Influence of functionalized S-SBR on silica-filled rubber compound properties
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(2) Rubber for Tread of Tire Tread Performance SBR NR BR Filler (Silica) Oil. Tread. 3. E-SBR and S-SBR S-SBR (Solution SBR) Solution-polymerized Styrene Butadiene Rubber E-SBR (Emulsion SBR) Emulsion-polymerized Styrene Butadiene Rubber. E-SBR. S-SBR. Process. Emulsion. Solution. Polymerization. Radical. Anionic. Styrene (%). 0 – 50 %. Controllable (0 ֞ 90 %). Styrene Chain. Random. Controllable (Random ֞ Block). Vinyl in Butadiene. 15 – 18%. Controllable (0 ֞ 80%). Functionalization. Introduce 3rd monomer. Chain end. Branching. Multi branched. Controllable (linear ֞ multi branched). MW distribution. Wide. Controllable (Wide ֞ narrow) Saito, A.: Nippon Gomu Kyokaishi, 71, 41(1998). 4. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. z Low-RR z Grip z Wear resistance. Material.
(3) How to improve S-SBR?. Macro structure. Functionalization. Bad point. High molecular weight (less free chain ends). Lower tanG. Lower Processability. Narrow molecular distribution (less free chain ends). Lower tanG. Lower Processability. Less branch or graft structure (less free chain ends). Lower tanG. Lower Processability. Low vinyl content (lower Tg). Lower tanG. Lower grip. Low styrene content (lower Tg). Lower tanG. Lower grip and processability. Lower tanG (Good filler dispersion). Lower processability. Less free chain ends. Saito, A.: Nippon Gomu Kyokaishi, 71, 41(1998) 5. How to introduce functional group in S-SBR? 1. Functionalization of the chain end +. C-Li+. Functional Group. SBR. 2. Functionalization of initiator -Li+. + Styrene + Butadiene. Initiator. Polymerization. 3. Functionalization of main chain with functionalized monomer Styrene + Butadiene + Functionalized Polymerization monomer. 4. Functionalization of side chain + SBR. Functional Group 6. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. Microstructure. Advantages.
(4) The aim of this study ,QYHVWLJDWHWKHHIIHFWRIIXQFWLRQDOJURXSRQVLOLFDFRPSRXQGV 2QN[OGTU Am ine group Alkoxy am ine group. Mw (kg/mol). 240-280. ML (100C). 42-47. Styrene (wt%). 27. Vinyl (wt%). 42-43. Effect. Method. 1. Silica micro dispersion. TEM, USAX. 2. Flocculation of filler. RPA2000. 3. Filler-polymer interaction. Bound rubber, Payne effect. 7. Formulation, mixing procedure and cure condition Master batch (MB1) Brabender. Formulation (phr) SBR. 80. BR (UBEPOL BR150). 20. Silica (ULTRASIL 7000GR). 75. TESPT. 5.6. TDAE oil (total). 33. Zinc Oxide. Time 0:00. Add Polymers. 0:20. Mix. 1:20. 1/2 Silica, 1/2 TESPT, Oil. 1:50. Mix. 2:50. 1/2 Silica, 1/2 TESPT, Stearic Acid, Zinc Oxide. 2.5. 3:10. Mix (Control rpm. up to target temp.). Stearic Acid. 2.0. 4:10. Ram sweep. Antioxidant (6PPD). 2.0. 6:40. Discharge (145-150 Co). Sulfur. 2.2. CBS. 1.7. DPG. 2.0. Master batch (MB2) Brabender 0:00. Add MB1. 4:00. Discharge (145-150 Co). Final Mix (Productive) Roll (50° C) MB2 + Sulfur and Accelerators Cure condition Temp. 160 Co. Time. t90 8. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. 'ZRGTKOGPVU.
