Chemistry Reference
In-Depth Information
Table 3.6 The glass-transition temperatures of RPEuO prepared at various initiator
concentrations.
Polym.
temperature/1C
Initiator
loading /mmol
Sample
T
g
/1C
RPEuO-I
25
1.87
22.7
RPEuO-II
25
2.79
15.9
RPEuO-III
25
4.66
15.0
Table 3.7 Data related to the extracted soluble substances from RPEuO polymers.
Soxhlet extraction/
wt%
Soluble
Polym.
temperature/1C
Initiator
loading/mmol
Monomer
loading/g
Sample
Insoluble
RPEuO-I
25
1.87
30
30
70
RPEuO-II
25
2.79
30
29
71
RPEuO-III
25
4.66
30
14
86
RPEuO-IV
25
4.66
40
22
78
RPEuO-V
25
4.66
50
35
65
Table 3.8 Thermal stability data for the RPEuO polymers.
Sample/Temperature
a
200-220 1C 240-320 1C 340-450 1C
RPEuO-I stable 2 wt% loss 87 wt% loss
RPEuO-II stable 3 wt% loss 85 wt% loss
RPEuO-III stable 4 wt% loss 85 wt% loss
RPEuO-IV stable 3 wt% loss 84 wt% loss
RPEuO-V stable 3 wt% loss 88 wt% loss
a
Roman numbers here are only to identify the samples prepared at different conditions, such as
temperature, catalyst amounts and initiator amounts.
EuO are mild, such as at room temperature, low pressure and shorter
reaction times. The polymerization of SBO needs harsh reaction conditions,
such as temperature more than 100 1C, pressures of 110 bar and longer
reaction times. This is because the internal 1,2-disubstituted non-
conjugated double bonds create diculties in the polymerization reaction.
When those double bonds in SBO are converted into oxirane (or epoxide)
moieties, they show more reactivity.
3.4.2 Characterization of the Polymers
Confirmation of the resulting polymer structures was accomplished by a
number of different techniques,
1
H-NMR,
13
C-NMR, FT-IR, solid-state NMR
and GPC. Figure 3.4 shows the
1
H-NMR spectra of SBO and PSBO.
The signals at 5.40 ppm are characteristic of olefinic hydrogens and the
signals at 5.1-5.3 ppm represent the methine proton of -CH
2
-CH-CH
2
-(the
glycerin backbone). The signals at 4.0-4.4 ppm are from the methylene pro-
tons of -CH
2
-CH-CH
2
-. The peak at 2.80 ppm corresponds to the protons in
