Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222

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Advanced Industrial and Engineering Polymer Research

journal homepage: http://www.keaipublishing.com/aiepr

Sustainable development of waste tires recycling technologies e

recent advances, challenges and future trends
Krzysztof Formela

sk University of Technology, Gabriela Narutowicza 11/12, 80e233 Gdan
Department of Polymer Technology, Faculty of Chemistry, Gdan
sk, Poland

a r t i c l e i n f o a b s t r a c t

Article history: Dynamic development of the automotive industry and the growing number of various vehicles generate
Received 12 May 2021 demand for the global production of tires. Simultaneously, high performance of tires cause serious
Received in revised form problems with further management and recycling of end-of-life tires. Therefore, searching for novel,
5 June 2021
environmentally-friendly and cost-effective rubber recycling methods is currently one of the biggest
Accepted 16 June 2021
environmental challenges in the 21st century.
This work aims to report the recent progress in sustainable development of waste tires recycling
Keywords:
technologies. A special attention was focused on current advances in waste tire rubber grinding tech-
Waste tires
Recycling
nologies; ground tire rubber treatment methods and characteristics of ground tire rubber and reclaimed
Ground tire rubber rubber.
Sustainable development Moreover, the main challenges affecting the future trends of the industrial application of waste tire
Quality control rubber recycling technologies are also discussed.
© 2021 Kingfa Scientific and Technological Co. Ltd. Publishing services by Elsevier B.V. on behalf of KeAi
Communications Co. Ltd. This is an open access article under the CC BY license (http://creativecommons.
org/licenses/by/4.0/).

1. Introduction up to 2030 the number of waste tires generated to the environment

Three-dimensional cross-linked structures formed in rubbers
during vulcanization significantly improve the performance prop-
erties of rubber goods (e.g. tensile properties, abrasion resistance,
chemical resistance or thermal stability). Simultaneously, cross-
linked rubbers are non-biodegradable and cannot be easily
reprocessed, such like thermoplastics. Above mentioned features of
rubber goods cause serious difficulties with management and
recycling of post-production and post-consumer waste rubbers
[1e3].
European Tyre and Rubber Manufacturers’ Association (ETRMA)
estimated that around 65% of the general rubber goods production
is dedicated for automotive sector (e.g. tires, wiper blades, seals,
hoses seatbelts, gaskets, insulators, etc.) [4]. Gerrard and Kandlikar
performed comprehensive analysis of materials used in a passenger
vehicles and showed that tires are 3.5 %wt., while the other rubber
goods are 1.6 %wt [5]. This indicates that the mainstream of waste
rubbers are end-of-life tires. The estimated data showed that
globally in each year, approximately 1000 million tires are not
suitable for further use or retreading [6]. According to predictions,
E-mail address: kformela.ktp@gmail.com.
will increase to 1200 million tires/per year [7]. Assuming that the
predicted data are correct and development of rubber recycling will
held the current relatively low level, this means increase by 20%
within next 10 years.
Increasing number of waste tires are serious threat to the nat-
ural environment and human health. Illegally dumped or stock-
piled waste tires are potential risk of uncontrolled combustion.
For example, in 2016 around 9000 people were evacuated from
their homes located in Sesen ~ a near to Madrid (Spain) due to the
combustion of the biggest illegal waste tire dump in European
Union (EU). Estimation showed that around 70e90 thousand tons
of tires were accumulated in Sesen ~ a for more than 15 years [8].
Fire in rubber recycling plants also occur, but fortunately in
lower scale. For example, in 2020: fire of around 1 ton of rubber
granulate in Vinderen Sp. z o.o. (Rubtiler) in Owadowie, Sławno,
Poland (technical rubber goods producer) or fire of 1000 L fuel tank
in Elan Recycling Plant Welshpool, Perth, Australia (producer of
pyrolysis products e carbon black, light oil, steel).
Fire of waste tire rubber resulted in emissions of sulfur oxides,
polycyclic aromatic hydrocarbons, fine particulates and other
hazardous compounds [8,9]. As a consequence, risk of cancer is
higher for population living near to illegal waste tire dumps and
also selected recycling rubber plants, especially those based on

https://doi.org/10.1016/j.aiepr.2021.06.004
2542-5048/© 2021 Kingfa Scientific and Technological Co. Ltd. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article
under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
K. Formela Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222

Abbreviations list SBR styrene-butadiene rubber

SBS styrene-butadiene-styrene copolymer
CR crumb rubber scCO2 supercritical carbon dioxide
DTG derivative thermogravimetry SSSE solid state shear extrusion
ETRMA European Tyre and Rubber Manufacturers' STR scrap rubber tire
Association RP rubber powder
EU European Union phr parts per hundred of rubber
FTIR Fourier transform infrared spectroscopy PSD particle size distribution
GC-MS gas chromatography mass spectroscopy VOCs volatile organic compounds
GTR ground tire rubber wt. by weight
GPC gel permeation chromatography WTR waste tire rubber
H2O2 hydrogen peroxide WTD waste tire dust
NR natural rubber WJP water-jet pulverization
TGA thermogravimetric analysis

