Rubber compoundingFormulation of Rubber Compounds Datwyler.pdf · Rubber compoundingFormulation of Rubber Compounds Dr Jakub Kadlcak Manager Material Development Automotive Dr Matthias

Dr Jakub KadlcakManager Material Development Automotive

October, 2nd 2016

Rubber compoundingFormulation of Rubber Compounds

Dr Jakub KadlcakManager Material Development Automotive

Dr Matthias SoddemannHead of Material Development Automotive

RIEG Conference, 7th and 8th December 2016, London, UK

Rubber compounding, October, 2nd 2016 / © Datwyler, www.datwyler.comRubber compounding, October, 2nd 2016 / © Datwyler, www.datwyler.com

Agenda

• Introduction to Datwyler AG

• Problem introduction

• Problem solving

• Conclusions

2 RIEG Conference, 7th and 8th December 2016, London, UK


– STABILITY AND STRENGTH OF A LARGE INDUSTRIAL GROUP

– Swiss origin,

established in 1915– Revenues some CHF

1.200 million– Focused industrial

player with two divisions: Sealing

Solutions & Technical

Components– Listed on the SIX Swiss

Exchange


INTERNATIONAL PRESENCE

WITH MORE THAN 5.800 EMPLOYEES

WORLDWIDE

4

ASIA 41%2.380 EMPLOYEES SALES CHF 136 M

AMERICAS 12%710 EMPLOYEES SALES CHF 124 M

EUROPE 47%2.740 EMPLOYEESSALES CHF 479 M



Employees: 1.700

Revenues: 320 m CHF

Applications:

− Prefilled syringe and cartridge drug deliverysystems

− Medical devices− Elastomeric closures

and aluminum seals

Employees: 3.730

Revenues: 272 m CHF

Applications:

− Brake systems− Fuel and tank systems− CNG and LPG− Exhaust gas treatment− Powertrain, suspension− Thermoplasts and LSR

Employees: 200

Revenues: 100 m CHF

Applications:

− Packaging solutions− Liquid sealing

applications− Customised containers− Capsules

Employees: 200

Revenues: 47 m CHF

Applications:

− Tunnelling− Building construction− Civil infrastructure− Industrial applications− Track superstructure

O-RINGS AND OTHER INDUSTRIAL APPLICATIONS Sealing solutions for machinery and equipment

Health care Automotive Consumer Goods Civil Engineering

4 industrial segments

Datwyler Sealing Solutions


SUPPLIERSUPPLIER

Introduction to the problem

6

Problem: A plant closure of a material supplier


A source of raw

materials, chemicals

Mixing compounds

and production of parts

Assembly of parts

1. A raw material supplier closes its plant – the product at ’’end of life’’

2. A raw material supplier moves production from one place to another

The aim of suppliers is usually to produce a product of the same quality

Not always possible – different environmental/production conditions, a new technology, etc.

CUSTOMER CUSTOMER’S

CUSTOMER


Problem solving

The goal was to prepare compounds based on the new elastomers

that show the same processing and performance properties as the

original compound.

Step one:

– 1:1 exchange of the original elastomer with the other two elastomers

7

Polymer Producer Plant

Original Original Closed

Elastomer 1 Original New

Elastomer 2 Alternative


In this case, an elastomer supplier has moved a production line from one plant

to another all at a very short notice to the customer (less than a year).


