Rubber Day

Budapest
19. March 2019

High Performance EPDM 1

Agenda

EPDM Basics

EPDM Platforms

Bimodal EPDM Types

New Grades and New Opportunities

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What is EPDM?

▪ E= Ethylene, C2
Typically, between 45 - 80% of the monomer composition by weight
▪ P=Propylene, C3
Disrupts crystallinity of polyethylene segments, inducing elastomeric properties

▪ D= Diene
Diene content typically varies from 0 to 10% by monomer weight

▪ M= polyMethylene backbone
Saturated polymer chain of the poly Methylene type
D
E P

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Designing EPDM products

Basics
o Molecular Weight (MW) ~ Mooney viscosity (20-200)
o Molecular weight distribution (MWD)
o Ethylene content (45 – 80 %)
o Diene type and content (0 – 10 %)Variations
Variations
o Branching
o Ethylene distribution
o Ethylene sequence distribution
o Diene distribution
o Oil extension
Also important
o Physical form (bales, crumbs, granules, bale density)
o Packaging

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 Effects of ...

Increasing MW

Vulcanizate Processing
+ increased tensile/tear strength + increased green strength
+ improved collapse resistance

+ higher filler acceptance

‒ poorer dispersion possible
‒ slower extrusion
‒ poorer calenderability

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 Effects of ...

Narrowing MWD

Vulcanizate Processing
+ increased cure rate/state + increased extrusion rate

+ improved vulcanizate properties + lower die swell

‒ poorer extruder feeding

‒ poorer mill handling
‒ poorer green strength
‒ poorer calendering

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 Mooney Viscosity Measurement

▪ EPDM sample preparation:

• re-massed on mill at 150°C
• uniform film without entrapped process aids for consistency

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 Effects of ...

Increasing Ethylene content

Vulcanizate
+ increased tensile
+ higher hardness
+ improved peroxide cure
‒ poor low temperature set
‒ lower elasticity
Processing
+ increased cold green strength
+ easier palletization
‒ lower hot green strength
‒ more difficult mixing

E P

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 Effects of ...
Increasing Diene content
Vulcanizate
+ faster cure rate
+ improved compression set
+ improved modulus
‒ decreased elongation
‒ decreased heat aging resistance
‒ increased cost
Processing
+ improved contiunuous cure
+ increased flexibility in accelerators
‒ decreased scorch safety
‒ decreased shelf life
D
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EPDM Grade positioning

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Agenda

✔ EPDM Basics

EPDM Platforms

Bimodal EPDM Types

New Grades and New Opportunities

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2 Platforms of EPDM

The conventional Ziegler Natta

catalyst for high MW and high ENB
capability

The metallocene catalyst for new

EPDM grades with enlarged
properties (low ethylene, low MW)

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 EPDM Platforms are complementary

Conventional ZN Metallocene Result

MW / Low (ML= 20 ) to very Very low (ML=5) to max limited low hardness
Mooney high (200+) with oil ML=90 at 125C (no oil and
Viscosity extension extension possible) resilience

MWD Medium to broad and Narrow-mid range, no Limited extrusion

MLRA bimodal, LCB branching processing, requires
blend with broad
MWD
Ethylene From 50 to 80%, random from low (10%) to very Improved low
content with limited propylene high (>80%), non blocky temperature
incorporation sequences compression
set / flexibility
ENB content Up to 11%+ , Limited to 7% (ENB Good high
Other diene possible incorporation), efficient temperature
cure compression set, fast
cure rate / high cure
state
at low diene content 13
 Mooney Viscosity Measurement

▪ EPDM sample preparation:

• re-massed on mill at 150°C
• uniform film without entrapped process aids for consistency

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Agenda

✔ EPDM Basics

✔ EPDM Platforms

Bimodal EPDM Types

New Grades and New Opportunities

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Bimodal EPDM

Bimodal Vistalon combines benefits of narrow and

broad molecular weight distribution (MWD)

• Controlled amount of high MW fraction

• Balances processing and physical properties
• Reduces need of polymer blending

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 EPDM with Bimodal Molecular Weight Distribution

Small molecules act as

Very long molecules are
plasticizer at high shear
effective at low shear
•decrease viscosity
•increase viscosity
•decrease elasticity
•increase elasticity
•key for easy mixing and
•key for collapse resistance
extrusion

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Relaxation Depends on MW, LCB, MWD

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Test Results for Vistalon 8700

