Thermal Degradation of mixed Plastic Solid Waste HDPE, LDPE, PP and PS Halla Ibrahim1*, RamadanMohmmed2,Hasabo A. Mhd Ahmed3, Sahar M. Ahmed4,R. M. Abualsoud5,Motawie, A.M1,6 1,5Africa 4,6Petrochemicals
City of Technology, Khartoum Sudan
Department, Egyptian Petroleum Research Institute, Nasr City, Cairo, Egypt
2, 3Sudan
University of Science and technology, Khartoum Sudan *
[email protected]
Abstract Pyrolysis of mixed waste plastic (Low density polyethylene (LDPE), High density polyethylene (HDPE), Polypropylene (PP) and polystyrene (PS)) were conducted in temperature range (200- 400 °C).The pyrolysis produced 95% of liquid fuel, 3% solid residue (char), and 2% gases.The oil obtained from the pyrolysis was fractionatedusing distillation process in different temperatures.Fractions were characterized using gas chromatographymass spectroscopy (GC-MS) and infrared spectroscopy (FTIR). The analysis of the fractions shows the presence of a mixture of different fuel fractions components such as kerosene, gasoline and diesel. Key
words:
fractional
distillation,
GC/MS,
pyrolysis,
waste
plastic
1. Introduction Due to the steadily increasing of plastic over Due to the increase in generation, waste
the last years and the disposal of waste
plastics are becoming a major stream in solid
plastic in Landfill, dump sites and open
waste, even the cities with low economic
burning without energy recovery lead to
growth have started producing more plastic
resource loss beside causing a serious health
waste due to plastic packaging, plastic
problems and environmental pollution[5-7].
shopping bags, PET bottles and other goods/appliances which uses plastic as the
Aplastic material is (Society of Plastics.
major component Solid waste has become
Industry, cited in Brady and Clauser, ‘any
one of the global environmental issues [1-4].
one of a large group of materials consisting
The proper waste management strategy is an
wholly or in part of combinations of carbon
important aspect of sustainable development.
with oxygen, hydrogen, nitrogen, and other 1
organic
or
inorganic
elements[8,
9].In
efficiency of the pyrolysis process can be up
common usage the terms plastics, polymers
to 90 % and the liquid end products are used
and resins are roughly equivalent[9-12]. The
as fuels [20].
plastics are mainly two types; thermoplastics
Several studies are reported for pyrolysis or
and thermosetting plastics. The first type is composed
of
polyethylene
polyolefin (LDPE),
(low high
thermal degradation of plastic wastes the
density
majority of these studies focused on LDPE
density
and the yield of liquid fraction is low and
polyethylene (HDPE), polypropylene (PP),
most of it is heavy and waxy.
polystyrene (PS), polyethylene terephthalate (PET) and polyvinyl chloride (PVC)) and
The thermal process utilized tobreak down
they are mainly used in containers and
the hydrocarbon chains of the polymers and
packing, and can be recycled[13, 14].
convert
and
industrial
the plastics produced a high yield of anoil\wax product in the range, 81-97 wt.
suitable
%.[22], the melting and thermal cracking
treatment of plastic wastes is one of the key
processes were carried out in a single batch
questions of the waste management and is
process at the temperature range is 200–420
important from energetic, environmental,
ºC. The final product consisted of light gas
economic and political aspects[15].
6.3 % and liquid product 90%. 3.7% solid
A Tertiary (chemical) recycling uses a chemical
procedure
to
recover
with
liquid product[21].Non-catalytic pyrolysis of
recycled product or monomer recovery), and The
fuel,
process. The process yields about 80-90%
recovery), true material recycling (similar
recovery.
liquid
utilized for the plasticthermal degradation
plastic
waste, i.e. landfill, incineration (energy
chemical
into
temperature range from 100 ºC to 400 ºC is
There are several methods for disposal of municipal
them
black products were produced. The light,
the
‘‘gas” fraction consist of the hydrocarbons
petrochemical components in plastics is
mixture (C1–C4) and rest of liquid fuel made
pyrolysis [16]. Pyrolysis, in general, means
over 90% of the liquid product. It may be
heating organic or inorganic material in the
used
absence of oxygen which leads to a
for
electricity
production of solid, liquid and a gaseous end
fuel
production
refinery
generation.[23]Pyrolytic
or oil,
consisting of almost 26% hydrocarbons
product [17]. The possible raw materials for
within the gasoline range and almost 70%
pyrolysis can be for example different
within the diesel range, is upgraded to
biomass products as well as organic wastes
transportation fuel in the existing refinery.
