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Load-type olefin oligomerization catalyst and preparation method thereof

A catalyst, supported technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as catalytic activity and selectivity reduction

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

[0018] The preparation method of supported olefin oligomerization catalyst of the present invention, comprises the steps:

[0019] (1) After roasting the mesoporous silicon-alumina material, add aromatic hydrocarbons or halogenated alkanes to fully stir,

[0020] (2) Add the aromatic hydrocarbon or halogenated alkane solution of the complex described in formula (I) to the material after the stirring treatment in step (1) to continue the stirring reaction, collect the solid matter and then dry it.

[0021] In the method, step (1) is to process the carrier, the calcination temperature of the mesoporous silicon-aluminum material is preferably 200-800° C., and the stirring temperature after adding aromatic hydrocarbons or halogenated alkanes to the mesoporous silicon-alumina material is 0-120°C, preferably 20-60°C, the mass ratio of the added aromatic hydrocarbon or halogenated alkane to the carrier is 10-50:1, preferably 15-40:1.

[0022] The step (2) of the method is the loadin...

example 1

[0030] Preparation of mesoporous silica-alumina materials.

[0031] 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 2 With 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

[0033] Preparation of the complexes described in the present invention.

[0034] Add 0.15 mol of salicylaldehyde and 0.15 mol of aniline into the reactor, add 100 ml of absolute ethanol and reflux at 80°C for 4 hours, cool down to 0°C, precipitate crystals, and filter. The obtained solid was recrystallized with 100 ml of absolute ethanol, and dried under reduced pressure at 25° C. for 2 hours to obtain yellow needle-like crystals, which were salicylaldehyde aniline.

[0035] 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, and washed the filter cake with 30 ml of hexane for 3 times, and dried the filter cake at 60°C for 6 hours under reduced pressure to obtain grass green solid powder, which was bis(salicylaldehyde aniline) nickel complex , the...

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Abstract

The invention discloses a load-type olefin oligomerization catalyst, which comprises a complex loaded on a medium-pore aluminum silica material and having an expression shown as formula (I). The catalyst contains 0.1 to 5.0 mass percent of nickel; in the formula (I), R is selected from hydrogen, alkyl of C1 to C12, 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 medium-pore aluminum silica material 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 used for olefin oligomerization and has higher reaction activity; and oligomerization products have wider distribution range without generating polymers.

Description

technical field [0001] The invention relates to an olefin oligomerization catalyst and a preparation method, in particular to a supported catalyst with a nickel complex as an active component and a preparation method. 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 is too high. High, reaching about 20MPa, which limits the econ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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