Journal of Cleaner Production 228 (2019) 1048e1061

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Journal of Cleaner Production

journal homepage: www.elsevier.com/locate/jclepro

Ground tire rubber and bitumen with wax and its application in a real
highway
Guilliana Agudelo a, b, Sergio Cifuentes b, Henry A. Colorado a, *
a
CCComposites Laboratory, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín, Colombia
b
Conasfaltos S. A, Medellín, Colombia

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

Article history: This research shows results over the structure-property relation of Ground Tire Rubber (GTR) modified
Received 16 September 2018 after a high shear mixing process using wax as rejuvenator agent in a product under the environmental
Received in revised form and technical regulations. The GTR was used after a milling process which produced a mean particle size
25 April 2019
of 1.19 mm. Bitumen 60/70 type was mixed with the rubber waste at 4000 rpm at 190
C. A set of 15
Accepted 26 April 2019
Available online 29 April 2019
formulations with rubber waste ranging from 10 to 20 wt% were prepared by following the Box-Behnken
experimental design. Gradation tests were conducted over the GTR. Penetration, softening point, elastic
recovering and viscosity tests were conducted over all formulations. Scanning electron microscopy with
Keywords:
Ground tire rubber
energy dispersed spectroscopy was used to analyze the microstructure and the chemical composition of
Bitumen samples. The effects of the main variables and their combinations over the properties have been
Recycling analyzed. Using the desirability criterion, three different formulations were found to follow the speci-
Waste fications, and the best composition of them was the sample with GTR 15 wt%, 40min agitation time, and
Applied research 3 wt% of rejuvenator, with a coefficient of determination of R2 ¼ 0.9924. Results were successfully scaled
up in a large manufacturing process by a road construction company and applied in a heavy traffic road at
Colombia.
© 2019 Elsevier Ltd. All rights reserved.

1. Introduction Bitumen consumption worldwide has been estimated to be 102

Many countries currently face significant environmental issues
derived from an inadequate solid waste management, which has an
important contribution from the improperly handling of used tires.
The use of rubber tire wastes (rubber waste known as ground tire
rubber, GTR) in roads in many places still are not applied, regulated,
and more importantly, adapted and investigated for the particular
materials and environmental conditions of the road need it. On the
other hand, some of the most common problems that occur in
pavements are fatigue cracking, rutting, and the interaction
aggregate-binder, which can decrease the useful life of the pave-
ment and increases the maintenance and operation costs. For this
reason, using GTR in the rods requires research and process opti-
mization, necessary to tailor the characteristics of bitumen with
GTR with different modifiers, additives and process parameters
(Feng and Hu, 2015), (Spechta and Khatchatourian, 2014).
* Corresponding author. Universidad de Antioquia, Facultad de Ingeniería. Bloque
20, Calle 67 No. 53 - 108, Medellín, Colombia.
E-mail address: henry.colorado@udea.edu.co (H.A. Colorado).
million tons per year, from which about 85% is used as binder for
stone based aggregates, 10% in roofs, and 5% in diverse applications
that include waterproofing, adhesives, corrosion protection, and
automobile (Euro Bitumen, 2011). Asphalt concrete has been
extensively used during many years, with issues such as cracking,
intensified by the temperature changes susceptibility, a problem
diminished when different modifiers such as GTR are used (Feng
and Hu, 2015).
In Colombia, more than 53000 tons per month of bitumen is
used in roads (Galvis Ramírez y Cía. S.A., 2015; Munera y
Ossa;_2014). However, there is a poor use of GTR in asphalt for-
mulations, which not only limits its research and development, but
also has a negative impact on the environment, considering the
poor utilization of waste tires (Munera y Ossa;_2014), (Heshmat
et al., 1995). Waste tires can cause very significant problems
worldwide, not only to the environment, but also in to the same
industry due to the ever increasing social and regulation pressure
for making green processes, problems in deteriorating the visual
appearance of the cities, issues related to a more complicated waste
logistics of the used tires, and complications related to the public

https://doi.org/10.1016/j.jclepro.2019.04.353
0959-6526/© 2019 Elsevier Ltd. All rights reserved.
 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061 1049

