Az32340347

Satyendra Singh Tomar, Dr.S.P.Singh / International Journal of Engineering Research and
Applications (IJERA) ISSN: 2248-9622 www.ijera.com
Vol. 3, Issue 2, March -April 2013, pp.340-347
Regaining Of Hydrocarbon Liquids From Discarded Polyethylene
By Thermolysis In Semi Batch Reactor
Satyendra Singh Tomar, Dr.S.P.Singh
Department of Chemical Engineering, BIT, Sindri, Jharkhand, 828123

Abstract
Thermolysis of waste plastics in an inert Recycling of plastics already occurs on a wide scale.
atmosphere has been gazed at as a useful method, Extensive recycling and reprocessing of plastics are
because this technique can convert waste plastics performed on homogeneous and contaminant free
into hydrocarbons that can be used either as fuels plastic wastes. Most recycling schemes require a
or as other valued chemicals. In this work, waste feedstock that is reasonably pure and contains only
polyethylene (PE) was chosen as the raw material items made from a single polymer type, such as
for thermolysis. A well designed semi batch Polyethylene (PE) commonly used to make milk
reactor has been used for thermolysis of waste bottles, or polyethylene terephthalate (PET) soft
polyethylene (PE) with the objective of enhancing drink bottles. However, a substantial fraction of
the liquid product yield at a temperature range of theplastics in municipal waste still ends up in
350ºC to 500ºC. Results of thermolysis landfills. Realistically, most post-consumer wastes
experiments showed that, at a temperature of contain a mixture of plastic types and are often
400ºC and below the major product of the contaminated with non-plastic items (Hegberg et al.,
thermolysis was oily liquid which became a 1992)[3].
viscous liquid or waxy solid at temperatures
above 425ºC. The yield of the liquid fraction An alternative thermal approach for dealing
obtained increased with the residence time for with waste plastics is the so-called chemical
waste polyethylene (PE). The oily liquid fractions feedstock or chemical recycling. This term has been
obtained were examined for composition using used to describe a diversity of techniques
FTIR and GC-MS. The physical properties of the includingthermolysis, hydrolysis, hydrogenation,
thermolytic oil show the presence of a mixture of methanolysis and gasification. Some of these
different fuel fractions such as gasoline, kerosene techniques are suitable for use only with
and diesel in the oil. homogeneous polymer wastes but others can accept
a feed of mixed wastes.
Keywords: Thermolysis;PE; FTIR; GCMS;
liquid fuel. The most attractive technique of chemical
feedstock recycling is thermolysis. Thermal cracking
INTRODUCTION or thermolysis involves the degradation of the
Plasticsareone ofthe mostwidelyused polymeric materials by heating in the absence of
materials due to their variousadvantagesand oxygen. Unlike mechanical recycling techniques, in
numerous applicationsin ourday-to-day life. Plastics which the long polymeric chains of the plastic are
production has increased by an average of almost preserved intact, thermolysis produces lower
10% every year on a global basis since 1950. The molecular weight fragments. The process is usually
total global production of plastics has grown from conducted at high temperature and results in the
around 1.3 million tons (MT) in 1950 to 230 MT in formation of a carbonized char and a volatile
2009 (Plastic-The facts 2010). PE is the third largest fraction that can be separated into condensable
commodity plastic material in the world, after hydrocarbon oil and a non-condensable high
polyvinyl chloride and polypropylene in terms of calorific value gas. The proportion of each fraction
volume. According to aBritish market-research and their precise composition depend primarily on
consulting agency, “Merchant Research & the nature of the plastic waste, but also on process
Consulting Ltd”.Polyethylene (PE) has accounted conditions. The effect of temperature and the type of
for a major share of ethylene consumption in the reactor on the pyrolysis of waste PE studied by
recent years. The demand for PE has increased 4.4% different researchers are summarized below.
a year to 31.3 million MT in 2009 (CEH report) [1]. Wallis et al. (2007) performed the thermal
The treatment of waste plastics has become a serious degradation of polyethylene in a reactive extruder at
problem and the pyrolysis (thermolysis) of these various screw speeds with reaction temperatures of
materials can be one of the most suitable processes 400°C and 425°C[4]. A continuous kinetic model was
for upgrading them [2]. used to describe the degradation of the high density
polyethylene in the reactive extruder.

