Preparation method of ethylene oligomerization catalyst and use thereof
A technology for ethylene oligomerization and catalysts, which is applied in the field of preparation of olefin oligomerization catalysts, and can solve the problems of many ligand synthesis steps
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Embodiment 1
[0051] 1. Catalyst chlorination of 2-n-butyryl-1,10-phenanthroline 2,6-diethylanilinate iron (II) complex preparation
[0052] The synthesis of a.2-n-butyryl-1,10-phenanthroline (see the following reaction scheme)
[0053]
[0054] Put 15g (76mmol) of 1,10-phenanthroline monohydrate into a three-neck flask, add 100ml of toluene that has been dehydrated and deoxygenated in advance to dissolve, and dissolve under nitrogen protection and magnetic stirring. Then, 93 ml of a 1.2 M cyclohexane solution of n-butyllithium (112 mmol) was slowly added dropwise at -10° C., and the addition was completed within 3 hours. After the dropwise addition, the reaction solution was brownish black, and was stirred overnight at 0°C. Then add 90ml of deionized water and hydrolyze at 0°C. Separate the liquid, take out the organic phase, reduce the pressure, and remove the solvent under 10mmHg. Afterwards, 8.06 g of selenium dioxide (72 mmol) and 50 ml (0.6 mol) of 1,4-dioxane were added, and re...
Embodiment 2
[0071] Catalyst for the preparation of 2-acetyl-1,10-phenanthroline chloride 2,6-diethylanilinate iron(II) complex
[0072] The synthesis of a.2-acetyl-1,10-phenanthroline (see the following reaction scheme)
[0073]
[0074] Repeat step a of Example 1, the difference is that the 1.2M cyclohexane solution of ethyllithium (112mmol) is used to replace the 1.2M cyclohexane solution of n-butyllithium, and finally through silica gel column chromatography, a khaki solid product is obtained , weighing 5.77g, yield 65%. The product was identified as the compound described in title a., ie, 2-acetyl-1,10-phenanthroline, by NMR and mass spectrometry analysis.
[0075] Mass Spectrum MS-EI:222.
[0076] NMR analysis: 1 H NMR (300MHz, CDCl 3 ): δ9.26(d, J=3.9Hz, 1H); 8.37(s, 2H); 8.29(d, J=8.1Hz, 1H); 8.7(dd, J=8.7Hz, 2H); 7.69(dd , J=7.8Hz, 1H); 3.09(s, 3H, CH 3 ).
[0077] b. Synthesis of ligand 2-acetyl-1,10-phenanthroline 2,6-diethylaniline (see the following reaction scheme) ...
Embodiment 3
[0090] Preparation of 2-n-propanoyl-1,10-phenanthroline chlorinated 2,6-diethylanilinate iron(II) complex as catalyst
[0091]Repeat Example 1 with the difference that in step a the 1.2 M cyclohexane solution of n-propyl lithium (112 mmol) is used instead of the 1.2 M cyclohexane solution of n-butyllithium, and in step b use the The resulting 2-n-propanoyl-1,10-phenanthroline (2.12 mmol) replaced 0.53 g (2.12 mmol) of 2-n-butyryl-1,10-phenanthroline, and was obtained in step c with step b 2-n-propionyl-1,10-phenanthroline 2,6-diethylaniline (1.36mmol) instead of 0.52g (1.36mmol) 2-n-butyryl-1,10-phenanthroline 2, 6-diethylaniline finally obtained 2-n-propanoyl-1,10-phenanthroline chloride 2,6-diethylanilinate iron (II), and its elemental analysis results are as follows.
[0092] Elemental Analysis: C 25 h 25 Cl 2 FeN 3 (494.24), Theoretical: C, 60.75; H, 5.10; N, 8.50. Measured values: C, 60.71; H, 5.00; N, 8.53.
[0093] The total yield of the target product 2-n-propan...
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