Use of Recycled Tyre Material in Natural Rubber based Tyre Tread Cap Compound: Part I ...

Use of Recycled Tyre Material in Natural Rubber

based Tyre Tread Cap Compound: Part I (with Ground
Crumb Rubber)
S. Bandyopadhyay*1, S. Dasgupta1, N. Mandal1, S.L. Agrawal1, S.K.
Mandot1, R. Mukhopadhyay1, A.S. Deuri2 and Suresh C. Ameta3
1Hari Shankar Singhania Elastomer and Tyre Research Institute (HASETRI), Jaykaygram,
P.O. Tyre Factory, Rajsamand – 313 342, Rajasthan, India
2R&D Centre, J.K. Tyre, Jaykaygram, P.O. Tyre Factory, Rajsamand, Rajasthan, India

3Department of Chemistry, Mohanlal Sukhadia University, Udaipur – 313 001, Rajasthan, India

Received: 19 November 2004 Accepted: 24 February 2005

ABSTRACT
For both environmental and economic reasons, there is a continuing broad-based
interest in the recycling of scrap rubber and therefore in the development of
recycling technologies. In the present work three different sizes of mechanically
ground Indian crumb rubbers were used in a natural rubber (NR) based tyre
tread cap compound. Varying doses of crumb rubber were used as an additional
compounding ingredient. The minimum torque and Mooney viscosity values
were marginally increased with increasing dose and mesh size of crumb rubber.
In a Rubber Process Analyser (RPA) study, the Payne effect before curing was
marginally higher for compounds containing crumb rubber, while, after curing
a comparable Payne effect was observed with respect to the control compound
without having crumb rubber. A marginal deterioration in tensile strength, fatigue
to failure and abrasion properties was observed. At all levels of usage, the 100
mesh size ground crumb rubber retained the properties better than other lower
mesh size crumb rubbers.

INTRODUCTION
Interest in the recycling of rubber has increased over the last few years, driven
by concern about the effect of scrap tyres and other rubber products on the
environment. Many tyre companies, trade associations, government agencies
and private recycling firms have joined together to solve this problem(1).

1Telefax:+91 2952 232019; e.mail: sbanerjee@ktp.jkmail.com

* Corresponding author

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Though reclaim rubber has been known since the middle of the nineteenth
century, use of recycled rubber materials remained restricted in the tyre industry
for the following reasons(2 ):

• The lack of technologies capable of economically producing a recycled

material of consistent quality.

• The market perception that products containing recycled materials are of

lower quality or value than those made from virgin materials.

• Export Import policies for imported materials for south-east Asian

countries.

• Others like development of Tyre Derived Fuels from scrap tyres.

Grinding rubbers to a granulate or a rubber powder is mainly a tyre matters

because tyres represent about 60 – 70% of all rubber consumed. A wide variety
of ground rubbers is available on the market differing in properties because of
variations in the feed stock, the grinding, and sieving processes, de-ironing,
fibre removal steps and logistics(3).

Hamed et al.(4-7) studied the effect of ground tyre rubber on a styrene butadiene
rubber (SBR) based vulcanisate. Kim and Burford(8) investigated the effect of
powdered rubber as filler on a non-polar rubber - natural rubber (NR), and a
polar rubber – acrylonitrile butadiene rubber (NBR). Deanin and Hashemiolya(9)
studied the compounding of ground tyre rubber with commercial polyolefins
like polypropylene. Osborn(10) investigated the effect of powdered rubber in
thermoplastic elastomers (TPE). Bauman(11) investigated the value of recycled
materials as an engineering product. Naskar et al.(12) studied the characterisation
of ground tyre rubber and its effect on a natural rubber (NR) based compound.
Naskar et al.(13) also modified ground tyre rubber by chlorination and studied its
effect on a plasticised poly vinyl chloride (PVC) compound. Jacob et al.(14-15)
studied the utilisation of powdered ethylene propylene diene modified (EPDM)
scrap rubber in virgin EPDM rubber. Kale and Tipanna(16) have investigated
the effect of ground tyre rubber on a composite of PVC. Grigoryeva et al.(17)
investigated the effect of partially (thermo-chemically) devulcanised ground
tyre rubber on virgin rubbers like styrene butadiene rubber (SBR), synthetic
poly isoprene (IR), poly butadiene rubber (BR) and with their combinations.