health (Pachecol, Yining y Said, 2012; Peng et al., 2017). Logistics
issues such as the high cost of the transportation and storage result
in that tires are be badly disposed, and in developing countries, this
can produce problems such as uncontrolled burning of used tires, in
most cases by homeless people trying to extract the steel to be
illegally commercialized. This activity releases hazardous sub-
stances such as CO, SO2, NO2, volatile organics, and hydrocarbons
like aromatic polycyclics, dioxins, furans, and benzene (Andressa F.
et al., 2015; Ali Shah et al., 2013). From several decades, GTR in
bitumen has shown (Feng and Hu, 2015) an improved product in
terms of a higher strength due to a higher viscosity, higher soft-
ening point, better resilient modulus, reduced fatigue, higher
durability, lower maintenance costs for the pavement rods, and not
less important, a less negative impact by the properly use of rubber
derived from tire waste (Feng and Hu, 2015). Although the benefits
of this technology are multiple, the use of GTR in bitumen adversely
increases the final product costs associated with the GTR prepara-
tion and the necessary additives, and also produces an increase in
mechanical strength that need higher processing temperatures and
compaction (Ramírez, 2006).
The first patent for modified asphalt with polymers was devel-
oped in 1843 (Yildirim, 2007, p. 66), widely used right after the end
of the second war world (Zhu et al., 2014). Also used in Europe and
in USA in the 700 s, and China in the 800 s. In 2004, China produced
239 million tons of new tires, generating about 112 millions of tons
of waste (Feng and Hu, 2015); while in 2006 and 2010, the pro-
duction was 280 and 200 millions of tons respectively, ranking first
worldwide (Heitzman, 1992). This negative increase also lead to an
increase in research in China in order to optimize their use of tire
waste in roads.
In Latin-America, several countries have been working in
bitumen blended with tire waste (Villegas et al., 2011), (Martinez y
Avellan, 2011). In general, the procedure began with grinding
rubber particles from tires up to particles size between 800 and
1000 mm, then mixed with bitumen. These mixes look for an
improvement in the elastic behavior, fatigue strength, temperature
susceptibility, and aging strength. Rubber can be incorporated in
the bitumen via both wet and dry methods. In the wet method,
rubber modifies the bitumen and is part of it, while in the dry
method, rubber is part of the aggregates. Depending of the method
and from the raw materials characterization, following the
Colombian Invias regulations (Invias, 2012), rubber particles can be
added in contents between 7 and 15% for the wet method, and
between 2 and 5% for the dry method (Martinez y Avellan, 2011).
These contents reduce not only the need of traditional raw mate-
rials but also improves the bitumen pavements performance (Feng
and Hu, 2015).
Research (Feng and Hu, 2015) with bitumen modified with
ground tire rubber (GTR) has revealed that the improvement in the
pavements depends of diverse factors such as the particle size,
surface of rubber, mixing conditions, binder properties, and the
microstructure of the mix. Additionally, extensive work has been
done by adding polymer additives to rubber-mixes at high tem-
perature (typically between 180 and 200
C) and at high shear
stresses. One of the most used materials is polystyrene-
polybutadiene, which forms a 3D network in the bitumen,
providing beneficial mechanical properties (Rodríguez et al., 2011).
strength; lower maintenance costs by having a more stable
aggregate distribution; and lower the noise contamination coming
from the roads (Heitzman, 1992).
The following investigation is part of a country strategy in
incorporating waste materials in the construction and building
materials (Loaiza, 2017; Loaiza, 2018; Colorado, 2014; Colorado
et al., 2016; Colorado et al., 2016; Revelo, 2019); in nano-
composites (Wei, 2014; Colorado, 2018) and in a circular economy
(Rua-Restrepo, 2019). Particularly this research uses waste rubber
grain introduced by the wet method in asphalt. Due to the limited
workability of these blends because of the high viscosity and
increased costs, this project focuses on the study of various rubber
formulations including the wax agent as a rejuvenator, in order to
achieve formulations economically competitive and with an
acceptable viscosity. The study is centered on the effect of pro-
cessing time, rubber, and wax contents. This project develops
bitumen-rubber mixtures incorporating GTR as an environmental
and economic solution for the reuse of this tire-derived solid waste
solution (Heitzman, 1992) (Gawel et al., 2006). The use of GTR as
pavement component can help to reduce the thickness of the
pavement layers, with a similar or even longer working life when
compared with traditional pavement. The following investigation
shows a methodological development to modify conventional
bitumen with process implemented in a pilot plant using the
manufacturing wet process, which includes catalyzed tests of
rubber incorporation, performance analysis of the obtained
bitumen mixtures and conceptual design of an -rubber production
process. Finally, there was an industrial production of asphalt
concrete with ground tire rubber (GTR) applied on the northern
highway in Medellin, Antioquia.
2. Experimental
2.1. Raw materials
Bitumen grade 60e70 was supplied by the Colombian National
Oil Company (Ecopetrol) as summarized in Table 1. The specifica-
tions for use of ground tire rubber (GTR) are established in the
general specifications for the road construction in Table 2, from the
Colombian National Institute of Roads (Instituto Nacional de Vías,
INVIAS), as INVIAS 2013 Chapter 4.1 (equivalent to ASTM D 6114).
The GTR were obtained as the byproduct of car tires processed by
the Colombian company Ekogroup. The sample for the gradation
tests weighted 300 g and the maximum size used was 1.19 mm
(sieve No. 30), which corresponds to gradation type B. Results are
presented in Table 2.
A rejuvenator wax TB-1 type from Surfax was used to restore the
original properties to aged (or oxidized) bitumen binders by rees-
tablishing the original ratio bitumenenes/maltenes. This additive
helps to decrease the viscosity of the bitumen and to improve the
adherence of the asphalt with the aggregates. Also, sulfur was used
Table 1
Properties of unmodified.
Test Result Requirement Standard

On the other hand, when asphalt is modified with the leftover of Penetration 68 (min 60-max 70) ASTM D5
natural rubber materials (styrene-butadiene-styrene SBS), Viscosity 60
C 200000 cP e ASTM D 4400
Viscosity 135
C 358.3 cP ASTM D 4402
(Rodríguez et al., 2011), increases the elastic recovery (increases in
Viscosity 150
C 173.7 ASTM D 4402
the strength to permanent strain upon high temperature, high load, Ductility 140 cm 100 minimum ASTM D 113
and slow conditions); increases the fracture strength (mostly due to Softening point 47.2
C (min 45, max 55) ASTM D 36
low temperature exposure and impact type loads); increases the Flashpoint 370 (min 232) ASTM D 92
strength to cracking (by the good bonding and swelling of rubber Density 15
1022. kg/m3 ASTM D4062
Mass Loss (RTFOT) 0.28 G/100 g 1.0 maximum ASTM D 4402
particles due to the effect of light elements); increases the fatigue
1050 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061

