Ethylene oligomerization method

An ethylene oligomerization and ethylene technology, applied in the field of olefin polymerization, can solve the problems of unattainability, harsh environmental requirements and high unit price, and achieve the effects of high oligomerization reaction activity, simplified production process and high selectivity

Active Publication Date: 2015-05-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
At present, it is generally believed that water is very unfavorable to the ethylene oligomerization process
In addition, the oligomerization reaction has very strict requirements on the initiation environment, and it is strictly required to be carried out in an anhydrous and oxygen-free environment. Due to the special conditions, it is very difficult to achieve, so the reaction initiation, stability and repeatability of the oligomerization process are also very poor.
In addition, the organic solvent used in the oligomerization process is generally toluene. As we all know, toluene is a toxic aromatic hydrocarbon, which is irritating to the skin and mucous membranes and has an anesthetic effect on the central nervous system; and in the oligomerization products, the toluene content is relatively large , unable to meet the requirements for aromatic hydrocarbon content when used as a comonomer

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

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

[0040] Synthesis of a.2-benzoyl-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 60ml of benzyllithium 1.2M n-hexane solution (72mmol) 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 30°C About, continue to stir 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 dichloro...

Embodiment 2

[0058] The method of Example 1 was adopted to carry out the ethylene oligomerization reaction, 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

[0060] The method of Example 1 was adopted to carry out the ethylene oligomerization reaction, 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, which comprises that ethylene is subjected to an oligomerization reaction in a reaction system containing an iron 2-benzoyl-1,10-phenanthroline polyamine chloride coordination compound main catalyst represented by a formula (I), an aluminum-containing cocatalyst, water and an organic solvent, wherein the organic solvent is alpha-olefin of Cn (n is more than 4 and is less than or equal to 10), and in the formula, 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, and the oligomerization reaction process is optimized, such that the oligomerization activity is high, the ethylene oligomerization reaction process has characteristics of rapid initiation, stable operation, low toxicity, environmental protection, good catalysis effect and cost balancing, and strong practicality, the ethylene oligomerization reaction cost is substantially reduced, the catalytic effect and the production cost are comprehensively considered, and the industrial prospect is 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/32C07C11/02B01J31/22
CPCY02P20/52
Inventor 张海英刘珺王怀杰郑明芳李维真王争
Owner CHINA PETROLEUM & CHEM CORP
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