The present paper reports the results of studies on the characterisation of

mechanically ground Indian crumb rubbers with different mesh sizes, and their
effect on a tyre tread cap compound based on natural rubber.

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EXPERIMENTAL

Material used
The suppliers of all the materials used in this study are listed in Table 1.

Chemical characterisation
The ground crumb rubber received from the source was sieved by a mechanically
operated sieve shaker that imparted a uniform rotary and tapping motion to
a stack of sieves of steel as per ASTM mesh numbers 20, 30, 35, 40, 60, 80,
100, 120, 140, 170 and 200, in accordance with ASTM D 1511. The mass of
ground crumb rubber retained on each sieve was measured. The mesh size
distribution of the samples is shown in Figure 1.

Table 1. Materials and source

Material Supplier
Sheet Natural rubber, RMA #4 MARDEC International,
Kualalumpur, Malayasia
Block Natural rubber, SMR 20 MARDEC International,
Kualalumpur, Malayasia
40, 80 and 100 mesh crumb rubber The Rubber Reclaim Company,
Sonepat, Haryana, India
Penta chloro pthio phenol (PCTP) based Acmechem Limited, Ankeleshwar,
Peptiser, PEPTIZOL - 7 India
High abrasion furnace black (HAF, N330) Cabot India Ltd., Mumbai, India
Aromatic oil, RPO 701 Sah Petroleum Limited, Daman,
India
Red seal zinc oxide Zinc – O – India, Ltd., Alwar,
Rajasthan, India
Stearic acid Godrej Industries Ltd., Mumbai,
India
Antiozonant 6PPD, PILFLEX 13 NOCIL, Thane, India
Antioxidant TMQ, PILNOX TDQ NOCIL, Thane, India
Rubber makers sulfur (soluble sulfur) Jain Chemicals, Kanpur, India
Accelerator, N-oxy-diethylene benzo pthiazyl NOCIL, Thane, India
sulfenamide, (NOBS), PILCURE MOR
Scorch Inhibitor, N-Cyclo hexyl pthio ICI, Rishra, India
pthalimide, CTP, (Pre-vulcanising inhibitor)
PVI 100, ACCITARD RE

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Figure 1. Mesh size distribution for different mesh size crumb rubbers

Subsequently the ground crumb rubbers were acetone extracted for 16 hours
using an extraction apparatus. After extraction, the rubbers were dried at
105 °C for 2 hours.

The extracted and the unextracted ground crumb rubbers were heated at 40 °C/min
in a nitrogen atmosphere up to 600 °C and up to 850 °C in an oxygen atmosphere
in a thermo-gravimetric analyser (TGA), TGA 7 from M/s Perkin Elmer, USA
in accordance with ASTM D 6370. The weight loss over a specific temperature
range and in a specific atmosphere provided the composition analysis of the
ground crumb rubber. The percent ash content (A) and the percent carbon black
content (B) of the unextracted crumb rubber were determined from the TGA
thermograms. The carbon black and ash percentage thus measured were the
actual carbon black and ash content of the crumb rubber. The percent polymer
content (C) and percent carbon black content (D) of the acetone-extracted samples
were also noted from the TGA thermograms. The percent polymer hydrocarbon
content (RH) of the crumb rubbers was calculated as (RH) = [(C) X (B)/(D)] X
100. The percentage of volatile material (V) in the ground crumb rubber was
calculated from the following equations:

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Volatile % (V) = 100 – [Polymer hydrocarbon % (RH) + carbon black % (B)

+ ash content % (A)]

The TGA results are shown in Table 2.

The semi-quantitative ash analysis was done in accordance with ASTM D

297. The metal content in the HCl soluble ash was determined using an atomic
absorption spectrophotometer, AAS 3300 from M/s Perkin Elmer, USA in
accordance with ASTM D 4075. The ash analysis data are shown in Table 3.

The sulfur content present in the crumb rubbers was determined by means of
an Elemental Analyser, NCS 2500 from M/s Thermoquest, Italy. The sulfur
data obtained are reported in Table 4.