Table 2 ASTM D-5 standard at 25
C. In Colombia, the INVIAS 2013 standard

Gradation of ground tire rubber (GTR).
Standard Sieve N
8 Nº 10 Nº 16 Nº 30 Nº 50
Sieve (mm) 9.52 4.75 2.00 0.43 0.180
Passing (%) 100 100 100 80.7 30.0
Standard for Type B - 100 65e100 20e100 0e45
Retained weight (g) 0.0 0.0 0.0 58.0 152.0
as cross-linking agent between the polymer and the bitumen,
which has been ground in a ball mill apparatus up to a 0.3 mm
particle size.
2.2. Experimental design
The experimental design followed in this investigation was the
Box-Behnken, see Table 3, which has been successfully utilized as a
practical method to explore multivariable problems with less
design points that other methods. In this design, each factor or
independent variable take equally spaced values, generally as 1, 0,
and 1. For the experiments, the main variables were: the rubber tire
waste content, taken between 10 and 20 wt%; the mixing (agita-
tion) time taken between 40 and 90 min (Onyango et al., 2015); the
wax content, taken between 0 and 3 wt%; and the sulfur content
which was left constant at 0.2 wt% of the bitumen. A total of 15
samples with different materials combination have been manu-
factured. Each sample weighted 2 Kg. The design of experiments
that were carried out has three replicas of the same formulation,
which were included in order to analyze the results.
2.3. Sample fabrication process
The methodology used in this work to obtain bitumen-GTR
mixtures consisted in the modification of the bitumen with a
digestion time of 30 min (Soon-Jae et al., 2007), (Sienkiewicz et al.,
2017). Thereafter, the mixing time was varied according to the
design of experiments proposed: the modified bitumen was mixed
at 4000 rpm (Aflaki and Memarzadeh, 2011) with a paddle stirrer
conducted over a heating plate with temperature control in order to
keep the temperature at 190
C during 40e90 min. The agitation
temperature for the asphalt modified with recycled rubber grain
usually followed is between 180
C and 200
C, which is relatively
high as the rubber grain requires not only higher temperature but
also longer digestion times (Yildirim, 2007, p.66). Therefore, an
intermedium value of 190
C was used in this research, which has
been proved to guarantee a good interaction of the recycled poly-
mer with the asphalt (M. Sienkiewicz, 2017). The rubber tire waste
particles and sulfur were added to the hot mix 30 min before the
mixing process ended. Wax has been introduced to the mix just
10min before the end of the mixing process.
Thereafter, bitumen binder was characterized with penetration
tests at 4 and 25
C with a digital Controls device, following the
Table 3
Experiment design for -rubber blends.
(article 413, table 413-3, Invias, 2013) contemplates the penetration
Nº 200 tests at both at 25
C and 4
C as part of the specifications for a
0.15
modified asphalt cement with recycled rubber grain. In this way,
18.3 this test is required locally as a complementary test to guarantee an
0e5 adequate production and quality control of these type of asphalts
35.0 and because of this, this experiment has been added to this
research.
The asphalt modified with GTR is not stable to storage. After five
days, the components of this asphalt are separated: the polymer
remains in the upper part and the asphalt goes to the lower part.
This is the reason why the solution given by the company (Con-
asfaltos) is producing the mixture immediately the modified
asphalt is produced, and manufacturing just required amount of
material, without the problem of the hot store stability present for
long periods.
2.4. Characterization tests
The softening point has been obtained according to ASTM D-36.
The viscosity (Bitumen Institute, 2007) was tested in a Brookfield
viscometer at 175
C, following the ASTM D-2196. Elastic recovery
in the torsion mode was also measured in an Insoltec apparatus at
25
C. Gradation tests were conducted in a Sieve (mm/U.S. Stan-
dard) gradation apparatus. Table 4 summarizes the conducted tests
for the GTR modified bitumen based on the ASTM specifications.
The rubber content was less than 15% of the total modified bitumen
mass, in order to obtain acceptable properties of the rubber-
bitumen mix.
In order to analyze the powdered GTR waste distribution inside
the bitumen binder, the modified bitumen was deposited on a glass
slide using a regular dropper, and then samples were observed in a
Leica optical microscope. A scanning electron microscope with
energy dispersed spectroscopy (SEM-EDS) type JEOL JSM 6490LV
operated in a high vacuum mode was used to observe in detail the
microstructure and chemical composition. Some samples surfaces
were observed as obtained, while others were fractured after
putting them in liquid nitrogen, and then prepared to the micro-
scope in order to see the internal microstructure. All samples were
mounted on an aluminum stub and gold sputtered with a Hummer
6.2 system, at conditions of 15 mA AC for 30 s, this in order to obtain
a thin film of Au.
With all experimental results, a statistical study was conducted
over the effects that each variable (such as GTR contents, agitation
time, and rejuvenator agent) has on the modified bitumen perfor-
mance. Also, the criterion of desirability was estimated to find the
optimal formulation to be used in a real production plant. Charac-
terization by grade PG was included. Finally, some real tests were
including regarding the application of all these results in a real
large-scale manufacturing highway, carried out by the Colombian
company Conasfaltos S.A. in a heavy traffic street, located at
Medellin, Colombia. Thermal images were taken in order to have
control and to show that the temperature was homogeneous in the
road surface.
3. Analysis and results

Name Factors Units 1 1

Fig. 1 summarizes the ground tire rubber (GTR) classification
A Rubber % 10% 20% used in this research, where the upper and lower limits are the
B Shaking time in high cut min 40 90
maximum and minimum allowed by the standard. The solid curve
C Wax Rejuvenator % 0 3%
is the gradation used.
Factor/Sample 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
Fig. 2 is the scanning electron microscopy (SEM) characteriza-
A 15 20 15 10 10 20 20 10 15 20 15 10 15 15 15 tion for the GTR. The method adopted to process the scrap tires
B 40 65 90 65 40 40 90 90 40 65 90 65 65 65 65 significantly affects the digestion of GTR and the intermediate to
C 0.0 0.0 0.0 0.0 1.5 1.5 1.5 1.5 3.0 3.0 3.0 3.0 1.5 1.5 1.5
high temperature properties of bitumen-rubber waste. The
 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061 1051

Table 4
Rubber modified specifications (ASTM, 2015).

Properties Testing Standard Type of -rubber

Type I Type II Type III

Min Max Min Max Min Max

Apparent viscosity at 175
C (Pa.s) ASTM D-2196 Method A Modified 1.5 5.0 1.5 5.0 1.5 5.0
according ASTM D-6114
Penetration at 25
C, 100 g, 5s (1/10 mm) ASTM D 5 25 75 25 75 50 100
Penetration at 4
C, 200 g, 60s (1/10 mm) ASTM D 5 10 e 15 e 25 e
Softening point (
C) ASTM D 36 57 e 54 e 52 e
Resilience at 25
C (%) ASTM D-5329 25 e 20 e 10 e
Cleveland open cup ignition point (
C) ASTM D 92 230 e 230 e 230 e
Conditioning in thin film test ASTM D 4402
Penetration of residue after conditioning in thin ASTM D 5 75 e 75 e 75 e
film test, % of original penetration

Fig. 1. Gradation curves for the rubber tire waste.
processing method changes the size and shape of rubber particles,
and therefore, changes the surface area of the rubber particles, the
reaction rate, and viscosity (Davide Lo Presti et al., 2012) (Yildirim,
2005).
The low magnification image from Fig. 2a shows whole particles
with different sizes and amorphous shapes from the grinding
process. The particle size was about 1190 mm (1.19 mm). The cut
surface show some unclean borders typical in the cutting process of
elastomers. Fig. 2b shows a detail of a GTR with a cleaner cut. Fig. 2c
and d are higher magnifications with micro-pores and small par-
ticles from the tire. Although some small voids were revealed, the
rubber is in general a compact material with limited bitumen
absorption.
Table 5 is the summary of all mechanical tests conducted over
the modified bitumen samples according to the experimental
design from Table 3, which corresponds to the basic parameters
from ASTM D6114. All tests show results in the required standard
limits, see Table 4, which not only validates the methodology but
also enables the mix to be used in real applications. This has been
obtained as function of the controlled variables and the process
followed: the rubber was added to a hot bitumen, which favors the
bitumen penetration in the particles. This produces that the
estyrene domains of the polymer dissolves, and melt for a better
interaction (Heitzman, 1992). When this happens, the shear stress
over the particles is critical, which contributes to an optimal

Fig. 2. SEM images of rubber waste particles as supplied magnified at a) 50, b) 200, c) 500 and d) 1000.
1052 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061

Table 5
Summary of the main results.

