A kind of ethylene oligomerization continuous reaction method
An ethylene oligomerization and reaction technology, applied in chemical instruments and methods, hydrocarbons, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of poor repeatability caused by oligomerization reaction process and harsh ethylene process conditions , high production cost and other problems, to achieve the effect of high selectivity, good oligomerization reaction activity, and stable operation
Active Publication Date: 2018-01-23
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology
[0003] The Institute of Chemistry, Chinese Academy of Sciences reported a catalyst for ethylene oligomerization and polymerization (Eur.J.Inorg.Chem.2009,4149–4156), which is 2-benzoxazolyl-6-acetylcondensate Amine Fe 2+ Chloride, under the action of co-catalyst methyl aluminoxane, when the molar ratio of the metal aluminum in the co-catalyst to the central metal in the main catalyst is 200-2000, and the reaction temperature is 30-50 ° C, oligomerization and Polymerization activity up to 10 7 g mol(Fe) -1 h -1 ; and whether methylalumoxane or modified methylalumoxane is used as a cocatalyst, the cost is too high and the consumption is too large. When the cocatalyst is used in large-scale ethylene oligomerization, it will inevitably lead to high cost
[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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Embodiment 1
[0029] 1. Synthesis of main catalyst chloride 2-benzoxazolyl-6-acetyl condensed 2′,6′-diethylanilinate iron (II) complex
[0030] According to the preparation method reported in the literature (Eur.J.Inorg.Chem.2009, 4149–4156), 2-benzoxazolyl-6-acetyl 2′,6′-diethylaniline iron chloride was prepared (II) Complexes.
[0031] 2. The continuous reaction of ethylene oligomerization specifically comprises the following steps: (1) in a 100ml continuous reaction device, aqueous ethylene, solvent toluene, main catalyst solution (concentration is 2.5 μ mol / ml, solvent is toluene) and cocatalyst solution (concentration is 715 μ mol / ml, and solvent is toluene) enters reactor respectively, and flow rate is respectively 80g / h, 168.26g / h, 3.40g / h and 2.34g / h, and Al / Fe is 196.8 in the reaction system, keeps the reaction mass in The residence time in the reactor is 30min; (2) reaction pressure is 1MPa and reaction temperature is 30 ℃, wherein, take ethylene as calculation basis, the mass co...
Embodiment 2
[0033] Same as Example 1, the difference is that the mass content of water is 60ppm. See Table 1 for the data.
Embodiment 3
[0035] Same as Example 1, the difference is that the mass content of water is 150ppm. See Table 1 for the data.
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Abstract
The invention discloses a continuous reaction method for ethylene oligomerization, which is specifically to use water-containing ethylene as a raw material, and add the main catalyst chlorinated 2-benzoxazolyl-6-acetyl acetamide iron ( II) The complex is a main catalyst, an aluminum-containing cocatalyst and an organic solvent: according to the present invention, the catalyst of the present invention is used for the ethylene oligomerization process, which has very high oligomerization activity and the selectivity of α-olefins High, and the oligomerization reaction initiates rapidly, runs smoothly, and is reproducible; even at low aluminum / iron ratios, it still has very good oligomerization reactivity; this has just overcome the technical bias of those skilled in the art, and achieved Unexpected technical effects have been achieved, the catalytic effect and cost are well balanced, the cost of ethylene oligomerization has been greatly reduced, the practicability is strong, and the industrialization prospect is broad.
Description
technical field [0001] The invention relates to the field of ethylene oligomerization, in particular to a method for continuous 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 c...
Claims
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IPC IPC(8): C07C2/22C07C11/02C07C11/08B01J31/22
CPCY02P20/52
Inventor 刘珺郑明芳张海英王怀杰栗同林李维真吴红飞祁彦平
Owner CHINA PETROLEUM & CHEM CORP