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Conesa et al. (1994) studied the production of gases in a stirred semi batch reactor on a laboratory
from polyethylene at five nominal temperatures scale was studied by Lee et al. (2003)[12]. As
(ranging from 500°C to 900°C) using a fluidized compared with thermal degradation, the catalytic
sand bed reactor. From the study of HDPE pyrolysis degradation showed an increase of liquid yield,
in a fluidized sand bed reactor, they have found that whereas that of residue was reduced due to the
the yield of total gas obtained increased in the range decomposition of heavier residues into lighter oil
500-800°C from 5.7 to 94.5%, at higher product.
temperatures[5]. Singh K.K.K. et al., reported maximum yield of
liquid when polymer catalyst ratio was 4:1 and after
Walendziewski et al. (2001) reported the this ratio the liquid yield decreases. The degradation
thermal degradation of polyethylene in the of waste plastic was over two commercial grade
temperature range 370-450°C. In the case of thermal cracking catalysts, HZY (20) & HZY (40) in a semi-
degradation of polyethylene, an increase in batch reactor [13].
degradation temperature led to an increase of gas
and liquid products, but a decrease of residue Seo et al. (2003) studied the catalytic
(boiling point >360°C)[6]. degradation of waste high density polyethylene to
The thermal degradation of waste PE can be hydrocarbons by ZSM-5, zeolite-Y, mordenite and
improved by using suitable catalysts in order to amorphous silica-alumina in a batch reactor and
obtain valuable products. The most common investigated the cracking efficiency of catalysts by
catalysts used in this process are: zeolite, alumina, analyzing the oily products, including paraffins,
silica-alumina, FCC catalyst, reforming catalyst etc. olefins, naphthenes and aromatics, with gas
The effects of various catalysts on the pyrolysis of chromatography/mass spectrometry (GC/MS)[14].
PE studied by different investigators are summarized
below. The liquid-phase catalytic degradation of
HDPE over BEA, FAU, MWW, MOR and MFI
Beltrame et al. (1989) have studied zeolites with different pores in a batch reactor at
polyethylene degradation over silica, alumina, silica- 380°C or 410°C has been studied by Park et al.
alumina and zeolites in small Pyrex vessel reactor (2002)[15].
without stirring, in the temperature range 200–
600°C[7]. Manos et al. (2000) studied the catalytic
degradation of high-density polyethylene to
The catalytic upgrading of the pyrolysis hydrocarbons over different zeolites[16]. The product
gases derived from the pyrolysis of polyethylene range was typically between C3 and C15
over zeolite in the temperature range 400–600°C has hydrocarbons.
been investigated by Bagri et al. (2002)[8].
The catalytic pyrolysis of high density
As the zeolite bed temperature was polyethylene was studied at different times using
increased, the gas yield increased with a decrease in different types of reactors: a pyro-probe apparatus,
oil and coke yield. Venuto et al. (1979) also showed where the volatile residence time is in the range of
that, as the catalyst temperature was increased from few milliseconds, and a fluidized bed reactor, where
480 to 590°C, coke formation in the zeolite catalytic the secondary reactions take place to a larger extent
cracking of petroleum was reduced and also alkene using HZSM-5 catalyst (Hernandez et al., 2006)[17].
gases increased in the gas product[9].
Garforth et al. (1998)[18]studied the catalytic
Sharratt et al. (1997) carried out the pyrolysis of polyethylene in a laboratory fluidized
catalytic degradation of polyethylene using ZSM-5 bed reactor operating in the 290°C-430°C range
zeolite. As the reaction temperature was increased under atmospheric pressure. The catalysts used were
from 290 to 430°C, the gas yield was increased, HZSM-5, Silicalite, HMOR, HUSY and SAHA and
whereas the oil yield was decreased[10]. the yield of volatile hydrocarbons (based on the
feed) was HZSM5>HUSY≈HMOR>SAHA.
Oil obtained in the thermolysis of
polyethylene contained a low concentration of The catalytic degradation of high density
aromatic compounds. The liquid-phase catalytic polyethylene (HDPE) under nitrogen using a
degradation of waste polyolefin polymers such as laboratory fluidized bed reactor operating at 360°C
HDPE, LDPE, and PP over spent fluid catalytic with a catalyst to polymer feed ratio of 2:1 and at
cracking (FCC) catalyst was carried out at 450°C with a catalyst to polymer feed ratio of 6:1
atmospheric pressure in a stirred semibatch under atmospheric pressure using ZSM-5, US-Y,
operation by Lee et al. (2003)[11].The difference in ASA, fresh FCC (fluid catalytic cracking)
the product yields between thermal and catalytic commercial catalyst (Cat-A) and equilibrium FCC
degradation of waste PE using spent FCC catalyst catalysts with different levels of metal poisoning

