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POLESTAR™ 200R Calcined Clay in EPDM Rubber
T H E A P P L I C A T I O N O F M I N E R A L S C I E N C E
A N O P T I M I S A T I O N O F :
- Filler: Oil Ratio
- Curing Systems
- Processability
- Physical Properties
A Study of Calcined Clay in EPDM Rubber
PoleStar™ 200R calcined clay is commonly used as filler for Ethylene Propylene Terpolymer (EPDM) rubbers in two specific applications – light coloured, extruded profiles and cable insulation.
A study of EPDM rubber has been made in which varying levels of PoleStar™
200R calcined clay (50-300 parts per hundred rubber) and extender oil
(0-100phr) have been incorporated. Mechanical, electrical and processing
properties have been determined. The data shows the way in which these
properties vary with filler and oil levels, and also the effect of vulcanisation
system on these properties.
I N T R O D U C T I O N
The combination of EPDM and PoleStar™ 200R is used in two applications in particular,
namely cable insulation and light coloured extruded rubber profiles. In both applications
physical and processing properties are important and in both process oil, a light paraffinic
oil which extends and aids processing of highly filled EPDM rubbers, are used extensively.
The data published here for both sulphur and peroxide vulcanised compound compares
the properties at various levels of PoleStar™ 200R and process oil additions.
Mechanical, electrical and processing properties are elucidated and tabulated.
E X P E R I M E N T A L
The EPDM rubber used (Vistalon 7602) in this study was selected
because of its general purpose character. The vulcanisation
chemicals were chosen as being representative of materials in
everyday use. Two series of compounds were prepared with
sulphur and peroxide vulcanisation chemicals using standard
mixing procedures. Formulation details are given in Table 1.
Within each series, compounds were varied only in the quantity
of extender oil and calcined clay. Silane coupling agents
(mercapto silane for the sulphur and vinyl silane for peroxide
vulcanised compounds) were added at a constant weight based
on the clay.
Compounds containing no extender oil could not be filled
beyond 200 phr due to the very stiff, unprocessable nature
of this product. Compounds containing 75 phr and 100 phr of
extender oil contained minimum levels of 100 and 200 phr
respectively of calcined clay. Lower additions of filler at these
high oil additions gave compounds that were unprocessable
due to their soft and sticky nature.
Rheological,1 mechanical2,3,4,5, and electrical6 properties were
determined using standard test procedures.
The sulphur vulcanised compounds were vulcanised at 160ºC
for 30 minutes and the peroxide vulcanised compounds for 30
minutes at 170ºC.
The results obtained can be expressed graphically as a
series of property contours in grid denoting filler and oil
additions. The resultant contours are shown in Figures 1-3
for rheological properties and in figures 4-10 for mechanical
properties. Figure 11 shows how compound’s density varies
against level of filler and paraffinic oil. Capicitance change,
Power Factor (Tan δ) and Volume Resistivity after two weeks
in water at 75°C, are abulated Tables IV and VI.
Sulphur Vulcanised EPDM
PeroxideVulcanised EPDM
Vistalon 7602 100 100
Zinc Oxide 5 5
Stearic Acid 1 1
TMQ - 1.5
Sulphur 1.5 -
TMTD 0.5 -
MBT 1.5 -
ZDC 0.5 -
Perkadox 1440 - 7
Aktivator TAC/S - 2
Sunpar 2280 Variable Variable
PoleStar™ 200R Variable Variable
MercaptoSilane 2% on Clay Weight -
VinylSilane - 1% on Clay Weight
T A B L E I
Process Oil (Sunpar 2280) phr
0 25 50 75 100
50 √ √ √ - -
100 √ √ √ √ -
PoleStar™ 200R (phr) 150 √ √ √ √ -
200 √ √ √ √ √
250 - √ √ √ √
300 - √ √ √ √
Process Oil (Sunpar 2280) phr
0 25 50 75 100
50 √ √ √ - -
100 √ √ √ √ -
PoleStar™ 200R (phr) 150 √ √ √ √ -
200 √ √ √ √ √
250 - √ √ √ √
300 - √ √ √ √
350 - √ √ √ √
T A B L E 2 : S U L P H U R V U L C A N I S E D C O M P O U N D S - T O TA L L E V E L S ( P H R ) O F P R O C E S S O I L A N D P O L E S TA R ™ 2 0 0 R
TA B L E 3 : P E R O X I D E V U L C A N I S E D C O M P O U N D S - T O TA L L E V E L S ( P H R ) O F P R O C E S S O I L A N D P O L E S TA R ™ 2 0 0 R
D I S C U S S I O N
The property contours produced in this investigation show
very clearly the way in which properties change with varying
filler and oil levels. Most properties change in a predictable
fashion. For example, hardness increases with increasing
levels of filler and decreasing
with increasing levels of oil. Some properties such as tear
strength pass through definite maxima at specific oil or filler
levels. Acceptance levels for these properties vary with the
application and are specified by the end user according to the
product requirements.
