Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021
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INTERNATIONAL ADVANCED RESEARCHES
and Volume 05
ENGINEERING JOURNAL Issue 02
e-ISSN: 2618-575X August, 2021
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Research Article
Chemical characterization of waste tire pyrolysis products
Gediz Uguz a and Abdulkadir Ayanoglu b,*
aOndokuz Mayis University, Faculty of Engineering, Department of Chemical Engineering, 55139, Samsun, Turkey
bMardin Artuklu University, Vocational School, Mechanical and Material School, 47200, Mardin, Turkey
ARTICLE INFO ABSTRACT
Article history: The significance of tire disposal, an attractive waste to convert into burning oil or absorber etc.,
Received 07 January 2021 has been increasing day by day. However, if it does not change into a useful form, it will damage
Revised 10 March 2021 the nature and the living things. Thus, pyrolysis, a well-known method, which is used to convert
Accepted 20 April 2021 recycle tire waste into gas, liquid and char. On the other hand, the waste pyrolysis oil or waste
Keywords: tire oil (WTO) has a substantial avaliable calorific value similar to those of fossil fuels. Due to
Gasoline like fuels pyrolysis reaction, high amount of sulfur is detected in the WTO; therefore, another step of
Diesel like fuels explosion applied to WTO to decrease sulfur and also re-upgrade quality of oil with such
Pyrolysis of waste tire catalysts as Calcium Oxide (CaO) and Natural Zeolite (NZ) at a ratio from 2 to 10 with an
increase of 2 for each step, individually. It is noticed that distillation test is a key analysis for
separation discrimination of rich or lean quality fuel. As a consequence of mixture of catalyst-
WTO reactions, the best curve was observed at a 10% CaO-WTO mixture which was close to
diesel#2 and the mixture was separated into two new fuels as light (Gasoline Like Fuel or
abbreviated as GLF) and heavy one (Diesel Like Fuel or shortened as DLF) due to temperature
differences. According to distillation, FT-IR, NMR and UV–vis were used to analyze WTO,
GLF and DLF for defining their characterization as well. Thus, the characterization result data of
samples have quasi-equivalent with standard petroleum in open literature, and can be combusted
in engine as well.
© 2021, Advanced Researches and Engineering Journal (IAREJ) and the Author(s).
1. Introduction Owing to high amounts of the residual, the WTs have
been used for landfill to minimize ecotoxicology
The world has come across a renew aspect by lowering
problems [5]. The cement kiln and incinerators use 35 %
traditional energy sources, so the energy gap requires to
of total WTs as fuel while 38% is recovered to utilize in
be filled by waste or natural sources. Unfortunately,
civil engineering usage by shredded chips or granulates
waste materials (waste tire, waste oil, garbage etc.) are
of WTs. [6]. Mechanical, biological, thermal incineration,
required to be utilized by minimizing their harmful
chemical and pyrolysis or catalytic pyrolysis methods
effects by recycling methods [1-2].
have been used for WTs in order to recycle them into
Recently, the amount waste tires (WTs) has increased
useful products [7].
due to the increase in transportation. However, tires have
Therefore, pyrolysis is a green and clean technique,
been worn out or abraded because of road problems or
which can be applied to WTs in order to obtain useful
other factors. Thus, high amount of WTs has been
products (non-condensable gas, liquid and solid material)
discarded to environment, which causes harmful
as a result of high temperature and pressure applied at
problems throughout human life and ecosystem [3]. The
several conditions [8–10]. Based on depolymerization of
US disposes 500 million tones WT every year [4]. And
the WTs, pyrolysis has brought in complex-mixture of
the amount of tire disposed in Australia for each year is
organics (paraffin, olefins, terpenes, mono-polyaromatics,
51 million tones [5].
* Corresponding author. Tel.: +90 482 213 00 02; Fax: +90 482 213 66 44.:
E-mail addresses: gediz.uguz@omu.edu.tr (G.Uguz), a.ayanoglu1@gmail.com (A. Ayanoglu)
ORCID: 0000-0002-6796-6067 (G.Uguz), 0000-0002-5835-558X (A. Ayanoglu)
DOI: 10.35860/iarej.856112
This article is licensed under the CC BY-NC 4.0 International License (https://creativecommons.org/licenses/by-nc/4.0/).
