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Supported late-transition-metal catalyst used for ethylene polymerization

A late-transition metal and ethylene polymerization technology, which is applied in the field of supported late-transition metal catalysts, can solve the problems of increasing catalyst preparation costs, limiting the industrial application of late-transition metal catalysts, and the like

Active Publication Date: 2014-09-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is also possible to functionalize the catalyst ligand structure and load the late transition metal catalyst on silica gel by chemical bonding (CN10169111; CN101173012; CN101531724) to improve the loading efficiency of the catalyst, but the cost of catalyst preparation in this method is greatly increased, and the above disadvantages Limiting the Industrial Applications of Silica-Supported Post-Transition Metal Catalysts

Method used

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  • Supported late-transition-metal catalyst used for ethylene polymerization
  • Supported late-transition-metal catalyst used for ethylene polymerization
  • Supported late-transition-metal catalyst used for ethylene polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] (1) Preparation of chlorinated alkyl silicon / silica gel support

[0066] Under the protection of nitrogen, take 10.0 grams of dry silica gel carrier and put it into a glass reactor, add 100 ml of dried hexane, disperse into a suspension, add 1 ml of SiCl 2 (n-Bu) 2 , start stirring, heat up to 30° C., react for 4 hours, and dry in vacuum to obtain a solid powder with good fluidity.

[0067] (2) Preparation of organoaluminum / alkyl silicon chloride / silica gel carrier

[0068] Under nitrogen protection, take 5.0 grams of the modified silica gel carrier obtained above and add it to a glass reactor, add 60 milliliters of dried toluene, disperse into a suspension, and add 18 milliliters of 10 wt% MAO (methylaluminoxane) toluene solution , heated to 50 ° C, stirred for 4 hours, then washed three times with 50 ml × 3 toluene, then washed with hexane, and dried in vacuum to obtain a solid powder with good fluidity, that is, a silica gel carrier containing methylaluminoxane.

...

Embodiment 2

[0078] (1) Preparation of chlorinated hydrocarbyl silicon / silica gel support

[0079] With embodiment 1 step (1), only SiCl in embodiment 1 2 (n-Bu) 2 Change to SiCl 4 .

[0080] (2) Preparation of organoaluminum / chlorinated hydrocarbyl silicon / silica gel carrier

[0081] Same as step (2) of Example 1.

[0082] (3) Preparation of supported transition metal catalyst B

[0083]Same as step (3) of Example 1, only 0.096 grams of (2,6-bis[1-(2,4,6-trimethylbenimine) ethyl]pyridine ferric dichloride in Example 1 is replaced by 0.111 g of [2,6-bis[1-(2,6-diisopropylphenylimine) ethyl]pyridine ferric dichloride] (see below for its structure, see Patent WO9827124A1, Example 8 for its synthesis), The supported transition metal catalyst B was obtained. Characterized by ICP, in the catalyst B, the weight content of Fe was 0.20%, and the weight content of Al was 11.28%.

[0084]

Embodiment 3

[0086] (1) Preparation of chlorinated hydrocarbyl silicon / silica gel support

[0087] Same as (1) preparation method in Example 1.

[0088] (2) Preparation of organoaluminum / chlorinated hydrocarbyl silicon / silica gel carrier

[0089] Same as step (2) of Example 1, only 18 ml of 10% MAO was replaced with 13 ml of 2M diethylaluminum chloride.

[0090] (3) Preparation of supported transition metal catalyst C

[0091] Same as step (3) of Example 1, only 0.096 g of [2,6-bis[1-(2,4,6-trimethylbenimine) ethyl]pyridine ferric dichloride] in Example 1 was replaced It is 0.098 grams [(2,6-bis[1-(2-methyl 6-chloro-phenylimine) ethyl] pyridine ferric dichloride] (see below for its structure, see patent WO9827124A1 for its synthesis, Example 2 ), to obtain the supported transition metal catalyst C. Characterized by ICP, the weight content of Fe in catalyst C was 0.19%, and the weight content of Al was 12.04%.

[0092]

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Abstract

The invention relates to a supported late-transition-metal catalyst used for ethylene polymerization and a preparation method thereof. The catalyst comprises a late-transition-metal compound, a chlorinated alkyl silicon modifier, an organo aluminium compound and a silica gel carrier reaction product; the preparation method comprises the following steps: 1) preparation of a chlorinated alkyl silicon modified silica gel carrier, 2)preparation of an organo-aluminium modified silica gel carrier, and 3)preparation of the silica gel supported late-transition-metal catalyst; and the obtained late-transition-metal catalyst has high polymerization activity for catalyzing vinyl polymerization or copolymerization. The preparation method of the silica gel carrier is simple, and the obtained supported catalyst particles have good morphology with adjustable size.

Description

technical field [0001] The invention relates to a supported late transition metal catalyst for ethylene polymerization, a preparation method, and the application of the obtained catalyst in olefin polymerization. technical background [0002] In the development of olefin polymerization catalysts, the late transition metal catalysts developed in the 1990s have received great development and attention. Especially Ni, Pd and Fe, Co diimine catalyst system (WO9623010, WO9827124), nickel, palladium catalyst can produce branched or even hyperbranched high molecular weight polyethylene with narrow molecular weight distribution through homogeneous polymerization of ethylene, iron, cobalt The catalyst can catalyze ethylene to produce linear polyethylene with broad molecular weight distribution. However, olefin polymerization is carried out in a homogeneous phase, and the obtained polymer is in an amorphous state, which cannot be used in the widely used slurry method or gas phase pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/02C08F4/70C08F4/02
Inventor 高榕李岩廖浩瀚周俊领刘东兵王丽莎
Owner CHINA PETROLEUM & CHEM CORP
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