Zirconium metal coordination polymer and synthesis method thereof and application thereof for catalyzing ethylene polymerization

A metal coordination and polymer technology, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problem of low activity, achieve high catalytic activity, convenient preparation, and low dosage low effect

Inactive Publication Date: 2014-08-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since its structure is not very suitable as a catalyst for olefin polymerization, the activity of polymerization is rather low (Tanski J.M., Wolczanski P.T.Inorg.Chem., 2001, 40:2026-2033)

Method used

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  • Zirconium metal coordination polymer and synthesis method thereof and application thereof for catalyzing ethylene polymerization
  • Zirconium metal coordination polymer and synthesis method thereof and application thereof for catalyzing ethylene polymerization
  • Zirconium metal coordination polymer and synthesis method thereof and application thereof for catalyzing ethylene polymerization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: Preparation of porous zirconium metal coordination polymer Zr-1

[0030]

[0031] Weigh 10.18g (0.22mmol) of ligand L and dissolve it in 10mL dry tetrahydrofuran solution under nitrogen, add 16.0mg (0.66mmol) sodium hydride and stir for 12 hours; add ZrCl to the reaction flask 4 (THF) 2 125 mg (0.33 mmol), refluxed for 3 days, the obtained yellow precipitate was washed with dry tetrahydrofuran, dichloromethane, and toluene, and then dried under vacuum at 120°C for 12 hours to obtain 0.21 g of yellow solid powder with a yield of about 75%. The composition of elemental analysis is: C56.57, H4.72, N3.28. The Zr content measured by ICP was 10.0%. The specific surface area of ​​Zr-1 measured by the specific surface area analyzer is 230m 2 / g. The single-point adsorption total pore volume of Zr-1 measured by the specific surface area analyzer is 0.17cm 3 / g, the total pore volume of micropores is 0.087cm 3 / g.

Embodiment 2

[0032] Embodiment 2: Preparation of porous zirconium metal coordination polymer Zr-2

[0033]

[0034] Weigh 20.19g (0.22mmol) of ligand L and dissolve it in 10mL dry tetrahydrofuran solution under nitrogen, add 16.0mg (0.66mmol) sodium hydride and stir for 12 hours; add ZrCl to the reaction flask 4 (THF) 2 125 mg (0.33 mmol), refluxed for 3 days, the obtained pale yellow precipitate was washed with dry tetrahydrofuran, dichloromethane and toluene, and then dried under vacuum at 120°C for 12 hours to obtain 0.24 g of yellow solid powder with a yield of about 85%. The composition of elemental analysis is: C55.55, H6.05, N3.29. The Zr content measured by ICP was 10.6%. The specific surface area of ​​Zr-2 measured by the specific surface area analyzer is 479m 2 / g. The single-point adsorption total pore volume of Zr-2 measured by the specific surface area analyzer is 0.31cm 3 / g, the total pore volume of micropores is 0.186cm 3 / g.

Embodiment 3

[0035] Embodiment 3: Preparation of porous zirconium metal coordination polymer Zr-3

[0036]

[0037] Weigh 30.20 g (0.22 mmol) of ligand L and dissolve it in 10 mL of dry tetrahydrofuran solution under nitrogen, add 16.0 mg (0.66 mmol) of sodium hydride and stir for 12 hours; add ZrCl to the reaction flask 4 (THF) 2 125 mg (0.33 mmol), refluxed for 3 days, the obtained yellow precipitate was washed with dry tetrahydrofuran, dichloromethane, and toluene, and then dried under vacuum at 120°C for 12 hours to obtain 0.19 g of yellow solid powder with a yield of about 68%. The composition of elemental analysis is: C54.64, H6.70, N3.72. The Zr content measured by ICP was 10.2%. The specific surface area of ​​Zr-3 measured by the specific surface area analyzer is 85m 2 / g. The single-point adsorption total pore volume of Zr-3 measured by the specific surface area analyzer is 0.13cm 3 / g, the total pore volume of micropores is 0.034cm 3 / g.

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Abstract

The invention discloses a zirconium metal coordination polymer and a synthesis method thereof and application thereof for catalyzing ethylene polymerization, and belongs to the technical field of porous coordination polymer materials. The method comprises the following steps: adding sodium hydride to an organic solution of a ligand at room temperature under the protection of nitrogen, reacting for 6-12 hours to prepare reaction liquid; adding a tetrahydrofuran adduct of zirconium tetrachloride to the reaction liquid, and carrying out reflux reaction for 2-3 days; carrying out drip washing respectively by using tetrahydrofuran, methylene dichloride and methylbenzene; drying in vacuum, so as to obtain the porous zirconium metal coordination polymer. The porous zirconium metal coordination polymer disclosed by the invention is taken as a catalyst and has good catalytic activity when used for catalyzing ethylene polymerization under the support of aluminum alkyl and boron cocatalysts, and the obtained polyethylene product has the characteristics of high molecular weight, wide molecular weight distribution, granular nanoscale and the like.

Description

technical field [0001] The invention belongs to the technical field of porous coordination polymer materials, in particular to the preparation of a porous zirconium metal coordination polymer olefin polymerization catalyst and its application in catalyzing ethylene polymerization. Background technique [0002] Polyolefin products have the advantages of low price, easy machining, good insulation and good corrosion resistance, and have been widely used in various fields of human life. Polyolefin products are essential elements in people's daily life. People's demand for polyolefin and its products is increasing. Therefore, it is necessary to develop novel olefin polymerization catalysts to prepare polyolefin materials with special properties. Compared with traditional Ziegler-Natta catalysts, single-site olefin polymerization catalysts such as metallocene catalysts, non-metallocene early-transition metal catalysts, and late-transition metal catalysts have a single active cente...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00C08F10/02C08F4/645
Inventor 母瀛李贺许博
Owner JILIN UNIV
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