prototype lines without strong basics in studies conducted at lab-

oratory scale.
Moreover, illegal disposal of waste tires can collect stagnant rain
water pools in their curvy shapes. These conditions enhance the
leaching of toxic compounds (e.g. heavy metals) from waste rubber,
which pollutes groundwater and have negative impact on aquatic
organisms [10]. High humidity inside disposed tires also creates
ideal conditions for breeding grounds for rodents and mosquitoes,
which can carry various diseases [11].
Nowadays, common method for waste tires management is
energy recovery, where whole or scrap tires are used as alternative
fuel in cement kilns, paper mills, or power plants. The newest
statistical report on the management of end-of-life tires published
by ETRMA showed that in 2018 around 91% of waste tires in the
European Union countries, as well as Norway, Serbia, Switzerland
and Turkey were collected and properly managed through material
recycling (56.4%) and energy recovery (34.9%) [12]. Fig. 1. Research works about rubber recycling, ground tire rubber and devulcanization
published in the period 2010e2020 (presented results according to Scopus® data base
It is worth to mention that in the statistical data presented by e data from April 06, 2021).
ETRMA, material recycling is mainly grinding/shredding of waste
tires, which in 2018 was the most popular solution among various
recycling methods of end-of-life tires. The shredding process in- products. This model was recently updated to 7Rs, in which the
cludes the production of the so-called “chips” commonly used as basic 3Rs model additionally contain new strategies for circular
alternative fuel (energy recovery). Other disturbing data presented economy model, such as redesign, renew, repair and recover. More
by ETRMA, points increase the level of unknown utilization of details about this approach dedicated to tires were comprehen-
waste tires in 2018 (318 800 t) by 12% comparing to value from 2017 sively reviewed in work [13].
(283 500 t). In this review paper recent progress, main challenges and future
Above mentioned data confirm that waste tires management is trends in sustainable development of waste tires recycling tech-
a global environmental problem and a huge challenge for scientists nologies are highlighted. A special attention was focused on i)
and industry representatives. Therefore research works focused on waste tire rubber technologies grinding; ii) ground tire rubber
material recycling technologies for waste tires are fully justified. treatment methods; and iii) characteristics of ground tire rubber
Fig. 1 showed data collected from Scopus® database (data and reclaimed rubber, which are described in next subchapters.
available on April 06, 2021) in which terms: rubber recycling;
ground tire rubber and devulcanization were searched in all fields
published in 2010e2020. As presented in Fig. 1, during last ten 2. Waste tire rubber grinding technologies
years, the number of research works in this area continually in-
crease. It was found that the total number of items for term: rubber Nowadays, the basic method of waste rubber recycling is their
recycling is 15 779 (2010 e 563/2020 e 3376; increase by 599%/10 shredding and grinding (~87.5% of all forms of recycling according
years); ground tire rubber is 4986 (2010 e 174/2020 e 1019; increase to ETRMA). In order to provide effective recycling of waste rubber,
by 587%/10 years) and devulcanization is 1001 (2010 e 43/2020 e prior to suitable shredding and grinding, waste rubber should be
156; increase by 363%/10 years). divided based on their source. This allows increase of process
This trend is related to current law (e.g. so called “Landfill repeatability and improve the quality of obtained products.
directive” - Council Directive 1999/31/EC from April 26, 1999), In case of waste tires the basic separation include two streams:
which successfully enforce the rubber industry responsibility for passenger car tires and truck tires. Sometimes also off-road tires are
waste rubber management and also higher awareness of society considered as third stream of waste tires. This is related to signifi-
about environment protection. Moreover, more and more efforts cant differences in the composition of these three types of tires,
are focused on circular economy model, according to 3Rs principles which is summarized in Table 1. As presented, truck tires are
including reducing waste, reusing and recycling resources and characterized by higher content of natural rubber and lower
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K. Formela Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222

Table 1
Typical composition of passenger, truck and off-road tires (data adopted from Refs. [1,14]).

Composition Passenger car tire Truck tire Off-road tire

Natural rubber 22% 30% 47%

Synthetic rubber 23% 15%
Carbon black 28% 20% 22%
Other additives (e.g. curing agents, textiles) 14% 10% 19%
Steel 13% 25% 12%
Estimated average weight of new tire 8.5 kg 65 kg e

content of carbon black as reinforcement filler in comparison to
passenger car tires. These difference are related to higher perfor-
mance properties of passenger car tires, such as low rolling resis-
tance, improved skid resistance and good wear [14]. Off-road tires
are characterized by higher content of textiles (10 %wt.) comparing
to passenger (5.5 %wt.) or truck tires (1 %wt.) [1], which might
cause difficulties related to purity of ground tire rubber based on
off-road tires.
According to information provided by Tyromer Inc. from Can-
ada, the tensile strength of reclaimed rubber obtained from tread of
truck tires (TSb ~ 8 MPa) is by ~ 33% higher comparing to reclaimed
rubber prepared from whole passenger car tires (TSb ~ 6 MPa).
However, it should be pointed out, that large scale separation of
passenger car tires and truck tires can be logistical problem and
additional cost of ground tire rubber. Other limitation is related to
volume of waste truck tires streams, which is lower than volume of
passenger car tires. Therefore, usually during shredding or grinding
mixes of passenger car tires and truck tires in ratio 50/50e70/30%
are used.
Depending on the grinding technology and conditions, ground
rubber is characterized by different particle sizes, surface charac-
teristics, etc. Products of waste tires grinding can be divided into
three streams: steel, textile cord and ground tire rubber.
It should be pointed out, that review of literature data indicated
the common problem with uniform nomenclature for the ground/
shredded waste tires. To highlight this problem data about the
finding for selected “keywords” were collected from www.google.
com, https://scholar.google.com, https://www.scopus.com,
https://apps.webofknowledge.com (searching performed on Apr.
10, 2021) and summarized in Table 2.
The issue with proper nomenclature of waste tires after grinding
process may cause misunderstanding in data interpretation. For
example, some of research works mention about using of ground
tire rubber, while presented results indicated that other type of
ground rubber (with similar appearance e black particles, but
not based on waste tires) was used in studies. This is also due to
very limited characterization of waste rubber prior to use in
research works, but this problem will be discussed in next sub-
chapter.
Moreover, data presented in Table 2 showed that according to
www.google.com findings three the most popular terms are “rubber
powder” (2 020 000 items), “waste rubber” (957 000 items) and
“crumb rubber” (775 000 items). For https://scholar.google.com,
https://www.scopus.com and https://apps.webofknowledge.com
database the most popular terms are “crumb rubber” (1st place in
all applied database https://scholar.google.com e 21 600 items,
https://www.scopus.com e 8016 items, https://apps.webofknowledge.
com e 2024 items), while second and third position varied depending
on used database. In https://scholar.google.com 2nd is “waste rubber”
(12 900 items), while 3rd place is “rubber powder” (9810 items). In
https://www.scopus.com 2nd is dedicated for term “waste rubber”
(5847 items), while 3rd place is “waste tire rubber” (4340 items). Ac-
cording to https://apps.webofknowledge.com on 2nd and 3rd place
are terms “waste rubber” (703 items) and “rubber powder” (497
items), respectively.
It is worth to mention that the most popular term “crumb
rubber” according to Web of Science is the most often used in such
field like: engineering civil (1036 items); materials science multi-
disciplinary (990 items) and construction building technology (873
items). Based on Scopus database, the highest number of works
with term “crumb rubber” is related to engineering (5595 items);
materials science (3582 items) and environmental science (1262
items). These data showed the main activity of research work are
related to application of waste rubbers as environmentally-friendly
materials in civil engineering, construction and building applica-
tion and material science (most desired target is automotive
industry).
It seems that the best option to uniform nomenclature is term:
ground tire rubber (GTR), which indicate the source of waste rubber
and final form of material obtained after shredding and grinding.
Alternatively, terms waste tire rubber (WTR) or waste tire dust
(WTD) can be considered. Moreover, it should be highlighted that
during searching term “tire” was used as form in American English,
while for term “tyre” in British English results might be different in

