CN114275769A - Method for separating C from fullerene mixture by utilizing silver salt60And C70Method (2) - Google Patents
Method for separating C from fullerene mixture by utilizing silver salt60And C70Method (2) Download PDFInfo
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Abstract
Method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the steps of completely dissolving a fullerene mixture in an organic solution to obtain a solution to be separated, mixing a silver salt with the solution to be separated according to a mass ratio of 20: 1-50: 1, reacting for 24-48 hours in a dark place at the temperature of 40-70 ℃, filtering out precipitates to obtain the solution containing C60And C70The filtrate of (1); then according to the prior art to the compound containing C60And C70The filtrate is separated to obtain pure C60With pure C70. The method utilizes silver salt to remove the large-size fullerene, and is favorable for quickly obtaining two kinds of fullerene C with the highest yield60And C70The mixture of (A) is simple to operate, does not require expensive equipment, is not limited by quantity, and combines the existing separation C60And C70Can realize the separation of pure C under the condition of completely not depending on any chromatographic technology60And C70Is very suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of fullerene separation, in particular to a method for separating C from a fullerene mixture by utilizing silver salt60And C70The method of (1).
Background
Fullerene is a novel zero-dimensional carbon material and has good application in the fields of biomedicine, energy and new materials. At present, fullereneThe only industrially applicable preparation method is the arc process, which produces a virtually fullerene mixture containing many molecules, such as C60、C70、C76、C78、C84And fullerenes of larger size. Due to the close nature of these fullerene molecules, it is difficult to simply separate one fullerene molecule. The separation method commonly used at present adopts High Performance Liquid Chromatography (HPLC) for separation, the separation method has high cost, the mixture which can be used for separation at a time is generally not more than 50mg under the conditions of expensive equipment and specially modified chromatographic columns, and the separation efficiency is very low. Therefore, the reduction or complete independence of chromatography during the separation process would be of great importance for the industrial production of fullerenes.
For this reason, researchers have also developed some new fullerene separations, which are currently focused primarily on the highest yields of the two fullerenes C60And C70Separation, first by means of AlCl3From C60And C70Separating out pure C from the mixed solution60(e.g., convention separation of high-purity C)60 from crude fullerene extract by selective complexation with AlCl3PNAS 91: 9019-60Can be oriented to absorb by the frame material to filter out C70(e.g., Effective Encapsulation of C60 by Metal-Organic Frameworks with polyamine macromolecular Linker, Angew. chem. int. Ed. 2021,60, 10814-; similarly, the pure C is separated by using a framework formed by silver nitrate molecules by a liquid-liquid interface deposition method70(e.g., Selective extraction of fullerene C)60 by in situinterweaved AgNO3 complex encapsulated C60molecular sieves, J Mater Sci (2021)56: 380-391; cage-shaped AgNO3Separation and purification of chelate structures C70CA 110902669B), in addition to C60Separation of pure C by its low reactivity60。
These techniques are all that is to first obtain pure C60And C70Mixed together and then separated by taking advantage of the difference in structural properties of the two. However, in the actual production process, there is no C60And C70Mixture, first obtaining a fullerene mixture containing not only C60And C70It also contains large-size fullerene, and although the content of the large-size fullerene is lower and the total content is less than 10%, the components are complex, and the properties are also similar to those of C60、C70Close, their presence greatly increases C60、C70The separation difficulty of (3). The most effective is the traditional HPLC separation at present, but the whole separation process is high in cost, time-consuming and labor-consuming.
Disclosure of Invention
The technical problem solved by the invention is to provide a method for separating C from a fullerene mixture by utilizing silver salt60And C70To solve the above problems in the background art.
