A kind of supported bridge bisphenoxy IVB metal catalyst and preparation method thereof

A metal catalyst, bisphenoxy technology, applied in the field of supported bridged bisphenoxy IVB metal catalyst and its preparation, can solve the problem of low activity

Inactive Publication Date: 2018-11-02
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the characteristics of the [ONNO] type bridged bisphenoxy IVB metal catalyst skeleton ligand, the [ONNO] type bridged bisphenoxy IVB metal catalyst is supported on MgCl 2 / Et n Al(OR) 3-n A new type of supported catalyst is formed on the carrier to solve the problem of low activity of the homogeneous [ONNO] type bridged bisphenoxy IVB metal catalyst. At the same time, its kinetic reaction is stable and efficient, and it has high catalytic activity. It can be prepared branched polyethylene

Method used

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  • A kind of supported bridge bisphenoxy IVB metal catalyst and preparation method thereof
  • A kind of supported bridge bisphenoxy IVB metal catalyst and preparation method thereof
  • A kind of supported bridge bisphenoxy IVB metal catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Example 1 Synthesis of Ligand Precursor L1

[0046] Add 100 mL of ethanol, 11.7 g of 3,5-di-tert-butyl salicylaldehyde, and 2.45 g of o-phenylenediamine into a 250 mL round-bottomed flask equipped with a magnet, N 2 Protected, heated to reflux for 6-8 h, cooled to room temperature and precipitated a yellow precipitate, after suction filtration, dried at 50 ℃ to obtain a yellow cotton flocculent solid, yield: 56.4%, to obtain diimine type [ONNO] type bridged bisphenoxy The base metal catalyst ligand precursor is denoted as L1. 1 H NMR (300 MHz, CDCl 3 ): δ :1.31 (s, 18H, C(CH 3 ) 3 ), 1.42 (s, 18H, C(CH 3 ) 3 ), 7.22(m, 4H, Ar-H), 7.30(m, 2H, Ar-H), 7.42(m, 2H, Ar-H), 8.63 (s, 2H,C=), 13.48(s, 2H , OH).

Embodiment 2

[0047] Example 2 Synthesis of Ligand Precursor L2

[0048] Add 100 mL of ethanol, 15.6 g of 3,5-di-tert-butyl salicylaldehyde, and 2.2 mL of ethylenediamine into a 250 mL round-bottomed flask equipped with magnets, N 2 Protected, heated to reflux for 4-6 h, cooled to room temperature and precipitated a yellow precipitate, filtered by suction, and dried at 50 ℃ to obtain a yellow cotton flocculent solid, yield: 89.4%, to obtain a diimine type [ONNO] type bridged bisphenoxy The metal catalyst ligand precursor is denoted as L2. 1 H NMR (300 MHz, CDCl 3 ): δ :1.28 (s, 18H, C(CH 3 ) 3 ), 1.43 (s, 18H, CH(CH 3 ) 3 ), 7.04(d, J=2.4 Hz, 2H, Ar-H), 7.34(J=2.4 Hz, 2H, Ar-H), 8.36 (s, 2H, C=), 13.59(s, 2H, OH)

Embodiment 3

[0049] Example 3 Synthesis of [ONNO] type bridged bisphenoxy metal catalyst 1

[0050] At a temperature of -20 ° Under C, add 2.536 g of ligand L1 to the Sehlenk bottle under nitrogen atmosphere, slowly add 5.0 mL of 1.0 mol / L titanium tetrachloride toluene solution dropwise, stir at this temperature for 60 min, then rise to room temperature and continue stirring After 24 h, the toluene solvent was removed by vacuum filtration; after washing with n-hexane, filtration, and removal of the n-hexane solvent by vacuum filtration, 2.81 g of gray powder was obtained, with a yield of 92%. Elemental analysis (C 36 h 46 Cl 2 N 2 o 2 Ti, mass %), theoretical value: C, 65.76; H, 7.05; N, 4.2.; found value: C, 64.93; H, 6.97; N, 4.2.

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Abstract

The invention discloses a supported bridged bis-phenoxy IVB metal catalyst and a preparation method thereof. The structural formula of the active component [ONNO]MX2 of the catalyst is disclosed as Formula (I) or Formula (II). The active component of the catalyst is supported on a triethyl-aluminum-modified MgCl2 / EtnAl(OR)[3-n] supporter, wherein R is C2-C5 straight-chain alkyl; and n represents the quantity of hydroxyl hydrogens substituted by triethyl aluminum in ethanol, and n=0-3. According to the characteristics of the [ONNO] bridged bis-phenoxy IVB metal catalyst framework ligand, the [ONNO] bridged bis-phenoxy IVB metal catalyst is supported on the MgCl2 / EtnAl(OR)[3-n] supporter to form a novel supported catalyst, thereby solving the problem of low activity in the homogeneous [ONNO] bridged bis-phenoxy IVB metal catalyst. The kinetic reaction of the novel supported catalyst is stable and efficient, has higher catalytic activity, and can be used for preparing branched polyethylene.

Description

technical field [0001] The invention belongs to the field of catalytic polymerization of olefins, and in particular relates to a supported bridged bisphenoxy IVB metal catalyst and a preparation method thereof. Background technique [0002] Polyethylene is the most demanded general-purpose plastic in the world. It is characterized by low price and good performance. It can be widely used in industry, agriculture and daily life, and occupies a pivotal position in the plastics industry. Therefore, the research on ethylene polymerization catalysts has always been an academic Research hotspots in the world and industry. Kol et al. (Tshuva, E. Y.; Goldberg, I.; Kol, M. J. Am. Chem. Soc. , 2000, 122, 10706.) In 2000, it was first discovered that [ONNO]-type bridging catalysts had certain activity for ethylene polymerization. With further research, it is found that the homogeneous [ONNO] type bridged catalyst has the following disadvantages for ethylene polymerization due to its o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/02C08F4/645C08F110/02
CPCC08F4/02C08F4/64189C08F110/02
Inventor 祝方明龙永江周启花梁华晴封硕魏婉楚李梅林伍青高海洋梁国栋
Owner SUN YAT SEN UNIV
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