Table 2
Comparison of nomenclature for grinded/shredded waste tires (searching performed in www.google.com, https://scholar.google.com, https://www.scopus.com, https://apps.
webofknowledge.com on Apr. 10, 2021).

“Keywords” Abbreviation Number of findings according to database

Google Google Scholar Scopusa Web of Sciencea

rubber powder RP 2 020 000 9810 2764 497

waste rubber e 957 000 12 900 5847 703
crumb rubber CR 775 000 21 600 8016 2024
scrap rubber e 632 000 4460 1235 160
ground rubber e 398 000 4040 1344 263
scrap tire rubber STR 45 800 2760 1814 110
waste tire rubber WTR 97 700 5360 4340 354
ground tire rubber GTR 45 200 4240 2541 426
granulate rubber e 10 100 66 4 2
waste tire dust WTD 6540 230 272 25
a
Search within: All fields.

211
K. Formela
dependence of used database. For example, according to Google-
Scholar database (data available on Jun. 06, 2021) term “ground tire
rubber” was used in 4390 items, while for term “ground tyre rub-
ber” only 894 items were found. For clarity, in this review term
ground tire rubber (GTR) was used.
The most popular industrial scale waste tires grinding technol-
ogies are: ambient method and cryogenic method. In first method,
waste rubber is passed through shearing mills or two rolls mills,
which working at room temperature. However, during grinding of
waste rubber by ambient temperature, the temperature of ground
rubber may increase even up to 130
C [15]. This phenomenon
increase the risk of uncontrolled combustion of rubber during
grinding.
Waste tires grinding by cryogenic method based on effective
cooling of waste rubbers below their glass transition temperature
using liquid nitrogen. This results in conversion of elastic rubber
material into frozen brittle form, which can be easily crushed by
using hammer mill [16].
Different mechanism of breaking during disintegration of waste
tire rubber by both mentioned methods affecting features of
ground tire rubber surface and shapes. In case of ambient method,
ground tire rubber is characterized by irregular particle shape and
spongy, well-development surface, while for cryogenic methods
rubber particles are regular and smooth characterized by low sur-
face area. A summary with comparison of ambient and cryogenic
methods of waste tires grinding is presented in Table 3.
Those obvious differences, cause that further processing (e.g.
mixing with fresh matrix) and application in recycling technologies
of GTR obtained by ambient method providing better results in
comparison to products obtained by cryogenic method [16e18].
Recently, Hoyer et al. [19] performed research focused on
comparison of the cryogenic grinding of waste tire rubber (truck or
passenger car) with different ambient grinding processes. During
research authors use: solid state shear extrusion e SSSE; cracker
mill (two roll mills); wet grinding (intermeshing grinding discs)
and hyperboloidal cutting mill (high-speed cutting mill equipped
with 3 rotor and stator knives (rotor diameter: 200 mm, rate of
rotation: 860 min1); at the bottom of the hyperboloidal cutting
mill is a sieve (600 mm) and waste rubber remains in the machine
until the desired size of rubber particles are obtained). The obtained
results are summarized in Table 4.
The results showed that the lowest specific energy consumption
during grinding truck tires (GTR e 400 mm fraction) was found in
the wet method in a wet grinding e 525 Wh/kg (truck tires) and
630 Wh/kg (car tires). Specific energy consumption value for the
other methods was, respectively, 967 Wh/kg for the method using a
hyperboloidal cutting mill, 1207 Wh/kg for the cryogenic grinding,
1250 Wh/kg for cracker mill and 3132 Wh/kg for the solid state
shear extrusion. In studied case, the cryogenic grinding line having
the highest throughput (588 kg/h) among the analyzed technolo-
gies (in the range of: 1.2e160 kg/h).
Table 3
A comparison of ambient and cryogenic methods of waste tires grinding.
Item
GTR properties specific gravity
particle shape
surface area
oxidation level
Product purity
Production costs
a
Grinding in inert atmosphere (liquid nitrogen), lower temperature during grinding.
b
Related to infrastructure, application of liquid nitrogen and product drying costs.
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
Moreover, other methods of waste rubber grinding, such as
grinding with support of ultrasounds, cutting with water under
pressure (water-jet), pulverization in presence of supercritical
carbon dioxide or other prototypes are gaining more and more
attention.
For example, Dobrota  and Dobrota  [20] investigated waste
rubber grinding technology activated with ultrasounds. Such
approach, allows on preparation of ground rubber with a very good
particle size distribution and average particle sizes in the range of
100e150 mm, which can replace reclaimed rubber used in industry.
Moreover, the results showed that application of ultrasounds dur-
ing grinding of waste rubbers reduce energy consumption and
simultaneously increase production efficiency by higher speed of
shredding.
Wang et al. [21,22] studied the impact of water-jet pulverization
(WJP) parameters, such as pump pressure, transverse velocity,
standoff distance and impacting angle, on the quality of obtained
GTR (e.g. particle size distribution; average particle size; cross-link
density and sol fraction). The WJP processing parameters were
optimized by response surface methodology, which allows mini-
malize specific energy consumption of pulverization process. Par-
ticle size of GTR obtained by this method was below 200 mm.
Moreover, the results showed that vigorous erosion and the high
compressive shear on the waste rubber during WJP might cause
partial devulcanization/degradation of GTR.
Zefeng et al. [23] used the GTR obtained by ultrahigh pressure
WJP (particle size 270 mm and surface area 0.153 m2/g) as rein-
forcement phase in natural rubber (NR) based composites. It was
observed that addition of GTR to NR had a negative effect on pro-
cessing of studied composites (Mooney viscosity increased with
higher load of GTR). On the other hand, tensile and tear strength
parameters were improved after incorporation of GTR into the NR
matrix at levels up to 40 parts per hundred of rubber (phr). Suffi-
cient dispersity and quite good compatibility of GTR phase and NR
matrix was confirmed by scanning electron microscopy.
Bowles et al. [24] compared the characteristics of GTR obtained
by ambient method with GTR obtained by ultrahigh pressure WJP.
The results confirm more developed surface of GTR obtained by
ultrahigh pressure WJP. The authors also investigated the impact of
