CN106006598B - A kind of embedded metal fullerene purification devices and purification process - Google Patents
A kind of embedded metal fullerene purification devices and purification process Download PDFInfo
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- CN106006598B CN106006598B CN201610308268.0A CN201610308268A CN106006598B CN 106006598 B CN106006598 B CN 106006598B CN 201610308268 A CN201610308268 A CN 201610308268A CN 106006598 B CN106006598 B CN 106006598B
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Abstract
The present invention provides a kind of embedded metal fullerene purification devices and purification process comprising the following contents：It includes solvent memory, and the top of solvent memory is connected by the top of the first pipeline and extractor, and the lower part of extractor is connect by the second pipeline with solvent memory；It is provided with condensing unit on the first pipeline；It is respectively arranged with valve on the first pipeline and the second pipeline；It is respectively arranged with heating device in the bottom of solvent memory and extractor.The solvent memory of the present invention by the first pipeline and the second pipeline with extractor due to being connect respectively, after extractor completes metal fullerene extraction, solvent dissolved with metal fullerene is passed through into the second Pipeline transport back dissolving agent memory, it is returned in extractor by the first Pipeline transport again after solvent gasification in solvent memory and continues to repeat the operation, therefore the continuous operation of extraction metal fullerene may be implemented, the treating capacity of charcoal ash and the recovery rate of metal fullerene are improved, metal fullerene content in extracting solution is allow to be improved to 10% by the 1% of conventional method.
Description
Technical field
The present invention relates to a kind of embedded metal fullerene purification devices and purification process, belong to fullerene purification art.
Background technology
1985, researcher mixed with the graphite target of LaCl3 when to carrying out laser evaporation, in the mass spectral analysis of soot
Detect the presence of LaC60.Then, the embedded metal fullerene of various metallic atoms or metal cluster be produced and
Characterization.Its basic preparation process is：The composite stone inker of graphite/metal alloy composition is electric in helium atmosphere as consumption electrode
Arc discharge collects the soot containing fullerene and metal fullerene and obtains soluble fullerene and metal fowler with solvent extraction
Alkene mother liquor, then detached with chemical reaction method or high performance liquid chromatography, you can obtain pure embedded metal fullerene.Its
In, the separation and Extraction of metal fullerene is an important branch of metal fullerene research always.The study found that metal fullerene
With unique structural property and potential application value, but because technology of preparing is complicated, low yield and by it from the sky of association
It separates relatively difficult in heart fullerene and its research is made to be very restricted.
Invention content
In view of the above-mentioned problems, the embedded of metal fullerene recovery rate in charcoal ash can be improved the object of the present invention is to provide a kind of
Metal fullerene purification devices and purification process.
To achieve the above object, the present invention takes following technical scheme：A kind of embedded metal fullerene purification devices, it is special
Sign is：It includes solvent memory, and the top of the solvent memory is connected by the top of the first pipeline and extractor, institute
The lower part for stating extractor is connect by the second pipeline with the solvent memory；Condensation dress is provided on first pipeline
It sets；It is respectively arranged with valve on first pipeline and second pipeline；In the solvent memory and the extractor
Bottom be respectively arranged with heating device.
The condensing unit is arranged in first pipeline close to one end of the extractor.
Sample holding box is provided in the extractor, each wall surface of the sample holding box is provided with sieve.
A kind of purification process of embedded metal fullerene purification devices comprising following steps：
1) object to be extracted is put into extractor, and the solvent of the required liquid of reaction is added into extractor；
2) heating device for starting extractor bottoms, makes the solvent of liquid be reacted with the object to be extracted in extractor, will wait for
Metal fullerene in extract extracts；
3) valve on the second pipeline is opened, the solvent of the liquid dissolved with metal fullerene is flowed by the second pipeline
In solvent memory；
4) valve on the second pipeline is closed, the heating device of solvent memory bottom is started, is opened on the first pipeline
Valve, the solvent gasification of the liquid dissolved with metal fullerene so that the solvent of liquid becomes being flowed into after gaseous solvent the
In one pipeline, and the solute metal fullerene extracted then stays in solvent memory；
5) the gaseous solvent being flowed into the first pipeline is flowed into extraction after being condensed into liquid again by condensing unit
Continue to react with object to be extracted in device, when the solvent of the liquid in solvent memory is reduced to the 1/10 of the solvent of stoste state,
The valve on the second pipeline is opened, the solvent of the liquid dissolved with metal fullerene flow back into solvent by the second pipeline and deposits again
In reservoir；
6) by the solvent for the liquid dissolved with metal fullerene flowing back into again in solvent memory by above-mentioned steps 4),
Step 5) continues cycling through the metal fullerene extracted in object to be extracted, until the solvent of the liquid after being reacted with object to be extracted becomes
It is colourless, that is, complete the purifying of metal fullerene.
Extractor is connect with pressue device, and in the step 2), argon gas is passed through into extractor by pressue device, will be carried
Pressure in device is taken to control in 5atm, the heating and temperature control of the heating devices of extractor bottoms under the pressure limit is 140
Between~160 DEG C.