164 Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021
nitrogen and sulfur compounds with heterocycles and 2.Material and Methods
oxygenates) like chemical contents of fuels. The initial 2.1. Raw Material
product of WTs was non-condensable gas which can be
WTs were cut into small particles (1mm) which were
burned directly in energy generating systems, because of
replaced in the reactor for organic decompositions [18].
high heating value. Other one, the solid product, could be
The simple schematic representation of cycling paths of
activated by nitrogen (N2) or carbon dioxide (CO2) flow
WTs is declared at Figure 1.
gases to upgrade as absorbent materials. Besides, the
liquid has disgusting odor, low power of hydrogen (pH), 2.2. Pyrolysis System
low heating value and high sulfur amount which causes
The batch pyrolysis system consists of a main reactor,
air pollution, high corrosion in engine with less burning
auto control, thermocouple, blender, safety valve, heat
capacity. Due to tire oil problems, it was treated with
exchanger and container (Figure 2). A cylindrical reactor
catalyst to improve properties of oil for burning [11–14].
has a dimension of Ø30x40cm with 5 cm glass wool
Ayanoglu and Yumrutas pyrolyzed WTs particles to
insulation. Additionally, a 5 kW electrical heater is used
oil and then mixed with catalysts to obtain well-quality
to verify temperature from room temperature to
fuels which have similarity to fuels. Moreover, each
demanded values. Furthermore, the blender is used for
sample was analyzed through chemical and physical tests
homogenous temperature variations. The last part of the
to check their comprehensive with petroleum fuels [15].
system is heat exchanger which liquefies gas into oil.
Kebritchi et al. [16] studied WTs pyrolysis to compare its
yield and properties with other fuels. Furthermore, 2.3. Reaction of Pyrolysis
Ground Tire Rubber (GTR) and Reclaim Rubber (RR) The main advantages of pyrolysis system are to be
were converted at 400–600 oC. The alkanes/aromatic cheap according to its parts, which minimized energy
ratios of FT-IR results and elemental analyses were consumption and maximized desired products.
close to each other. 1H-NMR and 13C-NMR spectra were Furthermore, the pyrolysis has other contribution to
declared at different concentrations of aromatics, and decrease residual of solid by increasing condensable (oil)
they exhibited similarities due to each property. Lopez et and non-condensable (gas) fractions via heating rates,
al. [17] investigated natural and synthetic rubber of WTs catalysts, pressure and other parameters for minimizing
conversion in conical spouted bed reactor between 425- harmful and polluting effects because of high amount of
600 oC. The liquid was tested by gas chromatography and sulfur [ 19–21].
mass spectrometry (GC-MS), two-dimensional gas WTs were converted into gas, liquid (WTO) and solid
chromatography (GCxGC) with distillation and elemental at first step of pyrolysis at a heating rate of 5 oC/min. And
tests. then, WTO was reacted with of CaO and NZ individually
The present study aims to characterize GLF and DLF at mass ratios of 2,4,6,8 and 10. Each sample was
with GF and DF in order to delineate organic distillated to compare with diesel fuel (DF).
compositions by means of FT-IR, NMR and UV-Vis Consequently, 10% CaO-WTO sample curve was fairly
methods which can be utilized in chamber of combustion. close to DF. However, the sample had a lower boiling
Each of analysis determined structure of composition temperature than DF.
with detection of organic compounds under advanced
technology of instrumental analysis.
Figure 1. Cycling paths of WTs
Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021 165
Figure 2. The batch pyrolysis system
Thus, the sample was divided into two new fuel by Agilent Premium Compact NMR600 MHz
samples at 54 oC to 150 oC which labelled as gasoline like spectrometer. The deuterated chloroform (CdCl3) was
fuel (GLF) and another one from 150 oC to 360 oC which used to dissolve sample at internal standard of NMR. 1H
was stated as Diesel like fuel (DLF) [22-24]. and 13C spectra were recorded from -2.00 ppm to 10.00
ppm and 20.00 ppm to 200 ppm, respectively at 600 MHz
2.4 Fourier Transform Infrared Spectroscopy (FT-IR)
frequency.
