Ethylene oligomerization method

A technology of ethylene oligomerization and ethylene, which is applied in the field of olefin polymerization, can solve the problems of oligomerization process reaction initiation, poor repeatability, unreachable, harsh environmental requirements, etc., and achieve the elimination of separation steps of aromatic solvents, high oligomerization activity, The effect of simplifying the production process

Active Publication Date: 2015-03-25
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Whether it is methylalumoxane or modified methylalumoxane, the unit price is relatively high, and when it is used for ethylene oligomerization on a large scale, it will inevitably lead to high production costs
And the oligomerization reaction is very harsh on the environment that initiates, it is generally believed that water is very unfavorable to the ethylene oligomerization reaction process
For example, CN200810111717.8 discloses a method for ethylene oligomerization, which is strictly controlled in an anhydrous and oxygen-

Method used

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Embodiment 1

[0039] 1. Catalyst synthesis of 2-isobutyryl-1,10-phenanthroline chloride 2,6-diethylanilinate iron (II) complex

[0040] a. Synthesis of 2-isobutyryl-1,10-phenanthroline (see the following reaction scheme)

[0041]

[0042] 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 15ml of triethylaluminum (d=0.75g / ml, 56.6mmol) 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, and then raise the temperature To about 30 ℃, continue to stir for 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 di...

Embodiment 2

[0057] The method of Example 1 was used for ethylene oligomerization, the difference being that the weight content of water was 20 ppm based on the weight of the solvent 1-hexene, and the analysis results were shown in Table 1.

Embodiment 3

[0059] The method of Example 1 was used for ethylene oligomerization, the difference being that the weight content of water was 50 ppm based on the weight of the solvent 1-hexene, and the analysis results were shown in Table 1.

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Abstract

The present invention discloses an ethylene oligomerization method, wherein ethylene is subjected to an oligomerization reaction in a reaction system containing an isobutyryl substituted 1,10-phenanthroline aminal iron (II) complex coordination compound main catalyst represented by a formula (I), an aluminum-containing assisted catalyst, water and a solvent, and the solvent is alpha-olefin of Cn (n is more than 4 and is less than or equal to 10), wherein in the formula (I), R1-R5 are respectively and independently selected from hydrogen, C1-C6 alkyl, halogen, C1-C6 alkoxy and nitro. According to the present invention, the technical prejudice is overcome, the oligomerization process is optimized, the oligomerization activity is high, and advantages of rapid ethylene oligomerization reaction process initiation, stable operation, low toxicity, environmental protection, good catalytic effect and cost balancing, and strong practicality; and the ethylene oligomerization reaction cost is substantially reduced, the catalysis effect and the production cost are comprehensively considered, and the industrialization prospects are broad.

Description

technical field [0001] The invention relates to the field of olefin polymerization, in particular to a method for ethylene oligomerization. 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 imine complex of (II)...

Claims

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Application Information

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IPC IPC(8): C07C11/02C07C2/22C07C2/34
CPCY02P20/52
Inventor 张海英王怀杰刘珺郑明芳栗同林李维真
Owner CHINA PETROLEUM & CHEM CORP
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