Table 2.
Influence of p-cresol equivalents on molecular weight and Tg of PIsSu
Equiv. p-cresol | Mn [kg/mol] | PDI | Tg [°C] | Unreacted isosorbide after esterification [mol%]* |
---|---|---|---|---|
0.5 | 28.1 | 2.5 | 81 | 0.8 |
0.9 | 40.3 | 2.7 | 83 | 1.2 |
1.5 | 40.4 | 2.4 | 82 | 2.0 |
2.2 | 31.6 | 2.0 | 82 | 2.9 |
Reaction conditions (unless noted otherwise): Reactions were conducted on a 60 mmol scale (respective diacid), with a 1:1 molar ratio of isosorbide:succinic acid and 0.1 mol% BuSnOOH catalyst (resp. diacid). The amount of p-cresol in each experiment was varied as indicated (respective diacid). Esterification was conducted for 5 h at 240 °C. For pre-polycondensation, the temperature was decreased to 220 °C and the pressure reduced from atmospheric pressure to 0.4–0.8 mbar within 2 h. Polycondensation was conducted for 1 h at 220 °C and 0.4–0.8 mbar.
*Determined from 1H NMR spectra after esterification, see Supplementary Information p. 5.