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N,O-double ligand metal catalyst with stereo structure and preparation method

A metal catalyst and three-dimensional structure technology, applied in the field of the main catalyst of the catalytic system, can solve the problems of poor resistance to polar groups, reduced activity, etc., and achieve the effects of high light transmittance, low moisture absorption rate, and good processing performance

Inactive Publication Date: 2012-06-20
江西耀泰铜业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Early Ziegler-Natta catalysis can be used to catalyze the polymerization of norbornene, but due to its poor resistance to polar groups, this catalyst is limited in the synthesis of norbornene with polar norbornene derivatives or 1-alkenes. Application in copolymerization; metallocene catalysts can also be used to catalyze the polymerization of norbornene, but the active centers of these catalysts are mostly pre-transition metal catalysts, which are highly electrophilic and easy to coordinate heteroatoms, so they are easy to be polarized. groups form stable complexes, which reduces activity and even prevents polymerization

Method used

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  • N,O-double ligand metal catalyst with stereo structure and preparation method
  • N,O-double ligand metal catalyst with stereo structure and preparation method
  • N,O-double ligand metal catalyst with stereo structure and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0038] (I) Preparation of α-ketophenylimine ligands with novel stereostructures.

[0039] Add 0.0143 mol of 9,10-dihydro-9,10-ethylene anthracene-11,12-dione, 0.0143 mol of aniline, and a catalytic amount of p-toluene into the reaction flask equipped with a reflux condenser and a water separator Sulfonic acid and 150 mL of toluene were used as solvents. After 2 hours of reaction, recrystallize from n-hexane or distill under reduced pressure to obtain a novel stereoscopic α-ketobenimine ligand with a purity of more than 99%.

[0040] (II) Preparation of bis(α-ketophenylimine)nickel(II) with novel stereostructure as main catalyst.

[0041] 50 o Add 0.014 mol of the ligand prepared in step I to the tert-butanol solution containing 0.01 mol of potassium tert-butoxide at C. After the reaction solution is clear and transparent, lower the temperature of the system to room temperature, and then add 0.007 mol of tetraethylamine tetra Nickel bromide was kept at room temperature for 3...

Embodiment 2

[0045] (I) Preparation of α-ketophenylimine ligands with novel stereostructure:

[0046] With embodiment 1.

[0047] (II) Preparation of bis(α-ketophenylimine)palladium(II) with novel stereostructure as main catalyst.

[0048] 50 o Add 0.014 mol of the ligand prepared in step I to the tert-butanol solution containing 0.01 mol of potassium tert-butoxide at C. After the reaction solution is clear and transparent, lower the temperature of the system to room temperature, and then add 0.007 mol of tetraethylamine tetra Palladium chlorate, kept at room temperature for 3 hours, filtered, and recrystallized to obtain bis(α-ketophenylimine)palladium(II) complex with a new stereostructure.

[0049] (III) Catalytic polymerization of norbornene.

[0050] Heat the reaction bottle equipped with a magnetic stirrer and a branch with a heat gun, and simultaneously vacuumize it, fill it with nitrogen, and replace it three times to ensure that the reaction system is in a dry nitrogen environ...

Embodiment 3

[0052] (I) Preparation of α-keto(2,6-dimethyl)phenylimine ligand with novel stereostructure.

[0053] Add 0.0143 mol of 9,10-dihydro-9,10-ethylene anthracene-11,12-dione, 0.0143 mol of 2,6-dimethyl Aniline, a catalytic amount of p-toluenesulfonic acid and 200 mL of toluene were used as solvents. After reacting for 4 hours, the α-keto(2,6-dimethyl)imine ligand with a new stereostructure with a purity of more than 99% was obtained by recrystallization from n-hexane or distillation under reduced pressure.

[0054] (II) Preparation of bis[α-keto(2,6-dimethyl)phenylimine]nickel(II) complexes with novel stereostructures as main catalysts.

[0055] 50 o Add 0.014 mol of the ligand prepared in step I to a tert-butanol solution containing 0.01 mol of potassium tert-butoxide at C. After the reaction solution is clear and transparent, lower the temperature of the system to room temperature, and then add 0.007 mol of tetraethylamine tetra Nickel bromide was kept at room temperature for...

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Abstract

An N,O-double ligand metal catalyst with a stereo structure and a preparation method. The catalyst has the following general formula; M is a nickel, palladium, cobalt, iron or copper central metal atom; R1 is bromine, chlorine, iodine, methyl, propyl, butyl, phenyl, naphthyl, methoxyl or ethyoxyl; when R2 is aromatic amine or aliphatic amine, R2 is ethylamine, propylanmine, isopropylamine, butylamine, tert-butylamine, hexylamine, or cyclohexylamine. The catalyst of the invention has high light transmittance, a high glass-transition temperature, good thermal stability, oxidation stability, low hygroscopicity, a low dielectric constant, and good processing performance, dissolving performance and adhesion performance.

Description

technical field [0001] The invention belongs to the technical field of catalysts and preparation, and relates to a catalytic system for addition copolymerization of norbornene and norbornene derivatives, in particular to a catalytic system for addition copolymerization of norbornene and norbornene derivatives main catalyst. Background technique [0002] Norbornene is a typical cyclic olefin, which can be polymerized in three ways: ring-opening metathesis polymerization, cationic or free radical polymerization, and vinyl addition polymerization. Polymers obtained by different polymerization methods have different structures and properties. Among them, vinyl addition polynorbornene is polymerized by opening double bonds, and the two-membered ring structure of norbornene is retained in the polymer chain (US Patent 5468819, 5569730), with high relative molecular mass and narrow molecular weight distribution. This material has high light transmittance, good thermal and chemical...

Claims

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Application Information

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IPC IPC(8): C08F4/80C08F4/72C08F232/08
Inventor 贺晓慧陈义旺王凯悌姚溢琼
Owner 江西耀泰铜业有限公司
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