Large-steric-hindrance neutral nickel catalyst, preparation method and application in preparation of ethylene/polar monomer copolymers

A nickel catalyst and catalyst technology are applied in the application field of large sterically hindered neutral nickel catalyst and preparation, and the preparation of ethylene/polar monomer copolymer, and the effect of simple and efficient synthesis method is achieved.

Active Publication Date: 2017-04-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the examples of the copolymerization of ethylene and vinyl polar monomers are mainly completed by palladium catalysts, but the expensive price of metal palladium will seriously limit its industrialization. Relatively speaking, nickel-based catalysts are cheap, and nickel-based catalysts successfully trigger ethylene and vinyl. There are very few reports on the copolymerization of vinyl polar monomers

Method used

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  • Large-steric-hindrance neutral nickel catalyst, preparation method and application in preparation of ethylene/polar monomer copolymers
  • Large-steric-hindrance neutral nickel catalyst, preparation method and application in preparation of ethylene/polar monomer copolymers
  • Large-steric-hindrance neutral nickel catalyst, preparation method and application in preparation of ethylene/polar monomer copolymers

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Experimental program
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Embodiment 1

[0061] The invention provides a method for synthesizing a phenol-phosphine neutral nickel catalyst with a large hindered phosphine, by combining a phenol-phosphine ligand with Py 2 NiMe 2 Mix directly, remove the nickel black produced by the deterioration of the nickel source during the reaction after the reaction, and then obtain the catalyst with the structure of formula a~j, and the operation is simple. X-ray single crystal diffraction shows that the complex has a planar tetragonal structure centered on nickel.

[0062]

[0063] The Ar group is 2-(2',6'-(OMe) 2 -C 6 h 3 )-C 6 h 4 ;

[0064] Preferably, the nickel source required for the reaction is Py 2 NiMe 2 ;

[0065] Preferably, the reaction solvent is toluene, and the reaction temperature is room temperature.

[0066] The specific implementation steps of the catalyst with formula a~j structure synthesized by this example:

[0067] The specific implementation steps of this example are firstly the synthesis...

Embodiment 2

[0113] The polyethylene in this embodiment is linear polyethylene. The catalyst used is a catalyst having a structure of formula a.

[0114]

[0115] The Ar group is 2-(2',6'-(OMe) 2 -C 6 h 3 )-C 6 h 4 ;

[0116] The preparation method of linear polyethylene in the present embodiment comprises the following steps:

[0117] (1) Under high vacuum, add 500mL toluene into a dry 1000mL autoclave, stir for 5 minutes, the reaction temperature is stabilized to 70°C, add 10μmol of toluene solution of the catalyst having the structure of formula a, and quickly feed 10atm ethylene Gas, polymerization under strong stirring for 20 minutes;

[0118] (2) After the polymerization, the ethylene gas in the autoclave was evacuated, and the polymer obtained in the autoclave was poured into 1L of ethanol to settle. Then filter, wash and vacuum dry to obtain high molecular weight linear polyethylene.

[0119] The product obtained above was subjected to DSC analysis and NMR analysis, and...

Embodiment 3

[0121] The polyethylene in this embodiment is linear polyethylene, and the catalyst used is a catalyst having the structure of formula c.

[0122]

[0123] The Ar group is 2-(2',6'-(OMe) 2 -C 6 h 3 )-C 6 h 4 ;

[0124] The preparation method of linear polyethylene in the present embodiment comprises the following steps:

[0125] (1) Under high vacuum, add 500mL of toluene to a dry 1000mL autoclave, stir for 5 minutes, the reaction temperature stabilizes to 30°C, add 10μmol of toluene solution of the catalyst having the structure of formula c, and quickly pass into 10atm ethylene Gas, polymerization under strong stirring for 20 minutes;

[0126] (2) After the polymerization, the ethylene gas in the autoclave was evacuated, and the polymer obtained in the autoclave was poured into 1L of ethanol to settle. Then filter, wash and vacuum dry to obtain high molecular weight linear polyethylene.

[0127] The product obtained above was subjected to DSC analysis and nuclear m...

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Abstract

The invention relates to a large-steric-hindrance neutral nickel catalyst, a preparation method and an application in preparation of an ethylene / polar monomer copolymer. A phenol-phosphorous mono-anionic ligand with different substituents of R1, R2 and R3 is dissolved in a good solvent and added to a good solvent of a metal nickel source for a reaction, and the catalyst is obtained, and X-ray single crystal diffraction indicates that an obtained complex adopts a plane quadrangle structure. The synthesized catalyst single component is used for triggering ethylene polymerization. An obtained polymer is a high-molecular-weight linear polymer with the molecular weight up to 770 kg / mol. Copolymerization of polar monomers such as ethylene, methyl acrylate and the like is realized, the copolymer with different polar monomer insertion rates is obtained, and the polar monomer insertion rate is up to 8mol%. Experimental results indicate that the polar monomers are inserted in polymer chain tails and molecular chains, which is the major breakthrough of the neutral nickel catalyst in the olefin polymerization history.

Description

technical field [0001] The invention relates to the technical field of synthesis of novel phenol-phosphine nickel complexes and the preparation of ethylene / polar monomer copolymers, in particular to a large sterically hindered neutral nickel catalyst and its preparation method and the preparation of ethylene / polar monomer copolymers Application; Application of polyethylene / polymethyl (butyl) acrylate random copolymer and preparation method thereof. Background technique [0002] Polyolefin is the polymer material with the largest output and the most wide application in the world. Polyolefins have excellent mechanical strength and processing properties, excellent chemical corrosion resistance and good electrical insulation properties, etc., and are inexpensive at the same time. Polyolefins are widely used in various fields such as transportation, construction, agriculture, national defense construction and people's daily life. Polyolefin contains only two elements, carbon an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F210/02C08F4/80
CPCC08F110/02C08F210/02C08F4/80
Inventor 李悦生张艳平穆红亮
Owner TIANJIN UNIV
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