prepared GTR on natural rubber/styrene-butadiene rubber (NR/
SBR) based composites. The results confirmed that composites
modified with GTR obtained ultrahigh pressure WJP had higher
performance. However, the improvement of tensile strength or tear
strength in comparison to reference sample (without GTR) was not
observed. This observation can be related to final particle size of
obtained GTR or presence of SBR in studied system and should be
verified during future research works.
Hydrapress Sp. z o.o. company (Białe Błota, Poland) patented an
interesting method of shredding whole tires by milling them using
special discs under the trade name Rotarex [25]. The proposed
station for shredding car tires takes up a small space (the size of a
Grinding technology
Ambient Cryogenic
same same
irregular regular
spongy/well-developed smooth/non-developed
high lowa
low high
low highb
K. Formela
Table 4
Comparison of cryogenic and various ambient grinding technology of waste tires (data adopted from Ref. [19]).
Item Grinding technology
Cryogenic Solid state shear extrusion
Waste tires source Truck tire Truck tire
Average energy demand (kW) 138 165
Particle size (mm) 400
Throughput (kg/h) 588 53
Energy consumption (Wh/kg) 1207 3132
container), which allows its transport (e.g. to collection points for
car tires or their illegal dumping) without numerous and compli-
cated logistic operations.
Kroll and Hoyer [26] invented a device called “Reaktruder”
dedicated to the grinding of elastomers by small and medium-size
companies. Construction is similar to extruders and its scheme is
shown in Fig. 2. The specific energy requirements for grinding of
crumb truck tires with particles below 5 mm is 0.16 kWh/kg
(0.32 kWh/kg for particles below 0.8 mm). The applied solutions
allowed for the reduction of investment and operating costs, and
according to the authors' calculations the purchase of the tech-
nology pays off after approximately 1500 h of device operation.
Recently, development of waste rubber pulverization/grinding
technologies combined with their suitable treatment by devulca-
nization or functionalization are gaining more and more attention.
Li et al. [27] investigated the cryogenic grinding process of GTR
modified by devulcanization in scCO2 performed in fluidized-bed
jet mill. The different content of scCO2 on devulcanization degree
and grinding efficiency of GTR were studied. Supercritical fluids
(scCO2, ethanol) [28,29] and subcritical fluids (water) [30] have the
ability to swell the waste rubber, which enhanced devulcanization
process due to higher selectivity of cross-linking bonds breaking.
The comparison of mechanisms of common devulcanization of GTR
and devulcanization in presence of scCO2 is presented in Fig. 3 [31].
As can be observe, common devulcanization process (path A) oc-
curs usually on surface of GTR and successfully proceed layer by
layer to core of waste rubber. This results in long time of devulca-
nization process, which affecting partial degradation of main chain
(see sol fraction). At the same time, inner core of cross-linked
rubber remains still almost untreated (see gel fraction). On the
other hand, scCO2 during devulcanization (path B) acts like plasti-
cizer and swell three-dimensional network of rubber, which
significantly improves devulcanization process efficiency in whole
volume of cross-linked rubber. Moreover, scCO2 as inert component
prevent uncontrolled oxidation and main chain degradation of GTR
during devulcanization.
Fig. 2. A grinding device called “Reaktruder” (as feed material waste rubber with particle size up to 5 mm can be applied): Left side - device appearance; Right side e scheme of the
device: 1 - screw; 2 - shredding disc; 3 - cylinder; 4 - working slot; 5 e engine (Reprinted with permission from Ref. [26]. Copyright (2021) Elsevier).
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
Cracker mill Wet grinding Hyperboloidal cutting mill
Car tire Truck tire Car tire Truck tire
200 32 32 1.2
160 61 51 1.2
1250 525 630 967
The results in work [27], showed that devulcanization of GTR
can promote particle size reduction, which is related to the trans-
formation of the cryogenic grinding mechanism from abrasion to
cleavage or fracture. It is expected that such approach allows
reduction of the consumption of refrigerants during cryogenic
grinding and consequently final cost of GTR production.
Wang and Zeng [32] highlighted novel concept of waste tire
rubber reclaiming using supercritical carbon dioxide (scCO2) jet
pulverization. The authors studied the effects of scCO2 jet pulveri-
zation parameters on particle size distribution (PSD) of GTR and
rubber devulcanization. The results showed that scCO2 jet pulver-
ization is energy intensive technology with energy consumption
4.3 kWh/kg, which is value similar to water jet pulverization in
laboratory scale (~4.5 kWh/kg). The estimated consumption of
scCO2 during process is around 3e5 l/kg, but it should be noticed
that this component can be recovered in the process. It was
observed that longer reaction of GTR with scCO2 enhanced devul-
canization process what result in GTR with coarser particle size
(formulation of reclaimed GTR agglomerates). This indicates that
rubber swelling in scCO2 and in consequence its higher devulca-
nization does not support of GTR pulverization.
The presented works confirm that grinding technologies will
develop in next years (especially methods acting in continuous
manner). It seems that works focused on utilization of post-
production waste rubber and special elastomers, which are char-
acterized by well-defined composition or relatively high-price, will
developed in future.
3. GTR treatment methods
Rubber reclaiming, which is accompanied by the devulcanization
(de-cross-linking), is one the oldest and most popular method for
treatment of ground tire rubber, which successfully develop in
recent years as summarized in comprehensive review works
[33e36]. This approach allows transformation of cross-linked rub-
ber use of thermal, mechanical or chemical energy into products
K. Formela
Fig. 3. Comparison between common devulcanization and devulcanization in presence of scCO2 of waste rubber (Reprinted with permission from Ref. [31]. Copyright (2021)
Elsevier).
commonly known as reclaimed rubbers, which can be easily
reprocessed, shaped and vulcanized.
Devulcanization allows highly selective breaking of sulfide
cross-linking bonds, while in rubber reclaiming also scission of
main chain occurs. Increasing level of main chain scission resulted