such as plastic [18, 19]. The thermal
[24]Thermal pyrolysis in a batch reactor 2
resulted in the highest yield of liquid
left inside the reactor was weighed. Then the
fractions. The liquid yield of HDPE, PP and
weight of gaseous/volatile product was
PS was found to be 80%, 82.6% and 80% by
calculated
mass, respectively. The characteristics of
Reactions were carried out at
HDPE and PP pyrolytic sample oils are
transferred into a fractional distillation unit.
similar
2.2.2
to
conventional
transportation
fuel[25].
from
the
material
balance. 400oCand
Fraction distillation
The oil obtained was fractioned using fraction distillation column in temperate
In this study thermal degradation of mixed
range from 45◦C to 370◦C.
waste plastics (high Density Polyethylene
2.2.3 Fourier transform- Infrared FT-IR
(HDPE), Low Density Polyethylene (LDPE),
The sample was loaded directly on the ATR
Polypropylene (PP), and Polystyrene (PS))
Zinc selenite (ZnSe) crystal, introduced into
depend on their presence in the garbage in
the FTIR and scanned at 4000-400 cm-1 at
Sudan into liquid fuel in temperature range
resolution intervals of 4.000 cm-1 using
(200- 400°C) were carried out.
NICOLET(370DTGS). *ATR:
2. Material and Method
Attenuated
total
reflection
2.1 Polymer Materials
*DTGS: Deuterium Tri Glycine Sulphate
Waste plastic material used in present work
2.2.4
were Low Density Polyethylene (L.D.P.E.)
MassSpectroscopy
30%, High Density Polyethylene (H.D.P.E.)
The analysis of samples was done using
25%,
15%,
GM/MS technique (GC/MS-QP2010-Ultra)
andPolypropylene (P.P.) 30% in the form of
from japans ’Shimadzu Company, equipped
plastic disposable glasses, poly shopping
with
bags, packaging poly bags. Andtheyare
Alltech)
obtained from house hold garbage.
mm×0.25µm).The injector temperature was
Polystyrene
(P.S.)
Gas
an
AT-WAX column
Chromatography
(Heliflex
capillary,
(Rtx-5ms-30m×0.25
set to 250 ºC, while the mass spectroscopy 2.2 Methodology
(Ms) oven temperature was 195 ºC. The
2.2.1 Pyrolysis
carrier gas used was He at 1 mL/min flow.
100g of mixed waste plastic was shredded
All the samples were analysed using scan
into small pieces and placed in the round
mode in the range of m/z 30-550 charges to
bottom flask of the simple distillation unit. The
condensable
collected
through
liquid the
ratio.
productswere condenser
and
3. Result and Discussion
weighted. After pyrolysis, the solid residue 3
Thermal cracking of mixed waste plastic takes place by means of a radical chain transfer mechanism, comprising the usual initiation,
3.1 FTIR spectra of plastic oil products
propagation, and termination steps. The random scission of the C–C bond of the main chain
FTIR is an important analysis technique that
occurs with heat to produce hydrocarbon radicals
detects the various characteristic functional
(HCRs), which form a broad hydrocarbon
groups present in the produced oil. (Fig. 1)
distribution wherein their main components in
shows the FTIR spectra of the produced oil
each fraction are the n-paraffin, the 1-alkene, and the
corresponding
alkadiene.
