Entry | Cat. | Temp. (°C) | Yield (g) | Activity (kgPE/(mmolV·h)) | Mw b (kg/mol) | PDI b | Tm/Tc c (°C) |
1 | 2a | 50 | 0.75 | 18.0 | 53.3 | 1.7 | 133/119 |
2 | 2b | 50 | 0.79 | 19.0 | 58.2 | 1.7 | 133/118 |
3 | 2c | 50 | 0.76 | 18.2 | 59.3 | 1.8 | 133/119 |
4 | 2d | 50 | 0.40 | 9.60 | 67.8 | 1.8 | 133/119 |
5 | 2e | 50 | 0.83 | 19.9 | 62.2 | 1.8 | 133/119 |
6 | 2f | 50 | 0.50 | 12.0 | 58.9 | 1.9 | 133/119 |
7 | 2e | 30 | 0.34 | 8.16 | 141 | 1.6 | 135/117 |
8 | 2e | 70 | 0.54 | 13.0 | 32.6 | 1.4 | 131/120 |
a Conditions: The feedstock of vanadium catalyst is 0.5 μmol; Et2AlCl, 2.0 mmol; ETA, 0.15 mmol; solvent, toluene; total volume, 50 mL; polymerization time, 5 min; ethylene pressure, 0.1 MPa; b Determined by HT-GPC at 150 °C; c Measured on DSC |

Citation: Ling-pan Lu, Kai-ti Wang, Yi Liu and Jia-jun Wu. Systheisis of Vanadium Complexes Bearing Tridentate β-Ketoimine Ligands and Their Catalytic Capabilities towards Ethylene (Co)polymerization[J]. Acta Polymerica Sinica. doi: 10.11777/j.issn1000-3304.2019.19128

三齿β-酮亚胺钒(III)配合物的合成及其催化乙烯(共)聚合行为研究
English
Systheisis of Vanadium Complexes Bearing Tridentate β-Ketoimine Ligands and Their Catalytic Capabilities towards Ethylene (Co)polymerization
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Key words:
- Vanadium complexs /
- Olefin polymerization /
- Polyethylene /
- Cyclic olefin copolymers
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[1]
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Table 1. Typical ethylene polymerization results a
Table 2. Typical ethylene/NBE copolymerization results a
Entry Cat. NBE
(mol/L)Yield
(g)Activity
(kgpolymer/(mmolV·h))Comonomer incorp. b
(mol%)Mw c
(kg/mol)PDI c Tg d
(°C)1 2a 0.5 0.66 15.8 33.2 58.1 1.3 84 2 2a 1.0 0.40 9.60 40.6 43.1 1.4 103 3 2b 0.5 0.81 19.4 34.3 63.7 1.3 89 4 2b 1.0 0.51 12.2 42.1 48.9 1.3 105 5 2c 0.5 0.74 17.8 32.1 64.0 1.3 87 6 2c 1.0 0.45 10.8 39.6 49.6 1.3 103 7 2d 0.5 0.58 13.9 31.4 64.5 1.4 88 8 2d 1.0 0.36 8.64 38.4 49.6 1.3 102 9 2e 0.5 1.12 26.9 30.9 66.4 1.3 86 10 2e 1.0 0.70 16.8 36.9 51.0 1.4 99 11 2f 0.5 0.51 12.2 34.0 52.9 1.4 84 12 2f 1.0 0.32 7.68 40.6 39.2 1.4 103 a Conditions: The feedstock of vanadium catalyst is 0.5 μmol; Et2AlCl, 2.0 mmol; ETA, 0.15 mmol; solvent, toluene; total volume, 50 mL; polymerization time, 5 min; ethylene pressure, 0.1 MPa; b Calculated according to the 13C NMR; c Determined by GPC; d Measured by DSC Table 3. Typical ethylene/HBM copolymerization results a
Entry Cat. HBM
(mmol)Yield
(g)Activity
(kgpolymer/(mmolV·h))Comonomer incorp.b
(mol%)Mw c
(kg/mol)PDI c Tg d
(°C)1 2a 0.2 0.84 20.2 15.5 90.2 1.7 135 2 2a 0.4 0.65 15.6 23.4 94.2 1.6 183 3 2b 0.2 0.86 20.6 16.9 99.6 1.6 137 4 2b 0.4 1.27 30.5 25.0 104 1.6 188 5 2c 0.2 1.13 27.1 16.4 110 1.6 137 6 2c 0.4 0.85 20.4 24.8 121 1.5 188 7 2d 0.2 0.43 10.3 14.7 104 1.6 131 8 2d 0.4 0.20 4.80 21.8 111 1.6 173 9 2e 0.2 0.93 22.3 14.7 116 1.6 131 10 2e 0.4 1.76 42.2 23.7 138 1.6 183 11 2f 0.2 0.60 14.4 15.6 91.6 1.6 133 12 2f 0.4 0.89 21.3 24.9 95.5 1.5 186 a Conditions: The feedstock of vanadium catalyst is 0.5 μmol; Et2AlCl, 2.0 mmol; ETA, 0.15 mmol; solvent, toluene; total volume, 50 mL; polymerization time, 5 min; ethylene pressure, 0.1 MPa; b Calculated according to the 13C NMR; c Determined by GPC; d Measured by DSC -