in decrease of molecular weight of polymer and increase of its
polydispersity, which usually deteriorate the mechanical properties
of vulcanized reclaimed rubbers, the so-called revulcanizates.
In fact, there is no simple parameter, which allows clear
distinction between reclaiming vs devulcanization of rubber. Most
of recently published scientific papers put accent on “rubber
devulcanization” (according Scopus database: 117 documents),
rather than “rubber reclaiming” (according Scopus database: 48
documents).
Differences between reclaiming and devulcanization based only
on a subjective assessment and the analysis of main chain degra-
dation degree usually supported by Horikx theory [37]. However, it
should be pointed out that swelling/extraction conditions (e.g.
temperature, time, sample weight, kind of used solvent, etc.) will
have impact on values of parameters used for estimation of main
chain scission selectivity based on Horikx theory.
Recent trends in research about waste rubber treatment tech-
nologies shown that low-temperature devulcanization and com-
bination of devulcanization with suitable functionalization are
gaining increasing attention.
Zhang et al. [38] considered application of hydrogen peroxide
(H2O2) during thermo-oxidative reclaiming of solid styrene-
butadiene rubber (SBR) vulcanizates performed at low tempera-
ture with the assistance of soybean oil. Reclaiming was performed
into drying oven within 0.5e4 h. The scheme of oxidative recla-
mation process of solid SBR vulcanizates is presented in Fig. 4.
The results showed that SBR vulcanizates were completely
transformed into liquid rubber (100% of sol fraction) at 100
C in the
presence of soybean oil (used amount 100 phr) and 3 %wt. solution
of H2O2 (used amount 2 phr).
Literature reports indicate that disintegration of three-
dimensional network in vulcanized rubber during partial devul-
canization might facilitate migration of curing system components
(e.g. sulfur, accelerators) between reclaimed GTR to the polymer
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
matrix [39,40]. Moreover, as presented in works [41,42], reclaiming
degree of GTR enhanced also migration of carbon black to the
polymer matrix, which have beneficial impact on mechanical
properties of composites modified by reclaimed GTR. The effect of
GTR treatment on rubber compound migration phenomenon is
schematically presented in Fig. 5.
Araujo-Morera et al. [43] performed mechano-chemical modi-
fication of GTR, which combine cryogrinding and chemical treat-
ment by hydrogen peroxide (for 3 h, at room temperature) or
inorganic acids (H2SO4, HNO3 and their mixture) (for 3 h, at 100
C).
GTR is hydrophobic material, however after controlled oxidation
new functional groups such as hydroxylic, carboxylic are formu-
lated (see Fig. 4). Fig. 6 shows stability of water-GTR suspension for
GTR treated by different methods: ambient grinding (Fig. 6a);
cryogenic grinding (Fig. 6b); H2O2 treated (Fig. 6c); H2SO4 treated
(Fig. 6d); HNO3 treated (Fig. 6e) and H2SO4/HNO3 mixture treated
(Fig. 6f). The results showed that only for GTR treated with inor-
ganic acids at 100
C stable suspension with water was possible.
This confirms that suitable level of oxidation enhance GTR
hydrophility, which in consequence will improve dispersion of
oxidized GTR into more hydrophilic matrices (e.g. polyurethanes,
concretes, etc.).
Rungrodnimitchai and Kotatha [44] prepare anion exchange
resin based on modified GTR. The scheme of three step modifica-
tion procedure is presented in Fig. 7. GTR treatment was performed
by a bromination reaction (modification for 2e3 h at room tem-
perature), followed by a reaction with ethylenediamine under
conventional heating (for 2e3 h at 150
C) or microwave heating
(domestic microwave oven was used; magnetron power:
300e600 W; time: 2e6 min, final temperature of mixture:
~120e180
C). Subsequently, ethylenediamine into the structure of
the ground tire rubber was protonated by HCl (for 12 h at room
temperature). After each step of GTR treatment, obtained product
was washed by distillated water and dried at 80
C for 12 h. The
results showed that modified ground tire rubber could be used as a
good adsorbent for defluoridation. Moreover, the experiment
confirmed that short time microwave treatment has similar reac-
tion efficiency like long term conventional heating. Selectivity and
highly efficiency in the heat transfer of microwave heating provide
K. Formela
Fig. 4. Scheme of oxidative reclamation process of waste SBR vulcanizates (R represents macromolecular radicals) (Reprinted with permission from Ref. [38]. Copyright (2021)
American Chemical Society.).
a huge advantage in industrial recycling and treatment of waste
rubbers, especially end-of-life tires, what was discussed in review
work [45].
Also other GTR modification approaches were considered in
order to extend GTR application in various composites and improve
matrix-GTR interactions. For example, grafting of GTR with: gly-
cidyl methacrylate and methacrylic acid [46,47]; acrylic acid
[48,49]; styrene [50,51]; polycardanol [52]; natural rubber [53] or
soybean oil [54] were described in the literature. Chlorination [55],
hydrosilylation [56] or plasma treatment [57] were also considered
for GTR treatment.
However, it should be pointed out, that the many of GTR treat-
ment methods described in the literature are usually performed
with low efficiency (~few grams of modified GTR) and in periodic
manner. Moreover, commonly GTR treatment is conducted in
presence of solvents or acids. This causes necessity of washing of
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
obtained products and also waste-water treatment, which affecting
the final costs of modified GTR production. Above mentioned
drawbacks are the main limitation for future implementation of
GTR treatment methods from laboratory to industrial scale.
Other approach is treatment of GTR by devulcaniation combined
with suitable modification or encapsulation, which efficiency
usually based on compatibility and physical interactions between
GTR and used modifier [58e60].
Fig. 8 presents scheme of GTR reclaiming in presence of bitumen
and bitumen modified with styrene-butadiene-styrene copolymer
(SBS). GTR treatment was performed for 30 min using two-roll mills
at ambient temperature [61].
The obtained results indicated that using of bitumen during
mechano-chemical treatment of GTR enhanced processing and
prevents oxidation of reclaimed GTR due to improved interfacial
interactions between GTR and bitumen.
K. Formela Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222

