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Preparation method of polyvinyl catalyst of loading semi-metallocene

A catalyst and metallocene technology, applied in the field of polyethylene catalyst preparation, can solve the problems of low polymer bulk density, poor shape, limited loading capacity, etc., and achieve good polymer particle shape, good fluidity and strength, good The effect of catalytic activity

Active Publication Date: 2009-10-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] CN00124667.4 discloses an ethylene polymerization catalyst prepared by loading the active component of a semi-metallocene catalyst containing a β-diketone derivative ligand on an inorganic chloride and a preparation method thereof, but because it adopts a co-precipitation method, Therefore, the shape of the catalyst particles prepared by this method is not good, and there is a saturation value when supporting the active components, resulting in a limited loading capacity, and the prepared supported catalyst has a low titanium loading, so the polymerization efficiency per unit mass of the catalyst is not high. The resulting polymer has low bulk density and poor morphology

Method used

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  • Preparation method of polyvinyl catalyst of loading semi-metallocene
  • Preparation method of polyvinyl catalyst of loading semi-metallocene
  • Preparation method of polyvinyl catalyst of loading semi-metallocene

Examples

Experimental program
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preparation example Construction

[0025] The preparation method of the semi-metallocene active component of the formula (I) is: in the presence of ether, make TiX 4 with the general formula R'-C(O)-CH 2 The β-diketone compound of -C(O)-R is reacted at the reflux temperature according to the molar ratio of 1:1-3, and the solvent is removed to obtain the β-diketone titanium compound. Then in an organic solvent, the alkali metal salt Cp'M of the cyclopentadiene skeleton compound and the β-diketone titanium compound are reacted in an equimolar ratio as in the presence of toluene, and the better method is to make the β-diketone titanium compound first Dissolve in toluene to prepare a solution, 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 needed, and the solvent used for recrystallization For polar organic solvents, such as halogenated alkanes. M in said Cp'M is an alkali metal, preferably sodi...

example 1

[0030] The supported catalyst is prepared by the method of the invention.

[0031] (1) Preparation of cyclopentadiene-(dibenzoylmethane) titanium dichloride

[0032] TiCl with a concentration of 4.74% by mass 4 Ether solution, the ether solution of 56.06% by mass of dibenzoylmethane (produced by 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.

[0033] 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 sodium cyclopentadiene.

[0034] Dissolve (dibenzoylmethane) titanium trichloride in toluene to form a solution of 94.35% by mass, then add a toluene solution with a conc...

example 2

[0040] Prepare supported catalyst B by the method for example 1, difference is (c) adds 40 milliliters and contains 3.7 grams (9.10 * 10 -3 mol) cyclopentadiene-(dibenzoylmethane)titanium dichloride dichloromethane solution, the obtained catalyst B had a titanium content of 6.23% by mass, a magnesium content of 9.12% by mass, and an aluminum content of 1.01% by mass.

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Abstract

This invention relates to a preparation method of polyethylene catalyzer for loading half metallocene. suspend anhydrous magnesium chloride in inertia hydrocarbon solvent, take abundantly contact reaction with Ti ( OR1) 4 and C2 to C8 fatty alcohol, obtain carrier after dryness. Use aluminium alkyl to hand le above dry carrier under inertia hydrocarbon solvent presence, then through dryness, under polar organic solvent presence takes abundantly contact reaction with half metallocene active constituent possess ( I) expression, collect solid for dryness. In ( I) expression, R and R' could homology or inequality, is alkyl of C1 to C12, alkaryl of C6 to C9 or perfluoro- alkyl of C1 to C12. Cp' is ligand group containing cyclopentadiene skeleton. cyclopentadiene skeleton has 1 to 5 substituting group R2, and adjacent substituting group can attach each other to form binary or more condensed nucleus. R2 chosen from alkyl or perfluoro- alkyl of C1 to C18, aralkyl or alkaryl of C6 to C24, X is halogen, n is whole number of 1 to 3. This catalyzer has higher titanium loading amount, polymer grain shape good.

Description

technical field [0001] The invention is a preparation method of a polyethylene catalyst loaded with semi-metallocene. Specifically, it is a preparation method of a polyethylene catalyst loaded with a semi-metallocene active component containing a β-diketone derivative ligand. Background technique [0002] After metallocene catalysts, another kind of non-metallocene compounds containing oxygen, nitrogen and other coordinated heteroatom ligands in the conjugated system has attracted more and more attention and attention in the application of polyolefins, especially polyethylene catalysts. . The non-metallocene compound that contains oxygen atom in the ligand, as the titanium compound with β-diketone and derivative as ligand usually can only be used for styrene polymerization, as CN1158859A discloses a kind of titanium chloride with β-diketone Catalyst system for the synthesis of syndiotactic polystyrene as the main catalyst. Its preferred main catalysts are titanium chlorid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/645C08F110/02
Inventor 宗明生许学翔纪洪波程薇
Owner CHINA PETROLEUM & CHEM CORP
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