Title: Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends
1Monitoring 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
2Outline
- Introduction
- Objective
- Modification of SAN in solution
- On-line Monitoring interlayer reaction by
ATR-FTIR in layered reactive polymer blends - Future work
3Introduction
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
4In situ compatibilization by reactive blending
A/B
B - Y
Y-functionalized B
Y-functionalized D (miscible with B)
5Introduction
Reactive blending
C. Koning, Prog. Pol. Sci (1998), 707
6Objective
- 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
7Oxazoline Universal compatibilizer
B.M. Culberston, Prog. Pol. Sci (2002), 579
8Modification of SAN in solution
Reaction scheme
9Polymer modification
- 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.
10Characterization (Mid-IR)
11Kinetics of solution modification
K 6.4104exp(-10.2103/T) ( g/mmolmin)
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13On-line monitoring of interfacial reaction by
ATR-FTIR
- 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)
14Instrumental set-up
400nm
15Results
190 oC
120 oC
5.4 wt oxazoline 400nm SAN-oxa layer
16Difference Spectroscopy
17Intensity Vs. Time
18Mirror image
overlapping
19Effect of temperatures
20Step annealing ?
190 oC 170 oC
21Step annealing II
150 oC/160 oC/170 oC 190 oC
22Step annealing II
Slope Slope in curve of 190oC
150oC 190oC 0.00707 0.00679
160oC 190oC 0.00329 0.00405
170oC 190oC 0.00148 0.00141
23Effect of content of oxazoline
3.45/1.9 5.4/1.9
ratio of oxazoline's content 1.815789 2.842105
ratio of amide I's intensity 1.974067 2.91471
24Effect of thickness of SAN-oxazoline layer
Temp. 190 oC
25Solution mixture of SAN and SAN-oxa
Temp. 190 oC
26Conclusions
- 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.
- Its 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.
27Future Work
- 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
28Acknowledgement
- 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
29Thanks for your attention !
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31Introduction
Morphology developement viscosity of
phases,interfacial properties, blend composition,
processing conditions
C. Koning, Prog. Pol. Sci (1998), 707
32Capillary Number ---- Drop deformation
33Why oxazoline??
Macosko et al., Polymer 42 (2001), 8171
34Ellipsometry
- The evolution of interface with time under
different temperatures
35Model for Ellipsometry
36Off-line investigation of the stretching process
by FTIR
37FTIR Microscopy
38Conversion of oxazoline
Which one is better
?
395.4 SAN-oxa with catalyst
5.4 without catalyst 190deg 2hrs
40?
5.4 with 55wt catalyst (to oxazoline) 190deg
2hrs