The Role of Carbon Black on Devulcanization of Natural Rubber by Microwaves

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DOI: http://dx.doi.org/10.1590/1516-1439.004915

The Role of Carbon Black on Devulcanization of Natural Rubber by Microwaves

_Fabiula Danielli Bastos de Sousa_ _a_ - _, Carlos Henrique Scuracchio_ _a_

_aCentro de Engenharia, Modelagem e Ciências Sociais Aplicadas – CECS,_

_Universidade Federal do ABC – UFABC, Santo André, SP, Brazil_

Received: May 5, 2015; Revised: June 11, 2015

One of the greatest problems of the modern society is the recycling of vulcanized elastomers, like
tires and industrial rejects. This work studies one of the techniques of devulcanization of natural rubber
(NR), the devulcanization by microwaves, as well as the influence of the amount of carbon black on
this process through devulcanization of the NR with controlled composition on it. The samples were
analyzed by Soxhlet extraction and some important correlations could be made based on its results and
also by the final temperature of the samples just after the time of exposure to microwaves. The results
highlighted that the increase of the temperature is responsible for the occurrence of devulcanization,
which is dependent on both the amount of carbon black present in the rubber and the time of exposure
to microwaves. These factors can influence its degree of devulcanization, since they are important for
the absorption of energy by the material.

Keywords: _NR, recycling, devulcanization, microwaves_

1. Introduction

Natural rubber (NR) is naturally produced through
bio‑synthesis by the _Hevea brasiliensis_ tree. It is constituted
by approximately 99.99% linear cis-1,4 polyisoprene.
The average molecular weight of polyisoprene in the NR
ranges from 200.000 to 400.000, with a broad distribution.
As a result of this broad molecular weight distribution, NR
has also a good performance during its processing 1 .

To acquire properties like elasticity and damping,
elastomers have to go through a complex process known
as vulcanization; the process in which the elastomers are
mixed with chemicals to reduce their plasticity, tackiness
and sensitivity to heat and cold, as well as to aggregate the
useful properties such as elasticity and mechanical resistance 2 .
This process converts, chemically, independent polymeric
chains of elastomers into a three-dimensional elastic network 1 .
However, while the vulcanization provides improvements in
the properties of the elastomers and, with it, the possibility
of a wide use as consumer goods, it brings difficulties for
recycling after use, once the vulcanized rubber becomes a
thermoset polymer, preventing its subsequent molding into
another product by heating 3 .

Devulcanization is a way of providing energy to destroy,
total or partially, the three-dimensional network formed during
vulcanization 4 . The known methods that use different ways
to promote the devulcanization of rubber include thermomechanical, thermo-chemical and mechano-chemical 5-9,
physical (by microwaves 3,10-20 and ultrasound 21-29 ) and
biochemical 30-33 . All of them involve complex transformations
that lead to depolymerization, oxidation, and in many cases,
the degradation of polymeric chains of rubber, with the
consequent reduction on its viscosity 34 .

The microwave devulcanization is currently one of the
most promising techniques, because the good properties
of the devulcanized material and the possibility of high
productivity. The process takes advantage of volumetric
heating of the material by microwaves, promoting a more
uniform heating than that achieved by more traditional
methods of heating, which depend on conduction and/or
convection 14,15,35 . Materials behave differently when exposed
to an electromagnetic field, like the one generated by
microwaves. In polar materials, molecules or free ions
can create a momentum of dipole, which results in the
volumetric heating throughout the mass of the material.
Elastomers such as NR, ethylene propylene diene monomer
rubber (EPDM) and styrene-butadiene rubber (SBR) have
low microwaves absorption capacity. This limitation can be
overcome by the addition of a conductive filler like carbon
black 36,37, that induces a phenomenon known as MaxwellWagner polarization 13,38 . The process has physical nature,
i.e. it does not involve chemicals during the process and
due to this reason is named ecofriendly 39 . Devulcanization
of elastomers by microwaves shows promising results for
recycling rubber 3,10,12-18,40 .

