Innovative High Performance ACE EPDM polymers

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Drusilla Summers
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1 Innovative High Performance ACE EPDM polymers Gosé van Zandvoort, Global R&D/TS&AD - EPDM LANXESS Business Unit Technical Rubber Products Mobility Days Prague, November 22, 2012

2 Innovative high performance ACE EPDM polymers Introduction New ACE catalyst technology Experimental section Results: - Polymer composition & structure - Mixing and rheometer data - Physical compound properties Conclusions 2

3 New innovations in EPDM production C H 2 C H 2 ethylene H 3 C H C C H 2 propylene Keltan ACE technology diene as termonomer (e.g. ENB) New Catalyst Technology!! Instead of Ziegler-Natta Bio based!! = Keltan ECO EPDM EPM 3

4 Introduction Keltan ACE Technology Showing long-term commitment to the EPDM market Keltan ACE technology is based on a specific family of advanced catalysts licensed from NOVA The technology has been further refined during eight years of catalyst development Various Keltan ACE runs Market being sampled A new catalyst family for EPDM production has been developed and patent-protected by LANXESS Keltan ACE is a key technology to achieve the sustainability vision of LANXESS and an enabler for EPDM capacity expansion projects 2008 Large-scale validation of Keltan ACE technology 2013 Full conversion of biggest EPDM plant in Geleen to ACE 4

Benefits of Keltan ACE technology Sustainability Reduced energy requirement Less pressure on increasingly scarce resources No catalyst waste No deashing

grade slate capability Unique ability to produce the same high quality grades regardless of catalyst technology Product diversification potential Breakthrough

5 Benefits of Keltan ACE technology Sustainability Reduced energy requirement Less pressure on increasingly scarce resources No catalyst waste No deashing necessary, yet lower catalyst residues Chlorine free product Avoidance of chlorine in catalyst system resulting in lower contact corrosion Innovation Full grade slate capability Unique ability to produce the same high quality grades regardless of catalyst technology Product diversification potential Breakthrough for peroxide vulcanized compounds with the High VNB technology platform Enabling reduced peroxide dosage, improved properties or increased compound loading Keltan ACE 5

Objective Polymer Compound Study Over the past years it seemed challenging to achieve excellent Ziegler-Natta like product performance with new (post-)metallocene catalysts Text (16 pt) LANXESS EPDM

6 Objective Polymer Compound Study Over the past years it seemed challenging to achieve excellent Ziegler-Natta like product performance with new (post-)metallocene catalysts Text (16 pt) LANXESS EPDM Production Site in Geleen, The Netherlands Aim of this study - To prove that the Keltan ACE technology is capable to produce a complete range of EPDM polymers with equal properties as their Keltan Ziegler-Natta counter types - To prove that the Keltan ACE technology covers the whole EPDM product range 6

7 Experimental Section Standard product development evaluation Three sets of 2 EPDM polymers were studied Broad selection of Ziegler-Natta products 3 polymers are commercially available and are produced with generic Ziegler-Natta catalyst 3 analogues have been produced with Keltan ACE technology in the pilot plant Polymers were analyzed with FT-IR, GPC and DSC Level of Long Chain Branching (LCB) was measured with DMS The polymers were evaluated in a standard compound, which was mixed with an intermeshing mixer Physical properties were tested on EPDM vulcanizates (Ageing conditions: C (ISO 188) 7

8 Broad selection of Ziegler-Natta products From multi-purpose to high performance Trade Name Polymer Characteristics Application area Polymer 1 Polymer 2 Polymer 3 Keltan 8550 Amorphous Medium ENB Long Chain Branched Keltan 6951 Amorphous Oil extended Very high Mooney Very high ENB Long Chain Branched Keltan 5469 Semi-crystalline Oil extended Extremely high Mol. Weight Fast mixing and extrusion All-round EPDM used in e.g. dense profiles, radiator hoses, window gaskets Good mixing, ultra fast vulcanization and excellent physical properties, like collapse resistance. Best in class for automotive sponge seals Suitable for production of high performance parts and for mechanical goods with high compound Loading 8