Beside
(all the produced fractions have the same
the
branched products obtained via reaction between
spectra with different
two radicals[26-28].
different assignments of the FTIR spectra are
Thermal cracking of mixed waste plastic (PP,
summarized in (Table 2) which shows the
LDPE, PS and HDPE) with percentage (30%,
presence of mostly alkanes, alkenesand some
30%, 25%, 15%), yields about 95% liquid fuels,
aromatic compounds. The results were
3% light gas and about 2% solid residues. The
consistent with the GC/MS results.
produced fuel is then transferred into fractional distillation column. Three fractions were collected in different temperature ranges as shown in (Table 1), and then characterized using FTIR and GC/MS. Table 1: Colour, Volume and temperature range of the three fractions Fractions Temperature Volume/ml range (45-170) °C 25 1st
Color
2nd
(170-265)°C
52
Bright yellow Yellow
3rd
(265-370)°C
21.5
Orange
4
intensities). The
Fig. 1: FTIR of the pyrolytic oil obtained from mixed waste plastic Table 2: FTIR of the pyrolytic oil obtained from mixed waste plastic
Functional group
Vibrational mode
Assigned (cm-1)
-CH=CH2 or >C=CH2 alkene
C-H stretching
3080
-C-H2
C-H asymmetrical stretching
2956
-C-H2
C-H symmetrical stretching
2871
C=C stretching
1630
-CH2-
C-H scissoring
1456
-CH3
C-H symmetrical bending
1376
-CH=CH aromatic
C=C stretching (aromatic)
1647, 1602 and 1575
-CH=CH2 or >C=CH2 or CH=CH-
3.2 Gas chromatography mass spectroscopy (GC/MS) The GC/MS analysis of first fraction shows
in percentage of 0.14, 1-Pentene, 2-methyl-
that it contains light hydrocarbon (C5-C11) as
(C6H12) at retention time 1.664 and trace mass
in (Fig. 2 and Table 3). All compounds are
56, Toluene (C7H8) at retention time 3.834 and
short chain hydrocarbon because when we
trace mass 91, Styrene appears at retention
fractionate waste plastic fuel to first fractional
time 7.644
fuel low temperature of (45 to 170) ºC was
percentage of 21.1 and trace mass 104 , 2,4-
used to collect all light fraction compound.
Dimethyl-1-heptene (C9H18) at retention time
Chromatogram and compound data show that
5.819 and trace mass 43, 1-Decene (C10H20) at
the first compound is 1-Hydroxy-3-methyl-2-
retention time 11.662 and trace mass 56, 1-
butanon (C5H10O2) at retention time 1.549 and
Heptanol, 2,4-diethyl- (C11H20O) at retention
trace mass 43 this compound intensity is low
time 15.736 and trace mass 69. 5
is compound intensity is high in
24
(x10,000,000)
28
2.5
2.5
5.0
7.5
10.0
12.5
15.0
17.5
20.0
22.5
25.0
71 72
64 66 65 67 68 69 70
44 46 45 47 48 5 0 4592 55 13 5 4 55 56 58 57 60 59 61 62 63
35 37 38 40 41 39 42 43
0.5
36
1.0
1 3 2617405 8 94 1 2 1 1 13 15 16 17 19 20 2 1 22 23 25 27 26 29 30 31 32 33 34
1.5
18
2.0
27.5
30.0
Fig. 2: GC/MS of the 1st fraction Temperature range: (45-170) ᵒC (light fraction) Table 3:GC/MS of the 1st fraction Temperature range: (45-170)ᵒC(light fraction) Peak Number 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26
Compound Name
Compound Formula
