Unlock instant, AI-driven research and patent intelligence for your innovation.

Dihydroxyfullerenol and preparation method thereof

A technology of dihydroxyfullerol and monohydroxyfullerol, which is applied in the field of fullerol, can solve the problems of inability to simply determine the reaction product, lack of selectivity, increase of experimental consumption, etc., so as to save manpower and improve products. The effect of purity, good selectivity

Active Publication Date: 2017-08-25
深圳市赛欣瑞科技创新中心 +2
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polyhydric fullererol is polyhydric fullererol. Since polyhydric fullereryl alcohol has multiple hydroxyl groups, when derivatization is performed on this basis, the reactants produced are diverse, and it is impossible to simply determine what the reaction product is. , and many side reactions, no selectivity, increased experimental consumption, not conducive to research

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Dihydroxyfullerenol and preparation method thereof
  • Dihydroxyfullerenol and preparation method thereof
  • Dihydroxyfullerenol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of bishydroxy fullerenol, its chemical structural formula (a) is:

[0028]

[0029] The preparation method of above-mentioned bishydroxy fullerenol, comprises the following steps:

[0030] S1. In terms of molar ratio, fullerene: p-toluoyl chloride: ferric perchlorate: o-dichlorobenzene = 1:50:2:25, wherein fullerene and p-toluoyl chloride react material, ferric perchlorate (Fe(ClO 4 ) 3 ·6H 2 0) is a catalyst, and o-dichlorobenzene (ODCB) is a solvent. First add 0.2mol ferric perchlorate and 5mol p-toluoyl chloride to the reaction bottle, vacuumize, protect with nitrogen, and activate the reactants at 60°C for 20min; then inject 0.1mol fullerene into the reaction bottle with a syringe 2.5mol saturated o-dichlorobenzene solution of alkenes, and reacted at this temperature for 20min, and the reaction process was strictly controlled in the absence of oxygen; after the reaction, 2ml of glacial acetic acid was added to further stabilize the target product. Sep...

Embodiment 2

[0038] A kind of bishydroxy fullerenol, its chemical structural formula (a) is:

[0039]

[0040] A preparation method of dihydroxy fullerenol, comprising the following steps:

[0041] S1. In terms of molar ratio, fullerene: p-toluoyl chloride: ferric perchlorate: o-dichlorobenzene = 1:50:3:25, wherein fullerene and p-toluoyl chloride react material, ferric perchlorate (Fe(ClO 4 ) 3 ·6H 2 0) is a catalyst, and o-dichlorobenzene (ODCB) is a solvent. First add 0.3mol ferric perchlorate and 5mol p-toluoyl chloride to the reaction bottle, vacuumize, protect with nitrogen, and activate the reactant at 80°C for 15min; then inject 0.1mol fullerene into the reaction bottle with a syringe 2.5 mol saturated o-dichlorobenzene solution of alkenes, and reacted at this temperature for 15 minutes, and the reaction process was strictly controlled in the absence of oxygen; after the reaction, 2ml of glacial acetic acid was added to further stabilize the target product. Separation and p...

Embodiment 3

[0049] A kind of bishydroxy fullerenol, its chemical structural formula (a) is:

[0050]

[0051] A preparation method of dihydroxy fullerenol, comprising the following steps:

[0052] S1. In terms of molar ratio, fullerene: p-toluoyl chloride: ferric perchlorate: o-dichlorobenzene = 1:50:3:25, wherein fullerene and p-toluoyl chloride react material, ferric perchlorate (Fe(ClO 4 ) 3 ·6H 2 0) is a catalyst, and o-dichlorobenzene (ODCB) is a solvent. First add 0.3mol ferric perchlorate and 5mol p-toluoyl chloride to the reaction bottle, vacuumize, protect with nitrogen, and activate the reactant at 70°C for 18 minutes; then inject 0.1mol fullerene into the reaction bottle with a syringe 2.5 mol saturated o-dichlorobenzene solution of alkenes, and reacted at this temperature for 18 minutes, and the reaction process was strictly controlled in the absence of oxygen; after the reaction, 2ml of glacial acetic acid was added to further stabilize the target product. Separation ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses dihydroxyfullerenol and a preparation method thereof. The preparation method comprises the following steps: S1, taking reactants including fullerene and p-methyl benzoyl chloride to be subjected to oxygen-free reaction at the reaction temperature of 60 DEG C to 80 DEG C under the conditions that ferric perchlorate is used as a catalyst and o-dichlorobenzene is used as a solvent; separating and purifying to obtain monohydroxyfullerenol; S2, hydrolyzing the monohydroxyfullerenol under an alkaline condition to obtain the dihydroxyfullerenol. According to the dihydroxyfullerenol and the preparation method thereof, a derivative of the monohydroxyfullerenol is obtained through free-radical addition and then is subjected to alkaline hydrolysis; finally, acidification is carried out to obtain a final target product of the dihydroxyfullerenol, which has the selectivity. The preparation method of the dihydroxyfullerenol, disclosed by the invention, has the advantages of short reaction time, simple flow and manpower saving and is relatively simple for laboratory preparation.

Description

technical field [0001] The invention relates to the technical field of fullerene alcohols, in particular to a dihydroxy fullerene alcohol and a preparation method thereof. Background technique [0002] Fullerene is a derivative of fullerene, which is obtained by chemically introducing a hydroxyl group on the carbon of fullerene. The polyhydric fullererol is polyhydric fullererol. Since polyhydric fullereryl alcohol has multiple hydroxyl groups, when derivatization is performed on this basis, the reactants produced are diverse, and it is impossible to simply determine what the reaction product is. , and there are many side reactions, it is not selective, increases the consumption of the experiment, and is not conducive to research. Contents of the invention [0003] In view of this, the present invention provides a dihydroxy fullerenol and a preparation method thereof to prepare the dihydroxy fullererol with selectivity. [0004] The technical means that the present inven...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C27/02C07C35/44
CPCC07B2200/11C07C29/095C07C67/14C07C69/76C07C35/44
Inventor 郑超王春儒居学成
Owner 深圳市赛欣瑞科技创新中心