The percentage moisture was determined using a Mettler IR Moisture Analyser

and the data are shown in Table 5.

Table 2. Thermo-gravimetric characterisation of ground crumb rubbers

Test parameter 40 mesh 80 mesh 100 mesh
Polymer content (%) 56.5 55.2 52.5
Carbon black content (%) 25.2 26.8 26.3
Ash content (%) 8.5 9.4 13.0
Volatile content (%) 9.8 8.6 8.2

Table 3. Semi-quantitative ash analysis

Test parameter 40 mesh 80 mesh 100 mesh
Ash at 650 oC (%) 8.5 9.4 13.0
HCl Insoluble (%) 53.3 55.9 64.4
HCl Soluble (%) 46.7 44.1 35.6
Zinc (%) 21.6 15.7 11.3
Iron (%) 1.13 0.30 2.50
Copper (ppm) 95.5 138.3 67.3
Lead (ppm) 220.2 225.1 217.8
Cadmium (ppm) 20.1 16.3 9.83
Manganese (ppm) 69.7 13.8 194.0
Note: All metal content determination was done on the basis of ash only

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Table 4. Determination of sulfur content of ground crumb rubbers

40 mesh 80 mesh 100 mesh

Sulphur (%) 1.59 1.58 1.60

Table 5. Moisture determination of ground crumb rubbers

40 mesh 80 mesh 100 mesh
Moisture (%) 0.40 0.50 0.52

Compound mixing and characterisation

Mixing of the rubber compounds was carried out using a two-wing rotor
laboratory Banbury mixer of 1.5 litre capacity (M/s Stewart Bolling, USA)
in two stages (master batch and final batch) and the formulations are given
in Table 6.

Master batch mixing was done keeping the temperature control unit (TCU) at
90 °C and the rotor speed at 60 rpm. First, the natural rubber was masticated
alongwith the peptiser (PCTP) for 45 s. Then the black, oil, zinc oxide, stearic
acid, crumb rubbers and the anti-degradants (6PPD and TMQ) were added. The
crumb rubbers were added as an additional ingredient in the formulation. The
ram was scraped in between and after an attainment of 0.32 kWh power in the
power integrator (PI), the master batch was dumped. The dump temperature of
the master batches was found to be within 140 – 150 °C.The master batches

Table 6. Tyre tread compound formulations (phr)

Ingredients Mix Id.

Control A B C D E F G H I
40 mesh crumb - 5 10 15 - - - - - -
rubber
80 mesh crumb - - - - 5 10 15 - - -
rubber
100 mesh - - - - - - - 5 10 15
crumb rubber
Other ingredients used in the above formulation and kept at constant loadings
were: RMA # 4-50.0, SMR # 20-50.0, N330 black -48.0, PCTP – 0.10, Aromatic
oil – 8.0, Zinc Oxide – 5.0, Stearic acid – 3.0, 6PPD – 1.5, TMQ – 1.0, Soluble
sulfur – 2.2, NOBS – 0.50 and PVI 100 - 0.15

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were sheeted out in a laboratory two-roll mill. The master batches were further
mixed after a maturation period of 8 h.

For final batch mixing the TCU was kept at 60 °C and rotor speed at 30 rpm.
The earlier prepared master batch was mixed with sulfur, accelerator and
scorch inhibitor. After a ram scraping in between, the batch was dumped at
an attainment of 0.12 kWh power in the power integrator (PI). The dump
temperature of the batches was found to be approximately 95 – 105 °C. The
final batches were also sheeted out in a laboratory two-roll mill.

Rheometric properties
Rheometric properties were determined at 141 °C for 1 h using 0.5° arc in
a moving die rheometer (MDR 2000E) in accordance with ASTM D 5289
and Mooney viscosity, ML (1+4) at 100 °C, was determined in a Mooney
viscometer (MV 2000E) in accordance with ASTM D 1646. Both pieces of
equipment were from Alpha Technologies, USA. The results are reported in
Table 7. The data relating to the rheometric curves obtained in the experiment
are shown in Figure 2a and 2b.

