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Double-core nickel, copper olefin polymerization catalyst, preparation method and application thereof

A technology of polymerization catalyst and copper olefin, which is applied in the field of copper olefin polymerization catalyst and its preparation, binuclear nickel, can solve the problems of low molecular weight of polyolefin, narrow molecular weight distribution of polyolefin, poor processability, etc., and achieve the effect of high catalytic activity

Inactive Publication Date: 2008-03-19
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the α-diimine nickel catalyst discovered by Brookhart and the pyridine bisimide iron and cobalt catalyst reported by Gibson and the neutral nickel catalyst reported by Grubbs are all mononuclear homogeneous catalysts, which are catalyzed by α-diimine nickel catalyst. The molecular weight of the obtained polyolefin is low, but the molecular weight distribution of the polyolefin catalyzed by iron pyridine bisimide, cobalt catalyst and the neutral nickel catalyst reported by Grubbs is narrow and the processability is poor.

Method used

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  • Double-core nickel, copper olefin polymerization catalyst, preparation method and application thereof
  • Double-core nickel, copper olefin polymerization catalyst, preparation method and application thereof
  • Double-core nickel, copper olefin polymerization catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]Example 1: Preparation of Ligand L1:

[0029] Under nitrogen protection, 1,3-bis(2,6-diisopropylphenyl)imidazolium salt (0.1 mmol), NaOt-Bu (0.1 mmol), Pd(OAc) 2 (0.05mmol), toluene (60mL) was placed in a 250ml Schlenk bottle, stirred at 80°C for 10 minutes, then added 1,2,4,5-tetrabromobenzene (5.00mmol), p-toluidine (35mmol), NaOt- Bu (20mmol), reacted at 110°C for about 14h, cooled to room temperature, added n-hexane 60ml, filtered, CH 2 Cl 2 After washing to remove inorganic salts, the mixture was stirred at room temperature for 2 days under an oxygen atmosphere, and the solvent was removed to obtain 1.49 g of brick-red solid powder with a yield of 60%.

Embodiment 2

[0030] Example 2: Preparation of Ligand L2:

[0031] Under nitrogen protection, 1,3-bis(2,6-diisopropylphenyl)imidazolium salt (0.15mmol), NaOt-Bu (0.25mmol), Pd(OAc)2 (0.05mmol), 1, 4-Dioxane (60mL) was placed in a 250ml Schlenk bottle, stirred at 80°C for 10 minutes, and then added 1,2,4,5-tetrabromobenzene (5.00mmol), o-methylaniline (50mmol), NaO t -Bu (20mmol), reacted at 110°C for about 14h, cooled to room temperature, added n-hexane 60ml, filtered, CH 2 Cl 2 Washed to remove inorganic salts, placed in an oxygen atmosphere and stirred at room temperature for 2 days to remove CH 2 Cl 2 , to obtain 1.38 g of red solid powder with a yield of 57%.

Embodiment 3

[0032] Example 3: Preparation of Ligand L3:

[0033] Under nitrogen protection, 1,3-bis(2,6-diisopropylphenyl)imidazolium salt (0.1 mmol), NaOt-Bu (0.1 mmol), PdCl 2 (0.05mmol), xylene (60mL) was placed in a 250ml Schenk bottle, stirred at 80°C for 10 minutes, and then added 1,2,4,5-tetrabromobenzene (5.00mmol), 2,6-dimethylaniline ( 20 mmol), NaO t-Bu (50 mmol), reacted at 110 ° C for about 14 h, cooled to room temperature, added n-hexane 60 ml, filtered, CH 2 Cl 2 Washed to remove inorganic salts, placed in an oxygen atmosphere and stirred at room temperature for 2 days to remove CH 2 Cl 2 , 0.95 g of orange-red solid powder was obtained, and the yield was 35%.

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Abstract

The invention relates to a dinuclear nickel and Cu olefin polymerization catalyst with the coordination between 2, 5-diamino-1, 4-p-Benzoquinone diimine ligand and nickel acetylacetonate and copper acetylacetonate, a preparation method and applications. The expression of the catalyst is [M (acac) LM (acac)], wherein, L represents a ligand containing 2, 5-diamino-1, 4-p-Benzoquinone diimine coordinated with metal, M represents metal Ni or Cu, and acac represents acetylacetone. The dinuclear catalyst prepared by the invention has the advantages of simple preparation and good stability and has high catalytic activity under the function of neutral Lewis acid, such as methylaluminoxane (MAO) or modified methylaluminoxane (MMAO), etc., and under a mild condition, and by changing the substituent group on the ligand and with different activity, the invention can catalyze norbornene and methyl methacrylate to prepare polynorbornene and polymethyl methacrylate, which have different molecular weights, by homopolymerization.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, and in particular relates to binuclear nickel and copper olefin polymerization formed by the reaction of 2,5-diamino-1,4-p-benzoquinone bisimine ligand with nickel bisacetylacetonate and copper bisacetylacetonate. Catalyst and preparation method thereof. technical background [0002] As the pillar industry of modern polymer materials, the development of polyolefin industry is an important symbol to measure the development of a country's petrochemical industry. Polyolefin products have greatly promoted the development of human civilization, and olefin polymerization catalysts are the key to the development of the polyolefin industry. core. Since the advent of olefin polymerization catalysts in 1953, there have been three important milestones in the Ziegler-Natta catalytic system, metallocene catalytic system and late transition metal catalytic system in just over fifty yea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F4/602C08F10/00C08F32/00C08F20/14
Inventor 金国新黄远标
Owner FUDAN UNIV
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