Method
2.6 Ultraviolet–Visible Spectroscopy Analysis (UV-Vis)
The physico-chemical properties with performance
and emissions of fuel have been influenced by different UV–vis spectra is used to detect the electronic
composition amount of hydrocarbon. The compositions properties of molecules. Each organic spectrum is taken
of fuel include different numbers of carbon which are via light into its structure to determine different aromatic
combined with various elements to form new types of compounds in samples at visible and ultraviolet fields
hydrocarbons at different ratios which can be classified as [33].
iso-paraffins, aromatics, naphthene, olefins (alkenes): In this study, UV absorption spectra of WTO, DLF, DF,
diolefins (alkins) [25]. The FT-IR is used to characterize GLF and GF were analyzed by using Agilent
bond structures of functional groups. Technologies Cary 60 UV–Vis Spectrophotometer in the
In this study, FT-IR was used to define functional wavelength range of 900-200 nm, at 1 nm intervals, at
groups and bands by a simple analytical technique which room temperature and scanned by using standard 1 cm
was related with kind of stretching and bending quartz cuvettes which are filled with samples for
vibrations of substances [26]. obtaining spectra. Additionally, samples were diluted by
FT-IR spectra were recorded between 4000-650 cm-1 ethanol to define the measurable absorbance interval in
range with a resolution of 4 cm-1 for 4 scans at room the spectrophotometer since samples absorbed light in
temperature by a Perkin Elmer Spectrum-Two high UV range to obtain spectra.
spectrometer for WTO, DLF, DF, GLF and GF, and the
chemical structure was observed. 3. Results and Discussion
2.5 Nuclear magnetic resonance spectroscopy (13C- 3.1 The physical properties of products
NMR, 1H-NMR)
A good indicator was physico-chemical analyses that
NMR has a special characterization analytical were applied to all samples. The initial product (WTO)
technique to satisfy available chemical compound was tested to measure calorific value and carbon amount
structures of renewable or conventional fuels. Besides, which was close to standard fuel except sulfur ratio. And
NMR has a good technique to find aromatic and aliphatic a second step of pyrolysis was carried out by adding
hydrogen and carbon atoms in fuel sample. The catalysts (2, 4, 6, 8 and 10 % of CaO and NZ separately)
resonance peaks area were characterized by the amount to WTO to minimize sulfur and increase features of new
of 1H or 13C atoms related with chemical compositions at mixture samples [18].
spectra [31]. The qualitative composition of WTO, DLF, The distillation was a good key for fuel properties to
GLF, DF and GF were determined in terms of high- notice best curve which was 10% CaO-WTO for the
resolution technique. Due to high resolution, NMR sample, while the mixture had to be extracted into two
spectroscopy provided detailed information on chemistry parts by boiling points of 54 oC-150 oC as GLF and 150
of petroleum fuels as proton and carbon [32]. The 1H, o
C-360 oC as DLF. Moreover, the carbon percentages,
13
C, 19F, 31P, 11B, APT and DEPT core probes were used density, flash point, and HHV of GLF and DLF were
166 Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021
close to fossil fuels. But, DLF sulfur amount require to be The peak of 891 cm−1 was determined C=C stretching
decreased by utilizing a novel process. Finally, GLF and which was presented in GLF, DLF and gasoline. The
DLF features were benefited for conventional engines residual aromatic groups were arranged at 768 cm -1, 742
[18]. cm-1, 729 cm-1 and 693 cm-1 which were seen at sharp
medium peaks of C-H cyclic deformations. The peak of
3.2 Fourier Transform Infrared Spectroscopy (FT-IR) C–H cyclic deformations were detected in all samples
The conventional fuels have complex ingredients as except DF [40]. The peaks of all samples revealed the
paraffins (alkanes), olefins (alkenes), diolefins (alkynes), main structure of hydrocarbons and their characteristics
naphthenic (cycloalkanes), and aromatic hydrocarbons by FT-IR spectrum analysis.
