
22.35
30.50

5
20
35
20
35
5
35
5
20
143.10
113.54
43.53
47.70
37.85
14.51
33.19

Temperature
(C)

1
2
3
4
5
6
7
8
9
K1
K2
K3
K1/3
K2/3
K3/3
R

Flotation
recovery (%)

with the result from orthogonal array of experiments. Since orthogonal array of experiments cannot provides enough insights into the
effects of experimental factors on the otation behavior of PET, single factor experiments were further carried out based on the result
of orthogonal array of experiments, and more practicable optimal
conditions were obtained from the results of the sequential experimentation of each controllable variable, one at a time.
3.2. Mechanism of alkaline pretreatment
It is, generally, suggested that chemical reactions occur
between alkaline solution and PET on the surface of PET
(Caparanga et al., 2009). Mancini and Zanin pointed out that thermodynamic estimates showed that the weakest chemical connection in the PET chain is the ester link (Mancini and Zanin, 1999).
NaOH can destroy ester bonds in polymer chains, and thus hydrolysis of PET occurs in NaOH solution, which can be viewed as the
reverse reaction of esterication. Thus, the reaction between NaOH
and PET surface can be shown as Eq. (1).

O
C OH + CH2OHCH2OH

As demonstrated in Table 3, the R value of the factors A, B and C

is 46.81, 30.50 and 33.19, respectively, implying that the most signicant factor is temperature followed by treatment time and
NaOH concentration. The optimal scheme is A3B3C3; the experimental conditions are temperature 70 C, NaOH concentration
15 wt% and treatment time 35 min. In order to prove the optimized
scheme, the otation test was conducted under optimal conditions,
and otation recovery of 0.15% was achieved, which is in agreement

FT-IR and atomic force microscope analysis, as well as contact

angle measurements, conrmed hydrolysis of PET (Caparanga
et al., 2009; Martin et al., 2011). Alkaline pretreatment results in
an increase in the number of hydrophilic groups (hydroxyl and carboxyl) on the PET surface and surface roughness, and thus renders
PET surface more hydrophilic. Therefore, the mechanism of alkaline pretreatment for facilitating otation can be shown in Fig. 1.
Although chemical reactions occur on PET surface, alkaline treatment has a little inuence on the bulk characteristics of PET since
just a few nanometers of PET surface were destroyed during treatment. Therefore, alkaline treatment basically does not affect the
post-recycling process.
3.3. Effect of NaOH concentration
The PET particles were subjected to treatment with alkaline
solutions at 70 C for 35 min, and after ltering and rinsing, otation was conducted under conditions of pH 7.0 0.2, terpilenol
concentration 52.7 mg/l and otation time 4 min. The experimental results are shown in Fig. 2.
As shown in Fig. 2, the PET sample is naturally hydrophobic, and
the otation recovery of PET is 99.85% without pretreatment. Flotation recovery of PET drops signicantly with increasing NaOH
concentration, which can be explained by the fact that an increase

87.42
48.48
20.06
64.8
17.14
46.73
6.33
8.95
0.26

Fig. 1. Mechanism of alkaline pretreatment for facilitating otation.

Please cite this article in press as: Wang, C.-Q., et al. Separation of polyethylene terephthalate from municipal waste plastics by froth otation for recycling
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C.-Q. Wang et al. / Waste Management xxx (2014) xxxxxx

Fig. 2. Effect of NaOH concentration on otation recovery of PET.

Fig. 4. Effect of treatment temperature on otation recovery of PET.

of NaOH concentration accelerates hydrolysis reaction of PET. The

otation recovery is declined to 0.26% when the NaOH concentration is 10%. Therefore, NaOH concentration of 10% was selected as
optimum for further experiments.

It can be seen from Fig. 4 that temperature has a considerable

effect on otation recovery of PET, implying that temperature is
a key factor for alkaline pretreatment, which is also conrmed by
orthogonal array of experiments. The inuence of temperature
can be divided into two stages; otation recovery of PET declines
slightly with an increase of temperature at low temperature
(below 50 C), and the otation recovery of PET is sharply
decreased to 2.75% at 60 C and further decreases with increasing
of temperature. This can be explained by the following reasons:
the activated molecules are fewer at low temperatures, and thus
hydrolysis reaction of PET is limited; higher temperatures signicantly increase the number of activated molecules and accelerate
molecular motion, and thus promote the reaction. Higher temperature involves more energy and may cause degradation of PET
(Caparanga et al., 2009), and thus 70 C was selected as optimum
for further experiments.

