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Preparation method of special chromatography separation medium for separating fullerene and derivatives of fullerene

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: 2015-04-29
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.
[0003] 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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  • Preparation method of special chromatography separation medium for separating fullerene and derivatives of fullerene
  • Preparation method of special chromatography separation medium for separating fullerene and derivatives of fullerene
  • Preparation method of special chromatography separation medium for separating fullerene and derivatives of fullerene

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Embodiment 1

[0028] A method for preparing a special chromatographic separation medium for the separation of fullerenes and their derivatives. Pyrene is bonded to the surface of the porous silicon ball matrix, and a smaller volume of pentabromobenzene is further bonded to the gaps of the pyrene molecules to make the silicon The surface of the ball produces two functional groups that affect the separation; the specific steps are:

[0029] (1) 5g of porous amino silicon balls with a particle size of 10μm are added to 50mL of toluene, stirred to make it wet and uniformly dispersed;

[0030] (2) 4g of pyrene hexanoic acid was added to the toluene suspended with porous amino silicon balls, stirred and mixed uniformly;

[0031] (3) Add 1-hydroxybenzotriazole (HOBt), a condensation agent of 0.5% by weight of pyrenehexanoic acid, react at 80°C for 24 hours, and filter;

[0032] (4) Add the bonded silicon balls to 50-500 mL of toluene again, and add 10 g of pentabromobenzyl bromide, react at 80°C for 24 ho...

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Abstract

The invention relates to a preparation method of a special chromatography separation medium for separating fullerene and derivatives of fullerene. The method is characterized by comprising the following specific steps: (1) adding 5-50g of a porous amino silicone ball to 50-500mL of methylbenzene, stirring, moistening and dispersing evenly; (2) adding 4-40g of pyrene caproic acid to methylbenzene suspending the porous amino silicone ball, stirring and mixing evenly; (3) adding a condensation agent, reacting at 80 DEG C for 24 hours, and filtering; (4) adding a bonded silica ball to 50-500mL of methylbenzene again, adding 10-100g of penta benzyl bromide, reacting at 80 DEG C for 24 hours, and filtering; and (5) washing with 50-500mL of methylbenzene for three times, and drying at 80 DEG C to obtain the chromatography separation medium. According to the chromatography separation medium bonded by two groups, the bonding density and the separation selectivity are superior to those of a bonded single group; especially the preparation load capacity is relatively large; and the preparation efficiency can be significantly improved.

Description

【Technical Field】 [0001] The invention relates to the technical field of chromatographic separation media, in particular to a preparation method of a chromatographic separation media special for the separation of fullerenes and their derivatives. 【Background technique】 [0002] Fullerenes and their different derivatives have been developed one after another. Under normal circumstances, the activity and effect of fullerene derivatives are better than that of a single fullerene. This is also 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 purification of these compounds have also brought great problems. [0003] Due to the increasing number of fullerene derivatives, the separation difficulties caused are increasing. The traditional single-bonded fillers can no longer meet the current separation requirements, so we are now bonding pyrene and penta...

Claims

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Application Information

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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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