(benzene derivatives), sulfur, oxygen, and nitrogen
molecules which cannot directly and easily break into 3.3 Nuclear magnetic resonance spectroscopy (13C-
components [30]. Due to conventional fuel ingredients,
NMR, 1H-NMR)
WTO has same complicated structure as well as aliphatic,
aromatic, hetero-atom and polar compounds. For NMR principal has been found on average molecular
instance, WTO contains aromatic hydrocarbons compounds for aromatic, olefin and aliphatic
compounds such as benzene, toluene, xylene, styrene and hydrocarbons. The latter structures have a mean of
limonene. And also, the hydrocarbon groups of alkanes various functional groups number, which were detected at
which cause an increase in cetane number. Thus, the the NMR spectra [41]. The WTO, DLF, DF, GLF and GF
alkanes amount was preferred to be high in fuel as an were analyzed by 1H-NMR spectra. The characteristic
advantageous factor [31]. Figures 3 and 4 indicate FT-IR spectral area was defined by aromatic, olefin and
absorbance spectra which aim to show functional group aliphatic of proton signals at high and low fields. The 1H-
individually while Figures 5 and 6 indicate FT-IR NMR spectra were separated into spectral regions by
transmittance spectra which target to define conflict signals which were determined by aromatic, olefin and
functional group of samples. The observed peaks defined aliphatic hydrocarbons, as shown in Figure 7. 1H-NMR
alkenes group for each sample. The functional groups, spectra defined the aromatic and aliphatic groups in
which were found in literature and compared with all samples.
samples, were tabulated at Table 1.
As seen in Table 1, IR spectra have been explained
deeply in some researches, as represented in Ref. [32–
35]. The wave number ranging between 3700 and 3200
cm-1 were defined O–H stretching which was shown in
the hydroxyl compounds as alcohols, phenols and
carboxylic acids. Another absorption between 3000 and
2800 cm−1 was determined as -CH3, -CH2, and C-H
functional groups to be specified by aliphatic group of
alkanes [36-37]. The peak of 3677 cm−1 was seen at O-H
stretching for GLF, DLF, DF and GF. The peaks of 2962
cm-1 and 2925 cm-1 were related with C-H stretching
which were vibrated to hybridized at sp3 layers. This Figure 3. FT-IR split absorbance (A) spectra of WTO, DLF,
aliphatic and aromatic compound were obviously DF, GLF and GF
indicated of alkane groups [38]. The peak around 1608
cm-1 was allocated at C=C stretching of aromatics and
alkenes [39]. Other peaks were observed between 1455,
1376 and 1247 cm-1 due to vibration of aliphatic C-H
molecules. The C-H stretching (alkanes), C=C stretching
(alkenes) and C-H bending (alkanes) were observed at all
peaks of samples. Besides, 1150 and 1100 cm -1 peaks
were described at C-H in plane bending of aromatics.
Furthermore, aromatic hydrocarbons were underwent
chemical reaction with oxygen at high temperatures more
than aliphatic hydrocarbons [40]. The wave number
ranges were altered between 1020 and 845 cm-1 to define
C=C stretching of alkenes. Figure 4. FT-IR split transmittance (%) spectra of WTO, DLF,
DF, GLF and GF
Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021 167
Figure 5. FT-IR overlay absorbance (A) spectra of WTO, DLF, DF, GLF and GF
Figure 6. FT-IR overlay transmittance (%) spectra of WTO, DLF, DF, GLF and GF
Table 1. FT-IR functional groups and compounds of WTO, DLF, DF, GLF and GF [32-35]
Wavenumber ranges Wavenumber Functional group Groups Samples
(cm-1) (cm-1)
3700-3200 3677 O-H stretching hydroxyl GLF, DLF, gasoline
3000-2800 2962,2925 C-H stretching alkanes Whole samples*
1675-1575 1608 C=C stretching alkenes Whole samples*
1525-1115 1455,1376,1247 C-H bending alkanes Whole samples*
1150-1100 1066 C-H in plane bending aromatics GLF, DLF, gasoline
1020-845 891 C = C stretching alkenes Whole samples*
810-600 768,742,729,693 C–H cylic deformations aromatics DLF, GLF, WTO, gasoline
*Whole samples: WTO, DLF, diesel, GLF and gasoline.
As seen in Table 2, DLF, GLF and GF were analyzed define carbon groups (i.e. methyl, methylene, methylene)
by 1H-NMR that aromatic peaks were observed between and information about their locations which were
9.00-6.00 ppm of 1H chemical shift. The aliphatic alkane assigned at various typical regions [42]. Thus, 13C-NMR
and aliphatic alkene peaks were detected at a range of informs about presence of aromatic and aliphatic carbon
1.74-0.88 ppm and 6.00-1.70 ppm, respectively. in samples which have an agreement with FT-IR spectra.