The main technique of characterization of devulcanized
rubber has been through Soxhlet extraction 41,42 . This technique
is widely mentioned by the literature to detect the status of
devulcanization of elastomers 4,5,14-16,24,31,32,39,41,43-52 . In general,
the content of soluble material (sol) increases with the
increasing of devulcanization degree, due to the breaks of
the cross-linkings and, consequently, the release of these
molecules from the three-dimensional network of vulcanized
rubber. Although the insoluble part (gel) still makes part of
the network, typically the devulcanization process tends
to decrease the cross-linkings density, making even this

il ld bl d b k bl h h i i l

vulcanized rubber 21 . According to Yashin & Isayev 23, as a
result of devulcanization, the rubber contains a significant
amount of sol, that allows the rubber to be reprocessed
and revulcanized in order to obtain a usable material with
reasonably good mechanical properties.

Scuracchio et al. 14,15 studied the characteristics of ground
tire rubber (GTR) after devulcanization by microwaves at
different exposure times. It was noted that, the greater the
exposure time of the sample to microwaves, the greater the
final temperature just after the treatment and, also, the lower
the gel content verified by Soxlhet extraction. In other words,
the higher the time of exposure of the rubber to microwaves,
the higher its degree of devulcanization. Similar results were
obtained by Zanchet et al. 16, who analyzed the devulcanization
of SBR by microwaves. According to the authors, the exposure
time of the sample to the microwaves had a strong influence
on the gel content, since for longer exposure times the material
reached higher temperatures and generated materials with
lower insoluble portion (gel content). A different behavior
was observed by Pistor et al. 13, who analyzed the properties
of EPDM devulcanized by microwaves. For exposure times
until 4 minutes, no significant changes in the gel content
values were observed. Only exposure times to 5 minutes
showed some changes in gel content.

In this work, special attention is paid to the influence
of the carbon black amount present in the NR in the
devulcanization process by microwaves, through the study
of the devulcanization of NR with controlled composition of
carbon black. It is important to bear in mind that the carbon
black in the rubber is the responsible for the heating of these
materials when exposed to microwaves, and the understanding
of the mechanisms that occur during the devulcanization
includes the role of the carbon black during the process.

2. Experimental

_2.1. Materials_

NR with controlled composition of carbon black
(0, 20, 45, 60 and 80 phr) was kindly supplied by IPAB SA.
The carbon black used was type N330 according to ASTM
classification (ASTM D1765-14) 53 . The exact composition
of the samples is not known, except the amount of carbon
black. All composites have the same additives and the same
amount for all the samples; they are vulcanized.

_2.2. Devulcanization of NR_

NR was devulcanized in a system comprised of a
conventional microwave oven adapted with a motorized
stirring system with speed control 14 . The speed of stirring
was set at 40 rpm. The devulcanization process was done by
using the maximum power of the oven (700 W). The time
at which the material was exposed to microwaves ranged
from 2 to 5 minutes. The temperature after devulcanization
was measured by using a rod thermometer.

The nomenclature used in this work is type NRX, where
NR represents the type of rubber used and X represents
the amount of carbon black present in the sample (in phr),
ranged in 0 (NR0), 20 (NR20), 45 (NR45), 60 (NR60) and
80 h ( 80)

_2.3. Characterization_

Granulometric analysis of the samples of NR0 and NR80
was performed according to ASTM D5644-01 [54] .

In order to verify the influence of the amount of
carbon black and the exposure time of NR to microwaves
on devulcanization, gel content of devulcanized NR with
controlled composition of carbon black was analyzed by
performing Soxhlet extraction, by using toluene as solvent.
The extraction time was 24 h and it was performed by using
approximately 5 g of material. After the extraction, the
material and the thimble filter were dried for 24 h at 80 °C
and its mass was measured.

3. Results and Discussion

_3.1. Granulometry_

The granulometric analysis of the NR0 and NR80 is
shown in the Figure 1.

According to the Figure 1, it can be seen that the NR80
has a more refined granulometry in comparison to the
compound NR0. Due to the presence of carbon black in
NR80, rubber was probably more rigid and, thereby, easier to
grind, resulting in a rubber with smaller particle sizes. So, the
higher stiffness promoted by the presence of carbon black
in the vulcanized sample, the easier the grinding process.

