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Application of a para-phenyl-containing α-diimine nickel (ii) complex in catalyzing the chain walking polymerization of 3-heptene

A technology of nickel diimide and complex, applied in the field of olefin polymerization, can solve the problem that 3-olefin polymerization monomer has not been successfully reported and so on

Active Publication Date: 2021-06-15
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, 3-alkenes have not been successfully reported as polymerized monomers

Method used

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  • Application of a para-phenyl-containing α-diimine nickel (ii) complex in catalyzing the chain walking polymerization of 3-heptene
  • Application of a para-phenyl-containing α-diimine nickel (ii) complex in catalyzing the chain walking polymerization of 3-heptene
  • Application of a para-phenyl-containing α-diimine nickel (ii) complex in catalyzing the chain walking polymerization of 3-heptene

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Experimental program
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Effect test

preparation example Construction

[0050] Preparation of cocatalyst dMMAO:

[0051] Modified methylaluminoxane (MMAO, 20.0 mL, 41.8 mmol) in toluene was vacuum dried at 60°C for 3 hours. The resulting colorless solid was redissolved in 20 mL of toluene. The cycle of drying and redissolution was repeated seven times to yield 3.32 g of a colorless solid. Titration of an aliquot of the resulting solid showed an aluminum content of 11.1 mmol / g (88% aluminum recovered). The prepared MMAO was used as stock solution in toluene (2.0M).

[0052] (3) Application of para-phenyl-containing α-diimine nickel (II) complexes in the chain walking polymerization of 3-heptene.

[0053] In the field of olefin polymerization, the preparation of new polyolefins has always been a very interesting challenge. Common olefin monomers that can be polymerized are very limited, generally including ethylene, propylene, long-chain α-olefins, styrene derivatives and different types of polar monomers. Olefins with alkyl substituent groups ...

Embodiment 1

[0058] (1) 3-heptene polymerization:

[0059] in N 2 Under atmosphere, toluene was used as the polymerization solvent, and the polymerization was carried out in a 10 mL dry glass reaction tube equipped with a magnetic stirrer. First weigh 0.61g of trans and cis 3-heptene mixture (trans / cis=0.82 / 0.18) with a reaction tube, then inject 5mL of toluene and cocatalyst dMMAO (1.0mL, 2.0M, n(Al) / n (Ni)=500) was sequentially added into the reaction tube, kept at the set polymerization temperature, and the mixture was fully stirred for 10 minutes. Then, the toluene solution containing 10 μmol nickel catalyst was added into the reaction tube with a syringe to start polymerization, and the reaction time was recorded. The polymerization was terminated with 50 mL of 3% HCl-MeOH solution. The resulting polymer was thoroughly washed with methanol, and vacuum-dried at 60°C for 3 hours.

[0060] (2) Evaluation of polymerization performance and analysis of polymer structure: weighing the ob...

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Abstract

The invention discloses the application of a para-phenyl-containing α-diimine nickel (II) complex in catalyzing the chain walking polymerization of 3-heptene, which is used as a chain walking catalyst to catalyze the synthesis of monomer 3-heptene Polymerization reaction, and the chain walking speed of internal olefins is accelerated due to the conjugation of phenyl groups; under the activation of cocatalyst dry modified methylalumoxane (dMMAO), the chain walking of 3-heptene is catalyzed by the chain walking catalyst Polymerization reaction, wherein the general structural formula and related polymerization process of the p-position containing phenyl α-diimine nickel (II) complex are as follows: the catalytic system of the present invention realizes the polymerization of 3-heptene through chain walking behavior, and produces stable branches degree of amorphous polymer (≈139 branches / 1000 carbons; T g ≈–68°C). NMR analysis of the polymer revealed that the resulting poly(3‑heptene) had ethyl, propyl, and butyl branches and a small amount of long-chain methylene sequences through monomer isomerization.

Description

technical field [0001] The invention relates to a preparation method of a novel polyolefin, in particular to the application of a para-phenyl-containing α-diimine nickel (II) complex in catalyzing 3-heptene chain walking polymerization, belonging to the technical field of olefin polymerization . It also involves the characterization of new polyolefins and the study of polymerization mechanism. Background technique [0002] In the field of olefin polymerization, late-transition metal catalysts are a new generation of metal-organic catalysts with high activity, especially Brookhart-type diimide nickel(Ⅱ) and palladium(Ⅱ) catalysts have a unique chain walking mechanism (Guo, L.H.; Dai, S.Y. ; Sui, X.L.; Chen, C.L. Palladium and nickel catalyzed chain walking olefin polymerization and copolymerization, ACS Catal. 2016, 6, 428-441). By changing the type of olefin monomer, catalyst structure and polymerization conditions can strongly affect the topology of the resulting polymer,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/14C08F4/70
Inventor 王福周陈昶乐徐国永张严朱文彬邢旭
Owner ANHUI UNIVERSITY
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