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
6
5
4
32
FIGURE 1A: T2
(MINUTES)
SULPHUR VULCANISED (160°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
3
5
10
15
FIGURE 2A: MAXIMUM TORQUE ( INCH LBF)
SULPHUR VULCANISED (160°C)
PEROXIDE VULCANISED (170°C)
FIGURE 1B: T2
(MINUTES)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)Filler (phr)
6
5
4
3
2
FIGURE 2B: MAXIMUM TORQUE ( INCH LBF)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
3
5
10
PEROXIDE VULCANISED (170°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
20
40
60
FIGURE 3A: MINIMUM TORQUE ( INCH LBF)
SULPHUR VULCANISED (160°C)
FIGURE 3B: MINIMUM TORQUE ( INCH LBF)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
20
40
60
80
PEROXIDE VULCANISED (170°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
30
25
20
FIGURE 6A: COMPRESSION SET (%) (70°C)
SULPHUR VULCANISED (30 MIN AT 160°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
30 40
50 60
70
80
FIGURE 5A: TEAR STRENGTH (N)
SULPHUR VULCANISED (30 MIN AT 160°C)
FIGURE 6B: COMPRESSION SET AT -70°C (%)
PEROXIDE VULCANISED (30 MIN AT 170°C)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
30
20
10
5
FIGURE 5B: TEAR STRENGTH (N)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
30
5404
50
55
PEROXIDE VULCANISED (30 MIN AT 170°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
7
8
9
10
11
12
FIGURE 4A: TENSILE STRENGTH (MPa)
SULPHUR VULCANISED (30 MIN AT 160°C)
FIGURE 4B: TENSILE STRENGTH (MPa)
PEROXIDE VULCANISED (30 MIN AT 170°C)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)Filler (phr)
5
7
10
12
The study also shows some of the differences between
sulphur and peroxide vulcanised compounds, the most
significant being tear strength and compression set.
Peroxide formed crosslinks take the form of
carbon-carbon interchain linkages whereas
sulphur derived crosslinks take the form
of mono or polysulphide bridges.
The carbon-carbon linkages are thermally very
stable (unlike polysulphide bridges) but do not
allow sufficient molecular mobility to distribute
evenly mechanical stresses as do the longer sulphur
bridges. As a result the tear strength of peroxide
crosslinked compounds are very much lower than
the sulphur vulcanised equivalents. For the same
reasons compression set properties (Figure 10B)
of peroxide crosslinked compounds are very much
lower than their sulphur vulcanised equivalents
(Figure 10A) despite being tested under more
severe conditions (120ºC compared with 100ºC).
In this report the electrical properties of sulphur
vulcanised compounds were found to be superior
to those obtained for the peroxide vulcanised
material. The peroxide vulcanised compounds
utilised only 1% vinyl silane which may be slightly
below the optimum level for this application.
Two areas of poor processability have already been
identified because of the impracticality of producing
compounds - those containing either low oil plus high
filler contents or high oil plus low filler contents.
The results presented in this report can be used by the
rubber compounder as a basis for practical formulations.
Levels of filler and process oil can be selected in
conjunction with method of vulcanisation to give
specific mechanical and processing properties. The
properties can also be changed by crosslinking chemicals
used and type of EPDM polymer used. Selection of these
compounding variables will be governed by individual
specific requirements of each enduser who will need to
consider parameters outside the scope of this report
such as product type and specifications and local
processing conditions.
C O N D I T I O N S
The data produced in this study shows the way in which
the properties of both sulphur and peroxide vulcanised
EPDM change as PoleStar™ 200R and process oil levels
change. The information provides a compounder with
information on which practical compounds can be based
in order to:
a) Select filler, oil and vulcanisation chemicals to meet
specific requirements in terms of mechanical,
electrical and processing properties.
b) Utilise maximum levels of filler and oil in order to
optimise cost and performance.
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
2
4
6
8
10
FIGURE 9A: MODULUS AT 100% (MPa)
SULPHUR VULCANISED (30 MIN AT 160°C)
FIGURE 9B: MODULUS AT 100% (MPa)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
2
4
6
8
PEROXIDE VULCANISED (30 MIN AT 170°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
300
200
500 400
FIGURE 8A: ELONGATION AT BREAK (%)
SULPHUR VULCANISED (30 MIN AT 160°C)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
500 400 300
200
100
PEROXIDE VULCANISED (30 MIN AT 170°C)
FIGURE 8B: ELONGATION AT BREAK (%)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
50 60
70
80
90
FIGURE 7A: HARDNESS (Shore A)
SULPHUR VULCANISED (30 MIN AT 160°C)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
40 5060
70
80
90
FIGURE 7B: HARDNESS (SHORE A)
PEROXIDE VULCANISED (30 MIN AT 170°C)
Sulphur Vulcanised Oil (phr)
0 25 50 75 100
50 1-14d7-14d
0.80
0.80
1.60.5
- -
100 1-14d7-14d
0.50.5
1.2 0.1
3.1 0.5
0.7 0
-
PoleStar™ 200R (phr) 150 1-14d 2.0 7-14d
1.1 1.2
1.6 0.4
0.8 0.4
- 0
200 1-14d7-14d
1.8 1.2
1.6 1.0
1.3 0
0.8 0
1.0 0.1
250 1-14d7-14d
- 1.6 0.5
1.8 0
0.2 0
1.3 0
300 1-14d7-14d
- 1.8 0.8
1.0 0
1.0 0
0.9 0
Peroxide Vulcanised Oil (phr)
0 25 50 75 100
50 1-14d7-14d
6.5 3.4
4.4 1.1
4.5 0.8
- -
100 1-14d7-14d
4.8 1.0
4.7 1.7
3.1 1.2
8.3 1.2
-
PoleStar™ 200R (phr) 150 1-14d7-14d
6.8 1.7
4.0 1.4
5.4 2.