However, the difference of the particle sizes (Figure 1) is
supposed not to have a significant effect on the devulcanization
process, since the microwave heating is volumetric and less
dependent on heat conduction.

_3.2. Temperature measurements after treatment_

Temperatures of the NR with controlled composition
of carbon black after the time of exposure to microwaves
are shown in Table 1.

In general, it can be observed the increase of the temperature
of the samples with the increase of the time of exposure
to microwaves, as also observed by other authors 3,14,15,18 .
Besides, it can be verified a trend towards the increase of
the temperature of NR after the treatment as the amount of

carbon black in the rubber got higher. As carbon black is
a conductive filler 13,36,37, it can absorb microwave radiation
and converts this energy into heat 3,18 . So, by increasing the
amount of carbon black in the NR, more microwave energy
is absorbed.

Even in the sample containing no carbon black, heating
was observed, but it was much smaller in comparison to
the samples containing this filler. The heating of the NR0
probably happened due to the presence of some residue of
any other chemical substance used during vulcanization,
since the real composition of the rubber is not known.

_3.3. Gel content_

Table 2 shows the results of Soxhlet extraction of the
samples.

As mentioned before, extraction technique is able
to separate the insoluble fraction of the rubber (known
as gel fraction - vulcanized part) of the soluble fraction
(sol fraction - devulcanized part). So, the gel content is an
index to evaluate the degree of vulcanization of the rubbers 18 .
In general, the higher the sol fraction, the more efficient the
devulcanization process is 5,15,55 .

According to the Table 2, in general, it could be observed
that the gel contend decreased with the increasing of the
exposure time of the NR to microwaves, as well as with the
increasing of carbon black content present in the sample. These
results show that the vulcanized rubbers were devulcanized
by the action of microwaves, and the carbon black acting as a
conductive filler was really efficient, increasing the efficiency
of the process in the samples as its content increases.

It is important to point out that, during heating, the oil
can evaporate when the rubber reaches high temperatures.
As the exact quantity of oil is the one detected for the
untreated sample, the value of the soluble phase can be
even greater than the one obtained through the analysis of
Soxhlet extraction, being that the process has been, in fact,
more efficient. According to Scuracchio et al. 14, the existence
of some part soluble in toluene even for the sample with no

treatment by microwaves is probably due to the presence of
auxiliary process oils in the rubber.

The interaction of charged particles in some materials
with the electric field component of electromagnetic radiation
causes heating on the material 38 . Carbon black presents a
sufficient electrical conductivity to promote this interaction
between the wave and the material 36 . In the case of dielectric
solid materials with charged particles, which are free to move
in a delimited region of the material (such as π-electrons
in carbon black), a current traveling in phase with the
electromagnetic field is induced. As the electrons cannot
couple to the changes of phase of the electric field, heat is
the result of dissipated energy (Maxwell-Wagner effect 56,57 ).

The ability of a microwave absorber material to be
heated in the presence of a microwave field is defined by
its dielectric loss tangent (Equation 1):

tan δ= ε " ε _'_ (1)

The dielectric loss tangent is composed of two parameters,
the dielectric constant (or real permittivity), ε′, and the
dielectric loss factor (or imaginary permittivity), ε″. ε’
quantifies the efficiency with which the electromagnetic
energy is converted to heat 38,58,59 . The tan δ value of carbon
black is between 0.35-0.83 60,61 .

Pistor et al. 12 studied the devulcanization of EPDM by
microwaves and the influence of paraffinic oil in the process.
They observed higher temperatures in the samples without
paraffinic oil due to an increase in carbon black content and
absence of evaporation or degradation of oil. According to
the authors, carbon black has high thermal conductivity and
heat capacity, what permit greater accumulation of internal
energy and a better distribution of energy in the material.
In the same way, some authors analyzed the conductivity
of elastomers or blends based on elastomers containing
carbon black. The conductivity got higher as the amount of
filler present in the samples increased 62-67, especially after

Table 1. Temperatures of the samples immediately after the microwaves treatment.