Sample Penetration 25
C (1/10 mm) Softening Point (
C) Elastic Recovery Viscosity (cP) Penetration 4
C (1/10 mm)
%

1 51.13 63.1 51.6 274.86 25

2 42.66 65.1 51.6 469.8 18.95
3 40.06 61 51.6 379.6 23.7
4 41.87 59.5 44.4 277.5 24.7
5 44.82 60.1 40.55 228.1 21.25
6 47.53 67.1 44.44 207.9 18.45
7 45.73 64 43.33 370.3 32.3
8 45.6 58.1 38.33 213.6 24.45
9 54.22 60.1 60.55 233.4 32.5
10 51.86 66.5 57.22 514.5 32
11 48.4 61.1 49.44 348.46 26.15
12 51.11 66.1 38.88 162 24
13 42.8 66.1 44.60 229.73 27.95
14 44.4 58.5 45.7 298.2 30.1
15 44.9 59.1 45.56 297.5 29.4

dispersion of the particles in an adequate time as the mixing speeds
of 4000 rpm.
Bitumen modified with recycled rubber is constituted by two
phases, one formed by small particles of swollen polymer and the
other by bitumen. In the compositions of low polymer concentra-
tion there is a continuous matrix of bitumen in which the GTR is
dispersed; but if the proportion of polymer in the bitumen is
significantly increased, an inversion of phases takes place, the
continuous phase is the swollen polymer and the discontinuous
phase dispersed therein (Heitzman, 1992).
The main effects of the different studied variables (A: rubber, B:
mixing time, C: additive wax as rejuvenator) over the properties
from the different fabricated mixes are summarized in Fig. 3 via
property-factors interaction graphs. These property-factors inter-
action graphs are obtained from the software used for the evalua-
tion of the factors importance (time,% of recycled rubber grain and
wax) and their interactions. Therefore, it is very important to
evaluate in more detail each factor to factor interaction and their
influence in each property (penetration to 25, penetration to 4,
viscosity, elastic recovery and softening point) when taken from the

Fig. 3. Property-factors interaction graphs for a) penetration at 25
C, b) Viscosity, c) Elastic torsional recovery, d) penetration at 4
C, e) softening point, f) Summary of factors and
their corresponding value.
 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061
Fig. 4. Main interactions for a) viscosity, b) penetration at 25
C, c) torsional elastic recovery, and d) penetration at 4
C.
low value (1) to the high value (1). The effects of the factors over
the penetration at 25
C is summarized in Fig. 3a. For the rubber
content interval studied, the penetration increased, and the mix-
tures harden as the rubber content (A) increased (Hainin et al.,
2015). Conversely, the penetration decreased as the agitation time
(B) increased, which suggests that for better penetration, the
agitation time must be kept low. On the other hand, as the additive
content increased, the penetration increased. This result is ex-
pected, since the wax improves the modified bitumen consistency
(Davide Lo Presti et al., 2012), mainly because wax prevents rubber
to absorb oils from bitumen, which is known to improve the
bitumen consistency (Davide Lo Presti et al., 2012). Therefore, the
amount of wax is a critical factor as the excess of these materials
could produce the penetration to be out of the recommended
values from the ASTM 6114.
Fig. 3b shows how viscosity changes with the variables (or
factors) studied (A, B and C, see Fig. 3f. As rubber content increases,
the viscosity increases as well (Putman and Amirkhanian, 2006) in
a linear trend for the interval studied (Mashaan and Karim, 2013).
Viscosity expected to increase with the rubber content as the
bitumen and GTR react, the absorption of aromatic oils from the
bitumen cement increases, the viscosity of the mixture increases,
and the amount of aromatic oils is reduced to lubricate the binder.
The swelling characteristics and adhesion properties of the reacted
GTR also contribute to increase the viscosity (Heitzman, 1992)
(Soon-Jae et al., 2007). The reaction of rubber with bitumen can
cause swelling and softening of these particles as well (Davide Lo
Presti et al., 2012). On the other hand, the viscosity increases and
has a maximum point as the agitation time increases, which can be
associated with depolymerization due to the large processing time
and its corresponding excess in the heating. Viscosity with the
additive content shows a curve with a clear minimum point, and
since the wax softens the bitumen, viscosity decreases (Davide Lo
Presti et al., 2012). Fig. 3c shows how the elastic recovery in-
creases with the rubber content, agitation time, and wax. Since the
bitumen 60/70 used in this research has not elastic recovery, the
addition of rubber significantly changes this to a much better
condition.
The elastic recovery goes up to a maximum value and then de-
creases, which can be associated with a large amount of oil absor-
bed by the rubber (Woo et al., 2007). On the other hand, the elastic
recovery decreases with the increase in the agitation time
1053
monotonically, indicating that for better elastic recovery values, the
mixing time must be low as well. For wax as additive, the elastic
recovery curve is concave, which indicates that using large amount
of wax can lead in a high elastic recovery. A certain degree of elastic
recovery is desirable in pavement to avoid permanent deformation
(Yildirim, 2007).
Fig. 3d shows different parameters effect on the penetration at
4
C, with a peak with the change in the rubber contents (A), which
is associated with the maximum absorbance capacity of oils by
rubber (F. Onyango, 2015). The agitation time (B) also reveals a
nonsymmetrical curve with a maximum point: the penetration is
small for a short and large agitation times. Thus, a mean value in the
agitation time could produce better penetrations (Sienkiewicz
et al., 2017). Penetration has almost a linear trend with the in-
crease in the wax content, which confirms that wax improves the
bitumen consistency (M. Sienkiewicz, 2017).
Fig. 3e shows how the softening point changes with rubber,
agitation time, and additive contents. The softening point increases
as the rubber content increases as well (Hainin et al., 2015), mainly
due to the addition of rubber. The rubber adhesion with the
bitumen is improved with sulfur used as catalyst, giving the
bitumen better resistance to the higher temperature conditions
(Nuha Salim Mashaan*, 2012). Since rubber increases the temper-
ature strength to bitumen, this increase is very significant in the
softening point. Both mixing time and wax contents have very
similar curves, both concave upright, but not have a strong mini-
mum point. This is due to the different interactions that occur
within the mixtures, which give better mechanical properties to the
modified bitumen.
Fig. 4 shows a combination of factors with its interactions
(rubber-time, rubber additive, and time-additive) and their corre-
sponding effects over different properties measured to the modi-
fied bitumen. The combine effects over viscosity are presented in
Fig. 4a. The rubber-time (AB) interaction shows a linear trend in
which viscosity increased as the interaction increased. Rubber (þ)
is more significant over viscosity, although their main interaction is
at low rubber/time contents. For the rubber-wax (AC) interaction, it
is observed an overlap, which is associated with a point of
maximum interaction among the factors and a potential influence
over the viscosity of the mix. When the rubber is increased, vis-
cosity does it as well. As the wax contents increases, the rubber
effect over the viscosity is diminished because it acts as a bitumen
1054 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061

