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Preparation method and application of micron acicular-structure N-methyl-2-phenyl-3,4-fullerenylpyrrolidine

A technology of fullerenyl pyrrolidine and micron needles, which is applied in the field of preparation of fullerene derivatives, can solve the problems of low product yield, low catalytic conversion rate, and low purity, and achieve high activity and long life. Effect

Active Publication Date: 2014-07-23
HUANGSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, the target product produced by the existing process for synthesizing fullerene derivatives generally has low product yield and low purity. At the same time, the above-mentioned fullerene derivatives are used for applications, such as catalyst supports, and there is catalytic conversion Low rate and other issues

Method used

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  • Preparation method and application of micron acicular-structure N-methyl-2-phenyl-3,4-fullerenylpyrrolidine
  • Preparation method and application of micron acicular-structure N-methyl-2-phenyl-3,4-fullerenylpyrrolidine
  • Preparation method and application of micron acicular-structure N-methyl-2-phenyl-3,4-fullerenylpyrrolidine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 (S1)

[0031] The preparation method of N-methyl-2-phenyl-3,4-fullerenylpyrrolidine, its step comprises:

[0032] (1) Under the protection of argon, the fullerene C 60 Dissolve in freshly distilled toluene and stir for 1 h to give fullerene C 60 Toluene solution;

[0033] (2) to the fullerene C 60 Add freshly distilled benzaldehyde and sarcosine to the toluene solution, and place it under reflux at 120°C for 2 hours to obtain a reaction solution, wherein, during the reaction, the three raw materials fullerene C 60 , The molar ratio of benzaldehyde and sarcosine is 1:6:4;

[0034] (3) Pass argon gas into the reaction solution, after it is cooled to room temperature, it is filtered, concentrated and separated by column chromatography to obtain a reaction concentrate;

[0035] (4) Use cyclohexane to wash out the fullerene C that has not participated in the reaction in turn for the reaction concentrate 60 , and then rinse the residue with an eluent that is a...

Embodiment 2

[0036] Example 2 (S2)

[0037] The preparation method of N-methyl-2-phenyl-3,4-fullerenylpyrrolidine, its step comprises:

[0038] (1) Under the protection of argon, the fullerene C 60 Dissolved in freshly distilled toluene and stirred for 2 h to give fullerene C 60 Toluene solution;

[0039] (2) to the fullerene C 60 Add freshly distilled benzaldehyde and sarcosine to the toluene solution, and place it under reflux at 120°C for 3 hours to obtain a reaction solution, wherein, during the reaction, the three raw materials fullerene C 60 , The molar ratio of benzaldehyde and sarcosine is 1:6:4;

[0040] (3) Pass argon gas into the reaction solution, after it is cooled to room temperature, it is filtered, concentrated and separated by column chromatography to obtain a reaction concentrate;

[0041] (4) Use cyclohexane to wash out the fullerene C that has not participated in the reaction in turn for the reaction concentrate 60 , and then rinse the residue with an eluent that ...

Embodiment 3

[0063] Example 3 (M3)

[0064] The N-methyl-2-phenyl-3,4-fullerenylpyrrolidine obtained in Example 1 was treated with toluene as a solvent, and the N-methyl-2-phenyl-3, 4-Fullerenylpyrrolidine is dissolved in toluene, and its concentration in toluene is 0.75mgmg / mL, and then a surfactant is added, wherein the surfactant is prepared by dissolving sodium dodecylsulfonate in methanol , the substance concentration of the surfactant is 3mmol / L; the volume ratio of methanol to toluene is 5:1, the temperature is 15°C, and the magnetic stirring time is 20min. After centrifugation, the speed of the centrifuge is 5000r / min, the centrifugation time is 10min, remove the upper layer solution, wash 3 times with absolute ethanol, after centrifugation, place it at room temperature and dry for 10min, you can get micron N-methyl-2-phenyl-3,4-fullerenylpyrrolidine with needle-like structure.

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Abstract

The invention relates to a micron acicular-structure N-methyl-2-phenyl-3,4-fullerenylpyrrolidine, and a preparation method and application thereof. The fullerene C60, benzaldehyde and sarcosine are used as raw materials to prepare the N-methyl-2-phenyl-3,4-fullerenylpyrrolidine and N-methyl-2-phenyl-3,4-fullerenylpyrrolidine in a micron acicular structure; and the micron acicular-structure N-methyl-2-phenyl-3,4-fullerenylpyrrolidine is used as a support to prepare the catalyst for preparing p-aminophenol from nitrobenzene by catalytic hydrogenation. The product prepared by the technique has the advantages of high yield and high purity; and the prepared catalyst has the advantages of high activity and long service life.

Description

technical field [0001] The present invention relates to a preparation method and application of fullerene derivatives, more specifically, to a preparation method and application of N-methyl-2-phenyl-3,4-fullerenylpyrrolidine . Background technique [0002] In terms of modern science and engineering technology, compared with the same material composed of conventional particles, materials composed of nanoparticles with a particle size in the nanometer range have great differences in performance. This material has physical and chemical properties. It has more advantages, and has potential application prospects in catalysts and optoelectronic devices. Fullerene-based nanomaterials have very important optical, electrical, magnetic, and catalytic properties, so scientists are working hard to find different methods in order to prepare fullerene-based nanomaterials with the same shape and uniform particle size distribution. Bokare and Patnaik directly use C 60 CS 2 The solution ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/96B01J32/00B01J31/02C07C215/76C07C213/00
CPCC07C213/00C07D209/96B01J31/0244B01J35/50C07C215/76
Inventor 黄飞魏先文陈国平
Owner HUANGSHAN UNIV
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