(5) Payne effect of uncured compounds 500 450. Amine group. 400. Alkoxy group. 300 250 200 150 100 50 0 0,1. 1. 10 Strain [%]. 100. 1000. 9 7KHUHVXOWZDVRSSRVLWHWRZKDWH[SHFWHG. 9. USAX measurement I (q) n[ Aexp{-q 2 ( 3r2 nd ) 2 /3}q Dm {I 2 nd (q) MI silica (q)} B{erf (qrsilica / 6 )}3( 6 Ds ) q ( 6 Ds ) ] 䐟fractal structure at small angle. 䐡fractal structure at large angle. 䐠Secondary agglomeration. 䐟. Solid line䠖measured line Dotted line䠖fitted line ʊVLOLFD ʊcompound. A,B䠖 constant n䠖 Number density of secondary aggregates M䠖 number of primary particles in the secondary aggregate r2nd, rsilica䠖 secondary aggregate, average primary radius of silica primary particle Dm, Ds䠖 fractal dimension at small and wide angle I2nd(q)䠖 Scattering equation of the same structure with uniform internal size and secondary aggregates Electron density difference䠖[v*Usilica+(1-v)*Upolymer)] – Upolymer v䠖silica volume fraction in the secondary aggregate Isilica(q)䠖 When the structure in the secondary aggregate is infinitely spread. Intensity. 䐠. 䐡. q (nm-1) 10. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. G' [kPa]. 350.
(6) USAX result and TEM images Average silica size from USAX profile (nm). Amine group Alkoxy group. 㻡㻠㻌. 㻡㻞㻌. ا. 500nm. 500nm. 500nm. 9 6JGTGUWNVUQH75#:CPF6'/FQPQVEQTTGNCVGYKVJ2C[PGGHHGEV ů)ğ • •. $PLQHJURXSVOLJKWO\DIIHFWVWKHVLOLFDGLVSHUVLRQ $ONR[\JURXSLPSURYHVWKHVLOLFDGLVSHUVLRQ 11. Payne effect of uncured compounds 500 450. Amine group. 400. Alkoxy group. G' [kPa]. 350 0 300 0 250 200 150 100 50 0 0,1. 1. 10 Strain [%]. 100. 1000. 9 +LJKHU*ĜDWKLJKVWUDLQLQIXQFWLRQDOL]HG6%5 9 3ODWHDXFXUYHLQDONR[\6%5FRPSRXQGV %HFDXVHRIKLJKHUILOOHUSRO\PHULQWHUDFWLRQ 12. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. <. 㻠㻤㻌.
(7) Comparison the result of payne effect and USAX Functionalized SBR. Non-functionalized SBR. Filler-filler interaction. Filler-filler interaction. Normal one. |G*|. Filler-polymer interaction. |G*|. Filler-polymer interaction Polymer-network Contribution. Hydrodynamic effect. Hydrodynamic effect Strain. Strain. 9 3RVVLELOLW\WKDWILOOHUSRO\PHULQWHUDFWLRQFDQEHGHSHQGHQWRQVWUDLQDV YDULRXVERQGLQJVW\OHVH[LVWEHWZHHQUXEEHUDQGVLOLFD 13. Measurement bound rubber Phy BR Chem BR. Rubber weekly connected to silica Rubber strongly connected to silica. Physical bound rubber 1. Occluded rubber 2. Rubber connected with silica via hydrogen bonding. Chemical bound rubber 1. Gel 2. Rubber connected with silica via covalent bonding. connected with silica via hydrogen bonding. Bound rubber 1. Occluded rubber 2. Gel 3. Rubber connecting via hydrogen bonding 4. Rubber connecting via covalent bonding. connected with silica via covalent bonding. 14. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. Polymer-network Contribution.
(8) Bound Rubber of uncured compound Amine group Alkoxy group. 60. 40 Phy BR. 30. Chem BR. 20 10 0. 9 $ONR[\JURXS 0RUHFKHP%5DQGSK\%5 9 $PLQHJURXS 6PDOOHIIHFWRQ%5 15. Payne Effect After Cure Cured. 5000 00 0. 500 0 450. Am ine group. 400. Alkoxy group. 350 0 3000. G' [kPa]. G' (100 Co) [kPa]. 4000. Uncured. 2000 00. 300 0 250 200 150 100. 1000. 50 0. 0 0,1. 1. 10 Strain [%]. 100. 1000. 0,1. 1. 10 Strain [%]. 100. 1000. 9 $ONR[\IXQFWLRQDOL]HG6%5V /RZHU*ĜDWORZVWUDLQ ȥRSSRVLWHEHKDYLRUWRXQFXUHG*Ĝ 16. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. Bound rubber [wt%]. 50.
