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Polythene catalyst loaded by semi-metallocene

A catalyst and metallocene technology, applied in the field of polyethylene catalyst and preparation, can solve the problems of low catalytic activity and other issues

Inactive Publication Date: 2004-03-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, silica-supported metallocene and non-metallocene catalysts show lower catalytic activity

Method used

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  • Polythene catalyst loaded by semi-metallocene

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0024] The preparation method of the semi-metallocene active component described in formula (I) is: make TiX 4 with R'-C(O)-CH having the general formula 2 The β-diketone compound of -C(O)-R is reacted at the reflux temperature according to the molar ratio of 1:1-2, and the solvent is removed to obtain the β-diketone titanium compound. Then in an organic solvent, such as the presence of toluene, the alkali metal salt Cp'M of the cyclopentadiene skeleton compound reacts with the β-diketone titanium compound in an equimolar ratio, and the better method is to dissolve the β-diketone titanium compound first. Prepare a solution in toluene, then add Cp'M, react at -15 ~ 25 ° C, remove the solvent, the obtained solid matter is preferably washed with ether, or the solid matter is recrystallized and purified as required. The solvent used for recrystallization is Polar organic solvents such as halogenated alkanes. M in said Cp'M is an alkali metal, preferably sodium. For a more detai...

example 1

[0032] The supported catalyst whose active component is cyclopentadiene-(dibenzoylmethane)titanium dichloride was prepared by co-precipitation method.

[0033] (1) Preparation of active component cyclopentadiene-(dibenzoylmethane) titanium dichloride

[0034] a. TiCl with a concentration of 4.74% by weight 4 Diethyl ether solution, the ether solution of 56.06% by weight of dibenzoylmethane (Shanghai Reagent Factory) is added in a closed container, and the TiCl 4 The molar ratio to dibenzoylmethane was 1:1, stirred and heated to reflux temperature, reacted for 1 hour, filtered, and the solid was washed 3 times with ether to obtain (dibenzoylmethane)titanium trichloride.

[0035] b. 5.5 milliliters of cyclopentadiene was dissolved in 25 milliliters of tetrahydrofuran, and 1.4 grams of sodium metal was added at -10° C. to react for 2 hours. The solvent was removed under reduced pressure to obtain 4.67 grams of cyclopentadiene sodium.

[0036] c. (dibenzoylmethane) titanium tric...

example 2

[0042] A supported catalyst whose active component is cyclopentadiene-(dibenzoylmethane)titanium dichloride is prepared by the second method.

[0043] Put 0.5 grams of dry magnesium powder and 50 milliliters of dry heptane into the reaction flask, heat to 70°C, add 2.5 milliliters of n-chlorobutane and react for about 5 hours until the magnesium powder has completely acted on it to obtain n-butylmagnesium chloride. It was cooled to -2°C, and 20 ml of dichloromethane solution in which 1 gram of cyclopentadiene-(dibenzoylmethane)titanium dichloride was dissolved was slowly added dropwise, stirred and reacted for 1 hour, and after rising to room temperature, slowly Slowly add 1.5 g of activated silica gel, stir the reaction at room temperature for 1 hour, filter, and dry the solid at 20° C. for 6 hours to obtain 3.9 g of Catalyst B, which has a titanium content of 1.95% by weight and a magnesium content of 10.2% by weight.

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Abstract

The present invention provides a polyethylene catalyst in which the semimetallocene is loaded on its carrier, its titanium content is 0.1-10 wt%. It is characterized by that the semimetallocene active component can be loaded on the silicon dioxide carrier treated by alkyl magnesium halide or the semimetallocene active component can be reacted with alkyl magnesium halide, then loaded on the silicon dioxide carrier. Said catalyst can be matched with alkyl aluminium cocatalyst, and used for ethylene polymerization, it possesses higher activity, and the prepared polyethylene possesses higher molecular weight and good molecular weight distribution.

Description

technical field [0001] The invention relates to a polyethylene catalyst loaded with semi-metallocene active components and a preparation method. Specifically, it is an ethylene polymerization catalyst prepared by loading the active component of a semi-metallocene catalyst containing a ligand of a β-diketone derivative on a magnesium halide / silicon dioxide carrier. Background technique [0002] Following the typical transition metal compounds with cyclopentadiene and its derivatives as ligands, that is, metallocene catalysts, another class of metallocene compounds containing oxygen, nitrogen and other coordinated heteroatom ligands in the conjugated system is in the The application of polyolefins, especially polyethylene catalysts, has attracted more and more attention and attention. [0003] Metallocene compounds containing oxygen atoms in the ligand, such as titanium compounds with β-diketones and derivatives as ligands, can usually only be used for styrene polymerization,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/643C08F10/02
CPCY02P20/52
Inventor 孙敏许学翔常溪燕于鹏程薇景振华
Owner CHINA PETROLEUM & CHEM CORP