The technical problem solved by the invention is realized by adopting the following technical scheme:
method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the following specific steps:
(1) completely dissolving a fullerene mixture obtained by a known method in an organic solution to obtain a solution to be separated, mixing a silver salt with the solution to be separated according to a mass ratio of 20: 1-50: 1, reacting for 24-48 hours in a dark place at the temperature of 40-70 ℃, filtering out precipitates to obtain a solution containing C60And C70The filtrate of (1);
(2) will contain C according to the prior art60And C70Evaporating the filtrate to obtain filtrate to be separated, dissolving carbon disulfide in the filtrate to be separated to obtain mixed solution to be separated, mixing aluminum trichloride and the mixed solution to be separated according to a mass ratio, and stirring under a dark condition to obtain the product containing pure C60The filtrate and the precipitate of (2);
(3) washing the precipitate obtained in the step (2) with water to obtain pure C70。
In the present invention, in step (1), the fullerene mixture is a hollow fullerene mixture or a metal-containing fullerene mixture.
In the invention, in the step (1), the silver salt is silver trifluoroacetate, silver nitrate, silver phosphate or silver acetate, preferably silver trifluoroacetate and silver nitrate, and the silver trifluoroacetate and the silver nitrate have high activity and high stability, and are easy to form precipitates with large-size fullerene in a solution to be separated to obtain the fullerene containing only C60And C70A fullerene mixture of (4).
In the present invention, in the step (1), the temperature condition is preferably 60 ℃.
Has the advantages that: the whole separation process only needs a small amount of silver salt and the solution to be separated to form precipitate, and then the precipitate is cleaned by water, so that the method is simple to operate and very economic, the cost of the silver salt and the organic solvent is low, the experimental conditions are common, no special environment is needed, all the operations can be carried out in a common laboratory, the defects of high cost, time consumption, complex operation and the like of general HPLC (high performance liquid chromatography) separation are effectively overcome, and the method is very suitable for separating C with the content of more than 90 percent from the fullerene mixture60And C70The fullerene greatly improves the separation efficiency of the fullerene; simultaneously combine existing C60And C70The technique of thorough separation, by means of which it is possible to carry out the separation of C under conditions which are completely independent of chromatography60And C70The separation and purification of the fullerene can greatly reduce the cost of industrial production and improve the industrial production efficiency of the fullerene.
Drawings
Fig. 1 is a mass spectrum before and after separation of a fullerene mixture according to preferred embodiment 1 of the present invention.
Fig. 2 is a chromatogram before and after separation of a fullerene mixture according to preferred embodiment 1 of the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below by combining the specific drawings.
Example 1
Method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the specific steps ofThe following were used:
(1) completely dissolving fullerene raw ash obtained by a known method in an organic solution to obtain a solution to be separated, mixing silver salt and the solution to be separated according to the mass ratio of 20:1, reacting for 24 hours in a dark place at the temperature of 60 ℃, filtering out precipitates to obtain a solution containing C60And C70The filtrate of (1);
(2) will contain C according to the prior art60And C70Evaporating the filtrate to dryness by rotary evaporation to obtain filtrate to be separated, dissolving carbon disulfide in the filtrate to be separated to obtain mixed solution to be separated, finally mixing aluminum trichloride with the mixed solution to be separated according to the mass ratio of 30:1, stirring for 24 hours under the condition of keeping out of the sun to obtain the product containing pure C60The filtrate and the precipitate of (2);
(3) washing the precipitate obtained in the step (2) with water to obtain pure C70。
Example 2
Method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the following specific steps:
(1) completely dissolving fullerene raw ash obtained by a known method in an organic solution to obtain a solution to be separated, mixing silver salt and the solution to be separated according to a mass ratio of 30:1, reacting for 48 hours in a dark place at the temperature of 60 ℃, filtering out precipitates to obtain a solution containing C60And C70The filtrate of (1);
(2) will contain C according to the prior art60And C70Evaporating the filtrate to dryness by rotary evaporation to obtain filtrate to be separated, dissolving carbon disulfide in the filtrate to be separated to obtain mixed solution to be separated, finally mixing aluminum trichloride with the mixed solution to be separated according to the mass ratio of 30:1, stirring for 24 hours under the condition of keeping out of the sun to obtain the product containing pure C60The filtrate and the precipitate of (2);