(9) Flocculation )ORFFXODWLRQLVUHDJJORPHUDWLRQRIVLOLFDGXULQJFXULQJSURFHVV 1200 1000. Temp 100C Strain 0.5%. G' / kPa. 800 600. Am ine group. 200. Alkoxy group 0 0. 2. 4. 6. 8. 10. 12. time / min. 9 $ONR[\JURXS 6LJQLILFDQWHIIHFWIRUUHGXFLQJIORFFXODWLRQ 9 $PLQHJURXS 6RPHHIIHFWIRUUHGXFLQJIORFFXODWLRQ +LJKHUILOOHUSRO\PHULQWHUDFWLRQȥ/RZHUIORFFXODWLRQ &RPSRXQGZLWKDONR[\6%5VKRZVORZHUFXUHG*ĜGHVSLWHRIKLJKHU XQFXUHG*Ĝ. 17. Payne Effect After Cure Cured. 5000 00 0. 500 0 450. Am ine group. 400. Alkoxy group. 350 0 3000. G' [kPa]. G' (100 Co) [kPa]. 4000. Uncured. 2000 00. 300 0 250 200 150 100. 1000. 50 0. 0 0,1. 1. 10 Strain [%]. 100. 1000. 0,1. 1. 10 Strain [%]. 100. 1000. 9 &XUHG*ĜVKRZVRSSRVLWHEHKDYLRUDVXQFXUHG*Ĝ ȥ)ORFFXODWLRQRFFXUVGXULQJFXULQJSURFHVV 18. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. 400.
(10) tanG 1. 0,10. tanG. 0,06. Amine group. 0,5. Alkoxy group. 0,04. 0,02. 0. 0,00. -80. 9 $ONR[\IXQFWLRQDOJURXS PRUHHIIHFWRQLPSURYLQJWDQG. -60. -40. -20 0 20 40 Temperature [oC]. 60. 80. 100. 9 $ONR[\IXQFWLRQDOJURXS +LJKHUSHDNRIWDQG. 9 $PLQHJURXS VOLJKWHIIHFWRQ WDQG 19. Why tanGG peak is higher in functionalized SBR compound? 5VTQPIHKNNGTRQN[OGTKPVGTCEVKQPEJCPIGUUKNKECVQCEVTWDDGTNKMG Only rubber can move under the deformation. No or week interaction with silica. Silica particle can move with rubber under the deformation Strong interaction with silica. 6JGTGKUNGUUQEENWFGFTWDDGTDGECWUGQHDGVVGTFKURGTUKQP. Worse dispersion ĺMore occluded rubber. Am ine group Alkoxy group. Better dispersion ĺless occluded rubber 30/6/18. 20. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. tanGG (60 oC). 0,08.
(11) The Summery 9 $ONR[\JURXSFDQLPSURYHVLOLFDGLVSHUVLRQDQGILOOHUSRO\PHU LQWHUDFWLRQDQGUHGXFHIORFFXODWLRQRQWKHRWKHUKDQGHIIHFWRI DPLQHJURXSLVVPDOOHU 9 3D\QHHIIHFWGRHVQRWDOZD\VUHODWHWRVLOLFDGLVSHUVLRQDQG GHSHQGHQWRIILOOHUSRO\PHULQWHUDFWLRQRQVWUDLQLVVXJJHVWHG 9 +LJKWDQG SHDNRIIXQFWLRQDOL]HG6%5FRPSRXQGFDQEHH[SODLQHG E\UXEEHUOLNHDFWLQJVLOLFDZKLFKKDVVWURQJLQWHUDFWLRQZLWKUXEEHU. How to analyze Amine group. Alkoxy group. Silica dispersion. TEM, USAX. +. +++. Flocculation of filler. RPA2000. +. +++. Filler-polymer interaction. Bound rubber Payne effect. +. +++ 21. This document is only for the exclusive use by attendees of the DKT 2018 scientific conference. Passing on to third parties or publishing the contents or parts of the contents requires the express consent of the author(s).. Effect.
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