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Ethylene oligomerization reaction method

A technology for ethylene oligomerization and water-containing ethylene, which is applied in the direction of chemical instruments and methods, hydrocarbons, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problem of poor reproducibility of oligomerization process reaction and ethylene process conditions Harsh, high production costs and other issues, to achieve high selectivity, good oligomerization reactivity, and stable operation

Active Publication Date: 2016-05-11
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

However, no matter 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 in large-scale ethylene oligomerization, 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
[0005] In addition, the water content of polymer grade ethylene is required to be below 5ppm, which makes the process conditions for producing ethylene more stringent

Method used

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preparation example Construction

[0045] The preparation of the procatalyst compound of the present invention is known per se, see CN102558243A, which is incorporated herein by reference.

[0046] According to a specific embodiment of the present invention, the main catalyst chlorinated 2-formyl-1,10-phenanthroline amide iron (II) complex represented by formula i can be prepared by the preparation method reported in Chinese patent application CN102532201A have to.

[0047] According to a specific embodiment of the present invention, the main catalyst chloride 2-acetyl-1,10-phenanthroline amide iron (II) complex shown in formula ii can be prepared by the preparation method reported in Chinese patent application CN102485733A have to.

[0048] According to a specific embodiment of the present invention, the main catalyst chlorinated 2-n-propionyl-1,10-phenanthroline amide iron (II) complex shown in formula iii can adopt the preparation method reported in Chinese patent application CN102558241A be made of.

[0...

Embodiment 1

[0055] 1. Synthesis of main catalyst 2-formyl-1,10-phenanthroline chloride 2,6-diethylanilinate iron(II):

[0056] The main catalyst is 2-formyl-1,10-phenanthroline chloride 2,6-diethylanilinium iron(II), which can be prepared by the preparation method reported in Chinese patent application CN102532201A.

[0057]

[0058] 2. Ethylene oligomerization reaction

[0059]The ethylene oligomerization reaction specifically comprises the steps: (1) in a 100ml continuous reaction device, the aqueous ethylene, solvent xylene, main catalyst solution (concentration is 2.5 μmol / ml, solvent is xylene) and cocatalyst solution (concentration is 715 μmol / ml, and solvent is xylene) enters reactor respectively, and flow rate is respectively 80g / h, 168.26g / h, 3.48g / h and 2.38g / h, and Al / Fe is 196 in the reaction system, keeps in reaction mass The residence time in the reactor is 30min; (2) the reaction pressure is 1MPa and the reaction temperature is 30°C, wherein, taking ethylene as the calc...

Embodiment 2-12

[0061] With embodiment 1, difference is that the weight content of water and reaction parameter are different. See Table 1 for the data.

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Abstract

The invention discloses an ethylene oligomerization reaction method; the method specifically comprises that water-containing ethylene is used as a raw material, and a complex chloro-2-acyl-1,10-phenanthroline amino-iron (II) represented by the formula (I) and used as a main catalyst, an aluminum-containing co-catalyst and an organic solvent are added; according to the method, an ethylene oligomerization reaction is carried out, the oligomerization reaction activity is high, the selectivity of alpha-olefin is high, the oligomerization reaction is fast to initiate, the operation is smooth and steady, and the repeatability is good; even when the aluminum / iron ratio is low, the catalyst still has good oligomerization reaction activity; therefore, the technical prejudice of technical personnel in the field is overcome, unexpected technical effects are obtained, and the catalytic effect and cost are better balanced, so that the cost of the ethylene oligomerization reaction is significantly decreased, the practicality is high, and the prospects for industrialization are broad.

Description

technical field [0001] The invention relates to the field of ethylene oligomerization, in particular to a continuous reaction 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. [0003] 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 tridentat...

Claims

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Application Information

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IPC IPC(8): C07C11/02C07C2/22B01J31/22
Inventor 王怀杰郑明芳张海英刘珺
Owner CHINA PETROLEUM & CHEM CORP
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