Table 6 since is evident an interaction point, but now with a different trend:
Desirability criteria. while rubber causes an increase (þ), additive wax causes a decrease
A B C (), and therefore the recommended working zone is where the
15% 40 3%
interaction occurred. Finally, additive and time do not show up
interaction as their curves are parallel and independently alter the
penetration at 4
C.
Table 6 shows the results obtained from desirability by the
rejuvenator (Davide Lo Presti et al., 2012). For the time-additive
evaluation in the elastic recovery and the softening point. The
(BC) system, no combined effect was found over the viscosity,
closest value to 1.0 is 0.8818 for the wanted desirability and 0.7908
which is observed from the parallel curves in Fig. 4a.
for the calculated desirability, which means that the mixture that
Fig. 4b shows the effects of the same interactions described
corresponds to these results is one that better fit the guidelines and
before but over the penetration at 25
C. In general it is found that
for which better results are obtained in the evaluated properties.
in the rubber-time interaction (AB) there is no combined effect of
Therefore, in Table 6, the formulation that is closest to the desir-
these two variables on the penetration because these curves are
ability criterion corresponds to the mixture 9.
parallel, which means that each variable affects the property in a
Table 7 shows the regressions and the coefficients found for
determined proportion but its influence has no relation if they are
each test. With the aim of looking for mixtures that gave optimal
combined. In a similar way, to relate the factors rubber-wax (AC)
results, the regressions were square, and the coefficients of
and time-wax (BC), is clear that there is no combined effect on the
penetration, as each variable affects the property indistinctly.
Fig. 4c summarizes the same interactions over the elastic re-
covery in the rubber-time interaction (AB) which shows that there
is no combined effect on the elastic recovery revealed by the par-
allel curves. Fig. 4d shows how some combinations influenced the
penetration at 4
C. By having the rubber-time interaction (AB), it is
evident that these two variables have a relation on the penetration,
since there is an intersection point of interaction: the rubber in-
crease (þ) causes the penetration to increase, but if this variable is
combined with the agitation time, the penetration at 4
C de-
creases. In the interaction rubber-wax (AC), these two variables
have a combined effect in the penetration at 4
C since they have a
point of interaction. However, they have different trends: while the
rubber (þ) causes an increase, the wax () causes a decrease.
Therefore, the acceptable values must be where the interaction was
presented. By relating time-wax (BC), it is evident that the variables
have no relation to the evaluated property since their graphs are
parallel, and these variables change the penetration indiscrimin-
ately at 4
C, but they do not have a relationship between them
when relating the factors rubber-wax (AC). A crossing interaction is
observed in the curves on the elastic recovery, which shows that
there is a point of interaction or effect on the elastic recovery of the
mixture: when increasing the rubber (þ), the elastic recovery in-
creases. However, with a higher amount of wax, the effect the
elastic recovery does not tend to increase. By relating the time-wax
(BC) variables, a crossing point in the elastic recovery is observed,
which shows that there is a point of interaction or effect on the
elastic recovery of the mixture. By increasing the agitation time (þ),
the elastic recovery decreases, however, with the presence of larger
amounts of wax, the elastic recovery increases until reaching a
plateau trend, a saturation value.
Fig. 4d shows the effect of the combined variables over the
penetration at 4
C. In the rubber-time interaction (AB), both var-
iables have a strong relation with penetration: the rubber increase
(þ) causes an increase in the penetration, but if combined with
time, this penetration decreases. The interaction additive (wax)-
rubber (AC) have a combined effect over the penetration at 4
C

Fig. 5. Desirability for a) the wax maximum content (wax of 1), b) mean wax content,
c) mean content of wax (wax of 0), c) for the minimum wax content (wax of 1).
Table 7
Coefficients of determination.
Table 8
Test R2 R2 adjusted Optimal mixtures found by means of desirability.
Penetration 25
C 0.9983 0.9924
Optimized Formulas Type I Type II Type III
Penetration 4
C 0.9918 0.9426
Elastic recovery 0.9841 0.9555 Rubber 15% 19.4% 17.2%
Rotational Viscosity 0.9995 0.9988 Shaking time in high cut 40 50 40
Softening point 0.9905 0.9339 Rejuvenating 3% 3.0% 3.0%
 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061
Fig. 6. Optical microscopy images for 10, 15 and 20-wt % of rubber waste in the bitumen mix.
Fig. 7. SEM images for 10, 15 and 20-wt % of rubber waste in the bitumen mix.
determination R2 and R2 adjusted. Results show that the determi-
nation coefficients for each test are very appropriate, since they are
higher than 0.9, which suggest that the methodology used to
1055
design the mixtures gave optimal results for each evaluated prop-
erty, with acceptable values as specified by the ASTM 6114. In this
Table, three optimal mixtures are presented in order to have points
of comparison.
Fig. 5 summarized the desirability, which must be close to 1 for a
required formulation. In all these curves, the wax content was kept
constant, with values of 1, -1, and 0. Fig. 5a shows the desirability
for a maximum content of wax, in which for a good desirability
value, a middle rubber content and a low agitation time are
required. Fig. 5b resumes results for the desirability with the wax
content in the minimum value, which says that for a good desir-
ability, low rubber content and middle agitation times are required.
Finally, Fig. 5c shows results for a middle wax content, in which for
a good desirability, middle rubber contents and high agitation
times are demanded.
Table 8 shows the three most appropriate formulations, ob-
tained after making the response surface graphs and R2 analyzes.
Three optimal formulations were found able to be implemented on
the roads. An essential characteristic of the three optimal formu-
lations obtained is that they all have a wax content, which shows
that the addition of this material to the bitumen-rubber mixture
promotes the formation of better mixes. This may be due to the
rubber absorption of oils from the wax rather than oils from the
bitumen, preventing the bitumen from being deteriorated as there
is no competition for the oils that the bitumen releases. It is also
important to note that it is not required to have high agitation time,
since it was found that a high value for this parameter can be
positive for some properties but adverse to others. Therefore, the
optimal formulations must be those with mean values for the
agitation time, guaranteeing that there will be no deterioration in
the bitumen-rubber mixes.
Fig. 6 presents optical images for 10, 15, and 20 wt% of GTR waste
in the bitumen mix. In general, a good distribution of the rubber
waste and a good bitumen impregnation over the particles have
been observed. Fig. 7 shows SEM images for 10, 15 and 20 wt % of
rubber waste in the bitumen mix, in all samples presented, rubber
particles are observed with the bitumen binder completely
impregnating them. Even though each sample was cryogenically
treated, it is quite hard to reveal clean particles, which is also an
indirect proof of the good adhesion between the rubber and the
bitumen matrix. Fig. 9 shows compositional maps with carbon,
oxygen and sulfur. The maps clearly shows a patron for the carbon
contents, clearer in the cracks, and darker in the oxygen exposed
asphalt. The opposite can be said for the oxygen contents. Sulfur
contents is also important as the distribution is quite homogeneous
in the full scanned area (see Fig. 8).
The previous results were all scaled up, in the asphalt-based
company Conasfaltos at Medellin-Colombia, with an optimization
process not showed here, but adequate for large scale processing in
a real hot plant. The process is summarized in Fig. 10. The full
manufacturing can be resumed as the preparation of the raw ma-
terials (bitumen and GTR), which were supplied for two different
companies. Then, bitumen was activated, followed by an agitation
1056 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061

Fig. 8. Scanning electron microscopy (SEM), map for spectrum 2.

