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Load-type olefin oligomerization catalyst and preparation method thereof

A catalyst and supported technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of catalytic activity and selectivity reduction, and achieve high catalytic performance The effect of activity and wide carbon number distribution

Active Publication Date: 2010-01-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large number of studies have shown that after the homogeneous catalyst is immobilized, its catalytic activity and selectivity are significantly reduced.

Method used

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  • Load-type olefin oligomerization catalyst and preparation method thereof
  • Load-type olefin oligomerization catalyst and preparation method thereof
  • Load-type olefin oligomerization catalyst and preparation method thereof

Examples

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preparation example Construction

[0020] The preparation method of catalyst of the present invention comprises the steps:

[0021] (1) After roasting the mesoporous silicon-aluminum material, add aromatic hydrocarbon, add organoaluminum compound under stirring condition, then wash and dry,

[0022] (2) Take the mesoporous silica-alumina material dried in step (1), fully react with the complex of formula (I) in the presence of aromatic hydrocarbon or halogenated alkane, wash with saturated hydrocarbon and then dry.

[0023] The step (1) of the method is to treat the carrier, first roasting the carrier, and then treating it with an organoaluminum compound. The calcination temperature of the mesoporous silica-alumina material is 200-800°C, preferably 400-600°C, and the calcination time is preferably 5-8 hours. The organoaluminum compound is preferably methylaluminoxane, isobutylaluminum-modified methylaluminoxane, diethylaluminum monochloride or triethylaluminum. The temperature for adding an organoaluminum com...

example 1

[0032] Preparation of mesoporous silica-alumina materials.

[0033] Take 100ml concentration as 90gAl 2 o 3 / L Al 2 (SO 4 ) 3 The solution was placed in a beaker, and ammonia water was added dropwise under stirring until the pH value of the system was 8, and the neutralization gelling temperature was 55°C. Add 50ml content of 60gSiO under stirring condition 2 / L of water glass, heated to 80°C for 4 hours; use NH 4 Cl solution according to precipitate (dry basis): ammonium salt: H 2With a mass ratio of O=1:0.8:15, the silicon-aluminum precipitate was ion-exchanged at 60° C. to remove sodium ions therein. The exchange was repeated twice, each time for 0.5 hours, washed with water, filtered after each exchange, and then dried at 120°C for 15 hours to obtain a mesoporous silica-alumina material with a chemical composition of 0.035Na 2 O·75.5Al 2 o 3 24.4SiO2 2 , the specific surface area is 378m 2 / g, the pore volume is 1.21ml / g, the average pore diameter is 10.55nm, t...

example 2

[0035] Preparation of the complexes described in the present invention.

[0036] Add 0.15 mol of salicylaldehyde and 0.15 mol of aniline into the reactor, add 100 ml of absolute ethanol to reflux at 80° C. for 4 hours, cool to 0° C., and precipitate crystals. After filtration, the obtained solid was recrystallized with 100 ml of absolute ethanol, and dried at 25° C. for 2 hours under reduced pressure to obtain yellow needle-like crystals, which were salicylaldehyde aniline.

[0037] 1 gram (0.004 mol) of nickel acetate tetrahydrate is added in 120 milliliters of dehydrated alcohol, stir, after the solid dissolves completely, add the salicylaldehyde aniline ligand of 1.58 gram (0.008 mol), stir 12 hours, have A large number of green solids precipitated, filtered, washed the filter cake 3 times with 30 ml of hexane, and dried the filter cake at 60° C. for 6 hours under reduced pressure to obtain a grass green solid powder, which was bis(salicylaldehyde aniline) nickel. The rati...

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Abstract

The invention relates to a load-type olefin oligomerization catalyst, which comprises a complex and an organic aluminum compound loaded on a medium-pore aluminum silica material and having an expression shown as formula (I). The catalyst contains 0.5 to 5.0 mass percent of nickel and 20 to 30 mass percent of aluminum; in the formula (I), R is selected from hydrogen, alkyl of C1 to C2, alkoxy or nitryl of C1 to C6, X is halogen or acetate moiety, and n is 1 or 2; the medium-pore aluminum silica material has a pseudo-boehmite phase structure, and comprises the anhydrous chemical composition based on the mass of oxide of (0-0.3)Na2O.(40-90)Al2O3.(10-60)SiO2, the specific surface area of the anhydrous chemical composition is between 200 and 400m<2> / g, the pore volume is between 0.5 and 2.0 ml / g, the average aperture is between 8 and 20nm and the most probable aperture is between 5 and 15nm. The catalyst is matched with the alkyl aluminum for olefin oligomerization, and higher reaction activity.

Description

technical field [0001] The invention relates to a supported olefin oligomerization catalyst and a preparation method thereof, in particular to a supported catalyst prepared by loading a nickel complex containing Schiff's base ligands on a carrier and a preparation method thereof. Background technique [0002] Olefin oligomerization is an important part of olefin polymerization. With the expansion of demand for specific products in modern production and life, the technology of olefin oligomerization, especially ethylene oligomerization, to prepare higher carbon number olefins has been rapidly developed. develop. [0003] Traditional and well-known ethylene oligomerization processes, such as Gulf, Ethyl, and SHOP processes, have problems such as harsh operating conditions, low single-pass catalyst activity, wide product carbon number distribution, difficult separation of products and raw materials, and difficult disposal of waste liquid, especially when the operating pressure ...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/28C07C2/22
Inventor 倪静荣峻峰景振华郑金玉
Owner CHINA PETROLEUM & CHEM CORP
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