Polymer-filler and filler-filler interaction

Payne effect
The addition of fillers to rubber compounds has a strong impact on the static
and dynamic behaviour of rubber. Besides the strain- independent contribution
of the hydrodynamic effect, the filler-to-rubber interaction and the crosslinking
of the matrix, the dynamic modulus, G* shows also a strong dependency at
low strains i.e. dynamic modulus decreases with increasing strain. This stress
softening at small deformations, also known as the Payne effect, plays an
important role in understanding reinforcement mechanisms in filled rubber
samples, and can be attributed to the breakdown of the filler-filler network,
an indication of the interactions between filler particles(18).

The filler networking or agglomeration of filler particles, which is controlled

mainly by filler-filler interactions in a rubber compound, was quantified
from the strain dependence of the elastic modulus G’. The filler network was
gradually destroyed on increasing the strain (at strains well below 100%). This
resulted in a decrease in elastic modulus G’ with strain amplitude. The ratio of
the elastic modulus G’ at low and high strain levels related to the filler-filler
interactions(19-22).

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Table 7. Rheometric properties
Sample Test Parameter
Minimum Maximum Scorch Time to 40% Time to 50% Optimum Mooney Mooney
torque torque safety time, cure, tc40 cure, tc50 (min) cure time, Scorch Viscosity
(dN-m) (dN-m) ts2 (min) (min) tc90 (min) (min) (MU)
Control 2.40 14.83 12.23 14.79 16.04 25.49 14.89 52
A 2.51 14.51 12.91 15.43 16.70 26.21 15.58 55
B 2.78 14.58 12.34 14.80 16.06 25.54 14.31 59
C 2.67 14.27 12.72 15.09 16.31 25.58 15.45 57
D 2.48 14.11 12.59 15.09 16.37 25.91 15.88 54
S. Bandyopadhyay et al.

E 2.67 14.55 12.12 14.57 15.82 25.12 14.57 59

F 2.72 14.29 12.31 14.77 16.04 25.63 15.51 58
G 2.88 15.24 13.30 16.02 17.35 27.52 15.44 64
H 3.15 15.12 13.14 15.69 16.99 26.82 15.03 70
I 3.35 15.03 12.94 15.44 16.77 26.74 14.81 70

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Figure 2a. Effect of different mesh size crumb rubbers on rheometric

properties

Figure 2b. Effect of different mesh size crumb rubbers on rheometric

properties

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The Payne effect before and after curing was measured using a Rubber Process
Analyzer (RPA2000) from Alpha Technologies, USA. A frequency sweep was
followed by a strain sweep before curing and a strain sweep after curing was
also performed.

The conditions for the Payne effect study are given in Table 8.

All the mixed compounds were conditioned in the RPA2000 at 100 °C, 120 cpm,
0.04 deg strain for 2 min before testing.

Before curing, a rubber compound can attain a higher strain without slippage,
whereas, after curing, the compound will slip at higher strain. A lower frequency
before curing and a higher frequency after curing were used to maintain the shear
rate at 30 s-1 maximum, which is the limit for the RPA 2000 equipment.

The elastic modulus G’ was measured in strain sweep before and after
curing.

The Payne effect before curing (Payne effect-1 and Payne effect-2) was
determined by measuring the difference between G’ values at 0.07 deg and
0.72 deg strain and the ratio of the G’ values at 0.07 deg and 0.72 deg strain
respectively. The Payne effect after curing (Payne effect-3 and Payne effect-4)
was determined by measuring the difference between G’ at 0.08 deg and
1.79 deg strain and the ratio of the G’ values at 0.08 deg and 1.79 deg strain
respectively.

Table 8. Test configuration used in RPA2000 for the Payne effect study
Test configuration Test condition
Temp. Time Frequency Strain
(°C) (min) (cpm) (deg)
Frequency sweep 40 _ 3, 6, 15, 30, 60, 150, 0.72
before curing 300, 600, 1500, 1920
Strain sweep 40 _ 12 0.07, 0.35, 0.72,
before curing 3.59, 7.17, 30.00
Curing 141 60 100 0.50
Strain sweep after 40 _ 600 0.04, 0.05, 0.08,
curing 0.12, 0.18, 0.28,
0.42, 0.63, 0.95,
1.43, 1.79, 2.00

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The elastic modulus G’ in strain sweep before and after curing, along with the
Payne effect for compounds mixed with different mesh sizes of crumb rubber
and the control compound are summarized in Table 9 and Table 10. The Payne
effect before and after curing is shown in Figures 3 and 4.

