Method for separating of metal fullerene m@C82 and isomer thereof

A technology for separating metal fullerenes and metals, applied in the chemical field, can solve problems such as inability to separate fullerenes, unfit for industrial production, harsh reaction conditions, etc., and achieve high-selectivity separation, fast separation speed, and simple equipment

Active Publication Date: 2019-04-19
BEIJING FUNAKANG BIOTECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the inventors found in actual production that TiCl 4 , SnCl 4 etc. are easy to deliquescence and need to be operated under the protection of inert gas. The reaction conditions are very harsh and are not suitable for industrial production.
In addition, TiCl 4 , SnCl 4 The selectivity of fullerenes is not strong, and high-purity fullerenes cannot be separated

Method used

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  • Method for separating of metal fullerene m@C82 and isomer thereof
  • Method for separating of metal fullerene m@C82 and isomer thereof
  • Method for separating of metal fullerene m@C82 and isomer thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Example 1: Metal fullerene Gd@C 82 separation and extraction of

[0056] (1) copper bromide (CuBr 2 ) to metallofullerene Gd@C 82 separation

[0057] (a) The metal Gd powder and spectroscopically pure graphite powder were mixed, filled into hollow graphite tubes and compacted, and arc discharge method was used to obtain soot containing fullerene products. Put the soot into a filter paper bag, put it into a Soxhlet extractor, and use N,N-dimethylformamide (DMF) as a solvent to extract at 150°C and low vacuum for 24 hours to obtain a black solution.

[0058] (b) Filter the above solution to remove a large number of suspended particles, take 500 mL of the filtrate in a round bottom flask, and use a rotary evaporator to completely evaporate the filtrate to dryness. Add 500mL of toluene, put it into an ultrasonic reactor (model: KQ-300DB; power: 300W; ultrasonic frequency: 40KHz) for ultrasonic reaction for 2h, and filter to obtain a clear brown-yellow filtrate, which is...

Embodiment 2

[0073] Example 2: Selective separation of Gd@C 82 isomer

[0074] (1) copper bromide (CuBr 2 ) to metallofullerene Gd@C 82 Separation of isomers

[0075] (a) Metallofullerene Gd@C prepared by traditional arc discharge method 82 Usually contains two isomers with relatively stable chemical properties: Gd@C 2v -C 82 and Gd@C s -C 82 , such as, the bright yellow filtrate obtained in step (d) of Example 1(1) contains two Gd@C 82 isomers, such as figure 2 shown. Take 500mL of this solution, add 10mg of CuBr 2 , precisely control the stirring (speed: 1000rpm) time to 40min. CuBr 2Priority with Gd@C s -C 82 The isomer reaction produces a complex precipitate, which is filtered through a solvent filter to collect the precipitate, and the filtrate contains only another isomer Gd@C 2v -C 82 .

[0076] (b) Washing in a solvent filter using aqueous sodium carbonate solution containing only Gd@C s -C 82 Precipitation of isomers three times, suction filtration completely r...

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Abstract

The invention provides a method for realizing high-efficiency, fast, high-selectivity and high-purity separating of metal fullerene m@C82 and an isomer thereof by using a specific lewis acid, the method can be used for simply and rapidly separating the metal fullerene and hollow fullerene, and meanwhile, the high-purity metal fullerene isomer can be further separated by strictly controlling chemical reaction kinetics. The method is simple to operate, low in cost and high in feasibility, and is suitable for large-scale production of the metal fullerene.

Description

technical field [0001] The invention relates to the field of chemistry, and further relates to a method for separating metal fullerenes M@C 82 and its isomers. Background technique [0002] Metallofullerenes refer to a special class of molecules in which metal ions or metal-containing ion clusters are embedded in fullerene carbon cages. Metallofullerenes not only have the physical and chemical properties of fullerene carbon cages, but also exhibit excellent optical, electrical, and magnetic properties of embedded metals or clusters, and have great potential application value in the fields of energy devices and biomedicine. [0003] In 1992, Gillan et al. found that most lanthanide metals can be expressed as M@C 82 The form of (M=Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb, Lu) is embedded in the fullerene carbon cage. Metallofullerenes such as Gd@C 82 , has important potential application value in the field of MRI contrast agent and antitumor drug. With the continuous de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/156
CPCC01B32/156C01P2002/87C01P2002/89C01P2002/84
Inventor 王春儒李杰
Owner BEIJING FUNAKANG BIOTECH CO LTD
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