A kind of supported late transition metal catalyst for ethylene polymerization, preparation method and application

A technology for polymerizing late transition metal and ethylene, which is applied in the field of preparation of supported late transition metal catalysts, and can solve the problems of uncontrollable, poor carrier particle shape, and complicated carrier preparation.

Active Publication Date: 2016-06-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many research reports (PCTInt.Appl.99 / 21898; US6,455,647; J.Mol.Catal.A2002,188,123; PCTInt.Appl.2004 / 078804) for magnesium chloride compound-loaded single-site catalysts, the carrier preparation And the cost of catalyst loading is high, and the particle shape of the carrier is poor, which cannot be controlled; although the use of spherical magnesium chloride can ensure that the supported catalyst has a good particle shape, the carrier contains components such as alcohol, water, and alkoxy groups, and the preparation of the carrier is complicated. The above shortcomings limit the industrial application of MgCl-supported single-site catalysts

Method used

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  • A kind of supported late transition metal catalyst for ethylene polymerization, preparation method and application
  • A kind of supported late transition metal catalyst for ethylene polymerization, preparation method and application
  • A kind of supported late transition metal catalyst for ethylene polymerization, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] (1) Preparation of chlorinated hydrocarbyl silicon / magnesium chloride support

[0068] Under the protection of nitrogen, take 10.0 g of magnesium chloride 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.

[0069] (2) Preparation of organoaluminum / hydrocarbyl chloride / magnesium chloride carrier

[0070] Under nitrogen protection, take 5.0 grams of the modified magnesium chloride 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 magnesium chloride carr...

Embodiment 2

[0080] (1) Preparation of chlorinated hydrocarbyl silicon / silica gel support

[0081] With embodiment 1 step (1), only SiCl in embodiment 1 2 (n-Bu) 2 Change to SiCl 4 .

[0082] (2) Preparation of organoaluminum / hydrocarbyl chloride / magnesium chloride carrier

[0083] Same as step (2) of Example 1.

[0084] (3) Preparation of supported transition metal catalyst B

[0085] 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 Replaced with 0.111 grams of [(2,6-bis[1-(2,6-diisopropylphenylimine) ethyl]pyridine ferric dichloride] (see below for its structure, see patent WO9827124A1 for its synthesis, examples 8) to obtain the supported transition metal catalyst B. Characterized by ICP, the weight content of Fe in catalyst B is 0.22%, and the weight content of Al is 11.41%.

[0086]

Embodiment 3

[0088] (1) Preparation of chlorinated hydrocarbyl silicon / silica gel support

[0089] Same as (1) preparation method in Example 1.

[0090] (2) Preparation of organoaluminum / hydrocarbyl chloride / magnesium chloride carrier

[0091] Same as step (2) of Example 1, only 18 ml of 10% MAO was replaced with 13 ml of 2M diethylaluminum chloride.

[0092] (3) Preparation of supported transition metal catalyst C

[0093] 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 Replaced with 0.098 g [(2,6-bis[1-(2-methyl 6-chloro-phenylimine) ethyl]pyridine ferric dichloride] (see below for its structure, see patent WO9827124A1 for its synthesis, examples 2) The supported transition metal catalyst C was obtained. Characterized by ICP, the weight content of Fe in catalyst C was 0.20%, and the weight content of Al was 11.92%.

[0094]

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Abstract

The invention relates to a supported late transition metal catalyst for ethylene polymerization, and a preparation method thereof, the catalyst comprising (a) a late transition metal compound; (b) hydrocarbyl silicon chloride; (c) an organoaluminum compound; (d) magnesium chloride A reaction product of a carrier; the preparation method thereof comprises: (1) preparation of a chlorinated hydrocarbyl silicon-modified magnesium chloride carrier, (2) preparation of an organoaluminum-modified magnesium chloride carrier, (3) preparation of a transition metal catalyst supported by magnesium chloride, and the obtained The late transition metal catalysts catalyzed ethylene polymerization or copolymerization have high polymerization activity. The preparation method of the magnesium chloride carrier used is simple, and the obtained loaded catalyst particle has good shape and adjustable size. The supported catalyst obtained by the method catalyzes the copolymerization reaction of ethylene and α-olefin, has high polymerization activity, and the obtained resin powder has good particle shape and high bulk density, and is applicable to slurry method and gas phase method polymerization technology.

Description

technical field [0001] The invention relates to a preparation method of a supported late transition metal catalyst for ethylene polymerization, 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 even hyperbranched high molecular weight polyethylene with narrow molecular weight distribution through ethylene homogeneous polymerization, 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 polymer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/646C08F4/658C08F4/656C08F4/655C08F4/654C08F4/02
Inventor 高榕廖浩瀚李岩周俊领刘东兵黄廷杰
Owner CHINA PETROLEUM & CHEM CORP
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