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Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends

Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends. J. Li a,b , M. Prusty a,c , H. Goossens a,c a Eindhoven University of Technology - Department of Chemical Engineering and Chemistry- Laboratory of Polymer Technology

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Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends

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  1. Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends J. Lia,b, M. Prustya,c, H. Goossensa,c a Eindhoven University of Technology - Department of Chemical Engineering and Chemistry- Laboratory of Polymer Technology P.O. Box 513, 5600 MB Eindhoven, The Netherlands b Fudan University -Department of Macromolecular Science, 200433 Shanghai, China c Dutch Polymer Institute, P.O. Box 902, 5600 AX Eindhoven, The Netherlands

  2. Introduction Objective Modification of SAN in solution On-line Monitoring interlayer reaction by ATR-FTIR in layered reactive polymer blends Future work Outline

  3. Introduction Polymer blends :Combination of existing polymers Advantage: Cheap Tuning properties easily high property/cost performances Disadvanatage: Immiscibility Coarse phase morphology C. Koning, Prog. Pol. Sci (1998), 707

  4. A/B immiscible blend  block or grafted copolymers “in situ” X-functionalized A* X-functionalized C* (miscible with A) In situ compatibilization by reactive blending A/B B - Y + Y-functionalized B* Y-functionalized D* (miscible with B)

  5. In situ generated copolymer Reactive additive for phase (A) Reactive additive for phase (B) Y X’ X Y’ (A)-graft-(B) X’ Y Y’ X (A)-branch-(B) Introduction Reactive blending: C. Koning, Prog. Pol. Sci (1998), 707

  6. Understand the reactive blending process from a fundamental point of view ---- the competition between processes like diffusion to interface and reaction between the components inside the interface Objective

  7. R N H 2 R ' C O N H C H C H N H R 2 2 Oxazoline: Universal compatibilizer B.M. Culberston, Prog. Pol. Sci (2002), 579

  8. Modification of SAN in solution Reaction scheme

  9. Materials: SAN, AE, catalyst, DCB (solvent) Procedure: Precipitation: 5 wt% of polymer in chloroform and then add to it 10 times methanol Drying: 48 hrs. at 45 °C Parameters: Ratio AN/AE, different catalysts, catalyst concentration, temperature and reaction time. Polymer modification

  10. Phenyl Nitrile Oxazoline Characterization (Mid-IR)

  11. Kinetics of solution modification K = 6.4*104exp(-10.2*103/T) ( g/mmol·min)

  12. Materials:SAN-oxazoline (1.9 ~5.4 wt% oxazoline) poly (ethylene-co-methacrylic acid) (15 wt% acid) Sample: a: thin film of SAN-oxazoline (100nm~ 400nm) b: thick film of PE-co-MA (~ 0.5mm) a b On-line monitoring of interfacial reaction by ATR-FTIR

  13. d=1~2 µm Instrumental set-up 400nm

  14. Amide I Oxazoline Ester Amide II Results 190 oC 120 oC 5.4 wt% oxazoline 400nm SAN-oxa layer

  15. Amide I Ester Oxazoline Difference Spectroscopy

  16. Intensity Vs. Time

  17. original After reversal Mirror image overlapping

  18. Equilibrium ? Diffusion limitation ? Effect of temperatures

  19. Equilibrium ? Step annealing І: 190 oC ~170 oC

  20. Step annealing II: 150 oC/160 oC/170 oC ~ 190 oC

  21. 150 oC/160 oC/170 oC ~ 190 oC Step annealing II:

  22. Temp. =190 oC Effect of content of oxazoline

  23. Effect of thickness of SAN-oxazoline layer Temp. =190 oC

  24. Solution mixture of SAN and SAN-oxa Temp. =190 oC

  25. ATR-FTIR can be used to monitor the interfacial reaction between oxazoline and acid groups and follow the kinetics. There is no side reaction in the system. It’s not an equilibrium reaction. low temperature – higher diffusion limitation and vice versa. The thickness of SAN-oxa layer and the position of the oxazoline group in SAN is not important for the reaction. Conclusions

  26. ATR-FTIR: do quantitative analysis on the data Ellipsometry: follow the interlayer formation The ellipsometry data will be correlated with the infrared data Off-line investigation of the stretching process by FTIR Future Work

  27. Otto van Asselen, TU/e Edgar Karssenberg, TU/e Martin van Duin, DSM Research, Geleen, The Netherlands Gert de Wit, GE Advanced Materials, Bergen op Zoom, The Netherlands Colleagues in the faculty of Chemical Engineering & Chemistry of TU/e Acknowledgement

  28. Thanks for your attention !

  29. Introduction Morphology developement viscosity of phases,interfacial properties, blend composition, processing conditions C. Koning, Prog. Pol. Sci (1998), 707

  30. Capillary Number ---- Drop deformation

  31. P(arom.) < P(aliph.) P’(arom.) < P’(aliph.) Why oxazoline?? Macosko et al., Polymer 42 (2001), 8171

  32. Ellipsometry • The evolution of interface with time under different temperatures

  33. Model for Ellipsometry

  34. Off-line investigation of the stretching process by FTIR

  35. FTIR Microscopy

  36. Conversion of oxazoline Which one is better ?

  37. 5.4% SAN-oxa with catalyst 5.4% without catalyst 190deg 2hrs

  38. ? 5.4% with 55wt% catalyst (to oxazoline) 190deg 2hrs

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