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Complex for catalyzing polymerization of 4-methyl-1-pentene and preparation method thereof

A technology of complexes and trimethylaluminum, applied in the direction of palladium organic compounds, platinum group organic compounds, chemical instruments and methods, etc., can solve the problem of deactivation of active centers, high manufacturing costs, and inability to catalyze the copolymerization of olefins and polar monomers and other problems, to achieve the effect of enhancing electrophilicity and improving catalytic activity

Inactive Publication Date: 2021-05-28
张洪胜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production cost of metallocene catalysts or non-metallocene catalysts of the early transition metal system is high, and the cocatalyst methylaluminoxane (MAO) is expensive and used in large amounts, and the active center is easily deactivated by polar functional groups and cannot be catalyzed. Defects such as copolymerization of olefins and polar monomers, difficulty in controlling the shape and particle size of the polymer
However, there are few studies on the polymerization of 4-methyl-1-pentene catalyzed by diimine nickel-palladium catalysts. The present invention provides a complex that catalyzes the polymerization of 4-methyl-1-pentene and a preparation method thereof

Method used

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  • Complex for catalyzing polymerization of 4-methyl-1-pentene and preparation method thereof
  • Complex for catalyzing polymerization of 4-methyl-1-pentene and preparation method thereof
  • Complex for catalyzing polymerization of 4-methyl-1-pentene and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The synthesis method of diimine ligand is as follows.

[0034] Under nitrogen atmosphere and room temperature, add 20mL of toluene, 2,6-dipropyl-4-nitroaniline (12mmol) in sequence to a 100mL branch bottle, and then slowly add 12mL of trimethylaluminum (1.0M, 12mmol) ; The reaction temperature was raised to 110° C., and after 2 hours of reaction, the reaction temperature was lowered to room temperature, and then acenaphthylquinone (5 mmol) was added; at this time, the reaction system changed from colorless to deep red, and released a large amount of heat; at 110° C. Continue to react for 6 hours, then lower the temperature to 0°C, and terminate the reaction system with 5% sodium hydroxide ice-water solution; extract the organic phase with ethyl acetate, and then use anhydrous MgSO 4 Dry and spin the solvent under reduced pressure to obtain an orange oil; the product is separated through a silica gel column, and the eluent (petroleum ether: ethyl acetate = 15:1); recryst...

Embodiment 2

[0036] The synthesis method of diimine palladium complex is as follows.

[0037] Under the protection of nitrogen, add diimine ligand (0.5mmol), (COD)PdMeCl (0.6mmol) and dichloromethane 20mL respectively in the Schlenk bottle with a branch, stir the reaction at room temperature for 12 hours, and then The solvent was evaporated under reduced pressure to about 5ml, and 20ml of n-hexane was added, at which time a large amount of precipitation occurred. Filtered with G4 filter ball, the precipitate was washed with 3×10mL n-hexane, and then vacuum-dried to obtain a yellow solid powder diimide palladium complex with a yield of 69.7%

Embodiment 3

[0039] This embodiment provides a poly(4-methyl-1-pentene), the preparation method of which is as follows.

[0040] All the glass instruments and magnets used for stirring were dried in an oven (120°C), and all polymerization experiments were carried out under anhydrous and oxygen-free conditions. Under continuous vacuuming, bake a 250mL branched-mouthed round-bottom flask under an infrared lamp at 150°C for more than 1 hour to remove all moisture and air; replace it with nitrogen twice and then fill it with nitrogen to normal pressure; keep the water bath to 0 ℃, add metered chlorobenzene, stir and dissolve, inject 2M monomer and 10 μmol diimide palladium complex dissolved in 2mL dichloromethane; stop the reaction after 4 hours of polymerization, and use Et 3 After SiH terminated, it was precipitated in methanol. The precipitated polymer was dissolved in petroleum ether, separated by silica gel column, concentrated, and precipitated in methanol. The obtained polymer was washe...

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Abstract

The invention discloses a complex for catalyzing polymerization of 4-methyl-1-pentene and a preparation method of the complex. A flexible group is introduced to the ortho-position of an imine nitrogen atom aromatic ring of the complex, so that the complex provides dynamic steric hindrance in the catalytic polymerization process, the space environment of a Pd catalytic active center is finely adjusted and the branching degree and molecular weight of the polymer are regulated and controlled; meanwhile, an electron withdrawing group is introduced to the para-position of an imine nitrogen atom aromatic ring, so that the electrophilicity of a metal active center is enhanced, insertion polymerization of 4-methyl-1-pentene is facilitated, and the molecular weight of the polymer is improved.

Description

technical field [0001] The invention belongs to the field of polyolefin preparation, in particular to a complex that catalyzes the polymerization of 4-methyl-1-pentene and a preparation method thereof. Background technique [0002] Poly 4-methyl-1-pentene, a new type of thermoplastic resin developed in recent years. Appearance is colorless transparent granular solid with a density of 0.833. It is the thermoplastic resin with the smallest density, excellent heat resistance, melting point 240°C, visible light transmittance up to 90%, ultraviolet transmittance better than glass and other transparent resins, and excellent electrical insulation and chemical resistance. [0003] The research on using 4-methyl-1-pentene as homopolymerization or comonomer mainly focuses on metallocene catalysts and non-metallocene catalysts of early transition metal systems. However, the production cost of metallocene catalysts or non-metallocene catalysts of the early transition metal system is h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C08F10/14C08F110/14C08F4/80
CPCC07F15/006C08F10/14C08F110/14
Inventor 张洪胜
Owner 张洪胜
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