Fig. 5. The effect of GTR treatment on rubber compound migration phenomenon [2].

Fig. 6. Stability of water-GTR suspension: (a) GTR after ambient grinding; (b) GTR after cryogenic grinding; (c) GTR treated with H2O2; (d) GTR treated with H2SO4; (e) GTR treated
with HNO3; and (f) GTR treated with H2SO4/HNO3 mixture [43].

Fig. 7. Reactions for preparation of the modified ground tire rubber (from up): bromination of carbon-carbon double bond (product: Ground tire rubber II); aminolysis of dibromide
product (product: Ground tire rubber III), and protonation of ethylenediamine modified ground tire rubber (product: Ground tire rubber IV). (Reprinted with permission from
Ref. [44]. Copyright (2021) Elsevier).

Zedler et al. [62] investigated the performance properties of GTR The results showed that a relatively small amount of ethylene-
reclaimed and modified with ethylene-vinyl acetate copolymer via vinyl acetate copolymer improves the mechanical properties of
low-temperature extrusion process. modified reclaimed GTR and also allows further recycling by

216
K. Formela
Fig. 8. Schematic illustration of GTR reclaiming using bitumen and bitumen modified with styrene-butadiene-styrene copolymer (SBS) (Reprinted with permission from Ref. [61].
Copyright (2021) Elsevier).
multiple processing without the deterioration of performance after
three cycles (tensile strength: 3.2 ± 0.5 MPa for reference and
2.7 ± 0.5 MPa for sample after three recycling cycles). The
appearance of GTR treated with ethylene-vinyl acetate copolymer
before and after recycling is presented in Fig. 9.
Examples presented in this sub-chapter confirm that GTR
treatment methods successfully develop and it seems that this
tendency will be continued in near future (especially in case of
methods based on reactive extrusion process). Summary of recent
trends in ground tire rubber treatment was comprehensively
described in work [63].
4. Characteristics of ground tire rubber and reclaimed rubber
One of the basic methods for characterization of ground tire
rubber is sieve analysis performed according to ISO 2591-1. Avail-
able on market GTR particles size usually vary in the range of:
0.4e7 mm. Fig. 10 presents comparison of particle size of GTR with
Fig. 9. Appearance of GTR treated with ethylene-vinyl acetate copolymer: A e refer-
ence sample; B e sample after material recycling (sample compressed in the same
conditions as reference sample) [62].
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
tradename Green Gran produced by Grupa Recykl S.A. (Srem,

Poland).
It is common rule, that lower particle size of GTR increase the
final cost of material, which is related to energy consumption
during waste tires shredding and grinding. Seghar et al. [64]
pointed out that for rubber particles of 1e3 mm size cost of
grinding is approximately 120 V/ton, for particles of 0.8e2.5 mm
size is 130 V/ton, while for rubber particles with dimension below
0.8 mm is 300 V/ton. Additionally, authors indicated that reason-
able economical size of waste rubber particles used in thermo-
mechanical devulcanization technology performed by extrusion is
in the range of 0.8e4 mm.
Currently, the particle size distribution and average particle size
are the main parameters determining the potential applications of
GTR, while the impact of waste rubber source (as mentioned in
previous sub-chapter, this fact might cause misleading interpreta-
tion of results), degradation level or cross-link density are usually
omitted.