9 EPDM Polymer Composition & Structure C2 content adjusted to match the crystallization behavior EPDM Polymer ZN1 ACE1 ZN2 ACE2 ZN3 ACE3 Catalyst system Ziegler- Natta Keltan ACE Ziegler- Natta Keltan ACE Ziegler- Natta Keltan ACE ML (1+4) 125 C [MU] C2 [wt%] ENB [wt%] Oil [wt%] M w /M n [-] Δδ [ ] Cryst.temp. [ C]

10 GPC and Crystallization Curves Polymer ZN1 & ACE1 Perfect match between ZN- and ACE polymer Polymer ZN1 ACE1 M n [kg/mol] M w [kg/mol] M w /M n [-] Polymer ZN1 ACE1 C2 [wt%] Cryst.temp. [ C]

11 DMS and Crystallization Curves Polymer ZN2 ACE2 Perfect match between ZN- and ACE polymer Polymer ZN2 ACE2 Δδ [ ] Polymer ZN2 ACE2 C2 [wt%] Cryst.temp. [ C]

12 Standard Compound Evaluation in a recipe Polymer rich compound oil correction oil-extended grades Ingredient [phr] ZN1 / ACE1 ZN2 / ACE2 ZN3 / ACE3 EPDM ZnO Stearic acid Carbon black N Carbon black N Oil MBTS-80 1,31 1,31 1,31 ZBEC-70 0,7 0,7 0,7 ZDBP-50 3,5 3,5 3,5 Vulkalent E/C 0,5 0,5 0,5 S-80 1,25 1,25 1,25 Total phr 293,26 293,26 323,26 12

13 Mooney, Mooney Scorch and Rheometer Data Curing package does not need adjustment EPDM Polymer ZN1 ACE1 ZN2 ACE2 ZN3 ACE3 ML (1+4) 100 C [MU] Scorch t5 [min] Rheometer data Ts2 [min] T90 [min.] State of cure ΔS MH-ML [dnm]

14 Mixing- Rheometer curves compounds ZN3 & ACE3 Perfect match ZN & ACE-polymer Polymer ZN3 ACE3 ML (1+4) 100 C [MU] Scorch t5 [min] Polymer ZN3 ACE3 Ts2 [min] T90 [min.] MH-ML [dnm]

15 Physical Properties EPDM Vulcanizates Similar crystallinity & similar X-link density Similar properties EPDM Polymer ZN1 ACE1 ZN2 ACE2 ZN3 ACE3 IRHD Hardness [-] M100% [MPa] M300% [MPa] TS [MPa] EB [%] Tear [N] C [%] C [%]

16 Median Tensile Curves for Vulcanizates from ZN3 and ACE3 Perfect match ZN- & ACE-polymer Tensile curves are identical for ZN- and ACEanalogues Again proof that the polymer structure and the crystallinity are very similar for the ZN- and ACE analogues 16

17 Physical Properties for the EPDM Vulcanizates after Aging The effect of heat aging is not negatively affected by the choice of catalyst EPDM Polymer ZN1 ACE1 ZN2 ACE2 ZN3 ACE3 IRHD Hardness [-] Δ IRHD after aging [-] M100% [MPa] M100% after aging [MPa] M300% [MPa] M300% after aging [MPa] TS [MPa] TS after aging [MPa] EB [%] EB after aging [%]

18 ACE high performance polymers Conclusion: Most advanced metallocene production technologies for EPDM have their limitations in Mooney viscosities (20-80 MU) and ENB content (usual<7 wt.%). The Keltan ACE technology covers the entire EPDM product range, including: - Polymers with very high molecular weight (oil extended) - Polymers with very high ENB content up to 9 wt% Keltan ACE technology is capable to produce products identical to their ZN-counter parts with: - Identical physical polymer properties - Identical compound and vulcanizate properties 18

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Ref: 04/2014. Robac SRM102. New Accelerator for Polychloroprene (CR)

Ref: 04/2014. Robac SRM102. New Accelerator for Polychloroprene (CR) Ref: 4/4 Robac SRM New for Polychloroprene (CR) Contents. Introduction to Robac SRM. Benefits of Robac SRM. General Purpose Polychloroprene Masterbatch 4 4. s 4. Rheological Properties.. Mooney Viscosity