8.2 2.8
-
200 1-14d7-14d
7.9 1.0
6.3 1.7
6.6 0.7
9.1 0
8.9 4.5
250 1-14d7-14d
- 6.7 0.2
7.7 0.2
7.2 1.1
7.1 4.8
300 1-14d7-14d
- 13.2 1.8
9.4 3.1
7.9 0.9
7.2 3.9
350 1-14d7-14d
- - - 9.2 2.0
8.0 5.3
TA B L E 4 : C A P A C I TA N C E C H A N G E ( % ) - A G E D 1 4 D A Y S I N WA T E R A T 7 5 ° C - 3 2 0 0 V / m m
Sulphur Vulcanised Oil (phr)
0 25 50 75 100
50 0.004 0.005 0.003 - -
100 0.006 0.007 0.004 0.004 -
PoleStar™ 200R (phr) 150 0.007 0.008 0.005 0.004 -
200 0.007 0.008 0.005 0.005 0.005
250 - 0.008 0.006 0.006 0.005
300 - 0.008 0.007 0.006 0.006
Peroxide Vulcanised Oil (phr)
0 25 50 75 100
50 0.017 0.012 0.008 - -
100 0.014 0.010 0.009 0.016 -
PoleStar™ 200R (phr) 150 0.017 0.012 0.008 0.010 -
200 0.020 0.014 0.009 0.008 0.019
250 - 0.016 0.015 0.008 0.012
300 - 0.024 0.016 0.009 0.012
350 - - - 0.014 0.012
TA B L E 5 : TA N δ - A F T E R 1 4 D A Y S I N WA T E R A T 7 5 ° C ( 3 2 0 0 V / m m )
Sulphur Vulcanised Oil (phr)
0 25 50 75 100
50 17 9 27 - -
100 14 8 14 10 -
PoleStar™ 200R (phr) 150 5 9 14 7 -
200 19 6 7 7 6
250 - 7 5 7 5
300 - 2 5 5 4
Peroxide Vulcanised Oil (phr)
0 25 50 75 100
50 12 12 10.5 - -
100 9.1 6.0 7.0 5.3 -
PoleStar™ 200R (phr) 150 4.9 6.7 7.3 5.2 -
200 2.9 7.2 6.4 3.5 3.0
250 - 3.8 13.2 5.7 3.0
300 - 2.5 3.1 3.9 3.7
350 - - - 3.2 2.2
TA B L E 6 : V O L U M E R E S I S T I V I T Y - A F T E R 1 4 D A Y S I N WA T E R A T 7 5 ° C U N I T S O H M . C M X 1 0 1 4
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
1.2 1.3 1.4 1.5
1.6
F IGURE 11: SPECIFIC GRAVITY
PEROXIDE VULCANISED (30 MIN AT 170°C)
100
75
50
25
050 100 150 200 250 300
Oil
(phr
)
Filler (phr)
70
60
50
40
FIGURE 10A: COMPRESSION SET AT 100°C (%)
SULPHUR VULCANISED (30 MIN AT 160°C)
FIGURE 10B: COMPRESSION SET AT 120°C (%)
100
75
50
25
050 100 150 200 250 300 350
Oil
(phr
)
Filler (phr)
30
20
10
PEROXIDE VULCANISED (30 MIN AT 170°C) R E F E R E N C E S
1. B.S. 1637 Part 10. Measurement of prevulcanising
and curing characteristics by means of curemeters.
2. ISO 34 and B.S. 903 Part A2.
Determination of Tensile Stress-Strain Properties.
3. ISO 34 and B.S. 903 Part A3.
Determination of Tear Strength.
4. B.S. 903 Part A6. Determination of Compression Set.
5. ISO 48 and B.S. Part A7.
Determination of Hardness.
6. K M Beazley and L E Cook, Transactions of the Institute
of the Rubber Industry, Vol. 38, No. 5.
7. ASTM-D 2230-68. Extrudability of unvulcanised
Elastomeric Compounds.
The information contained herein was obtained as a
result of work carried out on materials thought to be
representative of normal production using both IMERYS
and ISO standard procedures. Accordingly, the data are
believed to be correct.
Such information shall not, however constitute any
representation, condition or warranty as to any fact
contained herein, and accordingly IMERYS Minerals Ltd
hereby disclaims all and any liability arising from
the use of such information howsoever caused.
UKP/R006 - SECOND EDITION - 07/19
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