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Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends

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Characterization (Mid-IR) Kinetics of solution modification On-line monitoring of interfacial reaction by ATR-FTIR Materials: ... Polymer blends : ... – PowerPoint PPT presentation

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Title: Monitoring Interlayer Formation by Infrared Spectroscopy in Layered Reactive Polymer Blends


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

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
In situ compatibilization by reactive blending
  • A/B immiscible blend

A/B
B - Y

Y-functionalized B
Y-functionalized D (miscible with B)
5
Introduction
Reactive blending
C. Koning, Prog. Pol. Sci (1998), 707
6
Objective
  • 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

7
Oxazoline Universal compatibilizer
B.M. Culberston, Prog. Pol. Sci (2002), 579
8
Modification of SAN in solution
Reaction scheme
9
Polymer 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.

10
Characterization (Mid-IR)
11
Kinetics of solution modification
K 6.4104exp(-10.2103/T) ( g/mmolmin)
12
(No Transcript)
13
On-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)

14
Instrumental set-up
400nm
15
Results
190 oC
120 oC
5.4 wt oxazoline 400nm SAN-oxa layer
16
Difference Spectroscopy
17
Intensity Vs. Time
18
Mirror image
overlapping
19
Effect of temperatures
20
Step annealing ?
190 oC 170 oC
21
Step annealing II
150 oC/160 oC/170 oC 190 oC
22
Step 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
23
Effect 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
24
Effect of thickness of SAN-oxazoline layer
Temp. 190 oC
25
Solution mixture of SAN and SAN-oxa
Temp. 190 oC
26
Conclusions
  • 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.

27
Future 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

28
Acknowledgement
  • 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

29
Thanks for your attention !
30
(No Transcript)
31
Introduction
Morphology developement viscosity of
phases,interfacial properties, blend composition,
processing conditions
C. Koning, Prog. Pol. Sci (1998), 707
32
Capillary Number ---- Drop deformation
33
Why oxazoline??
Macosko et al., Polymer 42 (2001), 8171
34
Ellipsometry
  • The evolution of interface with time under
    different temperatures

35
Model for Ellipsometry
36
Off-line investigation of the stretching process
by FTIR
37
FTIR Microscopy
38
Conversion of oxazoline
Which one is better
?
39
5.4 SAN-oxa with catalyst
5.4 without catalyst 190deg 2hrs
40
?
5.4 with 55wt catalyst (to oxazoline) 190deg
2hrs
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