Catalytic system for ethylene selective oligomerization and ethylene selective oligomerization method
A catalytic system and selective technology, which is applied in the direction of chemical instruments and methods, catalysts, carbon compound catalysts, etc., can solve the problems of continuous production of products in production equipment, such as post-processing difficulties, and achieve the effects of low cost, high activity, and simple synthesis
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Embodiment 1
[0054] 1. Synthesis of ligand L1 (2,6-dimethyl-(bis-2-pyridinemethanone)aniline)
[0055] Dissolve 0.50g (0.0027mol) dipyridine (L) in 20mL toluene, add 0.33g (0.0027mol) 2,6-dimethylaniline, add a drop of glacial acetic acid as catalyst, add appropriate amount of molecular sieve to remove water, heat to reflux After three days, it was filtered to obtain a yellow liquid, the solvent was evaporated under reduced pressure, and recrystallized with ethanol to obtain a yellow solid with a yield of 93%.
[0056] 1 H NMR (δ, ppm, CDCl 3 , TMS): 2.086 (s, 6H, CH 3 ), 6.789-6.901 (m, 3H, C 6 h 3 ), 7.014(d, 1H, CH), 7.146(m, 1H, CH), 7.356(m, 1H, CH), 7.492(m, 1H, CH), 7.836(m, 1H, CH), 8.297(d , 1H, CH), 8.583(d, 1H, CH), 8.631(d, 1H, CH). 13 C NMR (δ, ppm, CDCl 3 ): 17.39, 122.17, 122.38, 123.63, 126.55, 134.52, 135.59, 147.08, 147.97, 148.15, 153.57, 153.79, 164.85.
[0057] 2. Preparation of catalyst
[0058] All operations were carried out in an anhydrous and oxygen-free ...
Embodiment 2
[0062] 1. Synthesis of ligand L2 (3,5-dimethyl-(bis-2-pyridinemethanone) aniline)
[0063] In the same synthesis method as L1, a light yellow solid was obtained with a yield of 87%. 1 H NMR (δ, ppm, CDCl 3 , TMS): 2.181 (s, 6H, CH 3 ), 6.419(s, 2H, Ph), 6.633(s, 1H, Ph), 7.049(d, 1H, CH), 7.201(m, 1H, CH), 7.344(m, 1H, CH), 7.56(m , 1H, CH), 7.825(m, 1H, CH), 8.213(d, 1H, CH), 8.604(m, 2H, CH).
[0064] 2. Preparation of catalyst
[0065] With embodiment 1. Ligand L1 was exchanged for L2 (1.38 mg) (9.6 μmol).
[0066] 3. Ethylene oligomerization
[0067] Same as Example 1, 80°C is changed to 70°C. The catalyst activity is 9.75×10 5 g oligomer / mol Cr·h. The distribution of the oligomerization products is shown in Table 1.
Embodiment 3
[0069] 1. Synthesis of ligand L3 (3-methylthio-(bis-2-pyridinemethanone) propylamine)
[0070] Dissolve 0.50g (0.0027mol) dipyridinone (L) in 20mL toluene, add 0.28g (0.0027mol) 3-(methylthio)propylamine, add a drop of glacial acetic acid to catalyze, add molecular sieve to remove water, and reflux for three days. Precipitation occurred, filtered to obtain a light green liquid, and the solvent was evaporated under reduced pressure to obtain a dark green oily product. 1 H NMR (δ, ppm, CDCl 3 , TMS): 2.023 (m, 2H, CH 2 ), 2.083 (s, 3H, CH 3 ), 2.575 (m, 2H, CH 2 ), 3.515 (m, 2H, CH 2 ), 7.332(m, 3H, CH), 7.75(m, 1H, CH), 7.794(m, 1H, CH), 8.112(d, 1H, CH), 8.524(m, 1H, CH), 8.735(d , 1H, CH).
[0071] 2. Preparation of catalyst
[0072] With embodiment 1. Ligand L1 was exchanged for L3 (2.4 mg) (9.6 μmol).
[0073] 3. Ethylene oligomerization
[0074] With embodiment 1, catalyst activity is 3.42 * 105 g oligomer / mol Cr·h. The distribution of the oligomerization produc...
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