Table 1.
Entry | Solvent | Catalyst [μmol] | Time [min] | Yield PE [g] | TO.h−1a |
M
n
(by GPC) [g mol−1] |
---|---|---|---|---|---|---|
1 | Toluene | L1Pd-NR3 (0.9) | 30 | 2.6 | 204,000 | 13,670 |
2b | Miniemulsion | L1Pd-NR3 (18) | 60 | <0.05 | <50 | n.d. |
3c | Water | L1Pd-NH2PEG (15) | 60 | 0.02 | 55 | n.d. |
4 | 9/1 Toluene/H2O | L1Pd-NR3 (0.9) | 30 | 1.5 | 121,000 | 9750 |
5 | 9/1 Toluene/H2O | L1Pd-NR3 (0.9) | 60 | 2.8 | 105,655 | n.d. |
6 | 9/1 Toluene/H2O | L1Pd-NR3 (0.9) | 90 | 3.8 | 98,513 | n.d. |
7 | Toluene | L2Pd-DMSO (0.4) | 15 | 2.0 | 774,000 | 96,330 |
8 | 9/1 Toluene/H2O | L2Pd-DMSO (0.4) | 15 | 0.65 | 226,000 | 68,050 |
Reaction conditions: 85 °C, 40 bar of constant ethylene pressure, total volume of solvent: 100 mL n.d. not determined
aMol of ethylene consumed per mol of Pd per hour
bAverage size of micelles or miniemulsion before (78.5 nm) and after (82.4 nm) ethylene polymerization determined by DLS
cWith additional 800 mg Tergitol® 15-S-20