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Dual core metallocene catalyst and preparation method and applications thereof

A metallocene compound and reaction technology, applied in the field of binuclear metallocene catalyst and its preparation and application

Active Publication Date: 2019-06-07
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN102942644, CN102180977, CN102993341 disclose a kind of preparation method of heterobinuclear metallocene catalyst, but only limited to the bimodal polyethylene that produces wide molecular weight distribution

Method used

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  • Dual core metallocene catalyst and preparation method and applications thereof
  • Dual core metallocene catalyst and preparation method and applications thereof
  • Dual core metallocene catalyst and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] {[(Me 3 Cp)PhN t Bu]TiCl 2} 2 C 10 h 6 The preparation method route of catalyst is as follows:

[0079]

[0080] 1) Preparation of component 1

[0081] Add 2,6-dibromonaphthalene (14.298g, 50mmol) into 50mL diethyl ether solvent, stir slowly at -50°C and add 40mL 2.5M n-BuLi hexane solution dropwise, and rise to room temperature ( 25°C or so) stirring and reacting for 6h, the obtained white turbid suspension was filtered to obtain a white solid lithium salt;

[0082] The resulting product was added to 40 mL of THF solvent, cooled to -78°C, and a mixed solution of 2,3,4-trimethylcyclopent-2-enone (12.433 g, 100 mmol) and 20 mL of THF was slowly added dropwise, After the dropwise addition, raise it to room temperature (about 25°C) and stir for 10 hours. After the reaction, filter the solid and remove the solvent to obtain a colorless oily liquid; A small amount of formic acid (0.046 g, 1 mmol) was added, stirred for 1 h, then 60 mL of n-hexane was added, stirre...

Embodiment 2

[0091] {[(Me 3 Cp)SiMe 2 N t Bu]TiCl 2} 2 C 10 h 6 The preparation method route of catalyst is as follows:

[0092]

[0093] 1) Preparation of component 1

[0094] Add 2,6-dibromonaphthalene (14.298g, 50mmol) into 50mL diethyl ether solvent, stir slowly at -50°C and add 40mL 2.5M n-BuLi hexane solution dropwise, and rise to 25°C after the dropwise addition Stir left and right to react for 6 hours, and filter the obtained white turbid suspension to obtain a white solid lithium salt; add 40mL THF solvent, cool to -78°C, slowly add 2,3,4-trimethylcyclopentyl- Mixed solution of 2-enone (12.433g, 100mmol) and 20mL of THF. After the dropwise addition, raise the temperature to about 25°C and stir for 10h. After the reaction, filter the solid and remove the solvent to obtain a colorless oily liquid. Continue to add 40mL Added p-toluenesulfonic acid (0.172g, 1mmol) at room temperature (around 25°C), stirred for 1 hour, added 60 mL of n-hexane, stirred and washed for 0.5 hour...

Embodiment 3

[0104] Ethylene / α-olefin solution copolymerization was carried out in a 2L stainless steel batch reactor with magnetic stirring.

[0105] Under the protection of inert gas, add 1000mL Isopar E solvent and 5mL 1.1M triisobutylaluminum hexane solution to the reaction kettle, stir quickly to remove the water and oxygen impurities in the reaction kettle, then dry it under high temperature vacuum and replace it with ethylene gas three times. Keeping the slight positive pressure in the kettle, add 1000mL of Isopar E solvent, 250mL of 1-octene and 6.7mL of 1.5M MAO hexane solution to the reaction kettle in sequence at a stirring speed of 500rpm, then raise the temperature to the reaction temperature of 90°C, and pass Enter ethylene gas to keep the pressure in the kettle stable at the required polymerization reaction pressure of 1.0Mpa; then add 5mL of 0.002M Isopar E solution of component 3 (prepared in Example 1) to the kettle by ethylene pressure to start polymerization reaction. ...

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Abstract

The invention relates to a dual core metallocene catalyst and a preparation method and applications thereof. The catalyst comprises two parts: a main catalyst and a co-catalyst; wherein the main catalyst is formed by bridging two molecules containing IVB-IIB group transition metal atoms with an organic metal complex formed by a cyclopentadienyl group or a substituted cyclopentadienyl group throughrigid groups. The catalyst is applied to ethylene / alpha-olefin solution co-polymerization reactions under the assistance of an activating co-catalyst, has extremely good polymerization activity and copolymerization performance, and can be used to prepare high molecular weight ethylene / alpha-olefin random copolymer with a high alpha-olefin content.

Description

technical field [0001] The invention relates to a binuclear metallocene catalyst, a preparation method and application thereof. Background technique [0002] In the process of polyolefin technology development, single-site catalysts represented by metallocene catalysts have played an important role in the development of new polyolefin materials due to their high polymerization activity, excellent copolymerization performance, and precise control of polymer structure, molecular weight, and distribution. show more and more obvious advantages. Metallocene catalysts with excellent copolymerization properties can realize the copolymerization of ethylene / α-olefins, which can be used to prepare linear low-density polyethylene (LLDPE) plastomers, and can obtain narrow molecular weight distribution and uniformity by increasing the amount of comonomer insertion Polyolefin elastomer (POE) with short chain branch distribution. Polyolefin elastomer (POE) is a kind of thermoplastic elas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/16C08F210/14C08F4/6592
Inventor 林小杰黄玲燕张彦雨李祥卢福广陈杰王勤隆王丹石正喜黄明路陈冠良刘帮明张田财王金强
Owner WANHUA CHEM GRP CO LTD
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