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were studied (Ali et al., 2002)[19]. the condenser and weighed. After thermolysis, the

Mastral et al. (2006) studied the catalytic solid residue left inside the reactor was weighed.
degradation of high density polyethylene in a Then the weight of gaseous/volatile product was
laboratory fluidized bed reactor at mild calculated from the material balance. The
temperatures, between 350°C and 550°C[20]. The uncondensed gases were separated out in a bladder
catalyst used was nanocrystalline HZSM-5 zeolite. from condenser. Apparatus setup and samples
collected for testing are shown in Figure. 1(a,b)
Lin et al. (2004) studied the pyrolysis of
polyethylene over various catalysts using a Reactions were carried out at different
laboratory fluidized-bed reactor operating temperatures ranging from 350-500°C. FTIR of the
isothermally at ambient pressure[21]. thermolysis oil obtained at the optimum condition
Karagoz et al. (2003) studied the conversion of high was performed and the product wasalso analyzed by
density polyethylene in vacuum to fuels in the GC-MS using flame ionization detector.
absence and presence of five kinds of metals
supported on active carbon catalysts (M-Ac) and 2. RESULTS AND DISCUSSION
acidic catalysts {HZSM-5 and DHC (Distillate 3.1 Proximate &Ultimate Analysis of Waste PE
Hydro Cracking- 8)} catalyst[22]. The proximate and ultimate analyses of
waste PE sample are shown in Table 1. The
Jan et al. (2010) studied the degradation of volatile matter is 100% in the proximate analysis,
waste high density polyethylene into a liquid due to the absence of ash in waste polyethylene
fraction thermally and catalytically using MgCO3 at sample; its degradation occurs with minimal
450°C in a batch reactor [23]. formation of residue. The oxygen is 5.19% in the
Different conditions like temperature, time and ultimate analysis of waste polyethylene. The oxygen
catalyst ratio were optimized for the maximum in the waste polyethylene sample may not be due to
conversion of polyethylene into a liquid fraction. In the fillers but rather to other ingredients that are
the present study, waste polyethylene was added to the resin in the manufacturing of
thermolized in a semi-batch reactor at a temperature polyethylene.
of 350°C to 500°C at a heating rate of 20°C/min.
The effect of thermolytic temperature and holding 3.2 TGA &DTG Analysis of the Waste PE
time on the reaction time and yield of liquid product, Sample
char, and gaseous product were studied. The fuel Thermogravimetric analysis (TGA) is a
properties of the oil (obtained at a temperature of thermal analysis technique that measures the weight
400°C from thermolysis of waste PE such as change of a material as a function of temperature
kinematic viscosity, flash point, fire point, cloud and time, in a controlled environment. This can be
point, pour point, specific gravity, and water content very useful to investigate the thermal stability of a
were determined using standard test methods. The material, or to investigate its behavior in different
chemical compositions of the waste PE thermolytic atmospheres.
oil were investigated using FTIRand GC/MS.
TGA was applied to study the thermal
1. MATERIALS AND METHODS stability/degradation of waste PE in various ranges
Waste Polyethylene was collected from the of temperature. From the TGA curve shown in
BITSindri, Dhanbad,Jharkhand, India campus waste Figure 2, the waste polyethylene degradation started
yard and used in this experiment. The catalytic at 340°C and was complete at 440°C for a heating
thermolysis of polyethelene was carried out in a rate of 20°C min. the degradation temperature at
semi-batch reactor. The thermolysis setup used in which a weight loss of 50% (T50) takes place
this experiment is shown in Figure 1. It consists of a was about 390°C for waste PE. The differential
semi batch reactor (steel made) of volume 2 liters, thermogravimetry (DTG) curve for waste PE in
vacuum-packed with two outlet tubes towards Figure 3 contains only one peak, this indicates that
vacuum pump and condenser. Vacuum pump with a there is only one degradation step in the dominant
gage is attached to the reactor so as carryout the peak from 330°C to 420°C where the conversion
reaction in vacuum. The condenser is attached to takes place.
collect condensed Liquid hydrocarbons and gases
separately. The reactor is heated externally by an 3.3 Effect of Temperature on Product
electric furnace, with the temperature being Distribution
measured by a Cr-Al: K type thermocouple fixed Thermolysis of PE yielded four different
inside the reactor, and temperature is controlled by products, i.e., oil, wax, gas, and residue. The
an external controller. 100 gm of waste plastics distributions of these fractions are different at
sample was loaded in each thermolysis reaction. The different temperatures and are shown in Table 2.
condensable liquid products was collected through The condensable oil/wax and the non-condensable