(3) washing the precipitate obtained in the step (2) with water to obtain pure C70。
Example 3
Method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the following specific steps:
(1) will be enriched using known methodsCompletely dissolving the leylen raw ash in an organic solution to obtain a solution to be separated, mixing a silver salt with the solution to be separated according to a mass ratio of 50:1, reacting for 60 hours in a dark place at the temperature of 70 ℃, filtering out precipitates to obtain a product containing C60And C70The filtrate of (1);
(2) will contain C according to the prior art60And C70Evaporating the filtrate to dryness by rotary evaporation to obtain filtrate to be separated, dissolving carbon disulfide in the filtrate to be separated to obtain mixed solution to be separated, finally mixing aluminum trichloride with the mixed solution to be separated according to the mass ratio of 30:1, stirring for 24 hours under the condition of keeping out of the sun to obtain the product containing pure C60The filtrate and the precipitate of (2);
(3) washing the precipitate obtained in the step (2) with water to obtain pure C70。
Example 4
Method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the following specific steps:
(1) completely dissolving fullerene raw ash obtained by a known method in an organic solution to obtain a solution to be separated, mixing silver salt and the solution to be separated according to the mass ratio of 40:1, reacting for 24 hours in a dark place at the temperature of 70 ℃, filtering out precipitates to obtain a solution containing C60And C70The filtrate of (1);
(2) will contain C according to the prior art60And C70Evaporating the filtrate to dryness by rotary evaporation to obtain filtrate to be separated, dissolving carbon disulfide in the filtrate to be separated to obtain mixed solution to be separated, finally mixing aluminum trichloride with the mixed solution to be separated according to the mass ratio of 30:1, stirring for 24 hours under the condition of keeping out of the sun to obtain the product containing pure C60The filtrate and the precipitate of (2);
(3) washing the precipitate obtained in the step (2) with water to obtain pure C70。
Example 5
Method for separating C from fullerene mixture by utilizing silver salt60And C70The method comprises the following specific steps:
(1) completely dissolving fullerene raw ash obtained by a known method in an organic solution to obtain a solution to be separated, and then mixing silver salt with silver saltMixing the separated solutions according to the mass ratio of 50:1, reacting for 48 hours in the dark at the temperature of 70 ℃, filtering out precipitates to obtain the product containing C60And C70The filtrate of (1);
(2) will contain C according to the prior art60And C70Evaporating the filtrate to dryness by rotary evaporation to obtain filtrate to be separated, dissolving carbon disulfide in the filtrate to be separated to obtain mixed solution to be separated, finally mixing aluminum trichloride with the mixed solution to be separated according to the mass ratio of 30:1, stirring for 24 hours under the condition of keeping out of the sun to obtain the product containing pure C60The filtrate and the precipitate of (2);
(3) washing the precipitate obtained in the step (2) with water to obtain pure C70。
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. Method for separating C from fullerene mixture by utilizing silver salt60And C70The method is characterized by comprising the following specific steps:
(1) completely dissolving the fullerene mixture in an organic solution to obtain a solution to be separated, mixing a silver salt with the solution to be separated according to a mass ratio of 20: 1-50: 1, reacting for 24-48 hours in a dark place at the temperature of 40-70 ℃, filtering out precipitates to obtain a solution containing C60And C70The filtrate of (1);
(2) according to the prior art on compounds containing C60And C70The filtrate is separated to obtain pure C60With pure C70。
2. The method of claim 1, wherein the C is separated from the fullerene mixture using a silver salt60And C70The method of (2), wherein in step (1), the fullerene mixture is a hollow fullerene mixture or a metal-containing fullerene mixture.
3. The method of claim 1, wherein the C is separated from the fullerene mixture using a silver salt60And C70The method of (2), wherein in the step (1), the silver salt is silver trifluoroacetate, silver nitrate, silver phosphate or silver acetate.
4. The method of claim 3, wherein the C is separated from the fullerene mixture by using a silver salt60And C70The method of (3), wherein the silver salt is preferably silver trifluoroacetate or silver nitrate.
5. The method of claim 1, wherein the C is separated from the fullerene mixture using a silver salt60And C70The method of (2), wherein the temperature condition in the step (1) is preferably 60 ℃.
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