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Ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst

A Mesoporous Silicone, Three-Dimensional Ordered Technology

Active Publication Date: 2015-05-20
佛山市莫斯卡有机硅实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to: provide a kind of preparation method of the three-dimensional order mesoporous organosilicon immobilized Pd(II) catalyst of ethylenediamine functionalization, by The ethylenediamine-functionalized three-dimensional ordered mesoporous organosilicon immobilized Pd(II) catalyst obtained by the preparation method can solve the problems that the homogeneous Pd(II) catalyst cannot be recycled, heavy metal ions and organic solvents pollute the environment, etc.

Method used

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  • Ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst
  • Ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst
  • Ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst

Examples

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Embodiment 1

[0026] Example 1: Preparation of ethylenediamine-functionalized three-dimensional ordered mesoporous organosilicon-immobilized Pd(II) catalyst according to the following steps

[0027] (1) Mix surfactant, alcohol and hydrochloric acid to make an aqueous solution with surfactant concentration of 3.8 mM, alcohol concentration of 0.32M, and HCl concentration of 0.11M. o C mixed evenly; add 1, 2-bistriethoxysilylbenzene, prepolymerize for 50min; then add ethylenediamine bridged silane, continue to react for 28 h; o C aging for 80 h; wherein, in step (1), the molar ratio of 1,2-bistriethoxysilylbenzene to ethylenediamine bridged silane is 5:1; the surfactant is P123; the The ethylenediamine bridged silane is two [3-(trimethoxysilyl) propyl] ethylenediamine;

[0028] (2) The solid obtained in step (1) is extracted to remove the surfactant, washed with alkali, and dried to obtain a three-dimensional ordered mesoporous organosilicon (DA-PMO) functionalized with ethylenediamine; where...

Embodiment 2

[0031] Example 2: Prepare ethylenediamine-functionalized three-dimensional ordered mesoporous organosilicon-immobilized Pd(II) catalyst according to the following steps

[0032] (1) Mix surfactant, alcohol and hydrochloric acid to make an aqueous solution with surfactant concentration of 4.0 mM, alcohol concentration of 0.4 M, and HCl concentration of 0.12 M. o C mix well; add 1, 2-bistriethoxysilylbenzene, pre-polymerize for 65min; then add ethylenediamine bridged silane, continue to react for 25 h; o C aging for 75h; wherein, in step (1), the molar ratio of 1,2-bistriethoxysilylbenzene to ethylenediamine bridged silane is 30:1; the surfactant is P123; the The ethylenediamine bridged silane is bis[3-(triethoxysilyl)propyl]ethylenediamine;

[0033] (2) The solid obtained in step (1) is extracted to remove the surfactant, washed with alkali, and dried to obtain a three-dimensional ordered mesoporous organosilicon (DA-PMO) functionalized with ethylenediamine; wherein, in step...

Embodiment 3

[0036] Example 3: Preparation of ethylenediamine-functionalized three-dimensional ordered mesoporous organosilicon immobilized Pd(II) catalyst according to the following steps

[0037] (1) Mix surfactant, alcohol and hydrochloric acid to make an aqueous solution with surfactant concentration of 4.2 mM, alcohol concentration of 0.45 M, and HCl concentration of 0.13 M. o C mix well; add 1, 2-bistriethoxysilylbenzene, pre-polymerize for 50min; then add ethylenediamine bridged silane, continue to react for 22h; o C aging for 70h; wherein, in step (1), the molar ratio of 1,2-bistriethoxysilylbenzene to ethylenediamine bridged silane is 60:1; the surfactant is P123; the The ethylenediamine bridged silane is bis[3-(trimethoxysilyl)propyl]ethylenediamine;

[0038] (2) The solid obtained in step (1) is extracted to remove the surfactant, washed with alkali, and dried to obtain a three-dimensional ordered mesoporous organosilicon (DA-PMO) functionalized with ethylenediamine; wherein, i...

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Abstract

The invention discloses an ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst. A preparation method of the Pd(II) catalyst comprises the following steps: firstly carrying out copolycondensation on ethylenediamine bridged silane and phenyl bridged silane in presence of a surfactant to obtain an ethylenediamine functionalized three-dimensional ordered mesopore organosilicone material; and then immobilizing Pd(II) on the ethylenediamine functionalized three-dimensional ordered mesopore organosilicone material to obtain the ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst. The ethylenediamine functionalized three-dimensional ordered mesopore organosilicone immobilized Pd(II) catalyst can be used for solving the problems that a homogenous Pd(II) catalyst can not be recycled and heavy metal ions and an organic solvent can produce pollution to the environment, is of an ordered three-dimensional hexagonal mesopore structure, has high specific surface area and shows high catalytic activity in water phase Suzuki reaction.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a Pd(II) catalyst functionalized with ethylenediamine and three-dimensionally ordered mesoporous organic silicon. Background technique [0002] In the field of fine chemical industry and pharmaceutical synthetic chemistry, organometallic-catalyzed carbon-carbon coupling reaction is one of the most effective tools for constructing carbon-carbon bonds, among which the palladium-catalyzed Suzuki reaction of halogenated arenes and terminal alkynes is the most important tool in organic synthesis. C sp -C sp One of the most important reactions of the bond, the construction of this structure occupies a very important position in the field of organic synthesis. Currently, typical reaction systems for palladium-catalyzed Suzuki reactions include classical homogeneous organometallic palladium catalysts such as Pd(OAc) 2 And heterogeneous metal palladium catalysts, such as Pd / C, etc. ...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J31/28B01J31/30C07B37/00C07C1/32C07C15/14C07C41/30C07C43/205C07C201/12C07C205/06
CPCY02P20/584
Inventor 朱凤霞安礼涛孙小军
Owner 佛山市莫斯卡有机硅实业有限公司
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