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External electron donor for olefin polymerization catalyst, catalyst system and preparation method of polyolefin

An external electron donor and olefin polymerization technology, which is applied in the field of olefin polymerization catalyst system to prepare polyolefin, can solve the problems of high branching efficiency, large amount of monomer, low long-chain branching efficiency, etc., and achieves increased melt elasticity, The effect of improving the efficiency of long chain branching

Active Publication Date: 2020-07-14
INST OF CHEM CHINESE ACAD OF SCI +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the problems existing in the prior art that it is difficult to form long-chain branched structures in situ for polyolefins prepared by using external electron donors; for polyolefins prepared by comonomers, the efficiency of long-chain branching is low , requires post-processing, and the problem of large amount of monomers. Provides an external electron donor for olefin polymerization catalysts, a catalyst system and a preparation method for polyolefins. The external electron donors for olefin polymerization catalysts catalyze olefin polymerization in a Ziegler-Natta catalyst system , the dosage is small, the isotacticity, molecular weight, and molecular weight distribution of polyolefin can be adjusted, and more importantly, polyolefin with long-chain branched structure can be obtained without post-treatment process, and the branching efficiency is high

Method used

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  • External electron donor for olefin polymerization catalyst, catalyst system and preparation method of polyolefin
  • External electron donor for olefin polymerization catalyst, catalyst system and preparation method of polyolefin
  • External electron donor for olefin polymerization catalyst, catalyst system and preparation method of polyolefin

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preparation example Construction

[0040] The third aspect of the present invention provides a method for preparing polyolefin, wherein the method comprises: performing bulk polymerization, gas phase polymerization or slurry polymerization of olefin monomers in the presence of the above catalyst system.

[0041] In the present invention, the olefin may be, but not limited to: ethylene or propylene.

[0042] In the present invention, bulk polymerization refers to liquid phase bulk polymerization, for example, liquid propylene is subjected to bulk polymerization in the presence of the above-mentioned catalyst system.

[0043] In the present invention, gas-phase polymerization refers to the polymerization of olefin monomers in a gasified state, for example, the polymerization of gaseous propylene is catalyzed in the presence of the above-mentioned catalyst system.

[0044] In the present invention, slurry polymerization refers to the polymerization of olefin monomers catalyzed by the above-mentioned catalyst syste...

preparation example 1

[0055] (1) Preparation of Dihexenyldiethoxysilane

[0056] The steps are: under the protection of nitrogen, the divinyl silane (Hexe 2 SiH 2 , 3.92g, 20mmol), absolute ethanol (Et 2 OH, 3.04g, 66mmol) and palladium chloride (PdCl 2 , 0.002g, 0.02mmol) of the mixture was dispersed in 80ml of benzene, the mixture was stirred at room temperature for 1h, and then the product A was obtained by distillation under reduced pressure.

[0057] (2) Characterization confirmation is the compound

[0058] The hydrogen spectrum of A: 1 H NMR (300MHz, CDCl 3 ,ppm)δ:0.64(t,4H),1.22(t,6H),1.43(m,8H),2.05(m,4H),3.81(m,4H),4.94(q,4H),5.80(m ,2H). The hydrogen spectrum is as follows figure 2 shown.

[0059] A carbon spectrum: 13 C NMR (300MHz, CDCl 3 , ppm) δ: 10.14, 32.21, 33.28 (CH 2 ), 18.16 (OCH 2 CH 3 ), 22.17 (SiCH 2 ), 58.18 (OCH 2 ), 114.06 (=CH 2 ), 138.87(CH). The carbon spectrum is as follows image 3 shown.

[0060] The silicon spectrum of A: 29 Si NMR(300MHz,ppm)δ:...

preparation example 2

[0063] (1) Preparation of dioctenyl dimethoxysilane

[0064] The steps are: under the protection of nitrogen, the dioctenylsilane (Octe 2 SiH 2 , 5.04g, 20mmol), absolute ethanol (MeOH, 3.26g, 102mmol) and palladium chloride (PdCl 2 , 0.004g, 0.04mmol) of the mixture was dispersed in 80ml of benzene, the mixture was stirred at room temperature for 1h, and then the product B was obtained by distillation under reduced pressure.

[0065] (2) Characterization confirmation is the compound

[0066] The hydrogen spectrum of B: 1 H NMR (300MHz, CDCl 3 ,ppm)δ:0.62(t,4H),1.35(m,16H),2.03(m,4H),3.56(m,6H),5.0(q,4H),5.78(m,2H). Figure such as Figure 5 shown.

[0067] Carbon spectrum of B: 13 C NMR (300MHz, CDCl 3 , ppm) δ: 11.86 (SiCH 2 ), 22.63, 28.75, 33.21, 33.80 (CH 2 ),50.26(OCH 3 ), 114.12 (=CH 2 ), 139.16(CH). The carbon spectrum is as follows Figure 6 shown.

[0068] Silicon spectrum of B: 29 Si NMR(300MHz,ppm)δ:-4.66(R 2 SiOCH 3 ).Silicon spectrum such as Fi...

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Abstract

The present invention relates to the field of catalysts for olefin polymerization, and discloses an external electron donor for olefin polymerization catalysts, a catalyst system, and a polyolefin preparation method, wherein the external electron donor has a structure represented by a formula (I) defined in the specification, m is an integer of 0-20, and R is methyl or ethyl. According to the present invention, with the application of the external electron donor to catalyze olefin polymerization in a Ziegler-Natta catalyst system, the consumption of the external electron donor is low, the isotacticity, the molecular weight and the molecular weight distribution of the polyolefin can be regulated, more importantly the polyolefin having a long chain branching structure can be obtained, the branching efficiency is high, and the post-treatment process is not needed.

Description

technical field [0001] The invention relates to the field of catalysts for olefin polymerization, in particular to an external electron donor for olefin polymerization catalysts, an olefin polymerization catalyst system, and a method for preparing polyolefins from the olefin polymerization catalyst system. Background technique [0002] Since Ziegler and Natta pioneered the field of polymer synthesis of Ziegler-Natta (Ziegler-Natta) catalyst system in the 1950s, the development of Ziegler-Natta catalysts can be divided into five generations, the first generation being δ-TiCl 3 AlCl 3 -AlEt 2 Cl system, the second generation is δ-TiCl 3 · R 2 O-AlEt 2 Cl system, the third generation is TiCl 4 / monoester / Mg 2 Cl 2 -AlR 3 / monoester system, the fourth generation is TiCl 4 / Diester / MgCl 2 -AlEt 3 / siloxane system, the fifth generation is TiCl 4 / diether / MgCl 2 -AlEt 3 . At present, the catalysts used in the industrial production of polypropylene are mainly the four...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/06C08F110/02C08F4/649C08F4/646
Inventor 杨婷婷王立才秦亚伟李伟董金勇郑国彤
Owner INST OF CHEM CHINESE ACAD OF SCI
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