Edge defects are enhanced by

narrow MW-Distributions

• variations in compound feeding

• initiation of scorch inside the

extruder due to high compound
viscosity at high sheer

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Agenda

✔ EPDM Basics

✔ EPDM Platforms

✔ Bimodal EPDM Types

New Grades and New Opportunities

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Vistalon EPDM Rubber Grade Slate

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Year 2016 – Vistalon 7700

▪ ExxonMobil’s unique bimodal molecular weight distribution (MWD)

o Easy processability of very high molecular weight VistalonEPDM rubber
o Enables higher filler loading and better filler dispersion
▪ Designed for high performance extrusion compounds
o Higher compound viscosity for low hardness profiles
o Better extrusion consistency and collapse resistance
o Improved elastic properties, such as resiliency / compression set
▪ •Enables cost reduction without sacrificing good physical and set properties

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V7700 Compound Hardness

• Optimum processing window

from 1.2 to 2.2 carbon black to
oil ratio

• Addition of CaCO3 reduces

the compound Mooney viscosity
up to 20 points

• It is a route to enlarge the

processing window at high
carbon black to oil ratio

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Vistalon 7700 EPDM Rubber for Extruded Profiles

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Vistalon EPDM rubber grade slate

Year 2018 – introduction of ultra high-Mooney grade 9600

C2 content Traditional limit

(% wt)
for dry EPDM
Vistalon X9600 Typical values
7001
70 mEPDM Mooney viscosity
Bimodal ZN EPDM ML (1+8) 125°C 1351
5601
ML (2+8) 150°C 92
Ethylene content
57.52
(% wt)
60 X9600 ENB content
8600 7700 ML (1+8) 125 °C 9.0
(% wt)
ML (1+8) 125 °C
7602
8800 MWD Bimodal
7500 8800D
ML (1+8) 125 °C

50
50 70 90 110 130
Mooney viscosity ML (1+4) 125 °C (MU)

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 Vistalon 9600 in Highly Filled Dense Profiles

Formulation phr Physical properties Extrusion Press cure

X9600 100 Hardness, [ShA ] 3" 66 72
N550 CB 180 Modulus 100%, [MPa] 4.0 4.3
CaCO3- Omya BL 80 Tensile strength, [MPa] 9.3 9.7
Flexon 815 oil 110 Elongation at break, [%] 250 265
Struktol 212 3
ZnO 6
Stearic acid 2
Sulfur 80% 0.1 • Compound extruded in a semi-industrial UHF line 3 x 2KW –
CaO 7 250°C hot air oven and also presscured in hot press
PEG 3 • Compound viscosity within typical extrusion range to deliver good
Sulfur cure package 8.4 collapse resistance despite high filler loading
Total 500
• Comparable physical properties of profile and press-cured plaques
Cmp. Mooney Viscosity demonstrate high cure state reached in continuous vulcanization when
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ML(1+4) 100°C [MU] using X9600

• High tensile strength at 500 phr with amorphous grade!

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Mechanical properties – highly filled dense profiles

Hardness, [ShA ] 3"

VW CS (%) 66
94h/70°C Tensile strength
50% defl., 2h (MPa) • 66 ShA compound suitable for dense
cooling, after 61 80 automotive weather seals
5 sec. 9.3
65 7
flat strip
VW TL 52704- • Strong mechanical properties despite high
X9600
B* filler loading (500 phr)
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60 250 250 • Potential to pass demanding VW
Elong. @ compression set tests on profile at high
VW CS (%) 4 break (%)
22h/90°C/50% temperature and after heat aging
defl., 3h cooling
after 5 sec. 6.7
Tear resist. Demonstrate capability to potentially pass VW
(kN/m)
specification with low EPDM content

*selected properties based on Volkswagen TL 52704

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 V9600 in Microdense Profiles

X9600/
Formulation X9600
7001 • EPDM rich formulations (31% polymer)
selected to favor expansion with limited
EPDM 100 50 + 50
amount of blowing agent
Plastomer 10 10
Zinc oxide 4 4 • Two options depending on OEM demands
Stearic acid 1.5 1.5
• Amorphous compound (X9600) for
CB Spheron 5000 110 110
low temperature performance
Flexon 815 oil 60 60
CaCO3 Omya BL 30 30 • Amorphous/crystaline blend (50/50 X9600/7001),
Sulfur 80% 1.5 1.5 for improved mechanical properties
CaO 80% 4 4
Sulfur cure pack 5.6 5.6
• 7001 introduction reduces compound viscosity
OBSH Celogen OT 0.6 0.5
Total (phr) 327.2 327.1

