Method for extracting endohedral metallofullerene

A technology of metallofullerene and extraction method, which is applied in the field of extraction of embedded metallofullerene, can solve the problems of not being able to adapt to the large-scale production of fullerene, waste of materials, and low purity of fullerene

Inactive Publication Date: 2017-05-31
HENAN INST OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for extracting embedded metal fullerenes, to solve the problem that the fullerenes extracted in the laboratory extraction process of the current fullerenes proposed in the above-mentioned background technology are not high in purity, resulting in a huge loss of materials. Waste, and cannot adapt to the problem of large-scale production of fullerenes

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  • Method for extracting endohedral metallofullerene

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Embodiment 1

[0024] An extraction method for embedded metallofullerenes, the specific steps of the extraction method for embedded metallofullerenes are as follows:

[0025] S1: Drill out the spectral grade graphite rod The deep holes are filled with pre-treated mixtures of various rare earth oxides and graphite powders. The rare earth oxides are dried and dehydrated at a high temperature of 280°C for 3.5 hours. The ratio of rare earth atoms to carbon atoms in the mixture is 1: 50;

[0026] S2: Roasting the filled graphite rod at 1700°C for 3 hours under vacuum conditions to change rare earth oxides into rare earth carbides;

[0027] S3: at 1.1 x 10 4 Discharge synthesis is carried out under the protection of Pa's helium, and a large amount of soot is produced during the discharge, and carbon deposition rods are produced at the end of the cathode. During the discharge synthesis process, the current is 140A and the voltage is 25V;

[0028] S4: Exchange the electrodes, and reverse dischar...

Embodiment 2

[0036] An extraction method for embedded metallofullerenes, the specific steps of the extraction method for embedded metallofullerenes are as follows:

[0037] S1: Drill out the spectral grade graphite rod The deep hole is filled with a mixture of pretreated various rare earth oxides and graphite powder. The rare earth oxide is dried and dehydrated at a high temperature of 300°C for 4.5 hours. The ratio of rare earth atoms to carbon atoms in the mixture is 1: 50;

[0038] S2: Calcining the filled graphite rod at 1900°C for 4 hours under vacuum conditions to change rare earth oxides into rare earth carbides;

[0039] S3: at 1.3×10 4 Discharge synthesis is carried out under the protection of Pa's helium gas, and a large amount of soot is produced during discharge, and carbon deposition rods are produced at the end of the cathode. During the discharge synthesis process, the current is 180A and the voltage is 35V;

[0040] S4: Exchange the electrodes, and reverse discharge, so...

Embodiment 3

[0048] An extraction method for embedded metallofullerenes, the specific steps of the extraction method for embedded metallofullerenes are as follows:

[0049] S1: Drill out the spectral grade graphite rod The deep holes are filled with pre-treated mixtures of various rare earth oxides and graphite powder. The rare earth oxides are dried and dehydrated at 290°C for 4 hours. The ratio of rare earth atoms to carbon atoms in the mixture is 1:50 ;

[0050] S2: Roast the filled graphite rod at a high temperature of 1800°C for 3.5 hours under vacuum conditions to change the rare earth oxide into rare earth carbide;

[0051] S3: at 1.2 x 10 4 Discharge synthesis is carried out under the protection of Pa's helium, and a large amount of soot is produced during the discharge, and carbon deposition rods are produced at the end of the cathode. During the discharge synthesis process, the current is 160A and the voltage is 30V;

[0052] S4: Exchange the electrodes, and reverse discharge...

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Abstract

The invention discloses a method for extracting endohedral metallofullerene in the technical field of fullerene extraction. The method for extracting the endohedral metallofullerene comprises the specific steps: S1, filling a pre-treated mixture of various rare-earth oxides and graphite powder in a deep hole; S2, enabling the rare-earth oxides to be changed into rare-earth carbides; S3, discharging to generate soot; S4, carrying out reverse discharging, so that a carbon deposition rod is consumed into soot; S5, extracting coarse ashes; S6, drying the extracted coarse ashes in a vacuum manner; S7, collecting and extracting the soot; S8, removing and drying the rest soot; S9, putting the ashes into a high pressure kettle to be extracted; S10, pumping, filtering and drying an extracting solution. According to the method for extracting the endohedral metallofullerene, the ashes generated in the discharging process are further extracted, so that the ashes can be sufficiently utilized and the content of high fullerenes in the product is obviously increased to develop a shortcut for further enrichment, separation and purification of the endohedral fullerene; therefore, the method for extracting the endohedral metallofullerene is especially suitable for larger-scale extraction.

Description

technical field [0001] The invention relates to the technical field of fullerene extraction, in particular to an extraction method for embedded metal fullerenes. Background technique [0002] Fullerene is the name of the solid state of fullerene and its derivatives, which is generally not specifically called in Chinese. The term superhard fullerene is generally used to describe fullerene obtained using high pressure and high temperature. Under such conditions, ordinary fullerene solids will form nanocrystals in the form of diamonds, which have relatively high mechanical strength and hardness. The embedded fullerene is a new type of embedded fullerene formed by embedding some atoms into the fullerene carbon cage, such as hydrogen, carbon, scandium, nitrogen, etc., most of which are produced in the process of producing fullerene by the arc method Formed, fullerene can also be filled with some atoms or molecules after opening the pores by chemical methods. [0003] At present...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/154
Inventor 崔乘幸王吉超刘露焦红艳张中印张裕平
Owner HENAN INST OF SCI & TECH
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