Table 9. Elastic modulus G’ (MPa) in strain sweep before curing

Strain Control A B C D E F G H I
(Deg.)
0.07 0.46 0.51 0.56 0.52 0.54 0.52 0.51 0.57 0.64 0.61
0.35 0.36 0.39 0.43 0.40 0.42 0.40 0.40 0.44 0.49 0.47
0.72 0.33 0.35 0.38 0.36 0.38 0.37 0.36 0.40 0.44 0.43
3.59 0.19 0.20 0.22 0.21 0.22 0.22 0.22 0.24 0.26 0.26
7.17 0.12 0.12 0.13 0.13 0.13 0.14 0.13 0.15 0.16 0.16
30.00 0.04 0.04 0.05 0.05 0.04 0.08 0.06 0.05 0.06 0.06
Payne 0.13 0.16 0.17 0.16 0.16 0.16 0.15 0.17 0.20 0.18
Effect-1
*Payne 1.40 1.44 1.46 1.43 1.43 1.43 1.42 1.43 1.46 1.43
Effect-2
* Payne Effect-2 is dimensionless

Table 10. Elastic modulus G’ (MPa) in strain sweep after curing

Strain Control A B C D E F G H I
(Deg.)
0.04 2.00 1.92 1.88 1.89 2.04 2.20 2.15 2.22 2.09 2.27
0.05 1.96 1.91 1.84 1.85 2.00 2.17 2.10 2.16 2.07 2.17
0.08 1.81 1.77 1.72 1.72 1.86 2.01 1.92 1.97 1.91 2.01
0.12 1.67 1.64 1.59 1.58 1.73 1.84 1.78 1.83 1.77 1.86
0.18 1.52 1.50 1.46 1.46 1.59 1.67 1.62 1.67 1.62 1.70
0.28 1.39 1.36 1.33 1.32 1.45 1.51 1.49 1.51 1.46 1.53
0.42 1.28 1.24 1.22 1.22 1.33 1.38 1.35 1.37 1.34 1.38
0.63 1.17 1.13 1.11 1.10 1.22 1.27 1.24 1.24 1.22 1.26
0.95 1.04 1.01 0.99 0.98 1.15 1.15 1.14 1.14 1.11 1.13
1.43 0.91 0.88 0.87 0.87 1.08 1.10 1.09 1.07 1.02 1.02
1.79 0.84 0.82 0.81 0.82 0.97 1.00 0.97 0.99 1.04 0.99
2.00 0.81 0.80 0.78 0.79 0.91 0.95 0.93 0.94 0.96 0.96
Payne 0.96 0.95 0.91 0.91 0.88 1.01 0.95 0.98 0.88 1.01
Effect-3
*Payne 2.14 2.15 2.12 2.11 1.90 2.02 1.98 1.99 1.84 2.02
Effect-4
* Payne Effect-4 is dimensionless

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Figure 3. Effect of different mesh size crumb rubbers on Payne effect before
curing

Figure 4. Effect of different mesh size crumb rubbers on Payne effect after
curing

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Volume fraction
For cured rubber vulcanisates, the volume fraction, Vr, of the test specimen in
the swollen state is the preferred way of expressing the amount of the rubber
component present at equilibrium swelling(23). When a crosslinked polymer
is placed in a suitable solvent, the polymer absorbs the solvent and undergoes
swelling to an extent determined mainly by the crosslink density, the nature
of the polymer and the solvent(24).

Volume fraction was also performed to get an indication of apparent crosslink

density. A weighed sample of cured rubber vulcanisate was immersed in
toluene for 48 h at room temperature. Excess solvent was then blotted from
the sample and the swollen weight was measured. The swollen sample was
dried in an oven at 100 °C to constant weight. The dried weight of the sample
was measured after cooling the sample in the desiccator.

The volume fraction, Vr(23-25) of the rubber vulcanisate was calculated using
the following formula:

Vr = [(D – FT)/ρr]/[(D – FT)/ρr + AO/ρs] (1)

where,
D is the weight of the deswollen sample;
F is the weight fraction of the insoluble non-rubber ingredients;
T is the original dry weight of the sample;
Ao is the weight of solvent absorbed;
ρr is the density of the rubber; and
ρs is the density of the solvent

Volume fraction values are given in Table 11.