Cmp. Mooney Viscosity

80 70
ML(1+4) 100°C [MU]

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 Mechanical properties – microdense profiles

X9600/
Microdense profiles X9600
7001 • Extruded in a semi-industrial UHF line 3x
Density (g/cm3) 0.96 0.93 2KW - 250°C hot air oven

Hardness [ShA 3"] 57 61 • 19-22% density reduction (= weight

savings) when moving from dense plaque
Modulus 100% [MPa] 3.3 3.2
to microdense profile
Tensile strength [MPa] 8.0 8.1
• ~60 ShA with tensile strength of 8 MPa -
Elongation at break [%] 290 320 meeting typical OEM targets
Compression set
ASTM 22h/70°C/25% defl.
21 32 • 7001 addition generates higher hardness,
tensile strength, tear strength and lower
Tear strength [kN/m] 22.7 26.7 surface roughness
Surface roughness Ri (µm) 2.2 2.0
Potential cost savings up to 6% vs
X9600 high filler dense compound*

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 V9600 in Sponge Profiles

Formulation 8600 X9600

X9600 • High MW EPDM formulations with high
high filler
filler and oil content
EPDM 100 100 100
CB FEF N-550 80 90 105 • Cure pack and blow agent adapted to filler
CaCO3 Omya BL 40 40 50 loading and compound viscosity
Paraffinic oil 70 85 100
Stearic acid 1.5 1.5 1.5
• Mixed in a 20 liter tangential mixer, upside
Zinc oxide active 4 4 4
down, 2 passes
PEG 3350 2 2 2 • Extruded in a semi-industrial UHF line 3x
Calcium oxide 80% 2 2 3 2KW - 250°C hot air oven
Sulfur cure pack 6.7 7.1 7.3
OBSH 2.0 2.5 3.5
Total phr 306 334 376
EPDM % 33% 30% 27%

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 Sponge Profile roperties

Compression set 22h, 100°C, 40%

Density (g/cc) 40

0.54

defl. (%)
0.57
Surface Tensile strength
roughness Ri (MPa)
(µm) 0.63 30
4.7 2.7
8600 X9600 X9600
4.9 6 2.8 High Filler
2.5
EPDM %: 33% 30% 27%

• Option to improve profile properties

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330 with similar EPDM content or
36 • Keep compression set and while reducing
340
EPDM content by 6%
Compression set Elong. @
(22h@100°C, %) break (%)
Potential cost savings up to 9% when
8600 X9600 X9600 High Filler reducing EPDM content by 6%!*
*based on internal value-in-use calculation tool

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V9600 benefits in weather seal applications

The latest developmental V9600 is an amorphous, dry ultra-high Mooney EPDM with
high Diene content for efficient cure in continuous vulcanization

▪ Dense: increase filler loading to 500 phr while potentially meeting typical OEM specifications

▪ Microdense: reduce weight by decreasing profile density

while still meeting main automotive specifications

▪ Sponge: enhance compound properties or

increase filler loading while keeping
finished part properties

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Thank you for your attention!

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Disclaimer

This presentation includes different statements referring to the future

development of the Biesterfeld Group. These statements are based on
assumptions as well as estimations. Although being convinced of our
forecasted statements, we are not able to guarantee the depicted
development.
Our assumptions include risks and uncertainty, which may lead to
deviations between actual and predicted results. It is not intended to
update the forecasted statements presented here. This presentation is
not complete without the oral explanations given.

State: xxx
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Understand EPR

How to cure?
≤ 100°C permanent operation Temperature: Standard Sulfur , EV

≤ 140°C permanent operation Temperature: Sulfur Donor

> 140°C permanent operation Temperature: Sulfur Donor, Peroxide

High elasticity, high resilience: Sulfur (Disulfide)

High temperature, low compression set: Peroxide (only polymeric

plasticizers)

Low temperature flexibility, softness: Sulfur (Polysulfide)

High hardness, strength, less flexing: Sulfur (Monosulfide),

Peroxide

Blooming issues: Rubber Basics 10.3 insoluble Sulfur,

36 add TMQ
09.04.2019 36
Understand EPR

CB Oil Absorption capability

Rubber Basics 10.3 37 09.04.2019 37

Rubber Knowledge

Formulate EPR compounds – design

hardness

NOTE: Also the type of CB is of importance!

Rubber Basics 10.0 EPR - STW 2013 38

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Formulation Guidelines with Application

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