Moreover, 1H chemical shift was identified in all samples In Table 2, 13C-NMR analysis was identified aromatic
(WTO, DLF, DF, GLF and GF). The samples were also peaks from 150.00 to 125.00 ppm by 13C chemical shift
tested by 13C-NMR spectroscopy to obtain more detail of for DLF, GLF, DF and GF. And also, alkane and alkene
their chemical structure. 13C nuclei of NMR sample of aliphatic compounds were seen in all samples which
spectra are seen in Figure 8. were detected via 13C chemical shift range of during
13C-NMR spectroscopy presents more detail on broad interval of 27.99-13.69 ppm and 150-110 ppm,
chemical shifts interval data (0-200 ppm) [41]. 13C-NMR respectively.
spectra have large numbers of distinguishable signals to
168 Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021
Table 2. 1H-NMR and 13C-NMR spectral regions for single components and structural groups of WTO, DLF, DF, GLF and GF
[43, 44]
1H chemical shift (ppm) 13C
Class chemical shift (ppm) Formulas Samples
Aromatics 9.00-6.00 150.00-125.00 Ar-H GLF,DLF, GF
Deuterated chloroform 7.27 77.36 CDCl3 Whole samples*
Aliphatics Alkenes 6.00-1.70 150-110 C=C Whole samples*
Aliphatics Alkanes 1.74-0.88 27.99-13.69 C-C Whole samples*
*Whole samples: WTO, DLF, diesel, GLF and gasoline.
Figure 9. UV-vis absorbance spectra of WTO, DLF, DF, GLF
and GF
3. Conclusions
Figure 7. 1H-NMR spectra of WTO, DLF, DF, GLF and GF WTs was liquefied into affluent organic products as
gas, oil and solid. Especially, the physical and chemical
features with calorific value of WTO were near to DF,
except for sulfur. Thus, CaO and NZ catalysts reacted
with different mass ratios to decrease sulfur quantity.
Then, the new products compared with DF. 10 % CaO-
WTO mixture curve was close to DF. Due to boiling
points, the mixture sample was separated into light (GLF)
and heavy (DLF) fractions. Both of GLF and DLF were
very similar to GF and DF. However, some available
characterization analyses were done for GLF and DLF
via FT-IR, NMR and UV–Vis which was explained as
items:
• FT-IR spectrum analyses of GLF and DLF had
peaks which demonstrated fundamental structure of
hydrocarbons, similar to standard fuels.
Figure 8. 13C-NMR spectra of WTO, DLF, DF, GLF and GF
• 1
H-NMR and 13C-NMR spectra of GLF and DLF
had aromatic and aliphatic carbon groups which
3.7. Ultraviolet–Visible Spectroscopy Analysis (UV-Vis) were compatible with FT-IR spectra which were
close to gasoline and diesel fuel.
UV-vis spectrometry is used for high accuracy quantity • UV-Vis spectra GLF and DLF had a similarity as
analysis for limited application interval due to range of visible and ultraviolet fields with standard
absorption. Thus, organic compounds were enlightened on petroleum fuels.
visible and ultraviolet fields to observe absorption spectrum
for functional sample groups. The absorbance curves of Declaration
diluted samples were observed at wavelength of 700– The authors declare no potential conflicts of interest
200 nm as seen in Figure 9. The curves were plotted by with respect to the research, authorship, and/or
UV-Vis spectra data to compare samples' shape and slope publication of this article. The authors also declare that
which have similarity with chemical compounds of fossil this article is original, and was prepared in accordance
fuels [45] with international publication and research ethics, and no
ethical committee permission or special permission is
required.
Uguz and Ayanoglu, International Advanced Researches and Engineering Journal 05(02): 163-170, 2021 169
Author Contributions upgradation of crude tire pyrolysis oil (CTPO) obtained
from a rotating autoclave reactor. Energy Conversion and
G. Uguz and A. Ayanoglu have equal contribution and Management, 2017. 250(1): p 339-351.
responsibility for the study. 14. Williams, P.T. Pyrolysis of waste tyres: A review. Waste
Management, 2013. 33(8): p 1714-1728.
Acknowledgment 15. Ayanoğlu, A., Yumrutaş, R. Production of gasoline and
diesel like fuels from waste tire oil by using catalytic
The authors wish to thank Tuna Demirci for the TGA,
pyrolysis. Energy, 2016. 103(1): p 456–468.
DÜBİT, Düzce University, Düzce, Turkey.
16. Kebritchi, A., Firoozifar, H., Shams, K., Jalali-Arani, A.
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