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Supported catalyst for olefin polymerization, as well as preparation method and application thereof

A supported catalyst and olefin polymerization technology, applied in the application field of 1-hexene and ethylene/1-octene copolymerization, can solve the problem that the new type of limited configuration double-bridge metallocene compound loading method has not been reported. , to improve the performance of the catalyst

Active Publication Date: 2013-09-11
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] There are many loading methods for metallocene catalysts, but there are no reports on the loading methods of novel constrained configuration double-bridge metallocene compounds

Method used

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  • Supported catalyst for olefin polymerization, as well as preparation method and application thereof
  • Supported catalyst for olefin polymerization, as well as preparation method and application thereof
  • Supported catalyst for olefin polymerization, as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Ligand [μ, μ-(SiMe 2 ) 2 (C 5 h 4 ) 2 ]Synthesis

[0057] Ligand [μ, μ-(SiMe 2 ) 2 (C 5 h 4 ) 2 ] The synthetic route is as follows:

[0058]

[0059]Add 50mL (0.42mol) of dimethyldichlorosilane to a 500mL three-neck flask, then add 100mL of n-hexane, and stir evenly. Add 260mL (0.84mol) of 1.6M sodium dicyanocene dropwise under ice-water bath conditions, react for 6 hours, add 50mL distilled water to wash, use a pear-shaped separatory funnel to separate liquid to remove the organic phase, wash the aqueous phase with 3 × 20mL ether, and combine the organic phase, dried over anhydrous magnesium sulfate, filtered, and the solvent was removed in vacuo. Distilled under reduced pressure, collected fractions at 40-42°C / 2mmHg to obtain 18.05 g of a light yellow liquid product with a yield of 22.9%.

[0060] Add the above product into a 250mL Schlenk bottle and dissolve it with 80mL of n-hexane. Under an ice-water bath, about 53 mL of 1.8M n-butyllithium was add...

Embodiment 2

[0062] Catalyst I [μ, μ-(SiMe 2 ) 2 (Allyl-C 5 h 2 )(C 5 h 3 )][(C 5 h 5 )ZrCl 2 ] 2 Synthesis

[0063] 1.04 g (4.3 mmol) of the ligand disilicon-bridged dicyclopentadiene prepared in Example 1 was added into a 100 mL Schlenk bottle, and 30 mL of n-hexane was added to dissolve it. In an ice-water bath, 2.4 mL (4.3 mmol) of 1.8M n-butyllithium was added dropwise, controlled for half an hour in the ice-water bath, and then naturally rose to room temperature, and stirred for 4 hours. The solvent was drained, the solid was washed with 2×10 mL of n-hexane, and then dried, the solid was dissolved in 30 mL of tetrahydrofuran, 0.52 g (4.3 mmol) of allyl bromide was added dropwise, and the reaction was stirred overnight at room temperature. The solvent was drained, and the remaining substance was extracted with 3×20 mL of n-hexane, and then 4.8 mL (8.6 mmol) of 1.8M n-butyllithium was added dropwise and reacted for 4 hours. Drain the solvent, wash the solid with 2×10mL n-hex...

Embodiment 3

[0065] Catalyst II [μ, μ-(SiMe 2 ) 2 (Allyl-C 5 h 2 )(C 5 h 3 )][(C 5 h 5 )TiCl 2 ] 2 Synthesis

[0066] The preparation steps are the same as in Example 2, replacing 1.52g (4.3mmol) CpZrCl with 4.3mmol titanium trichloride 3 · DME, a dark red solid was finally obtained with a yield of 36%.

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Abstract

The invention relates to a supported catalyst for olefin polymerization, as well as a preparation method and an application thereof. The catalyst comprises a double-silicon double-bridge metallocene compound, an aluminum alkyl or aluminoxane compound or a mixture thereof and an inert inorganic compound carrier. The preparation method comprises steps of: completing the reaction of the inorganic compound carrier with the aluminum alkyl or aluminoxane compound at a reaction temperature of 80 DEG C-110 DEG C according to a weight ratio of (1:1)-(1:5); dissolving the double-silicon double-bridge metallocene compound into a methylbenzene solvent, adding the mixture into the liquid of the inorganic compound carrier and the aluminum alkyl or aluminoxane at the reaction temperature of 0 DEG C-60 DEG C according to a weight ratio of double-silicon double-bridge metallocene compound to inorganic compound carrier of (1:3)-(1:10), then removing the solvent, filtering, washing and pumping at reduced pressure so as to obtain the catalyst. The catalyst can be used for olefin polymerization or the polymerization of ethylene and alpha-olefin with 3-20 carbon atoms, and the content of the alpha-olefin in a copolymer is high.

Description

technical field [0001] The invention relates to a supported catalyst for olefin polymerization and its preparation, and its application in ethylene polymerization, ethylene / α-olefin copolymerization, especially 1-hexene and ethylene / 1-octene copolymerization. Background technique [0002] Z-N catalysts and chromium-based catalysts catalyze the polymerization of α-olefins to produce polymers with a fairly wide molecular weight distribution; the distribution of molecular weight affects the physical properties of the polymer, which in turn determines the final use of the polymer. [0003] It is well known that "single-site catalysts" can produce ethylene polymers with narrow molecular weight distribution and excellent physical properties. WO 91 / 09882 reports that single-site metallocene-aluminoxane catalysts produce copolymers with narrower molecular weights than expected. Central cationic catalysts have outstanding catalytic activity, but are extremely sensitive to impurities...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/6592C08F10/02
Inventor 王亚丽米普科李建忠王斯晗褚洪岭许胜张宝军王桂芝刘敏贺德福吴志祥徐显明熊玉洁陈谦张洪达张志高王力搏任迎春张德顺王秀绘于部伟黄付玲韩雪梅魏福成曾群英赵贵桥王东军刘丽莹王淑兰官鹏鹏张君杨晓莹
Owner PETROCHINA CO LTD
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