1-Hydroxy-3-methyl-2-butanon 1-Butanol, 2-methyl 1-Pentene, 2-methyln-Hexane Cyclopentane, methyl 1,3-pentadiene,2-methyl, (E) 1-Pentene,2,4-dimethylBicyclo[2.1.0]pentane,1,4-dimethyle1-Heptene Heptane Toluene Heptane, 4-methyl-
C5H10O2 C5H12O2 C6H12 C6H14 C6H12 C6H10 C7H14 C7H12 C7H14 C7H16 C7H8 C8H18
1-Octene Octane Ethylbenzene
C8H16 C8H18
Styrene Heptane, 2,4-dimethyl-
C8H8
C8H10
C9H20
Cyclohexane, 1,3,5-trimethyl 2,4-Dimethyl-1-heptene
C9H18
Cyclohexene, 3,3,5-trimethylNonane alpha. -Methyl styrene 2-Octene, 2,6-dimethyl1-Decene Heptane, 3,3,5-trimethyl-
C9H16 C9H20 C9H10 C10H20 C10H20
C9H18
C10H22
Heptane, 2,5,5-trimethyl-
C10H22
6
Trace Mass (m/z) 43 57 56 57 56 67 56 81 56 43 69 91
Area%
Retention Time (M)
0.14 0.02 0.56 0.12 0.08 0.16 0.51 0.55 1.17 1.21 6.06
1.549 1.620 1.664 1.712 1.923 1.995 2.064 2.145 2.524 2.626 3.834
2.82
3.772
43 55 43
1.93 1.97
4.325 4.531
4.79
6.409
43 69
21.10
7.644
1.40
5.120
43 91
2.16
5.372
15.94
5.819
1.52 1.52 4.12 1.97 1.69
6.673 7.798 11.271 3.586 11.662
1.60
11.463
1.60
12.654
109 104 43 113 71 56 71
Benzene, butyl-
27
1-Heptanol, 2,4-diethyl-
28 29 30 31
91
C10H14
69
C11H24O
C11H22 56 C11H22 57 92 C11H16 Undecene (C11H22) at
1-Undecane Undecane Benzene, (3-methyl-3-butenyl The GC/MS analysis of 2'nd fraction
0.42
14.639
2.63
15.736
1.07 16.209 0.86 16.508 0.50 17.738 retention time 9.704
shows that it contains light hydrocarbon
and trace mass 55, 1-Decene,2,4-dimethyl-
(C8-C30) as in (Fig. 3 and Table 4). Most of
(C12H22) at retention time 9.440 and trace
these compounds are short and long chain
mass 69, Benzen,1,1'-(1,3-propandiyl(bis-
hydrocarbon.
and
(C15H16) at retention time 21.082 and trace
first
mass 92, Hexadecane (C16H3) at retention
compound is 1-Heptene, 2-methyl- (C8H16)
time 16.270 and trace mass 57, 3-2-
at retention time 3.196 and trace mass 56
Hexyldecyl acetate (C18H36O2) at retention
and show area percentage of 0.27, Styrene
time 14.596 and trace mass 69, Eicosane
(C8H8) at retention time 5.242 and trace
(C20H42) at retention time 24.347 and trace
mass 104 show high intensity 12.17, 2,4-
mass 57, Oxalic acid,hexadecylisohexyl
Dimethyl-1-heptene (C9H18) at retention
ester (C21H40O4) at retention time 14.779
time 4.153 and trace mass 43, 1-
and trace mass 43, Tridecane (C30H28) at
compound
Chromatogram data
table
shown
(C10H22O)
Octanol,2,7-dimethyl
at
retention time 14.296 and trace mass 57.
retention time 9.357 and trace mass 69, 1-
(x10,000,000) 2.0 1.5 1.0 0.5
5.0
7.5
10.0
12.5
15.0
17.5
20.0
22.5
Fig. 3 GC/MS of the 2ndfraction Temperature range: (170-265) ᵒC
7
25.0
27.5
Table4 :GC/MS of the 2nd fraction Temperature range: (170-265)ᵒC Peak Number 1 2 3 4 5 6 7 8
9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29
Compound Name 1-Heptene, 2-methyl1-Octene Octane Cyclopentane, 1,1,3,4tetramethyl-, cisHeptane, 2,4-dimethylCyclohexane, 1,3,5trimethyl2,4-Dimethyl-1-heptene Cyclohexane, 1,2,4trimethyl-, (1.alpha.,2.beta.,4.beta.)Ethylbenzene Styrene Nonane Benzene, (1-methylethyl).alpha.-Methylstyrene 1-Decene Decane Benzene, (1-ethyl 2methyl)1-Tridecene Benzene, butyl1-Decene,2,4-dimethyl1-Octanol,2,7-dimethylUndecane 1-Undecene Benzene,(3-methyl-3butenyl)Benzene ,pentyl1-Dodecanol Dodecane Cyclohexan,2,4-diethyl-1methyl1-Tridecene Tridecane
