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A technology of ethylene oligomerization and ethylene, applied in the field of ethylene oligomerization reaction technology, can solve the problems of harsh process requirements, large dosage, high production cost, etc., and achieve the effect of high oligomerization reactivity and high selectivity
Active Publication Date: 2015-02-11
CHINA PETROLEUM & CHEM CORP +1
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However, whether methylalumoxane or modified methylalumoxane is used as a cocatalyst, the cost is too high and the dosage is too large. When it is used as a cocatalyst for ethylene oligomerization on a large scale, it will inevitably lead to production costs. high
[0004] At present, it is generally believed that water is very unfavorable to the ethylene oligomerization reaction process. CN200810111717.8 discloses a method for ethylene oligomerization, which is strictly controlled in an anhydrous and oxygen-free environment. Therefore, the current ethylene oligomerization reaction is harmful to the process. The requirements are very demanding, resulting in very poor reaction initiation and repeatability of the oligomerization process
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Embodiment 1
[0043] 1. Catalyst synthesis of 2-acetyl-1,10-phenanthroline chloride 2,6-diethylanilinate iron (II) complex
[0044] a. Synthesis of 2-acetyl-1,10-phenanthroline (see the following reaction scheme)
[0045]
[0046] Put 5.1 g (28.3 mmol) of 1,10-phenanthroline into a 250 ml three-necked flask, and dissolve it with 100 ml of toluene under nitrogen protection and magnetic stirring. Slowly add 10ml of triethylaluminum (70.8mmol) dropwise to the three-necked flask under stirring at -60°C, the dropwise addition is completed in about 15 minutes, continue stirring at this temperature for 18h, then raise the temperature to about 30°C, and continue stirring 10h. Then the reaction mixture was cooled to about -30°C, 50ml of distilled water was slowly added thereto, and then heated to 30°C and stirred for 10h. Then separate the liquids, take out the organic phase, and extract the inorganic phase three times with dichloromethane, each time the consumption of dichloromethane is 20ml, ...
Embodiment 2
[0062] Same as Example 1, the difference is that the weight content of water is 20ppm. See Table 1 for the data.
Embodiment 3
[0064] Same as Example 1, the difference is that the weight content of water is 50ppm. See Table 1 for the data.
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Abstract
The invention discloses an ethylene oligomerization method. The method comprises the following steps: performing oligomerization reaction on ethylene in a reaction system which comprises a chloridized 2-acetyl-1,10-phenanthroline amine iron (II) complex main catalyst shown by a formula (I) in the specification, an aluminum-containing promoter, water and an organic solvent. According to the method disclosed by the invention, ethylene oligomerization reaction has relatively high oligomerization reaction activity and high alpha-olefin selectivity, and still has relatively good oligomerization reaction activity even under the condition of low Al / Fe ratio; and in addition, even the oligomerization reaction is performed at relatively low temperature, the relatively high oligomerization reaction activity can still be achieved. Moreover, in an oligomerization reaction process, the ethylene oligomerization method disclosed by the invention is rapid in reaction initiation, stable in operation and good in repeatability, and thus the technical biases of those skilled in the art can be overcome, unexpected technical effects can be achieved, and wide industrial prospects can be provided.
Description
technical field [0001] The invention relates to the field of ethylene oligomerization, in particular to an ethylene oligomerization reaction process method. Background technique [0002] Linear α-olefins are widely used in the fields of ethylene comonomers, surfactant synthesis intermediates, plasticizer alcohols, synthetic lubricating oils and oil additives. In recent years, with the continuous development of the polyolefin industry, the worldwide demand for α-olefins has grown rapidly. At present, the vast majority of α-olefins are prepared by ethylene oligomerization. The used catalyst of ethylene oligomerization mainly contains nickel series, chromium series, zirconium series and aluminum series etc., in recent years, Brookhart group (Brookhart, the people such as M, J.Am.Chem.Soc.,1998,120,7143-7144 ; WO99 / 02472,1999), Gibson group (Gibson, V.C. et al., Chem.Commun., 1998,849-850; Chem.Eur.J., 2000,2221-2231) found that some Fe(II) and Co The tridentate pyridine imin...
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