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Preparation method of piperazine functionalized ordered mesoporous phenolic resin solid base catalyst

A solid base catalyst, phenolic resin technology, applied in the preparation of organic compounds, physical/chemical process catalysts, chemical instruments and methods, etc. The effect of strength, good catalytic activity

Inactive Publication Date: 2010-08-25
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, various organic functional groups are connected to the carrier by means of post-modification. In the modification process, volatile and irritating raw materials such as oleum and chloromethyl ether are often used, and the reaction conditions are not mild enough.
Professor Lu Yunfeng and others used the copolymerization method to prepare a series of mesoporous phenolic resins functionalized with carboxyl, sulfonic acid and amino groups, which showed a good application in the separation of metal ions, but the order of the prepared materials was not high. worm-like mesopores

Method used

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  • Preparation method of piperazine functionalized ordered mesoporous phenolic resin solid base catalyst
  • Preparation method of piperazine functionalized ordered mesoporous phenolic resin solid base catalyst
  • Preparation method of piperazine functionalized ordered mesoporous phenolic resin solid base catalyst

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Effect test

Embodiment 1

[0026] At 308K, 2.4g of phenol (Phenol), 0.52g of 20% sodium hydroxide aqueous solution and 0.027ml of piperazine functionalized formaldehyde Formylpiperazine, 37% of formaldehyde solution were stirred and mixed, and then reacted at a temperature of 340~350K for 10min, A phenolic resin (Piperazidine-MPs) prepolymer with Piperazidine functional groups was obtained, which was subsequently formulated into a 20% ethanol solution by mass. Add 0.90g of triblock copolymer Pluronic F127 (EO106PO70EO106, M w =12600, Aldrich) 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 was washed with saturated aqueous sodium carbonate solution, then washed with a large amount of deionized water and alcohol until the washing liquid was neutral and the presence of carbonate ions could not be detected, then the sample was vacuum-dried, and finally obtained Ordered mesoporous phenolic resin mat...

Embodiment 2

[0028] At 318K, 2.4g phenol (Phenol), 0.52g 20% ​​aqueous sodium hydroxide solution and 0.082ml piperazine functionalized formaldehyde Formylpiperazine, 37% formaldehyde solution were stirred and mixed, then reacted at 350K for 1h to obtain There is the phenolic resin (Piperazidine-MPs) prepolymer of Piperazidine functional group, then it is made into ethanol solution with a mass ratio of 20%. Add 1.10 g of triblock copolymer Pluronic F127 (EO106PO70EO106, M w =12600, Aldrich) 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 was washed with saturated aqueous sodium carbonate solution, then washed with a large amount of deionized water and alcohol until the washing liquid was neutral and the presence of carbonate ions could not be detected, then the sample was vacuum-dried, and finally obtained Ordered mesoporous phenolic resin materials with piperazidine functional grou...

Embodiment 3

[0030] At 310K, 2.4g phenol (Phenol), 0.52g 20% ​​sodium hydroxide aqueous solution and 0.050ml piperazine functionalized formaldehyde Formylpiperazine, 37% formaldehyde solution were stirred and mixed, then reacted at 345K temperature for 30min to obtain There is the phenolic resin (Piperazidine-MPs) prepolymer of Piperazidine functional group, then it is made into ethanol solution with a mass ratio of 20%. Add 1.00 g of triblock copolymer PluronicF127 (EO106PO70EO106, M w=12600, Aldrich) ethanol solution, after standing at room temperature for 6h, further solidified at 380K temperature, 48w%H 2 SO 4 Extraction, the obtained dark brown solid was washed with saturated aqueous sodium carbonate solution, then washed with a large amount of deionized water and alcohol until the washing liquid was neutral and the presence of carbonate ions could not be detected, then the sample was vacuum-dried, and finally obtained Ordered mesoporous phenolic resin materials with piperazidine fu...

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Abstract

The invention discloses a preparation method of a piperazine functionalized ordered mesoporous phenolic resin solid base catalyst. The method comprises the specific steps: under the alkali condition, phenol, formaldehyde and piperazine functionalized formaldehyde are copolymerized; the solvent evaporation induced self-assembly (EISA) method is adopted to be in hot polymerization to prepare piperazine a functionalized ordered mesoporous phenolic resin heterogeneous catalyst (Piperazidine-MPs). The invention also relates to application thereof in Knoevenagel condensation reaction in aqueous medium. In the Knoevenagel condensation reaction in the aqueous medium, the Piperazidine-MPs prepared by the EISA method has similar catalytic activity as the heterogeneous catalyst.

Description

technical field [0001] The invention relates to a preparation method of a piperazine functionalized ordered mesoporous phenolic resin solid base catalyst, specifically, under alkaline conditions, through the copolymerization of phenol, formaldehyde and piperazine functionalized formaldehyde, and then using solvent volatilization to induce self-assembly ( EISA) thermally polymerized piperazine functional ordered mesoporous phenolic resin heterogeneous catalyst (Piperazidine-MPs), and relates to its application in Knoevenagel condensation reaction in aqueous medium. Background technique [0002] In organic synthesis, the use of solid acid or solid base instead of liquid acid-base can reduce the pollution of acid-base to the environment. A solid base refers to a solid that has the ability to accept protons or donate electron pairs. As a catalyst, its active center has a very strong ability to donate or accept electrons, and it has a surface anion hole, that is, the free electr...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C253/30C07C255/41
Inventor 杨旭石李和兴张昉朱凤霞郭成
Owner SHANGHAI NORMAL UNIVERSITY
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