Exposure time of
NR to microwaves

(min)

Temperature (°C)

NR0 NR20 NR45 NR60 NR80

2 56 66 101 109 166
3 74 94 153 175 244
4 80 117 185 271 250
5 103 138 217 280 307

Table 2. Gel content of the samples of NR with controlled composition of carbon black.

Exposure time of
NR to microwaves

(min)

Gel content (%)

NR0 NR20 NR45 NR60 NR80

0 83.04 80.38 89.52 82.70 80.09
2 79.19 80.31 82.26 79.77 79.66
3 78.43 79.37 79.91 76.74 64.93
4 78.29 78.82 77.71 65.45 59.17
5 77 51 77 84 60 32 53 61 55 09

achieving the percolation threshold, showing its efficiency
as a conductive filler.

The presented results are in agreement with other
authors 3,18,68, who studied the influence of variation of the
carbon black content present in SBR on its devulcanization by
microwaves. According to them, the degree of devulcanization
by microwaves is proportional to the amount of carbon black
on the rubber. In other words, the electrical conductivity of
rubber increases with the increase of the amount of carbon
black due to the higher energy absorbance.

In order to deepen the analysis of the results, Figure 2
presents the correlation between temperature of the samples
after exposure to microwaves and gel content.

From the results presented in the Figure 2, a correlation
between the temperature of the samples just after the
treatment and the gel content obtained by Soxhlet extraction
technique can be seen. In general, the higher the final
temperature of the sample, the smaller its gel content, what
proves that the devulcanization of the rubber was obtained.
Then, the temperature rise is responsible for the occurrence
of devulcanization. According to Hirayama & Saron 18, “the
heating of material, due to the presence of carbon black,
is the main factor that leads to devulcanization, which is
confirmed by an increase in the temperature of the rubber
as a function of carbon black content in the material”.
Based on the results found, it could be concluded that the
time of exposure of the sample to microwaves has also
great value, what can be highlighted from the analysis of
the Figure 3.

According to the Figure 3, it is clear the dependence of
the degree of devulcanization with the time of exposure of
NR to microwaves. The devulcanization process is efficient
from 3 minutes (or more) of exposure to microwaves, and
depending on the content of carbon black present in the
sample, the efficiency level of the process can be improved.

According to some authors 3,18, the degree of devulcanization
(Equation 2) can be calculated by the difference between
gel content of the devulcanized rubber (DR) and the one of
vulcanized rubber (VR).

_Degree of devulcanization_ = −( _DR_ - _VR_ ) (2)

The results of the degree of devulcanization of the NR
with controlled composition of carbon black are showed in
the Figure 4. It is noted, in general, that there is a tendency
of the increase of the degree of devulcanization values
as function of the amount of carbon black present in the
rubber, and as function of the increasing of the exposure
time of NR to microwaves. In addition, according to the
Figures 2 and 3, it could be observed that the relevant
amount of carbon black able to improve the process of
devulcanization by microwaves is from 45 phr. Smaller
quantities seem not to have influence on the process.
According to Paulo et al. 3, the amount of carbon black is
an important factor to achieve a successful recycling by
using devulcanization by microwaves.

As the increase of the final temperature of the compound
is the responsible for devulcanization, the amount of carbon
black and exposure time of the sample to microwaves

bl i i hi h i fl d i h

degree of devulcanization. The final temperature reached
by the sample is the determining factor for the degree of
devulcanization, being dependent on the time of exposure
of the sample to microwaves and the amount of carbon
black present on it.

Figure 2. Gel content _versus_ temperature of the samples after
exposure to microwaves.

Figure 3. Gel content _versus_ amount of carbon black of the samples
after different times of exposure to microwaves.

Figure 4. Degree of devulcanization of the NR with controlled

4. Conclusions

The compound containing carbon black (NR80) was
easily ground and presented a more refined granulometry
in comparison to the compound containing no carbon black
(NR0).

The amount of carbon black present in the rubber, as well
as the time of exposure of NR to microwaves, are able to
influence its devulcanization degree. The temperature of the
NR, immediately after the time of exposure to microwaves,
increased as the amount of carbon black present in the sample,
as well as the time of exposure to microwaves got higher.
As the increase of the temperature is the responsible for the

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