Preparation method of PPh2-ordered mesopore polymer-Pd(II) heterogeneous catalyst and use thereof

A technology of heterogeneous catalyst and homogeneous catalyst, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of environmental pollution and difficult to reuse, etc. achieve the effect of improving catalytic efficiency

Inactive Publication Date: 2009-06-17
SHANGHAI NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although compared with heterogeneous catalysts, homogeneous catalysts mostly have better catalytic activity and selectivity, but the latter has problems such as difficulty in reusing and easy to cause environmental pollution.

Method used

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  • Preparation method of PPh2-ordered mesopore polymer-Pd(II) heterogeneous catalyst and use thereof
  • Preparation method of PPh2-ordered mesopore polymer-Pd(II) heterogeneous catalyst and use thereof
  • Preparation method of PPh2-ordered mesopore polymer-Pd(II) heterogeneous catalyst and use thereof

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preparation example Construction

[0026] a PPh 2 -The preparation method of ordered mesoporous polymer-Pd (II) heterogeneous catalyst, comprises the following steps:

[0027] 1) At a temperature of 308K, mix 1.10g of phenol (Phenol), 20% aqueous sodium hydroxide solution and p-PPh 2 -Phenol, 37% formaldehyde solution was stirred and mixed, and then reacted at 340K for 2h to obtain 2 Polymers with functional groups (PPh 2 -MPs) prepolymer, which is subsequently formulated into PPh with a mass ratio of 20% 2 - MPs prepolymer ethanol solution.

[0028] 2) PPh obtained in step 1 2 -Add 0.90g of triblock copolymer Pluronic F127 (EO106PO70EO106, M w =12,600, Acros Chemical Inc.), 20.0g ethanol solution, after standing at room temperature for 5h, further solidified at 373K temperature, 48w%H 2 SO 4 Extraction, the obtained dark brown solid is PPh 2 Ordered mesoporous polymer materials with functional groups (PPh 2 -MPs).

[0029] 3) Add 0.50g of PdCl 2 (PPh 3 ) 2 The homogeneous catalyst was dissolved in...

Embodiment 2

[0031] 1) At 318K, 1.19g of phenol (Phenol), 20% aqueous sodium hydroxide solution and p-PPh 2-Phenol, 37% formaldehyde solution was stirred and mixed, and then reacted at 350K for 4h to obtain 2 Polymers with functional groups (PPh 2 -MPs) prepolymer, which is subsequently formulated into PPh with a mass ratio of 20% 2 - MPs prepolymer ethanol solution.

[0032] 2) PPh obtained in step 1 2 -Add 1.10g of triblock copolymer Pluronic F127 (EO106PO70EO106, M w =12,600, Acros Chemical Inc.), 20.0g ethanol solution, after standing at room temperature for 8h, further solidified at 383K temperature, 48w%H 2 SO 4 Extraction, the obtained dark brown solid is PPh 2 Functional group ordered mesoporous polymer materials (PPh 2 -MPs).

[0033] 3) Add 0.60g of PdCl 2 (PPh 3 ) 2 The homogeneous catalyst was dissolved in anhydrous toluene, and then the PPh obtained in step 2) was slowly added 2 -MPs solid material (the molar ratio of P content in the control material to Pd content...

Embodiment 3

[0035] 1) At 310K, mix 1.15g of phenol (Phenol), 20% aqueous sodium hydroxide solution and p-PPh 2 -Phenol, 37% formaldehyde solution was stirred and mixed, and then reacted at 345K for 3h to obtain 2 Polymers with functional groups (PPh 2 -MPs) prepolymer, which is subsequently formulated into PPh with a mass ratio of 20% 2 - MPs prepolymer ethanol solution.

[0036] 2) PPh obtained in step 1 2 -Add 1.0 g of triblock copolymer Pluronic F127 (EO106PO70EO106, M w =12,600, Acros Chemical Inc.), 20.0g ethanol solution, after standing at room temperature for 7h, further solidified at 380K temperature, 48w%H 2 SO 4 Extraction, the obtained dark brown solid is PPh 2 Functional group ordered mesoporous polymer materials (PPh 2 -MPs).

[0037] 3) 0.55g of PdCl 2 (PPh 3 ) 2 The homogeneous catalyst was dissolved in anhydrous toluene, followed by the slow addition of the PPh obtained in step 2 2 -MPs solid material (the molar ratio of P content in the control material to Pd ...

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Abstract

The invention discloses a method for preparing a Pd(II)-PPh2-MPs heterogeneous phase catalyst. The method comprises the following steps: 1) polymer (PPh2-MPs) prepolymer with PPh2 functional groups is prepared; 2) an ordered mesoporous polymer material (PPh2-MPs) having the PPh2 functional groups is prepared; and 3) the Pd(II)-PPh2-MPs heterogeneous phase catalyst is prepared. The preparation method can realize the uniform distribution of catalytic activity sites, the sufficient contact between a substrate and an active center, and can also realize the recycling of the catalyst, so as to realize the aim of green catalysis in the end.

Description

technical field [0001] The present invention relates to PPh 2 -A method for preparing an ordered mesoporous polymer-Pd(II) heterogeneous catalyst, specifically a functionalized ordered mesoporous polymer-immobilized organometallic Pd(II) heterogeneous catalyst (Pd(II) -PPh 2 -MPs) and relates to their use in clean Barbier reactions in aqueous media. Background technique [0002] In recent years, the use of water instead of organic solvents for organic synthesis has become an important branch of green chemistry. The Barbier reaction is an important class of organic reactions. The resulting homoallyl alcohol or homopropargyl alcohol is used as an intermediate in organic synthesis and is widely used in the synthesis of macrolides, polyhydroxy natural products, polyether antibiotics, etc. synthesis. Most of the organometallic catalysts currently used to catalyze the Barbier reaction in aqueous media are organometallic palladium complexes, such as Pd(PPh 3 ) 2 Cl 2 . Alth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C29/38C07C33/20
CPCY02P20/584
Inventor 杨旭石李和兴朱凤霞张昉朱瑞星郭成
Owner SHANGHAI NORMAL UNIVERSITY
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