Fig. 9. Industrial large scale process followed by Conasfaltos in Medellin, Colombia, for the recycling of tire rubber waste in bitumen.

and storage. The large scale agitation unit reveals the scale of the
materials production. A storage hopper and a conveyor belt are
used to move and prepare the aggregates to the mix. Thus, all
materials and bitumen were moved to a mixing plan. Finally, the
final mix is storage.
A set of tests were carried out to guarantee the quality of the
bitumen produced in the plant with results presented in Table 9,
including both raw and modified bitumen, following the procedure
for the design of high performance pavements, PG grade (Sebaaly y
Epps, 2002). With this method, it is concluded that the bitumen
modified with GTR increased its PG performance grade from 64 to
22 to 88-28, having the necessary characteristics to be used in
 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061 1057

Fig. 10. Road paving using the rubber waste mix (MGCR(Mix With Recycled Rubber Grain)-19) at Medellin-Colombia, a) during the application of material mix, b) in-situ tem-
perature evaluation for a), c) other area during the application, d) during the application and d) in-situ temperature evaluation for c).

Table 9
Physico-mechanical Characterization and rheology results for performance grade PG ASTM D-6373.

Test Testing Method Specification Result C/Nc Frequency

Min Max

Penetration at 25
C, 100 g, 5s (1/10 mm) ASTM D 5 25 75 36 C Lot

Softening point (
C) ASTM D 36 54 e 70 C Lot
Apparent viscosity at 175
C (Pa.s) ASTM D-2196 Method A Modified 1.5 5 1.5 C Lot
according ASTM D-6114
Resilience at 25
C (%) ASTM D-5329 20 e 26.3 C Lot
Cleveland open cup ignition point (
C) ASTM D 92 230 e 297 C Monthly
Rheological module G*/send (88
C, 10 rad/s) kPa ASTM D 7175 1.0 e 2.89 C Monthly
Fault temperature (G*/send ¼ 1,0 kPa),
C ASTM D 7175 e e 102.6 e Monthly
Phase angle (88
C, 10 rad/s),
ASTM D 7175 e e 63.3 e Monthly
Loss of mass,%, maximum ASTM D 4402 e 1 0.4 C Monthly
Penetration at 4
C, 200 g, 60s (1/10 mm) ASTM D 5 e e 19.7 e Monthly
Penetration of residue after conditioning in thin film ASTM D 5 75 e 84.2 C Monthly
test, % of original penetration
Rheological module G*/send (88
C, 10 rad/s) kPa ASTM D 2872 2.2 e 5.71 C Monthly
Fault temperature (G*/send ¼ 2,2 kPa),
C ASTM D 2872 64 e 102.3 e Monthly
Phase angle (88
C, 10 rad/s),
ASTM D 2872 e 56.8 e Monthly
Rheological module G*xsend (34
C, 10 rad/s) kPa ASTM D 2872 e 5000 974 C Monthly
Fault temperature (G*xsend ¼ 5000 kPa),
C ASTM D 2872 e e 16 e Monthly
Flexural creep rigidity st (28
C, 60 s), MPa ASTM D 6648 e 300 113.9 C Monthly
Slope m (12
C, 60 s), non-dimensional ASTM D 6648 0.3 e 0.31 C Monthly

Degree of performance original PG 64-22 403A-20-11-2017 Degree of performance 400A-20-11-2017