Fig. 10. Comparison of particle size of GTR produced by Grupa Recykl S.A. (Srem,
Poland).
K. Formela
The main categorization of waste tires covers passenger car and
truck tires, which differ essentially in the type/quantity: i) elas-
tomer matrix (e.g. the ratio of natural rubber to synthetic rubbers),
ii) reinforcement fillers (carbon black, silica) and iii) other additives
(e.g. curing additives, accelerators, plasticizers, antioxidants, etc.)
(please see Table 1).
The most appropriate method to determine composition of
waste tire rubber and rubber reclaiming or modification efficiency
is thermogravimetric analysis (TGA) and derivative thermog-
ravimetry (DTG) [65,66]. This analytical technique allows on
quantity identification of rubber compound composition (content
of elastomer, filler and additives). A detailed description of the
methodology for compositional analysis of rubber by TGA is pre-
sented in the ASTM D6370 standard.
During studies of GTR in DTG curve we should observe two
characteristics peaks related to the temperatures of maximum rate
of thermal degradation of natural rubber (Tmax1 ~ 400
C) and
styrene-butadiene rubber (Tmax2 ~ 450
C), which are rubbers
commonly used during tires manufacturing. The estimated carbon
black content should be in the range ~35 ± 5% [67].
Moreover, for better understanding of the complex changes
related to reclaiming or modification of GTR and characteristics of
volatile organic compounds emitted during GTR recycling, it is
recommend to extend TGA by combination with Fourier transform
infrared spectroscopy (FTIR) or with gas chromatography mass
spectroscopy (GC-MS) [68,69].
Another important parameter, which should be considered
during GTR processing is moisture content. A detailed description
of the methodology is presented in the ASTM D6980 standard. This
parameter is very important in the case of application of GTR in
polyurethane adhesives or other reactive systems (e.g. production
of wheels for trash cans, mats, etc.), where moisture content can
affecting reaction kinetics and curing efficiency of obtained com-
posites [70].
One of the basic methods for studies of GTR before and after
treatment based on determination of the sol fraction and cross-
linking density measured by equilibrium swelling method in
organic solvents. Acetone extraction allows studies of soluble
substances content (e.g. curing additives, plasticizers, etc.), while
the extraction in toluene/xylene/benzene determine sol fraction
content. A detailed description of the methodology is presented in
the ASTM D6814 standard. It should be pointed out that sometimes,
in order to eliminate the impact of reinforcement fillers (carbon
black, silica) present in GTR or reclaimed GTR on the value of their
cross-linking density, the Krauss correction dedicated for filled
compounds can be used [22,61]. However, this approach is more
suitable for rubber compounds modified with GTR or reclaimed
GTR, rather than for materials based only on GTR or reclaimed GTR
for which the content of filler is usually constant.
Moreover, in most published scientific papers, individual
research groups use their own developed procedures or laboratory
standards [71e73]. Differences in swelling/extraction conditions
(e.g. different temperature during extraction, solvent type, test
time, weight of sample, etc.) cause that comparison of the results
obtained by different groups research is very difficult.
Although the extracts with sol fraction, can be also used in order
to determine the average molecular weight and molecular weight
distribution of sol fraction by gel permeation chromatography
(GPC), the literature data about such measurements dedicated to
waste rubbers are rather limited [74,75].
It seems that more appropriate method for determination of
GTR reclaiming efficiency is Mooney viscosity measured according
to ASTM D1646 standard [76e78]. Mooney viscosity (MV) of rubber
is parameter strongly correlated with gel-sol fraction content.
However, MV value does not provide information about molecular
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
structure of reclaimed rubber, especially its polydispersity related
to selectivity of cross-linking bonds scission (devulcanization) vs
main chain degradation (reclaiming). Interesting approach in this
area is application of rubber process analyzer which can provide
more information about structure of natural rubber [79,80] (one of
basic matrices used in rubber industry) or rheological properties of
rubber compounds modified by reclaimed rubber [81e83].
Other suitable method to evaluate the quality of reclaimed or
modified GTR are measurements of curing characteristics (by using
of oscillating disc rheometer/moving die rheometer) or mechanical
properties (e.g. tensile strength, elongation at break, hardness, etc.)
performed according to dedicated ISO or ASTM standards. Such
approach allows comparison of results obtained by independent
research groups.
However, it should be noticed that some limitation in this field is
lack of standardized procedures with specification of sample
preparation and vulcanization conditions of reclaimed rubbers
based on GTR (or rubber compounds filled with reclaimed rubber).
As presented in work [84], curing system have significant impact on
final mechanical properties of reclaimed GTR. For the same material
tensile strength might vary in the range of: 4.8e7.4 MPa and for
elongation at break in the range of: 98e263%. For comparison, the
above-mentioned conditions were specified for reclaimed rubber
derived from products containing mainly natural rubber, as
described in the ISO/AWI TS 16095 standard.
Liang et al. [85] performed comprehensive investigations about
quality control of SBR (as model compound) and GTR by various
analytical techniques, such as: atomic absorption spectrometry,
inductively coupled plasma optical emission spectrometry, CHNS
elemental analysis, differential scanning calorimetry, solid-state
proton nuclear magnetic resonance, thermogravimetric analysis
and energy-dispersive X-ray fluorescence spectroscopy. The results
showed that among used techniques, the most promising methods
are: X-ray fluorescence spectroscopy (determination of zinc con-
tent) and differential scanning calorimetry (measurements of glass
transition temperatures). This is related to analyses duration and
costs of those techniques, which allow their implementation in
rubber recycling plants [85].
According to authors, TGA results are recommended for
determination of monomer weight ratios of SBR, but not for
GTR. TGA results can overestimate monomer weight ratios
(butadiene þ isoprene/styrene) in GTR, which was also confirmed
by solid-state proton nuclear magnetic resonance analysis.
Furthermore, the results showed that TGA technique is suitable for
determination of carbon black and inorganic residue content in SBR
and GTR.
Colom et al. [86] performed research about GTR microwave
treatment, which efficiency was evaluated by Fourier transform
infrared spectroscopy (FTIR), thermogravimetric analysis. FTIR
spectroscopy analysis indicated that microwave treatment of that
GTR causes a decrease in carbon black with generation of carbon
dioxide due to GTR thermo-oxidation. Moreover, reduction of sig-
nals from structural groups related to elastomeric components
(mainly methylene and methine) and a breaking of CeS and SeS
cross-linking bonds were also observed.
Moreover, in order to determine the surface changes after GTR
treatment contact angle [87], X-ray photoelectron spectroscopy
[88] are used, however more often scanning electron microscopy
[89e91] is applied.
Recently, problem of volatile organic compounds (VOCs) emis-
sion from ground tire rubber, especially this used in applied in
artificial turf fields, is gaining increasing attention as highlighted by
independent research groups [92e94].
This is due to fact that during degradation or reclaiming/
devulcanizaiton of rubber emission of low-molecular volatile
K. Formela
organic compounds related to disintegration of cross-linking
bonds, main-chain scission, as well as evaporation of additives
present in the rubber (e.g. plasticizers) naturally occur. Ga˛ gol et al.
[95] confirm that efficiency of VOCs emission is strongly correlated
with GTR devulcanization degree. GTR was thermo-mechanically
treated in different temperature (80, 120, 160
C) using a co-
rotating twin screw extruder. The highest concentration of VOCs
was determined for GTR treated at the highest temperature e
160
C. The study revealed that, during extrusion, emitted VOCs can
interact with each other and formed new chemical structures
which affected the total amount of volatile organic compounds.
It was found that benzothiazole was the most abundant sulfur