Physical properties
The green rubber compounds were cured in accordance with ASTM D 3182
in an electrically heated hydraulic curing press using compression moulding.
The moulding conditions followed to cure the compounds were: 141 °C for
45 minutes for the stress-strain and fatigue to failure test (FTFT) and 141 °C
for 1 h for the determination of abrasion loss and rebound resilience.

The tensile properties (including tear strength) were measured using a Zwick
UTM 1445 in accordance with ASTM D 412 and ASTM D 624. The hardness

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was measured with a Shore A Durometer, M/s Prolific Engineers, New Delhi,
India (ASTM D 2240) and with a dead load IRHD tester, M/s H. W. Wallance
and Company Ltd., UK (ASTM D1415). The fatigue to failure properties
(FTFT) at 100% extension ratio were measured in a Monsanto FTFT machine
(ASTM D 4482). The fatigue life was calculated using the Japanese Industrial
Standard (JIS) average method. The abrasion loss at 10 N load was measured
in a Zwick DIN Abrader (ASTM D 5963). In dynamic mechanical property
testing, the values of tan δ at room temperature and 70 °C, at 5% strain level
and at 11 Hz frequency were measured using a Metravib Dynamic Mechanical
Analyser, VA4000 (ASTM D5992). Rebound resilience at room temperature
and 70 °C, was measured using a Zwick Rebound Resilience Tester (SS-ISO
4662).

The tensile and tear specimen was air-aged in a Multicell Ageing Oven from
M/s Tempo Industries, New Delhi, India at 70 °C for 2 weeks.

The results for unaged and aged tensile, hardness and tear specimens, flex to
fatigue properties, tan δ, rebound resilience, volume fraction and abrasion loss
are reported in Table 11.

RESULTS AND DISCUSSION

Mesh size distribution

In sieve analysis, the 40 mesh crumb rubber was found to having major part
of crumb rubber particles retained in the range of 60 – 80 mesh, the 60 mesh
crumb rubber was having maximum particles in the range of 80 – 140 mesh,
whereas, the 100 mesh crumb rubber was having maximum particles in the
range of 100 – 140 mesh.

Thermogravimetric analysis
For all the crumb rubbers, the polymer content was found to be around 53 -
57%, the carbon black content was around 25 - 27% and the volatile content
was around 8 - 10%. The ash content increased with increase in the mesh size of
the crumb rubbers. During the manufacture of crumb rubbers by a mechanical
grinding process, the grinding time is increased to produce a higher mesh
size. This results in the temperature shooting up and softening the crushed
rubber. To counteract this, a silicate clay is added, so that the torque level is
maintained for the grinding process. This may be the reason why a higher ash
content is observed with an increase in the mesh size of the crumb rubbers.

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Table 11. Physical properties

Sample Test Parameter

M100% (MPa) M300% (MPa) TS (MPa) EB (%) Hardness Tear (N/mm)
(IRHD) (Shore A)
Control 1.9 (163) 9.5 (139) 24.9 (76) 591 (70) 61 (+4) 57 (+6) 68 (85)
A 1.9 (158) 9.4 (141) 22.6 (78) 573 (68) 60 (+4) 57 (+6) 64 (91)
B 1.9 (153) 9.4 (134) 22.5 (72) 560 (67) 60 (+3) 58 (+5) 77 (81)
C 1.9 (153) 9.5 (133) 20.4 (70) 515 (65) 60 (+3) 57 (+6) 69 (74)
D 1.9 (158) 9.6 (135) 21.6 (84) 540 (74) 60 (+4) 57 (+6) 72 (72)
E 1.9 (163) 9.6 (136) 21.6 (80) 538 (72) 60 (+5) 57 (+7) 82 (64)
F 2.0 (150) 9.7 (132) 21.7 (77) 532 (73) 61 (+5) 58 (+6) 68 (68)
G 1.9 (147) 9.8 (129) 24.7 (73) 564 (73) 61 (+7) 59 (+7) 65 (82)