Modified PG 88-28

Mixing and compaction temperatures

Laboratory temperatures Min Max

Mixing (
C) 169 172
Compaction (
C) 161 163

transit levels "E" (Extremely high designation according to AASHTO
M332-14 standard) (Sebaaly and Epps, 2002), for typical conditions
of traffic level greater than 30 million “equivalent axes” and up to
speeds of less than 20 km/h. At the bottom part of Table 9 are
summarized the mixing and compaction temperatures of the
mixture used for the modified asphalt with GTR. The temperatures
were selected based on the ASTM D2493 standard.
Finally, Fig. 11 shows the application of the developed mix in a
heavy traffic highway at Medellin (Autopista Norte-calzada orien-
tal). Fig. 11a shows workers applying the mix, while Fig. 11b and
d shows the in-situ temperature evaluation, revealing that there is
not significant differences among different areas of the just
1058 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061
Fig. 11. Reaction process of the bitumen with the recycled rubber grain.
manufactured road. Similar good results were obtained for many
other different evaluated sections of the road during the applica-
tion. Fig. 11c shows the mixture applied to one side of the highway
with good appearance and texture.
3.1. Asphalt mix with modified asphalt and with recycled rubber
grain MGCR-19
Design of asphalt mix MGCR-19: based on the requirements of
the INVIAS 467 specification, the asphalt mixture is designed by the
Marshall methodology, with five asphalt percentages ranging from
6.5 to 8.5 and using asphalt mix type MGCR-19 as selection criteria
and with asphalt-rubber type II intended for rolling layer with NT3
traffic level. For these asphalt-rubber contents, asphalt mixtures
were tested, and the theoretical maximum specific weight of the
mixture was determined. The Rice function was also found, which
relates the specific weight to the asphalt. The effective specific
weight of the stone aggregate was determined as well, and the
absorbed asphalt content was calculated. With this value, the
effective percentage of asphalt is finally determined as 7.9%, which
corresponds to an effective asphalt percentage of 6.0%. Table 10
summarizes the design parameters for the optimum percentage
of asphalt-rubber found in this research.
Production of the mix MGCR-19: the preparation of the asphalt
mix with asphalt modified with GCR was conducted in a similar
way to the asphalt mix modified with polymers, following the in-
dications in numeral 450.4.6 of article 450 of INVIAS. The aggre-
gates must be heated before the mixing process with the asphalt-
rubber. The mixture must be homogeneous, with the aggregates
completely wrapped in the asphalt-rubber, avoiding the carbon-
ization of the mixture, overheating, contamination, and humidity.
The mixing temperature of the aggregates with the asphalt-
rubber is established from the viscosity-temperature relationship
curve by the low-cut viscosity (LSV) method using a rotational
viscometer (Asphalt Institute, 2007), and the temperature was also
Table 10
Characteristics obtained for optimum percentage of asphalt-rubber.
Characteristic Reference value
Minimum stability 8250 N
Flow 2,5 - 4,5
Empty with air 3e5
Empty in mineral aggregate >16%
Empty filled with asphalt e 78,3%
Full asphalt/asphalt ratio e 0,88
Thickness of asphalt film >7,5 mm
Susceptibility to TSR Humidity >80%
established from the compaction of the mixture on site, taking into
account that at least an application temperature of 135
C must be
guaranteed. Table 9 shows the mixing and compaction tempera-
tures for the MGCR-19.
4. Discussion
First of all, the process presented in this research is a success
case study from the developing in a lab to a product in large scale
industry, which fulfill completely the regulation of a country in
terms of materials for infrastructure. In addition, it is a success for a
company as well, since changes the way the GTR rubber waste is
being utilized in Colombian roads. Therefore, this project is not only
good from the technical point of view because of all the new data
and statistical analysis presented, but also environmentally,
economically, and socially important, as the tire-based rubber
recycling in Colombian involves thousands of informal workers.
When asphalt cement and GTR are mixed, there is a complex
interaction between these materials: the asphalt-rubber reaction is
affected by complex microstructures of materials and process pa-
rameters. Specifically, the reaction is influenced by factors that
include the temperature at which the fusion reaction occurs, the
processing time at elevated temperature of the mix, the type and
amount of mechanical energy that is applied to the mixture during
the mixing process, the size and the texture of the GTR, and the
aromatic components of the asphalt cement. The temperature,
time, and mixing energy are parameters of the process used to
process the GTR in asphalt. Depending on the selected process,
these parameters can be adjusted in order to achieve the desired
product (Heitzman, 1992), and thus, from the results of the current
investigation, it is concluded that the selected parameter for the
mix design were ideal for the obtained results.
The reaction itself is composed by two simultaneous processes.
On one hand, partial digestion of the rubber in the bitumen. On the
other hand, adsorption of the aromatic oils within the polymer
chains that are the main components of the rubber, both natural
and synthetic (Lo Presti et al., 2012). Natural rubber polymers are
more reactive with asphalt cement than synthetic rubber polymers.
Each group of polymer chains give particular characteristics to the
Design value
modified binder (Heitzman, 1992). The reaction can be understood
11200 N as a hard and dry sponge upon the contact with water: as the
4,5 mm
sponge absorbs water, it swells and softens (Lo Presti et al., 2012).
3,9%
18% The GTR behaves in a similar way: as the GTR reacts with the
asphalt cement, it also swells and softens with the corresponding
consequences for the mix. In addition, the rubber particles that
14 mm have reacted become sticky and the adhesion to the bitumen matrix
86%
improves (Heitzman, 1992). A particle that reacted completely can
 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061
swell 3 to 5 times its original volume (Arizona Department of
Transportation, 1977).
A schematic representation of the phenomena is presented in
Fig. 12, representing the rubber particle interacting with asphalt,
first in the raw materials, see Fig. 12a, and then, the rubber particles
absorbing the bitumen of the oil phase at high temperatures (160-
220
C), see Fig. 12b. During this reaction, there is a simultaneous
reduction in the oil fraction and an increase in the rubber particle
size which decreases the particle-particle distance, see Fig. 12c. The
bitumen is hosted between the polymer chains, which gives a gel
consistency, and thus causes an increase in viscosity up to 10 times
(Lo Presti et al., 2012). When is necessary to stop the reaction, this
can be done by cooling the mix and avoiding an asphalt deterio-
ration. Rubber reacts depending on time and temperature: if tem-
perature is large enough, swelling continues until
depolymerization and even devulcanization can occurs, see
Fig. 12d. Depolimerization starts with the rubber components
released to the liquid asphalt phase, Fig. 12b, which causes a
decrease in the stiffness (G) and changes the asphalt recovery and
resilience. If the processing or reaction temperature is large
enough, or the reaction time is quite large, depolymerization will
continue until the deterioration of the modified asphalt (Lo Presti
et al., 2012).
This work will benefit the study of the modified asphalt with
GTR in Colombia, since a robust design of experiments was fol-
lowed, by means of which response surfaces are obtained and thus
helping to refine the models upon the determination of all impor-
tant factors that affect the mixtures. Therefore, the optimized for-
mulas can be found instead the trial and error process typical in
industry. The advantage of this type of design is that the design
points are placed in the combinations of factors in high, medium
and low levels, which decreases the number of combinations to be
made (Ferreira et al., 2007). The statistical analysis conducted in
this investigation has been derived from the experimental Box-
Behnken results, selected with the aim of a large scale imple-
mentation in the field, and as shown before, it was applied in a real
highway at Medellin, upon a company process optimization. The
experimental design allows a good combination of factors to eval-
uate high, intermediate and low levels parameters, in order to draw
general trends, very useful in the real applications. This design
requires a high level of previous knowledge in the applied field, as
well as experiments that helps in the interval selections. These
ranges were as follows: for rubber from 10 to 20%, for time from 40