– Recipe 1:1 plus polymer exxon plus resultsMaterial phr phr phr

Compound coding X 3606-01 X 3606-02 X 3606-03

Original elastomer 100.0 ---- ----

Elastomer 1 ---- 100.0 ----

Elastomer 2 ---- ---- 100.0

Carbon black

Paraffinic oil

Anti-ageing agents

Vulcanisation activators and accelerators

Peroxide 3.6 3.6 3.6

Compound composition



Rheological properties

9

0

5

10

15

20

25

0 1 2 3 4 5 6

To

rqu

e / d

Nm

Time / min

Characteristic X 3606-01 X 3606-02 X 3606-03

ML 1.39 1.41 1.23

MH 18.60 21.74 17.01

dM 17.21 20.33 15.78

ts2 0.38 0.36 0.40

t30 0.53 0.53 0.57

t70 1.08 1.09 1.18

X 3606-02

X 3606-01

X 3606-03



Physical properties

10

66

69

66

65

66

67

68

69

Microhardness / °IRHD

X 3606-01 X 3606-02 X 3606-03

15.5 15.5

16.4

15.0

15.5

16.0

16.5

Tensile Strength / N/mm2

X 3606-01 X 3606-02 X 3606-03

369

283

376

0

100

200

300

400

Elongation at Brake / %

X 3606-01 X 3606-02 X 3606-03

2.8

3.7

2.9

0.0

1.0

2.0

3.0

4.0

Modulus 100 / N/mm2

X 3606-01 X 3606-02 X 3606-03

8.7

5.2

8.3

0

2

4

6

8

10

Tear Strength / N/mm

X 3606-01 X 3606-02 X 3606-03

14.5

8.7

15.8

0

5

10

15

20

Compression Set 24 h, 130 °C / %

X 3606-01 X 3606-02 X 3606-03

Other characteristics X 3606-01 X 3606-02 X 3606-03

Glass transition (DSC) / °C -54.48 -53.97 -52.97

Density / g/cm3 1.09 1.09 1.09



ENB – ethylidene norbornene

Findings…

– Next to the usual non-conjugated diene ethylidene norbornene (ENB) also a percentage

of another diene has been used during polymerisation causing differences in molecular

structure between original and the new elastomer

– Additional double bonds and consequently creating crosslinks during vulcanisation all

resulting in different properties of the compound compared to the original elastomer



Raw elastomer investigation – Cross-over point

12

1

10

100

1,000

0.001 0.01 0.1 1 10 100

Shear

moduli

G',

G"

/ kP

a

Shear rate / s-1

Series1 Series2 Series3 Series4 Series5 Series6

broadMWD

lowMW

highMW

narrowMWD

Original G’ Original G’’ Elastomer1 G’ Elastomer1 G’’ Elastomer2 G’ Elastomer2 G’’



Raw elastomer investigation – Shear thinning

13

100

1,000

10,000

100,000

1,000,000

0.001 0.01 0.1 1 10 100

Vis

cosity

/ P

a.s

Shear rate / s-1

Series1 Series2 Series3Elastomer 1

1 – 10 s-1

compression moulding

Original Elastomer 2



Compound composition

Step two:

– The adjustment of the vulcanisation system level

14

Material phr phr

Compound coding X 3606-01 X 3606-06

Original elastomer 100.0 ----

Elastomer 1 ---- 100.0

Elastomer 2 ---- ----

Carbon black

Paraffinic oil

Anti-ageing agents

Vulcanisation activators and accelerators

Peroxide 3.6 ↓ ~ 20 %



0

5

10

15

20

25

0 1 2 3 4 5 6

To

rqu

e / d

Nm

Time / min

X 3606-06

Rheological properties

15

Characteristic X 3606-01 X 3606-06 X 3606-03

ML 1.39 1.35 1.23

MH 18.60 18.89 17.01

dM 17.21 17.54 15.78

ts2 0.38 0.40 0.40

t30 0.53 0.55 0.57

t70 1.08 1.13 1.18

X 3606-01

X 3606-03



14.5 13.815.8

0

5

10

15

20

Compression Set 24 h, 130 °C / %

X 3606-01 X 3606-06 X 3606-03

8.7

6.1

8.3

0

2

4

6

8

10

Tear Strength / N/mm

X 3606-01 X 3606-06 X 3606-03

2.8 2.8 2.9

0.0

1.0

2.0

3.0

4.0

Modulus 100 / N/mm2

X 3606-01 X 3606-06 X 3606-03

369 359 376

0

100

200

300

400

Elongation at Brake / %

X 3606-01 X 3606-06 X 3606-03

15.515.3

16.4

15.0

15.5

16.0

16.5

Tensile Strength / N/mm2

X 3606-01 X 3606-06 X 3606-03

66

67

66

65

66

67

68

69

Microhardness / °IRHD

X 3606-01 X 3606-06 X 3606-03

Physical properties

16

Other characteristics X 3606-01 X 3606-06 X 3606-03

Glass transition (DSC) / °C -54.48 -54.00 -52.97

Density / g/cm3 1.09 1.09 1.09



Conclusions

– Elastomers show differences even suppliers declare them to be the same

– Elastomers differ in molecular structure

– Difference in elastomer processing and physical properties

– Adjustment of the compound recipe necessary

– Major deterioration in tear strength even the recipe was adjusted

– The performance of the new elastomer is limited



Endurance test – before

18

Original elastomer Elastomer 1

Under high vacuum



Endurance test – after

19

Original elastomer Elastomer 1

Test OK High wear resulting in leakage.

Test not OK

Higher wear



Acknowledgements

TA Instruments for performing rheological testing.


Thank you

Documents

Rubber compoundingFormulation of Rubber Compounds Datwyler.pdf · Rubber compoundingFormulation of Rubber Compounds Dr Jakub Kadlcak Manager Material Development Automotive Dr Matthias