3.4. Effect of treatment time

The PET particles were subjected to treatment with 10% NaOH
solutions at 70 C, and otation was conducted under conditions
of pH 7.0 0.2, terpilenol concentration 52.7 mg/l and otation
time 4 min. The effect of treatment time on PET otation recovery
is shown in Fig. 3.
As shown in Fig. 3, otation recovery of PET declines sharply
with increasing treatment time. The orthogonal array of experiments illustrates treatment time has a signicant effect on otation recovery of PET, and results shown in Fig. 3 further conrm
the conclusion. The otation recovery drops from 99.85% to
3.57% when the treatment time is 10 min, and it reduces to
0.58% at treatment time of 20 min. Therefore, treatment time of
20 min was selected to conduct further experiments.
3.5. Effect of treatment temperature
Treatment with 10% NaOH solutions for 20 min was conducted
at different temperatures, and otation was carried out under conditions of pH 7.0 0.2, terpilenol concentration 52.7 mg/l and otation time 4 min. The effect of temperature on PET otation
recovery is displayed in Fig. 4.

3.6. Effect of particle size

Plastic components in most plastic products are adequately liberated at large particle sizes. The particle size of plastics subjected
to otation is usually 110 mm, one or two order of magnitudes
larger than that of ores. In previous studies, it is manifested that
particle size shows certain inuence on otation behavior of plastics (Fraunholcz, 1997; Shen et al., 2001; Marques and Tenrio,
2000). Thus, the effect of particle size should be taken into consideration. The PET samples and the oat products were screened into
four sections, namely 0.92.0 mm, 2.02.5 mm, 2.53.0 mm and
3.04.0 mm, and distribution of particle size is shown in Fig. 5. It
should be noted that the oat products were obtained after pretreatment 10% NaOH solutions for 20 min at 70 C and otation
under conditions of pH 7.0 0.2, terpilenol concentration
52.7 mg/l and otation time 4 min.
As demonstrated in Fig. 5, the particle size of PET samples is distributed relatively evenly. After pretreatment, small particles show
better oatability, and the percentage of particle size of 0.9
2.0 mm and 2.02.5 mm increases while that of large particles
(2.53.0 mm and 3.04.0 mm) declines. Experimental results by
Fraunholcz (1997), Shen et al. (2001), Marques and Tenrio
(2000) manifest that large particles are more difcult to oat than
small ones, and results shown in Fig. 5 are consistent with this fact
though alkaline pretreatment is employed before otation.
3.7. Effect of pH

Fig. 3. Effect of treatment time on otation recovery of PET.

After pretreatment of PET with 10% NaOH solutions for 20 min

at 70 C, otation was conducted under conditions of terpilenol

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Fig. 5. Distribution of particle size of PET sample and oat product.

Fig. 7. Flow sheet of separation PET plastic from MWP by froth otation and sink
oat separation.

conditions. Flotation separation of plastic mixtures can be conducted at neutral condition, namely pH 7.0, which reduces the difculty of disposal of waste water.
3.8. Flotation separation of PET

Fig. 6. Effect of pH on otation recovery of PET.

concentration 52.7 mg/l and otation time 4 min. The effect of pH

on PET otation recovery is displayed in Fig. 6.
It is obvious from Fig. 6 that the pH of otation medium has a
little effect on the otation recovery of PET, and the otation recovery is less than 2.7% at both acidic and alkaline conditions. Kirjavainen pointed out that the otability of particles being better in
acid than in alkaline liquid, which is a consequence of higher surface tension at acid pH (Kirjavainen et al., 2003), and the result
shown in Fig. 6 is consistent with the conclusion since the recovery
of PET at acidic conditions is slightly higher than that at alkaline