to 90 min, and for wax from 0 to 3%, values that have been used by
the company Conasfaltos in many big projects. The experimental
design gives three possible formulations to be replied, which gave
good results as presented above.
The GTR contents, the processing time, and the wax effect,
where analyzed with respect to the bitumen properties. The
optimal results were obtained for a medium rubber particle size, for
a medium value of mixing time, and for a high wax content. These
conditions enable the bitumen-rubber mixes to be used in infra-
structure from Colombia, which was supported by the desirability
criterion with variables in the required range conditions: the rub-
ber content between 15 and 17%, the mixing time between 40 and
50min, and 3% of wax as rejuvenator additive.
The sulfur has been studied (Palma et al., 2016) as part of an
alternate vulcanization process within the modification of the
asphalt with recycled rubber grain, and its contribution is evi-
denced in the positive results obtained in the research presented
here, from the penetration tests, softening point, and elastic re-
covery, when compared with conventional asphalt. Sulfur is known
to react mostly with the naphthenic and aromatic parts of the
asphalt (Elkholy et al., 2018), either binding the molecule, or by its
oxidation, upon the production of hydrogen sulfide. Since the
1059
processing temperature was over 150
C, the oxidation process
could be increased and thus cause an increase in the number of
asphaltenes. The use of the rejuvenator wax TB-1 in the GTR asphalt
produced a decrease in the viscosity of the mix, which helps to
decrease the processing temperatures and reduces the energy
involved in the manufacturing, therefore diminishing the emissions
of greenhouse gases (Súrfax, n.d.). The wax supplier company
recommend to use the additive between 3 and 4%, and upon the
experiment in this research it was found an optimal content of 3% of
wax, keeping in acceptable production costs and ensuring an
adequate viscosity values that enhance the durability of the pumps
and other devices involved in the process. The interaction of asphalt
molecules and wax is quite complex and a modeling is required due
to the complexity of both chemistries, so multiple interaction is
expected. Rejuvenators are mostly light hydrocarbons that decrease
aging in asphalt, in which asphaltenes are increased while other
lighter compounds (nitrogenated and sulphonated parts) are
decreased, limiting the good dispersion of the asphalt components,
(Kim, Mazumder, Lee and Lee, 2018a), (Kim, Mazumder, Lee and
Lee, 2018b).
In terms of the asphalt-wax interaction, three wax types are
typically used in literature: fatty acid amides (FAAs), polyethylene,
and Fischer-Tropsch wax (Reyes Ortíz et al., 2013). Wax is known to
reduce the fabrication temperatures and compaction of the asphalt
mix, and it is used as a coupling agent to improve the rubber-
bitumen interaction (Edwards et al., 2007). Different mechanisms
have been proposed for the asphalt-waxes interaction. Poly-
ethylene wax reacts with asphaltenes, which is the phase respon-
sible for the stiffness of asphalt (Redondo, 2011). Cera Fischer-
Tropsch (F-T) tends to form CeH bonds with the resins, aromatics
and asphaltenes molecules, thus producing the hardening of
asphalt. Fischer-Tropsch wax helps to reduce viscosity as can break
the CeH bonds (Redondo, 2011). The wax used in this research was
FAAs-amide wax, composed of hydrocarbon chains from 16 carbon
atoms bonded by amide groups (Redondo, 2011). This type of wax
increases the steric hardening by segregating the asphaltenes
present in the asphalt to a greater degree producing stiffer asphalts.
This wax has many amide groups, facilitating the interaction with
different heteroatoms present in asphaltenes, which should reduce
the spread of asphaltenes in bitumen by random movements
(Redondo, 2011).
In most countries worldwide there is a huge environmental
issue with the end of life tires besides the effort in developing new
applications for this waste. In 2015, USA and EU collected 4.038.800
and 3.868.000 tires respectively; while in 2016 Colombia collected
45.804 tires (Park et al., 2018). The recovery rates for these regions
(USA, EU, and Colombia) were 48, 28, and 22% respectively. Clearly,
there is a huge problem worldwide, but even more critical in
Colombia and other developing countries due to their poor reuse
and recycling numbers. In Colombia, with the current standard,
Resolucio
n 1236 de 2017 (Sostenible, 2017), the procedures for the
collection and environmental management of used tires now en-
forces companies to properly dispose tires. Nevertheless, the
technology of GTR used is still quite limited in real projects, perhaps
because the political interest in provide environmental solutions
are still not a real priority in the national agenda. Perhaps this
aspect is responsible for the high cost of modified asphalts, since
the cost increases from 2 to 3 times the cost with respect to a
conventional asphalt (60/70). Besides the costs due to the rubber
addition, the PG grade asphalt not only has better performance and
durability (can hold more than 30 million equivalent axes) but also
can operate at higher temperatures and constitutes an environ-
mental friendly solution, which justify by far its use in roads. The
fabrication of 1 ton of asphalt modified with GTR needs between
175 and 194 Kg of GTR, which supports the goal of increasing its use
1060 G. Agudelo et al. / Journal of Cleaner Production 228 (2019) 1048e1061
in these type of mixes, giving an important contribution for having
a better environment and for technical improvement such as the
increase in the asphalt pavement durability.
4.1. Conclusions
o The use of Box-Behnken, as an experimental design method
developed to optimize the results of the evaluated mixtures
provides an ideal formulation for large-scale production in GTR
modified asphalt with 15% recycled rubber grain, 40 min of
agitation time, and 3% wax addition.
o In this research, the optimal formulations were developed with
recycled rubber and with Colombian raw materials showing
better properties than those for the conventional bitumen. This
modified bitumen increased the softening point from 47.2
C to
70
C, which allows its use in higher temperature conditions.
This result evidenced that the asphalt can supports higher
working temperatures. An elastic recovery of 47.18 was also
found, which allows the pavement to retain more loads without
deformation.
o The effect of the wax rejuvenator significantly improved several
properties of the rubber mixture, such as the reduction of the
viscosity to 1.5 P s, which guarantees that the asphalt has the
necessary fluidity for the production of the hot asphalt mixture.
Also, the wax promotes in the process the use of a lower pro-
duction temperature, since the production of asphalt with
rubber grain was achieved in the company's plant at 180
C
(10
C reduction in the production temperature), which gener-
ates less greenhouse gas emissions.
o In terms of the mechanical properties of the samples, the
penetration decreased with the rubber addition, going from 68
(1/10 mm) to 36 (1/10 mm), which translates into a harder
material, with higher compressive strength.
o During the manufacturing and later characterization was
evident that the bitumen particle impregnation was good,
which ensures not only samples but also infrastructure with a
proper -particle interaction, particle distribution and property
homogeneity.
o The utilized rubber particles from this research certainly
contributed to improve the negative environmental impact of
tire rubber waste in Colombia, by using this waste in the roads.
The selected mix was applied in a bitumen road near Medellin
and successfully proved until today. Therefore, the research was
not only important for the company but also for the local
community.
o Considering PG grade classification for asphalts, the modifica-
tion with GCR improves its grade. An asphalt 60/70 has a PG
grade of 64-22, with a JNR ¼ 4.5kPa-1, which can be used in
conditions with traffic standard designation "S" according to the
AASHTO M332-14 standard, which is equivalent to a traffic of
less than 10 million equivalent axes and speeds greater than
70 km/h. While the PG grade of asphalt-rubber is 88-28, with a
JNR ¼ 0.46kPa-1, which can be used in extremely high transit
levels designation "E", for typical conditions of traffic levels
greater than 30 million of equivalent axes and up to speeds of
less than 20 km/h.
o All the trials addressed in this paper showed that the mixtures
made with GCR can meet all the quality parameters established
in both regulations, the Colombian National Institute of Roads
and ASTM regulations.
Acknowledgement
Authors want to acknowledge Prof Mauricio Sanchez from
Department of Chemical Engineering Universidad de Antioquia for
his support during part of this research.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.jclepro.2019.04.353.
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