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gas/volatiles fractions of the reaction constituted the oil, chemical bonds can absorb infrared radiation in
major product as compared to the solid residue specific wavelength ranges regardless of the
fractions. The condensable product obtained at low structure of the rest of the molecules Figure 6 shows
temperature (350°C and 400°C) was low viscous the FTIR spectra of waste PE oil. The different
liquid. With an increase in temperature, the liquid assignments of the FTIR spectra of waste PE oil are
became a viscous/wax at and above 425°C. The summarized in Table 3, which shows the presence of
formation of a viscous and waxy product was due to mostly alkanes and alkenes. The results were
improper cracking of the plastic to high molecular consistent with the results of GC-MS.
mass hydrocarbon components. The recovery of the
condensable fraction was very low at low .3.7 GC-MS of the Oil Sample
temperature, i.e., at 350°C, and increased with a The GC-MS analysis of the oil sample
gradual increase of temperature. obtained from waste PE was carried out to verify the
exact composition of the oil (Figure 7) and is
From the table, it is observed that, at low summarized in the Table 4. The components present
temperature, the reaction time was longer, due to in PE are mostly aliphatic hydrocarbons (alkane and
secondary cracking of the thermolysis product that alkenes) with carbon number C9-C24.
occurred inside the reactor, which resulted in highly
volatile product. Similarly, the low liquid yield at 3.7 Physical Properties of the Oil Sample
high temperature was due to the formation of less- Table. 5 shows the results of physical
cracked high molecular weight wax and more non- property analysis of the oil obtained from
condensable gaseous/volatile fractions due to thermolysis of waste PE. The appearance of the oil is
rigorous cracking. dark brownish free from visible sediments. From the
distillation report of the oil it is observed that the
3.4 Effect of Temperature on Reaction Time boiling range of the oil is 82-352°C, which suggests
The effect of temperature on the reaction the presence of a mixture of different oil components
time for the thermolysis of waste Polyethylene is such as gasoline, kerosene and diesel in the oil. The
shown in Figure 4. The thermolysis reaction rate oil obtained from the thermolysis was fractionated to
increased and the reaction time decreased with an two fractions by distillation and the fuel properties
increase in temperature. High temperature supports of the different fractions were studied. From this
the easy cleavage of bonds and thus speeds up the result, it is observed that the fuel properties of
reaction and lowers the reaction time. PE, with a thethermal thermolysis oil match the properties of
long linear polymer chain with low branching and a petroleum fuels.
high degree of crystallinity, led to high strength
properties and thus required more time for
decomposition. This shows that temperature has a
significant effect on reaction time and yield of
liquid, wax and gaseous products.

3.5 Effect of Holding Time on Yield of Oil
The effect of holding time on the yield of
the oil is shown in Figure 5. The reaction was
carried out by keeping the plastics in the reactor at
350°C with different holding times from 1-6 hours,
followed by an increase of the reaction temp to
400°C. It was observed that this additional reaction
phase increased the oil yield from 23% to 28% for a
1 hour holding time and to 50.8% with a 4 hour
holding time, but then decreased gradually with Figure. 1(a) Apparatus setup
further increase in the holding time. The introduction
of this reaction phase loosens the polymer bonds that
are easily cleaved to liquid hydrocarbons, which
leave the outlet at 400°C without being converted to
gas due to the decrease in reaction time compared to
350°C.

