MPG 2016 Bespoke compound. used in extreme environments. Clwyd Compounders Ltd.

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1 MPG 2016 Bespoke compound engineering for elastomers used in extreme environments Clwyd Compounders Ltd.

2 Introduction Challenging service conditions and engineering specifications are now more prevalent Analysis of processing and service requirements plus innovative compounding gives the best chance of success We will showcase some compounds designed for extreme service conditions look at tested properties and performance in ED tests Discuss difficulties facing compounders today as tougher requirements call for engineering solutions. Also discuss a novel sealing solution and the associated rubber technology

3 Developing compounds for enhanced oil recovery Component service conditions are becoming increasingly challenging particularly in oil & gas industry Exposure to CH 4, CO 2, steam and sour conditions (H 2 S) at high temperature and pressure Material which passes engineering specification and industry-standard explosive decompression (ED) testing may be difficult to mould, leading to defects in finished components

4 Screening experiments : compounds for enhanced oil recovery Screening experiments on a range of compound types produced by Clwyd Compounders, which included: HNBR Aflas (TFE/P) various subtypes of FKM FFKM Tested steam resistance, resistance to sour conditions (H 2 S) and rapid gas decompression (RGD) resistance Test Pressure Temperature (ºC) Test type medium (bar) CO RGD (1 cycle) using 312 O-rings Steam wks ageing, then tensile testing 65% H 2 S/ wks ageing, then tensile testing 35% CO 2

5 Screening test results: compounds for enhanced oil recovery Viton ETP 90, Aflas 90 and High fluorine FKM (type 2) compounds gave best results for chemical resistance against steam and sour conditions Best results for RGD resistance were obtained from a compound containing a specific specialist filler system Formulations were further refined by using a specialist filler system in revised versions of chemically resistant compounds Material description Aflas 90 FKM High Fluorine 90 ETP 90 Aflas 80 Comments Designedfor ED resistance,good steam and H 2 S resistance Designedfor non-sourenvironment at high temperatures and improved ED resistance Designedfor good ED resistance, steam and H 2 S resistance at high temperatures Designedfor ED resistance,good steam and H 2 S resistance with high E@B

6 Test results on refined compounds Aflas 90 FKM High Fluorine 90 ETP 90 Aflas 80 Hardness (IRHD) TS (MPa) B (%) % (MPa) % (MPa) Tear strength (N/mm) Compressionset (%) 22 h at 200 ºC Heat Age Resistance 70h at 200 ºC Hardness Change (IRHD) Tensile Strength Change (%) B Change(%)

7 Rheology at 185 C on refined compounds Aflas 90 FKM High Fluorine 90 ETP 90 Aflas ML (dnm) Aflas FKM ETP Aflas

8 Test results on refined compounds The following properties were independently tested at a recognised test house: After steam exposure (220ºC and 150 bar for 2 weeks) TS change (%) E@ B change (%) Mod@ 50% change (%) Aflas 90 < -25 < -25 < +25 FKM High Fluorine 90 > -50 > -50 > -50 ETP 90 < -25 < -25 < -25 Aflas 80 < +25 < +25 < +25 After exposure to sour conditions (150ºC and 20 bar for 2 weeks ) TS change (%) E@ B change (%) change (%) Aflas 90 < +19 < -19 < +19 FKM High Fluorine 90 < +19 < -19 < +19 ETP 90 < +19 < -19 < +19 Aflas 80 < +19 < -19 < +19

9 Test results on refined compounds The following properties were independently tested at a recognised test house: After exposure to hydrocarbons (NORSOK oil test 7 days at 150ºC), followed by exposure to steam (220ºC and 150 bar) TS change (%) E@ B change (%) change (%) Aflas 90 Not tested Not tested Not tested FKM High Fluorine 90 Not tested Not tested Not tested ETP to -50 < to +50 Aflas 80 < -25 < to -50 Aflas 90 Failure RGD resistance testing Aflas 90 FKM High Fluorine 90 ETP 90 Aflas 80 NORSOK RATING FAIL PASS FAIL PASS FKM 90 Pass

10 Conclusions on refined compounds Tested refined compounds for resistance to sour gas, steam and RGD Best all-round performance was seen from Aflas 80 compound Aflas 80performed well in steam, even at higher temperatures (250 C and 265 C) and showed good resistance to sour conditions 312 O-rings passed RGD testing Moved on to moulding trials Compression moulding did not produce a good quality part Transfer moulding gave good quality parts free from moulding flaws when examined along the cross-section

11 Example of compression moulded packer showing splits from poor consolidation Example of transfer moulded packer free from moulding defects