From above results, it can be concluded that alkaline pretreatment can change signicantly the hydrophobicity of PET, which
is responsible to the hydrolysis of PET. Hence, separation of PET
plastic from MWP by froth otation combined alkaline pretreatment can be achieved for recycling. After treatment with 10%
NaOH solutions for 20 min at 70 C, otation separation of binary
plastic mixtures was conducted with the liquid/solid ratio of
80:1 ml/g under conditions of pH 7.0 0.2 and otation time
5 min. The terpilenol concentration became 70.3 mg/l since more
particles were added. The results of otation separation of PET
are shown in Table 4.
From Table 4, it can be seen that otation separation of PET
from ABS, PC, PVC or PS plastics was obtained efciently. The purity and recovery of separated PET were above 92.35% and 92.47%,
respectively; in terms of other plastics (ABS, PC, PVC or PS), the
purity and recovery of were also above 93.11% and 91.37%, respectively. In the case of PET/PC, the purity of PET is highest and up to
98.46%; in terms of PET/PS, best separation is achieved since both

Table 4
Flotation separation of PET from binary plastic mixtures.
Plastic mixtures

Products

Yield (%)

Purity (%)

Recovery (%)

PET

OPa

PET

OPa

PET/ABS

Float
Non-oat
Feed

45.61
54.39
100.00

3.40
92.35
51.78

96.60
7.65
48.22

2.99
97.01
100.00

91.37
8.63
100.00

PET/PC

Float
Non-oat
Feed

53.78
46.22
100.00

6.89
98.46
49.21

93.11
1.54
50.79

7.53
92.47
100.00

98.60
1.40
100.00

PET/PVC

Float
Non-oat
Feed

50.58
49.42
100.00

1.78
93.57
47.14

98.22
6.43
52.86

1.90
98.10
100.00

93.98
6.02
100.00

PET/PS

Float
Non-oat
Feed

43.12
56.88
100.00

0.72
96.66
55.30

99.28
3.34
44.70

0.56
99.44
100.00

95.76
4.24
100.00

OP denotes the other plastics, namely ABS, PC, PVC or PS.

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C.-Q. Wang et al. / Waste Management xxx (2014) xxxxxx

the purity and recovery are above 95.76% and the purity of PS is up
to 99.28%.
Flotation separation of PET from ABS, PC, PVC or PS plastics was
obtained with high efciency and purity, and separation PET from
MWP containing PP, HDPE, PET, ABS, PC, PVC and PS plastics was
further studied. As manifested in Fig. 7, a ow sheet of separation
PET from MWP was designed by a combination of froth otation
and sink oat separation. As shown in Table 1, the density of PP
and HDPE is 0.911 g/cm3 and 0.951 g/cm3, respectively, lower than
that of water (1.0 g/cm3). Complete separation of light components
(PP and HDPE) was obtained by sink oat separation using water as
medium; and PP and HDPE were further separated by sink oat
method using alcohol solution (0.93 g/cm3) as medium. In the case
of heavy components, PET can be puried through alkaline pretreatment followed by froth otation, while other plastics can be
further separated by otation.
4. Conclusions
Separation of PET from municipal waste plastics by froth otation combined with alkaline pretreatment was investigated for
recycling industry. Orthogonal array of experiments demonstrate
that the most signicant factor with respect to alkaline pretreatment is temperature followed by treatment time and NaOH concentration. Single factor experiments conrm that the optimum
conditions of alkaline pretreatment are 10 wt% NaOH, 20 min and
70 C. After alkaline pretreatment under optimum conditions, otation separation PET from ABS, PS, PVC or PC was achieved with
high purity and efciency. The purity of PET is up to 98.46% and
the recovery is above 92.47%.
Flotation separation of PET is a reliable and relatively inexpensive technology. A ow sheet of separation PET from MWP containing PP, HDPE, PET, ABS, PC, PVC and PS plastics by a combination of
froth otation and sink oat separation was further designed. This
work facilitates industrial application of plastics otation and provides technical insights into recycling of waste plastics.
Appendix A. Supplementary material
Supplementary data associated with this article can be found,
in the online version, at http://dx.doi.org/10.1016/j.wasman.2014.
09.025.
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Please cite this article in press as: Wang, C.-Q., et al. Separation of polyethylene terephthalate from municipal waste plastics by froth otation for recycling
industry. Waste Management (2014), http://dx.doi.org/10.1016/j.wasman.2014.09.025