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A kind of preparation method of special chromatographic separation medium for separation of fullerene and its derivatives

A technology for chromatographic separation and derivatives, which is applied in the field of preparation of special chromatographic separation media for the separation of fullerenes and their derivatives, can solve the problems of increasing separation difficulties, achieve the effect of large preparation load and improve preparation efficiency

Active Publication Date: 2017-02-15
SOOCHOW HIGH TECH CHROMATOGRAPHY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the similarity of their structures, it also brings great problems to the separation analysis and separation and purification of these compounds.
[0005] As there are more and more derivatives of fullerene, the difficulty of separation is also increasing. The traditional single-bonded packing can no longer meet the current separation requirements, so we now bond pyrene and pentabromobenzene in two parts. on the same silicon sphere

Method used

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  • A kind of preparation method of special chromatographic separation medium for separation of fullerene and its derivatives
  • A kind of preparation method of special chromatographic separation medium for separation of fullerene and its derivatives
  • A kind of preparation method of special chromatographic separation medium for separation of fullerene and its derivatives

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Embodiment 1

[0033] A method for preparing a special chromatographic separation medium for the separation of fullerenes and their derivatives. Pyrene is bonded to the surface of a porous silicon sphere matrix, and pentabromobenzene with a smaller volume is further used to bond to the gap between pyrene molecules, so that The surface of the ball produces two kinds of functional groups that affect the separation; the specific steps are:

[0034] (1) Add 5g of porous amino silicon spheres with a particle size of 10μm into 50mL of toluene, stir to make it wet and evenly disperse;

[0035] (2) The pyrenecaproic acid of 4g joins in the toluene that is suspended with porous amino silicon ball, stirs, mixes;

[0036] (3) Add condensing agent 1-hydroxybenzotriazole (HOBt) with pyrenecaproic acid weight percent of 0.5%, react at 80° C. for 24 hours, and filter;

[0037] (4) Add the bonded silicon spheres to 50-500mL of toluene again, and add 10g of pentabromobenzyl bromide, react at 80°C for 24h, a...

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Abstract

The invention relates to a method for preparing a special chromatographic separation medium for the separation of fullerenes and their derivatives, which is characterized in that the specific steps are: (1) adding 5-50 g of porous amino silicon spheres to 50-500 mL of toluene, Stir to make it wet and disperse evenly; (2) Add 4-40g of pyrenecaproic acid to the toluene suspended with porous amino silicon balls, stir and mix evenly; (3) Add a condensing agent, React for 24 hours, filter; (4) add bonded silicon spheres to 50-500 mL of toluene again, and add 10-100 g of pentabromobenzyl bromide, react at 80 ° C for 24 hours, filter; (5) 50-500 mL of toluene Wash three times and dry at 80°C to obtain a chromatographic separation medium. The performance of the chromatographic separation medium bonded with two groups of the present invention is better than that of a single group in terms of bonding density and separation selectivity, especially the preparation capacity is larger, which can significantly improve the preparation efficiency.

Description

[0001] 【Technical field】 [0002] The invention relates to the technical field of chromatographic separation media, in particular to a preparation method of a special chromatographic separation medium for the separation of fullerenes and their derivatives. [0003] 【Background technique】 [0004] Fullerenes and their various derivatives have been successively developed. Usually, the activity and effect of fullerene derivatives are better than that of a single fullerene, which is the main reason why new fullerene derivatives, including metal fullerenes, have become research hotspots. However, due to the similarity of their structures, the separation analysis and separation and purification of these compounds have also brought great problems. [0005] As there are more and more derivatives of fullerene, the difficulty of separation is also increasing. The traditional single-bonded packing can no longer meet the current separation requirements, so we now bond pyrene and pentabrom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08C07C69/616C07C67/56C07D209/94
CPCB01D15/08B01J20/286B01J2220/54C07B2200/11C07C67/56C07C2604/00C07D209/94C07C69/616
Inventor 张维冰邵平戈兆松
Owner SOOCHOW HIGH TECH CHROMATOGRAPHY
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