12 ED Testing on Clwyd Compounds Validated some designed compounds against the rigorous requirements of the Norsok M710 speciation next step was to expand the product range CCL have portfolio of materials for use in these environments Validated the formulation design and gained better understanding of the requirements design compounds tailored for individual processes that will meet the specifications and service conditions offer impartial choice on suitable grades for best processing and performance

13 Test results on Clwyd ED resistant compounds We designed further ED resistant compounds using different base elastomers and tested basic physical properties internally FFKM Aflas FKM Type 1FKM Type 2 HNBR Hardness IRHD Specific Gravity g/cm Tensile Strength MPa Elongation to Break % % MPa Compression set % C C C C C

14 Test results on Clwyd ED resistant compounds We designed further ED resistant compounds using different base elastomers and tested ED resistance in accordance with ISO Rapid gas decompression testing ISO Test piece and fill factor Gas mixture 312 O ring size at 85% fill factor 10/90 CO2/CH4 FFKM Aflas FKM Type 1 FKM Type 2 HNBR Rating

15 Designing Compounds for non-standard ED Resistant Parts Sometimes other parts than o-rings are required for these extreme environments which may need similar ED resistance, such as packers Elastomers are often used in critical applications, need to understand engineering requirements Design engineers are designing parts for purpose which may need evaluating in service conditions When testing to N710 and chemical testing good information is ascertained but actual parts may not reflect this test performance Global catastrophes have emphasized the need for rigorous testing

16 Designing Compounds for non-standard Parts Test methods are for o-rings -in service testing is paramount Cooperation between compounder, design engineer and component manufacturer feedback is key in order to adapt and refine There is a huge diversity of materials within the sector FKM and HNBR are generalisations that are often asked for there are many grades available offering a wide range of chemical and physical resistances FKM grades available for extremes of high or low temperature (- 45 C) with high chemical resistance need to understand service requirements for correct selection

17 Designing Compounds for non-standard Parts Formulation Design Correct Grade Selection Best Chance of Success High Compound Quality Processing Considerations

18 Challenging Conventions -Water Swellable Compounds Rubber very often required to resist the ingress of fluids for sealing applications - elastomers are selected for low swell in fluids Some applications require this concept to be turned on its head Water swellable compounds can provide an inexpensive seal against ground water down bore holes The function is still to stop fluids but by a different mechanism

19 Challenging Conventions -Water Swellable Compounds Elastomer seals overcome the shortcomings in engineered contact points Large engineering projects require elastomer seals more than ever less precise materials such as concrete tunnel segments Where the sealing faces cannot be mapped such as rough cut bore holes the function of a swellable elastomer is vital Conditions can range from ambient low pressure areas to high pressure high temperature scenarios requiring swell sealing up to 600 F These are very extreme conditions and present problems for the swell medium and the elastomer itself.

20 Water Swellable Components Elastomeric gaskets make up one of the most effective systems for segmentally lined tunnels where sealing is required against water ingress, or for retention in tunnels used for fluid transport or storage. The complex section of the gaskets is designed to provide the energy within the seal, generating the sealing function once the segments have been assembled, whilst minimising closure forces.

21 Water Swellable Compounds An example of a water swell graph for a conventional swelling NBR compound An example of a water swell graph for a conventional swelling PCR compound

22 Water Swellable Compounds Conventional water swell proceeds by an osmotic mechanism Ions are replaced by water molecules by osmotic pressure which expands the polymer matrix In high temperatures conventional mechanisms will not survive Certain ceramics can absorb water into interstices to expand up to 100% Engineering on the part minimises distance until swell sealing is achieved Certain elastomers inherently offer high resistance to steam including FFKM, Aflas (TFE/P) and to a degree EPDM Further enhancements can be made to steam resistance of the base elastomers by special compounding techniques

23 Water Swellable Components An example of a conventional water swellable packer An example of a higher temperature and pressure swellable packer

24 Conclusions Knowledge of compounding techniques to design materials suitable for extreme conditions is required Materials then need independent testing to check suitability in function Standardised tests, such as Norsok, are widely recognised and give a degree of confidence in the compound/parts capability However these tests are not always associated with the parts performance With such a wide variety of parts, environments, service and chemical conditions in-situ test data is more relevant to performance Feedback is essential for compounder to fulfil the service requirements can be used to adapt and refine compounds further for optimum performance in extreme environments By use of innovative technology and novel ingredients we can find solutions to even the most demanding and extreme applications

25 Thank you for your time Clwyd Compounders Ltd., Gardden Industrial Estate, Ruabon, Wrexham, LL14 6RG t:+44 (0) e: