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A kind of plate type α-diimine catalyst and its preparation method and application

A diimine and catalyst technology, which is applied in the field of plate-type α-diimine catalyst and its preparation, can solve the problems of high branching degree, poor catalytic performance, low molecular weight of polymer products, etc., and achieves low branching degree, The effect of low cost of raw materials and high molecular weight

Active Publication Date: 2021-06-22
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a plate-type α-diimine catalyst and its preparation method and application, so as to solve the problem of poor catalytic performance of existing olefin polymerization catalysts, resulting in low molecular weight of polymerization products and high degree of branching

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  • A kind of plate type α-diimine catalyst and its preparation method and application
  • A kind of plate type α-diimine catalyst and its preparation method and application
  • A kind of plate type α-diimine catalyst and its preparation method and application

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Effect test

Embodiment 1

[0032] 1) Preparation of α-bis(2,6-diisopropyl)phenylimine ligand:

[0033] Add 100mL of toluene and 0.005mol of 5,7,12,14-tetrahydro-18λ with a plate structure into the reaction flask connected to the water separator 5 ,19λ 5 -5,14; 7,12-bis([1,2] endophenylene)pentacene-6,13,18,19-tetraketone and 0.020mol of 2,6-diisopropylaniline, heating Reaction at 120°C for 24h. After the reaction was completed, it was concentrated to 30 mL, placed in a refrigerator for crystallization, and the obtained crystal substance became a platy α-bis(2,6-diisopropyl)phenylimine ligand.

[0034] The obtained ligands were analyzed by NMR mass spectrometry, such as figure 1 shown.

[0035] It can be concluded from the figure that the structure of the ligand is as follows:

[0036] Same result as expected.

[0037] 2) Preparation of plate-type α-bis[(2,6-diisopropyl)phenylimine]palladium(II) catalyst

[0038] Add 30 mL of dichloromethane to the reaction flask, then add 0.005 mol of platy α-b...

Embodiment 2

[0042] 1) Preparation of platy α-bis(2,6-diisopropyl)phenylimine ligand:

[0043] Add 100mL of toluene and 0.005mol of 5,7,12,14-tetrahydro-18λ with a plate structure into the reaction flask connected to the water separator 5 ,19λ 5 -5,14; 7,12-bis([1,2] endophenylene)pentacene-6,13,18,19-tetraketone and 0.020mol of 2,6-diisopropylaniline, heating Reaction at 120°C for 72h. After the reaction was completed, it was concentrated to 30 mL, placed in a refrigerator for crystallization, and the obtained crystal substance became a platy α-bis(2,6-diisopropyl)phenylimine ligand.

[0044] 2) Preparation of plate-type α-bis[(2,6-diisopropyl)phenylimine]nickel(II) catalyst

[0045]Add 30 mL of dichloromethane to the reaction flask, followed by 0.005 mol of platy α-bis(2,6-diisopropyl)phenylimine ligand and 0.005 mol of (DME) 2 NiBr 2 , and reacted at 30°C for 1 hour. After the reaction, it was concentrated to 5 mL, and 20 mL of n-hexane was added for recrystallization and purificat...

Embodiment 3

[0049] 1) Preparation of α-diphenylimine ligand:

[0050] Add 100mL of toluene and 0.005mol of 5,7,12,14-tetrahydro-18λ with a plate structure into the reaction flask connected to the water separator 5 ,19λ 5 -5,14; 7,12-bis([1,2] endophenylene)pentacene-6,13,18,19-tetraketone and 0.020mol of aniline, heated to 120°C for 24h. After the reaction was completed, it was concentrated to 30 mL, placed in a refrigerator for crystallization, and the obtained crystalline substance became a platy α-diphenylimine ligand.

[0051] 2) Preparation of plate-type α-bis[(2,6-diisopropyl)phenylimine]palladium(II) catalyst

[0052] Add 30 mL of dichloromethane to the reaction flask, then add 0.005 mol of platy α-diphenylimine ligand and 0.005 mol of (COD)PdClMe, react at 30°C for 24 h, after the reaction, concentrate to 5 mL, 20 mL of n-hexane was added for recrystallization and purification, and the obtained powder solid was the plate-type α-diphenylimine palladium (II) catalyst.

[0053] 3...

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Abstract

The invention provides a plate type α-diimine catalyst and its preparation method and application. The general structural formula of the catalyst is as follows: wherein, M is a central metal atom; R 1 and R 2 is a methyl group, a chlorine atom or a bromine atom; the bridging group is phenyl, benzoquinone, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl, tetrahydrothiophene, tetrahydrofuran or tetrahydropyrrole; R is an aliphatic group groups or aromatic groups. The catalyst of the invention has high catalytic activity, and can catalyze functionalized polyolefin materials with high molecular weight, low branching degree, high polar group content, and highly controllable structure and performance. The invention has low cost of preparation raw materials, short synthesis route, high reaction yield and easy realization of industrialized production.

Description

technical field [0001] The invention belongs to the technical field of catalysts and preparation, and in particular relates to a plate-type α-diimine catalyst and its preparation method and application. Background technique [0002] Polyolefin is the polymer material with the largest output and widest application, which can be used to prepare food packaging, medical equipment, optical components, etc. In recent years, my country's annual production and consumption of polyolefins have steadily increased, but the annual import volume has also gradually increased. This is mainly due to the fact that the degree of intensification of my country's polyolefin industry is low, and the products tend to be low-end. In order to improve the global competitiveness of my country's polyolefin industry, it is necessary to increase the output and production capacity of my country's high-end polyolefin products, and the most important and effective way in this regard is to design and develop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/70C08F10/00C08F110/02C07F15/00C07F15/04
CPCC07F15/0066C07F15/045C08F4/7006C08F10/00C08F110/02C08F2500/01
Inventor 王凯悌刘翼吴佳骏向红霞曾晓燕李又兵
Owner CHONGQING UNIV OF TECH
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