compound due to degradation of vulcanization accelerators residue
present in GTR. This indicates that the results of quantify analysis of
benzothiazole (vulcanization accelerators residue) emission could
be use as marker for reclaiming/devulcanization degree [96,97].
Other compound from the VOCs group, which could provide
information about the level of main chain scission in GTR is limo-
nene, a degradation product of natural rubber [62,98,99]. The level
of limonene is strongly correlated with degradation level of natural
rubber characterized by lower thermal stability comparing to
synthetic rubbers (butadiene rubber, styrene-butadiene rubber)
commonly used in tire rubber manufacturing.
The progress in this field was recently summarized by Sibeko
et al. [100], who discussed experimental approaches in the analysis
of polycyclic aromatic hydrocarbons from rubber crumbs.
5. Conclusions, challenges and future trends
Increasing number of waste tires generated to the environment
each year is a huge and global problem. This situation enforced
industry and researchers to develop existing technologies and
searching of new direction of rubber recycling, which is one of
strategies supporting circular economy in tire industry.
Over the last 10 years many attempts in waste tires recycling,
especially those focused on direct application of GTR in various
matrices (e.g. polymers, bitumens, concretes, etc.) or GTR devul-
canization treatment were depicted.
This work summarized recent advances related to sustainable
development of waste tires recycling technologies. A special
attention was focused on current advances in waste tire rubber
grinding technologies and treatment methods, which allow
tailoring of particle size distribution and suitable modification/
functionalization of GTR surface by reactive functional groups or
physical encapsulation by compatibilizers.
New features of modified GTR affecting on matrix-GTR interfa-
cial interactions, which increase the range of potential application
of treated GTR. This solution should allowing use higher content of
GTR in composites and consequently resolve the current problems
with still relatively low level of waste tires recycling.
The main drawback in this field of research is fact that in the
most of investigated methods GTR modification require complex
reaction procedures with multiple steps (including e.g. solvent re-
covery, washing, drying and generated waste-water utilization) and
long treatment time, performed usually in periodic manner. Above
mentioned disadvantages results in high cost of GTR modification
methods performed at laboratory scale, which limits industrial
implementation of GTR treatment technologies.
This paper also highlighted the issues related to limited charac-
teristics of GTR or ground rubber (in appearance similar to GTR) used
during research focused on the search for new forms and methods of
material recycling. General specification of commercially available
GTR based on estimation of particle size distribution or average
particle size, while the chemical composition (especially rubber
content and type (natural rubber/synthetic rubber), reinforcement
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Advanced Industrial and Engineering Polymer Research 4 (2021) 209e222
filler (carbon black/silica) content, etc.) is usually unknown. Ther-
mogravimetric analysis procedure based on the ASTM D6370 seems
to be the best option to apply for GTR. Additionally, such parameters
moisture content or degradation degree (acetone extract, sol frac-
tion) of ground rubber should be also considered prior recycling
process. Lack of more detailed characteristics of GTR or ground
rubber before processing/recycling might results in incorrect or
overestimated findings and conclusions.
Moreover, during future works application of “standardized”
procedures for assessment of new reclaiming/devulcanization
technologies and reclaimed GTR characterization are highly rec-
ommended for research groups working on this topic.
The basic information about reclaiming/devulcanization tech-
nologies should considered detailed description of: characteristics
of used GTR (as pointed above), reclaiming conditions (especially
temperature, shear forces, throughput), temperature of reclaimed
GTR measured directly after processing (infrared thermometers or
thermal-imaging cameras are useful for this purpose), cooling
method of reclaimed GTR, total energy consumption or specific
mechanical energy (kWh/kg). Mentioned parameters provide use-
ful information about process profitability and environmental-
friendlies (e.g. volatile organic compounds emission related to
applied processing temperature; waste-water treatment necessary
after product cooling, etc.), which are crucial for future imple-
mentation at industrial scale.
Considering pros and cons of various methods applied for
reclaimed rubber characterization its seems that as a basic standard
Mooney viscosity according to ASTM D1646 should be determined.
However, for GTR with low reclaiming/devulcanization degree
(changes only on surface of GTR) this method will not work.
Therefore future work in this field should considered development of
procedures dedicated for reclaimed rubbers and rubber compounds
modified by GTR, which based on rubber process analyzer.
Other important parameter which should be investigated for
reclaimed rubbers is tensile strength determined according to ISO/
ASTM standards. However, it should be noticed, that the final value
of this parameter is affected not only by reclaiming/devulcanization
efficiency but also by curing system composition and vulcanization
conditions of revulcanizates.
Mooney viscosity and tensile strength of reclaimed GTR are
standardized (ISO/ASTM) parameters which provide useful infor-
mation about processing and performance. Standardization allows
easy comparison of results obtained by independent research
groups and provide good platform for discussion about differences
or similarities of obtained results. Based on values of these two
simple parameters potential application of neat reclaimed GTR
or its behavior during blending with fresh matrices can be esti-
mated. Moreover, test cost for these parameters is relatively low,
comparing to other more sophisticated methods of reclaimed or
modified GTR characterization.
The presented state of art indicates that the rubber recycling by
suitable grinding and treatment technologies of waste tire rubber
and the characterization techniques of obtained products will
continue to grow in the future.
However, it seems that the most promising routes for further
investigations can be categorized into three main directions. First
route, is grinding, modification, functionalization of ground tire
rubber (or combination of these methods), preferably conducted by
reactive extrusion or high-shearing mixing technologies which
working in continuous manner. This approach allows tailoring
of matrix-GTR interfacial interactions and preparation of novel
rubber recycling based products, which could found application as
reinforcing or semi-reinforcing fillers, bitumen modifiers or engi-
neering materials dedicated for construction and building or
automotive industry.
K. Formela
Second direction for further research should be focused on
quantitative and qualitative characterization of liquid by-products
and volatile organic compounds formed and emitted during devul-
canization, modification or functionalization of ground tire rubber.
Moreover, the impact of above mentioned compounds (some of
them are carcinogenic) on the final product properties and stability
(possible migration of degradation products on surface or evapora-
tion during storage), environment or human health should be also
investigated. Without those data at laboratory scale further imple-
mentation in industry will be very difficult (or even impossible).
Third direction for further investigations about rubber recy-
cling technologies, should dealing with: solutions to convert
promising batch methods of GTR modification to continuous
method. This part should include profitability estimation of such
conversion. Moreover, optimization and up-scaling of laboratory
scale prototype lines dedicated for GTR recycling should be per-
formed in order to verify laboratory results at larger semi-
technical or industrial scale.
Declaration of competing interest
There is no conflict of interest.
Acknowledgements
Financial support of project LIDER/6/0035/L-8/16/NCBR/2017
provided by the National Centre for Research and Development
(NCBR, Poland) is gratefully acknowledged. The author devotes this
paper to the 85-th anniversary of Prof. Stoyko Fakirov with the best
wishes for a good health and further contributions to the polymer
science.
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