Differential scanning calorimetry (DSC) thermograms of the heat-treated hybrids are
shown in Fig. 2. The DSC scans did not change significantly as the heat treatment time
increased from 10 to 60 min at 190
C. Chemical changes thus do not take place to any
appreciable extent at the extrusion processing temperature of 190
C. It was also
confirmed by
1
H- and
13
C-NMR spectroscopy that no detectable transesterification
reaction occurred in TLCP under the processing conditions (not shown here).
O
O
HOC
COH
1) Synthesis of EHBT
2) Organoclay
3) Synthesis of EHBT hybrid
EHBT
EHBT hybrid
C25A
melt
Intercalation
pyridine
Cloisite 25A
;C25A
- HCL
SOCl 2
CH 3 CH 2 O
CH 3 CH 2 O
Br
O
O
C
O
O
n
CO
Br
EHBT
O
CCl
HO
OH
ClC
+
Br
Scheme 2 Synthetic routes for the EHBT hybrid
0 min
10 min
20 min
30 min
60 min
300
200
Temperature (°C)
100
0
Endotherm.
Fig. 2 DSC thermograms of
4 wt% C25A in EHBT hybrid
annealed at 190
C for
different times
584
T. Y. Ha et al.
shown in Fig. 2. The DSC scans did not change significantly as the heat treatment time
increased from 10 to 60 min at 190
C. Chemical changes thus do not take place to any
appreciable extent at the extrusion processing temperature of 190
C. It was also
confirmed by
1
H- and
13
C-NMR spectroscopy that no detectable transesterification
reaction occurred in TLCP under the processing conditions (not shown here).
O
O
HOC
COH
1) Synthesis of EHBT
2) Organoclay
3) Synthesis of EHBT hybrid
EHBT
EHBT hybrid
C25A
melt
Intercalation
pyridine
Cloisite 25A
;C25A
- HCL
SOCl 2
CH 3 CH 2 O
CH 3 CH 2 O
Br
O
O
C
O
O
n
CO
Br
EHBT
O
CCl
HO
OH
ClC
+
Br
Scheme 2 Synthetic routes for the EHBT hybrid
0 min
10 min
20 min
30 min
60 min
300
200
Temperature (°C)
100
0
Endotherm.
Fig. 2 DSC thermograms of
4 wt% C25A in EHBT hybrid
annealed at 190
C for
different times
584
T. Y. Ha et al.