Palladium-containing catalyst and preparation method thereof, composition prepared from palladium-containing catalyst, and application of composition

A palladium catalyst and catalyst technology, applied in the field of olefin catalysis, can solve the problems of low copolymerization activity of olefins and polar/functional monomers, low insertion rate of comonomers, etc. the effect of leaving

Active Publication Date: 2018-01-19
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defects of low transition metal catalyst catalyzed copolymerization activity of olefins and polar / functional monomers in the prior art, low comonomer insertion rate, and the need to add a large amount of co-catalysts to improve catalytic activity or insertion rate, and provide Olefin polymerization catalyst with high catalytic activity and high comonomer insertion rate

Method used

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  • Palladium-containing catalyst and preparation method thereof, composition prepared from palladium-containing catalyst, and application of composition
  • Palladium-containing catalyst and preparation method thereof, composition prepared from palladium-containing catalyst, and application of composition
  • Palladium-containing catalyst and preparation method thereof, composition prepared from palladium-containing catalyst, and application of composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] A preparation method containing palladium catalyst, the steps are as follows:

[0068] (1) Dissolve 2-hydroxy-1,4-naphthoquinone and substituted aniline in n-heptane, add trifluoroacetic acid to react to obtain anilinonaphthoquinone ligands, the reaction temperature is 100°C, the time is 15h, the reaction Initially, the molar ratio of 2-hydroxy-1,4-naphthoquinone to substituted aniline was 1:1.15, and the molar ratio of trifluoroacetic acid to 2-hydroxy-1,4-naphthoquinone was 0.33:1,2-hydroxy- The concentration of 1,4-naphthoquinone in n-heptane is 0.125mol / L, and the structural formula of substituted aniline is as follows:

[0069]

[0070] In the formula, R 1 is ethyl, R 2 is ethyl, R 3 is methyl, R 4 is methyl, R 5 It is a methyl group, and after the reaction, the anilinaquinone ligands are purified by toluene recrystallization;

[0071] (2) Dissolving the anilino-naphthoquinone ligands in toluene, adding sodium hydride to react to obtain a ligand salt compo...

Embodiment 2

[0078] A preparation method containing palladium catalyst, the steps are as follows:

[0079] (1) Dissolve 2-hydroxy-1,4-naphthoquinone and substituted aniline in toluene, add trifluoroacetic acid to react to obtain aniline naphthoquinone ligands, the reaction temperature is 110°C, the time is 6h, when the reaction starts , the molar ratio of 2-hydroxyl-1,4-naphthoquinone to substituted aniline is 1:1, the molar ratio of trifluoroacetic acid to 2-hydroxyl-1,4-naphthoquinone is 0.32:1, 2-hydroxyl-1, The concentration of 4-naphthoquinone in toluene is 0.1mol / L, and the structural formula of substituted aniline is as shown in embodiment 1, and in the formula, R 1 is methyl, R 2 is methyl, R 3 is ethyl, R 4 is ethyl, R 5 After the reaction, the anilinaquinone ligands are purified by n-hexane extraction;

[0080] (2) Dissolving the anilinaquinone ligands in tetrahydrofuran, adding sodium hydride to react to obtain a ligand salt compound, the temperature of the reaction is 40°C...

Embodiment 3

[0085] A preparation method containing palladium catalyst, the steps are as follows:

[0086](1) Dissolve 2-hydroxy-1,4-naphthoquinone and substituted aniline in chlorobenzene, add trifluoroacetic acid to react to obtain anilino-naphthoquinone ligands, the reaction temperature is 130°C, the time is 6h, and the reaction starts , the molar ratio of 2-hydroxy-1,4-naphthoquinone to substituted aniline is 1:1.02, and the molar ratio of trifluoroacetic acid to 2-hydroxy-1,4-naphthoquinone is 0.32:1,2-hydroxy-1 , the concentration of 4-naphthoquinone in chlorobenzene is 0.11mol / L, and the structural formula of substituted aniline is as shown in embodiment 1, and in the formula, R 1 is isopropyl, R 2 is isopropyl, R 3 is methyl, R 4 is methyl, R 5 It is a methyl group, and after the reaction, the anilinaquinone ligands are purified by tetrahydrofuran recrystallization;

[0087] (2) Anilinaquinone ligands are dissolved in dichloromethane, and potassium hydride is added to react to...

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Abstract

The invention relates to a palladium-containing catalyst and a preparation method thereof, a composition prepared from the palladium-containing catalyst, and application of the composition. The structural formula of the palladium-containing catalyst is described in the description. The preparation method of the palladium-containing catalyst comprises the following steps: firstly, dissolving 2-hydroxy-1,4-naphthoquinone and substituted aniline into an organic solvent for carrying out a reaction so as to obtain an aniline naphthoquinone ligand; dissolving the aniline naphthoquinone ligand into an organic solvent, and adding a hydrogen extraction reagent for carrying out a reaction so as to obtain a ligand salt compound; adding a palladium precursor into the ligand salt compound for carryingout a reaction so as to obtain an intermediate metal complex; finally, adding a pyridine reagent into the intermediate metal complex for carrying out a reaction to obtain the catalyst. The compositioncan be prepared from the palladium-containing catalyst and a catalyst promoter. The palladium-containing catalyst uses palladium as a metal center, is higher in activity of catalyzing homopolymerization of ethylene and copolymerization of olefin and a polar monomer, also can reach a certain activity without needing a catalyst promoter, and is good in economical efficiency and high in polarity/functional monomer insertion rate. The composition prepared from the palladium-containing catalyst has higher catalytic activity when a very small amount of the catalyst promoter is used.

Description

technical field [0001] The invention belongs to the field of olefin catalysis, and relates to a palladium-containing catalyst, a preparation method thereof, a composition prepared therefrom and applications thereof, in particular to a palladium-containing catalyst for catalyzing ethylene or ethylene and polar / functional monomers, and its preparation Methods, compositions made therefrom and applications. Background technique [0002] With the in-depth research on coordination polymerization catalysts, several major types of olefin polymerization catalysts have emerged: Ziegler-Natta catalysts, metallocene catalysts, non-locene early transition metal catalysts and late transition metal catalysts. The development of these catalysts has greatly promoted the progress of industrialization. In recent years, late transition metal olefin polymerization catalysts have been greatly developed. Late transition metal olefin polymerization catalysts refer to a type of olefin polymerizatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F110/02C08F210/02C08F232/08C08F218/12C08F218/08C08F220/14C08F212/08C07F15/00
Inventor 蔡正国丁琳伏夏张凌隽
Owner DONGHUA UNIV
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