3.6 FTIR of Oil Samples
Fourier Transform Infrared spectroscopy
(FTIR) is an important analysis technique that
detects various characteristic functional groups
present in oil. Upon interaction of infrared light with Figure. 1(b) Samples collected for testing

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Figure 5: Effect of holding time on the yield.

Figure 2: TGA curve of waste polyethylene

Figure 6: FTIR spectrum of waste PE oil obtained at
400°C.

Figure 3: DTG curve of waste polyethylene

Figure 4: Effect of Temperature on Reaction Time

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Figure 7: GC/MS chromatogram of the oil that was
obtained at 400°C R.Time Area Name of Molecul
(min) % Compound ar
Properties Present (Parikh (Kim et Formula
study et al., al., 3.050 1.50 1-Nonene C9H18
(Waste 2009) 2010) 3.147 0.96 Nonane C9H20
PE) [24] [25] 4.465 2.60 1-Decene C10H20
Proximate analysis 4.463 1.25 Decane C10H22
Moisture 0.00 0.00 1.37 5.914 3.22 1-Undecene C11H22
content 6.116 1.76 Undecane C11H24
Vol. matter 100 100 92.90 7.525 3.30 1-Dodecene C12H24
Fixed carbon 0.00 0.00 1.14 7.628 2.25 Dodecane C12H26
Ash content 0.00 0.00 4.59 8.960 3.80 1-Tridecene C13H26
Ultimate Analysis 9.075 2.50 Tridecane C13H28
Carbon 80.50 84.95 79.9 10.346 4.70 1-Tetradecene C14H28
Hydrogen 13.90 14.30 12.6 10.450 2.90 Tetradecane C14H30
Nitrogen 0.60 0.55 - 11.618 4.87 1-Pentadecene C15H30
Sulphur 0.080 - - 11.714 3.18 Pentadecane C15H32
Oxygen 5.35 0.20 5.10 12.846 5.09 1-Octadecene C18H36
Chlorine - - 1.13 12.935 3.68 Hexadecane C16H34
GCV 45.78 - 44.40 14.011 4.87 1-Heptadecene C17H34
(Mj/Kg) 14.084 3.70 Hexadecane C16H34
15.096 4.70 1-Nonadecene C19H38
15.170 369 Hexadeane C16H34
Table 1: Proximate and ultimate analysis of waste 16.135 4.40 1-Nonadecene C19H38
polyethylene 16.211 3.68 Hexadecane C16H34
17.145 3.76 1-Nonadecene C19H38
17.190 3.19 Eicosane C20H42
Temp (°C) 350 400 450 500
18.079 3.17 1-Nonadecene C19H38
Oil (wt.%) 11.2 23.8 21.9 7.9 2.97 Heneicosane C21H44
18.139
Wax (wt.%) 0 0 50.0 71.1 18.995 2.55 1-Nonadecene C19H38
Gas/ volatile 84.2 72.4 25.1 18.5 19.047 2.47 Docosane C22H46
(wt.%) 19.859 1.99 1-Nonadecene C19H38
Residue(wt.%) 4.6 3.8 3.0 2.5 19.920 1.99 Tricosane C23H48
Reaction time 760 290 68 54 20.687 1.27 1-Nonadecene C19H38
(min) 20.751 1.28 Tetracosane C24H50
21.501 0.94 1-Nonadecene C19H38
Table 2: Distribution of the different fractions at 21.538 0.69 Docosane C22H46
different temperatures in the Polyethylene 22.274 0.44 n-Tetracosanol-1 C24H50O
thermolysis 22.310 0.36 Tetracosane C24H50
23.015 0.27 1-Nonadecene C19H38
Wave Type of Name of 25.051 0.21 4,6- C14H30
Number Vibration Functional Dimethyldodecane
(cm-1) group
2955/296 C-H stretching Alkane
6
1373 C-H Scissoring Alkane
and Binding
2851 C-H stretching Alkane
1642 C=H stretching Alkane/Fingerpr
int region
1462 C=H stretching Alkane/Fingerpr
int region
991 C-H Bending Alkane
908 C-H Out-of- Alkane
plane bending
720 C-H Bending Alkanes Bands

Table 3: FTIR assignments of waste PE oil obtained
at 400°C Table 4: GC-MS composition of oil obtained at

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450°C arranging and providing all the facilities for the
completion of work.

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