Thermal Degradation of mixed Plastic Solid Waste

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


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



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


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


(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,


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


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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