Compound Formula
Area%
Retention Time (M)
C8H16 C8H16 C8H18 C9H18
Treace Mass (m/z) 56 55 43 83
0.27 0.59 0.84 0.53
3.196 3.258 3.389 3.574
C9H20 C9H18
43 69
0.50 1.20
3.766 3.962
C9H18 C9H18
43 69
4.65 1.76
4.153 4.431
C8H10 C8H8 C9H20 C9H12 C9H10 C10H20 C10H C9H10
91 104 43 105 118 56 57 117
2.93 12.17 1.25 0.77 4.02 1.76 1.50 0.51
4.582 5.242 5.323 5.913 7.245 7.382 7.574 8.251
C13H26 C10H14 C12H22 C10H22O C11H24 C11H22 C11H40
57 91 69 69 57 55 91
0.45 1.07 4.23 3.79 1.76 1.94 1.31
8.382 8.938 9.440 9.537 9.893 9.704 10.866
C11H60 C12H26O C12H26 C11H22
91 43 57 69
0.54 2.37 2.02 0.51
11.257 11.958 12.136 12.265
C30H26 C30H28
55 57
2.09 2.62
14.102 14.269
8
30 31 32
33 34 35 36 37 38 39 40 41 42 43 44
2-Isopropyl-5-methyl-1heptanol 1. 2-Hexyldecyl acetate 2. Oxalic acid,hexadecylisohexyl ester 3. 1-Heptadecene 4. Hexadecane Heptadecane Benzene, (2,3dimethyldecl)Pentadecane 5. Benzen,1,1'(1,3-propandiyl(bis6. 1-Nonadecene Heneicosane Octadecane Eicosane Tetracosane Docosane
C11H24O
69
6.19
14.430
C18H36O2
69
4.31
14.596
C21H40O4
43
6.81
14.779
C17H34 C16H34 C17H36 C18H30
55 57 57 57
2.32 1.96 0.56 0.57
16.122 16.270 17.468 17.627
C15H32 C15H16
57 92
2.07 3.34
18.163 21.082
C19H38 C21H44 C18H38 C20H42 C24H50 C22H46
83 57 57 57 57 57
1.76 1.56 1.73 1.31 1.16 0.65
21.509 21.614 23.061 24.347 25.517 26.593
The GC/MS analysis of 3'rd fraction
19.954 and trace mass 57, 3-Hexadecene,
shows that it contains light hydrocarbon
(Z)- (C16H32) at retention time 16.111 and
(C8-C36) as in (Fig. 4 and Table 5). Most of
trace mass 55, Heptadecane (C17H36) at
these
chain
retention time 18.019 and trace mass 57,
hydrocarbons because most of the light
Octadecane (C18H38) at retention time
fraction were fractionated in the other
24.345 and trace mass 57, Nonadecane
fractions. Chromatogram and compound
(C19H40) at retention time 23.054 and trace
data table shown first compound is 1-
mass 57, Eicosane (C20H42) at retention
Heptene, 2-methyl- (C8H16) at retention
time 25.514 and trace mass 57, 1-
time 3.192 and trace mass 56 and show the
Heneicosanol (C21H44O) at retention time
lower area percentage of 0.21, Styrene
27.551 and trace mass 97, Behenic alcohol
(C8H8) at retention time 5.191 and trace
(C22H46O) at retention time 25.451 and
mass 104, Nonane (C9H20) at retention
trace mass 83, n-Tetracosanol-1 (C24H50O)
time 5.306 and trace mass 43, 1-Decene
at retention time 26.537 and trace mass 97,
(C10H20) at retention time 7.371 and trace
1-Heptacosanol (C27H56O) at retention
mass 56, 1-Undecene (C11H22) at retention
time
time 9.692 and trace mass 55, 1-Dodecene
Tetratetracontane (C34H70) at retention
(C12H24) at retention time 11.949 and trace
time
mass 55, 2-methyl-5-propyl- (C13H28) at
57,Hexatriacontane (C36H74) at retention
retention time 14.253 and trace mass 57,
time 27.739 and trace mass 57.
