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Polypropylene catalyst preparation method

A polypropylene catalyst and catalyst technology are applied in the field of preparation of supported metallocene catalysts, which can solve the problems of low bulk density, poor sPP morphology, and inapplicability, and achieve the effects of high activity and excellent morphology.

Active Publication Date: 2020-01-31
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sPP obtained by using a homogeneous metallocene catalyst has poor morphology an

Method used

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  • Polypropylene catalyst preparation method

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preparation example Construction

[0036] The preparation method of polypropylene catalyst of the present invention specifically comprises the steps:

[0037] After the carrier is dispersed in the solvent, add aluminum alkyl, boric acid and water, add the metallocene complex to continue the reaction after the reaction, wash and dry after the reaction to obtain the target catalyst system; wherein the carrier is silicon dioxide, two The specific surface area of ​​silicon oxide is in the range of 200m 2 / g~600m 2 / g, the particle size ranges from 10 to 60 μm, and the pore volume ranges from 0.8 to 3 mL / g. The carrier silica should be heat-treated (activated) before the reaction, that is, treated at 400-600° C. for 2-24 hours under the protection of nitrogen flow. The surface hydroxyl content of the obtained silica gel is in the range of (1-5) OH / nm 2 .

[0038] In the supported metallocene catalyst system for preparing syndiotactic polypropylene, the (water+boric acid) / alkylaluminum molar ratio is 0.7-0.95, an...

Embodiment 1

[0044] Silica gel activation (heat treatment)

[0045] Brand name is 2408D (Grace Corporation) silica gel, in N 2 Under protection, activate at 200°C for 2 hours, raise the temperature from 200°C to 600°C within 4 hours, activate at 600°C for 4 hours, cool down to room temperature, and store under nitrogen gas.

Embodiment 2

[0047] Catalyst preparation

[0048] Add 3.0g of activated silica gel to the reaction flask, add 30mL of toluene, cool down to 0°C, slowly add 50mL of 1M trimethylaluminum solution dropwise, react for 1 hour, cool down to -15°C, add 0.79g of 3,5-difluoro Phenylboronic acid, after reacting for 1 hour, slowly add 0.63g of water dropwise, heat up to 40°C and react for 12h, slowly add 0.08g of isopropylidene (cyclopentadiene) (9-fluorenyl) zirconium dichloride in toluene ( 10mL) solution. After continuing to react for 1 h, filter, wash with 15 mL of toluene three times, and drain to obtain 5.2 g of supported catalyst.

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Abstract

The invention discloses a polypropylene catalyst preparation method, wherein the catalyst is a supported metallocene catalyst for preparing syndiotactic polypropylene. The preparation method comprises: adding a heat-treated carrier into a solvent, dispersing, adding aluminum alkyl, boric acid and water, reacting, adding a metallocene coordination compound after the reaction is finished, and continuously carrying out a reaction to obtain the catalyst, wherein the metallocene coordination compound is represented by a general formula (1) R<1>(CpR<2>n)(FluR<3>m)MQ2, Cp is cyclopentadienyl, Flu isfluorenyl, R<2> and R<3> are respectively and independently selected from H, C1-C12 alkyl, aryl and halogen, m and n are integers of 0-4, R<1> is a bridging group of cyclopentadienyl and fluorenyl, Mis zirconium or hafnium, and Q is halogen or C1-C6 alkyl.

Description

technical field [0001] The invention relates to a preparation method of a polypropylene catalyst, in particular to a preparation method of a supported metallocene catalyst used for preparing syndiotactic polypropylene. Background technique [0002] Syndiotactic polypropylene sPP was first reported in patent US 3305538, and the catalyst in this patent can only prepare sPP obtained by a small amount of extraction. Since Ewen JA adopted a C s Symmetrical metallocene catalyst system can prepare high syndiotactic polypropylene (J.Am.Chem.Soc., 1988, 110, 6255-6256.). However, the sPP obtained by using a homogeneous metallocene catalyst has poor morphology and low bulk density, and is not suitable for existing polypropylene industrial devices. If the metallocene catalyst is to be applied to the existing polypropylene process, it generally needs to be used after loading. The earliest and most commonly used loading method in industry is to pre-mix the alkyl aluminoxane (such as m...

Claims

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Application Information

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IPC IPC(8): C08F10/06C08F110/06C08F4/02C08F4/6592
CPCC08F10/06C08F110/06C08F4/025C08F4/65927C08F2500/16C08F2500/03C08F2500/01
Inventor 许蔷袁苑义建军张洪滨吴伟于锋邸得利王莉李荣波
Owner PETROCHINA CO LTD
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