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H 1.9 (158) 9.9 (130) 23.6 (75) 565 (71) 62 (+6) 60 (+6) 66 (89)
I 2.0 (155) 10.1 (130) 22.0 (79) 537 (72) 62 (+5) 60 (+6) 77 (73)
Note: Results in parenthesis ( ) are the percentage retention of physical properties after air aging at 70 °C for two weeks. In the case
of hardness, the + values indicate an increase in hardness after ageing
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Table 11. Physical properties continued…
Sample Test Parameter
FTFT (kC) Tan δ Rebound Resilience (%) Volume Fraction Abrasion loss (mm3)
@RT @70 °C @RT @70 °C
Control 89.2 0.218 0.163 49.8 57.0 0.221 132
A 60.0 0.218 0.163 47.4 54.3 0.223 160
B 47.1 0.214 0.165 50.5 56.7 0.226 163
C 54.6 0.212 0.165 49.8 54.6 0.228 172
D 75.4 0.213 0.160 50.2 56.6 0.239 160
S. Bandyopadhyay et al.

E 63.5 0.202 0.151 49.4 56.6 0.243 159

F 56.0 0.210 0.166 49.5 56.2 0.232 163
G 82.5 0.210 0.162 50.1 57.0 0.230 141
H 64.2 0.207 0.155 51.4 58.6 0.243 153
I 50.1 0.209 0.154 47.4 55.5 0.241 149

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 Use of Recycled Tyre Material in Natural Rubber based Tyre Tread Cap Compound: Part I ...

The explanation is also supported by the acid-insoluble data shown in Table 3.

The percentage of acid-insoluble material also increased with an increase in
mesh size of the crumb rubbers.

Semi-quantitative ash analysis

The acid-soluble and insoluble portions of ash both increased with an increase
in the mesh size of crumb rubbers. The acid-soluble part indicated the presence
of zinc metal, whereas, the acid-insoluble part indicated the presence of silica
or silicates. Copper, lead, manganese and cadmium levels were negligible.

Sulfur content
All the crumb rubber samples were found to have much the same levels of
sulfur.

Rheometric properties
Among rheometric properties, the minimum torque and Mooney viscosity values
were slightly increased with increase in dosage and mesh size of crumb rubber.
All other rheometric properties of the compounds containing the different mesh
size crumb rubber were comparable with those of the control compound.

Polymer-filler and filler-filler interaction

The compounds containing different mesh size crumb rubbers before curing
showed a marginally higher Payne effect (which is an indication of more filler
–filler interaction) than the control compound. However, all the compounds
had comparable Payne effects after curing.

Physical properties
Considering the stress - strain properties of the unaged samples, a marginal
deterioration in tensile strength was observed for the compounds containing
crumb rubber. In the case of tear strength and modulus at 100% elongation,
hardly any effect was observed. The stress-strain properties of the aged
samples were not much affected by the presence of crumb rubbers. There was a
significant deterioration in the fatigue to failure (FTFT) and abrasion properties
of the compounds having crumb rubber. The abrasion loss and FTFT were
worst for the compounds containing - 40 mesh crumb rubber. The dynamic
mechanical properties of all the compounds were similar. The rebound resilience
properties of the compounds having crumb rubbers were also comparable to
those of the control compound both at room and at elevated temperatures.

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 S. Bandyopadhyay et al.

The volume fraction of the cured rubber specimen was marginally higher for
the compounds containing crumb rubber than for the control compound. The
crumb rubbers had a significant effect on some of the critical rubber compound
properties and the deterioration in properties increased with the increase in
level of crumb rubbers.

CONCLUSIONS
The use of recycled materials in tyre compounding, in general is not encouraged
for the reason stated earlier in the text. The recent rise in raw material prices and
the greater prominence of environmental issues has now forced the tyre industry
to explore the possibilities of using recycled material along with virgin or as a
complete replacement for virgin rubber. The main hurdle is the availability of the
right grade of recycled material with consistent quality at a competitive price.
In the present experiment, the 100 mesh crumb rubber retained its properties to
a greater extent than those with other lower mesh sizes.

ACKNOWLEDGEMENT
The authors would like to thank HASETRI and JK Tyre Management for kind
permission to publish this work.

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