compounds
are
long
Pentadecane (C15H32) at retention time 9
28.500
27.597
and
trace
and
mass
trace
97,
mass
(x1,000,000) 5.0
2.5
5.0
7.5
10.0
12.5
15.0
17.5
20.0
22.5
25.0
27.5
Fig.4: GC/MS of the 3rd fraction Temperature range: (265-370) ᵒC Heavy Fraction
Table 5: GC/MS of the 3rd fraction Temperature range: (265-370) ᵒC Heavy Fraction Heavy Fraction Peak Number 1 2 3 4 5
Compound Name 1-Heptene, 2-methyl1-Octene Octane Cyclopentane, 1,1,3,4tetramethyl-, cisHeptane, 2,4-dimethyl-
Compound Formula
Area%
Retention Time (M)
C8H16 C8H16 C8H18 C9H18
Trace Mass (m/z) 56 55 43 83
0.21 1.17 1.26 0.27
3.192 3.256 3.386 3.572
C9H20
43
0.33
3.762
10
6 7 8
9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48
Cyclohexane, 1,3,5trimethyl2,4-Dimethyl-1-heptene Cyclohexane, 1,2,4trimethyl-, (1.alpha.,2.beta.,4.beta.)Ethylbenzene Ethinamate 2,4-Heptadiene, 2,6dimethylStyrene 1-Nonene Nonane Benzene, (1methylethyl).alpha.-Methylstyrene 1-Decene Undecane Octane, 3,3-dimethylHeptane, 2,5,5trimethyl1-Decene, 2,4-dimethyl2-Undecene, 4,5dimethyl-, [R*,S*-(Z)]1-Undecene 1-Dodecene Dodecane 1-Tridecene Nonane, 2-methyl-5propyl11-Methyldodecanol 3-Eicosene, (E)2-Isopropyl-5-methyl-1heptanol 3-Hexadecene, (Z)Hexadecane 1-Heptadecene Heptadecane 1-Pentadecene Pentadecane 1-Heptadecene Heptadecane 1-Nonadecene Nonadecane 1-Octadecene Octadecane 1-Dodecanol, 2octylBehenic alcohol Eicosane n-Tetracosanol-1 Heneicosane 1-Heneicosanol
C9H18
69
0.46
3.958
C9H18 C9H18
43 69
6.14 0.89
4.131 4.425
C8H10 C9H11NO2 C9H16
91 91 109
2.19 0.71 0.13
4.578 4.731 4.916
C8H8 C9H18 C9H20 C9H12
104 56 43 105
6.92 1.44 1.69 0.41
5.191 5.130 5.306 5.909
C9H10 C10H20 C11H24 C10H22 C10H22
118 56 57 71 43
1.36 1.81 1.76 0.47 0.57
7.228 7.371 7.564 7.779 7.875
C12H22 C13H26
69 69
1.13 0.93
9.420 9.517
C11H22 C12H24 C12H26 C13H26 C13H28
55 55 57 55 57
1.81 1.94 1.80 1.59 1.88
9.692 11.949 12.125 14.090 14.253
C13H28 C20H40 C11H24O
69 69 69
1.38 0.75 1.01
14.396 14.572 14.746
C16H32 C16H34 C17H34 C17H36 C15H30 C15H32 C18H34 C18H36 C19H38 C19H40 C18H36 C18H38 C20H42O
55 57 55 57 55 57 55 57 83 57 83 57 69
1.78 1.57 1.49 1.88 1.62 2.18 1.57 1.90 1.57 2.08 1.40 2.10 0.58
16.111 16.259 18.019 18.019 19.822 19.945 21.501 21.605 22.967 23.054 24.270 24.345 25.027
C22H46O C20H42 C24H50O C21H44 C21H44O
83 57 97 57 97
1.26 2.37 1.50 1.92 2.23
25.451 25.514 26.537 26.592 27.551
11
49 50 51 52 53 54 4. Conclusion
Tetratetracontane Hexatriacontane 1-Heptacosanol Tetratriacontane Cyclotetracosane Tetratetracontane
Consumption of plastics has increased over the years and the concern with their waste generated too. Because of these many studies have been done with the aim to recover or recycle the waste. Pyrolysis has been effective compared to other recycling methods, because it can reuse the energy and the raw materials contained in those waste. Liquid resulting from the simple distillation with a percentage 95 % was a mixture of alkanes and alkenes up to 36 carbon chains. After Fractional distillation three fractions were collected in various temperature range, the first fraction is light with short hydrocarbon from C5-C11, it was suitable for the production of light kerosene. the second one contains a mixture of light and some heavy fractions from C8-C30 it was suitable for the production of light gasoline. And the third fraction contain higher alkenes of long chains hydrocarbons C8-C36 it good for diesel oil.
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