Solvent memory is connect with decompressor, in the step 4), by decompressor by the pressure in solvent memory
Power controls between -0.08atm~-0.09atm, the heating temperature of the heating device of solvent memory bottom under the pressure limit
Degree control is between 100~120 DEG C.
In the step 1), solvent uses n,N-Dimethylformamide.
In the step 4), when the solute metal fullerene content in solvent memory is excessively high, after gasifying in order to prevent
The solvent of liquid is dry, and the solvent of the liquid dissolved with metal fullerene is taken out, and the solvent that new liquid is added continue into
The extraction of row metal fullerene.
The invention adopts the above technical scheme, which has the following advantages：The solvent memory of the present invention is due to respectively
It is connect with extractor by the first pipeline and the second pipeline, after extractor completes metal fullerene extraction, it is rich metal will to be dissolved with
The solvent of alkene is strangled by the second Pipeline transport back dissolving agent memory, passes through the first pipeline again after the solvent gasification in solvent memory
It is transmitted back in extractor and continues to repeat the operation, therefore the continuous operation of extraction fullerene may be implemented, improve charcoal ash
The recovery rate for the treatment of capacity and metal fullerene allows metal fullerene content in extracting solution to be improved extremely by the 1% of conventional method
10%.
Description of the drawings
Fig. 1 is the overall structure diagram of apparatus of the present invention.
Specific implementation mode
The present invention is described in detail below with reference to the accompanying drawings and embodiments.
As shown in Figure 1, the present invention includes solvent memory 1, the top of solvent memory 1 by the first pipeline 2 with it is closed
Extractor 4 top connection, the lower part of extractor 4 is connect by the second pipeline 3 with solvent memory 1.On the first pipeline 2
It is provided with condensing unit 5, for condensing the gas entered by solvent memory 1 in first pipeline 2.In the first pipeline 2 and
It is respectively arranged with valve 6 on two pipelines 3.It is respectively arranged with heating device 7 in the bottom of solvent memory 1 and extractor 4, is used for
Solvent in heated solvent memory 1 and extractor 4.
In above-described embodiment, solvent memory 1 is also connect with decompressor 8, for reducing the pressure inside solvent memory 1
Power is conducive to keep metal fullerene not oxidizable and is conducive to solvent vapour condensation.
In above-described embodiment, extractor 4 is also connect with pressue device 9, for improving the pressure inside extractor 4.
In above-described embodiment, condensing unit 5 is arranged in the first pipeline 2 close to one end of extractor 4.
In above-described embodiment, sample holding box 41 is provided in extractor 4, each wall surface of sample holding box 41 is provided with
Sieve, for making sample fully be reacted with solvent in extractor 4.
The invention also includes a kind of purification process based on above-mentioned metal fullerene purification devices comprising following steps：
1) charcoal ash dissolving packet 11 to be extracted is put into extractor 4, and liquid needed for addition reaction is molten into extractor 4
Agent 10 makes liquid solvent 10 dissolve packet 11 with charcoal ash and comes into full contact with；
2) heating device 7 for starting 4 bottom of extractor, opens pressue device 9, the liquid solvent 10 under high-pressure high-temperature environment
It is reacted with the charcoal ash dissolving packet 11 in extractor 4, the fullerene in charcoal ash dissolving packet 11 is extracted, especially by metal richness
Alkene is strangled constantly to extract；
3) valve 6 on the second pipeline 3 is opened, the liquid solvent 10 dissolved with metal fullerene is flowed by the second pipeline 3
It returns in solvent memory 1, completes the extraction of a metal fullerene；
4) valve 6 on the second pipeline 3 is closed, the heating device 7 of 1 bottom of solvent memory, open pressure reducing device 8 are started
With the valve 6 on the first pipeline 2, the liquid solvent 10 dissolved with metal fullerene gasifies under low-voltage high-temperature environment so that liquid
State solvent 10 becomes gaseous solvent 10 and is flowed into the first pipeline 2, and the solute metal fullerene extracted stays in solvent storage
In device 1；
5) gaseous solvent 10 being flowed into the first pipeline 2 is condensed into be flowed into after liquid by condensing unit 5 and be carried again
It takes and continues to react with charcoal ash dissolving packet 11 in device 4, when the liquid solvent 10 in solvent memory 1 is reduced to former liquid solvent 10
When 1/10, the valve 6 on the second pipeline 3 is opened, the liquid solvent 10 dissolved with metal fullerene is flowed again by the second pipeline 3
It returns in solvent memory 1；
6) liquid solvent 10 dissolved with metal fullerene flowing back into again in solvent memory 1 is sequentially repeated and is followed
Ring above-mentioned steps 4), 5), the metal fullerene in extraction charcoal ash dissolving packet 11 is continued cycling through, until 11 being reacted with charcoal ash dissolving packet
Liquid solvent 10 afterwards becomes colorless, that is, completes the purifying of metal fullerene, and the content of metal fullerene after purification can reach
To 10%.
In above-described embodiment, when the solute metal fullerene content in solvent memory 1 is excessively high, after gasifying in order to prevent
Liquid solvent is dry, can take out the liquid solvent 10 dissolved with metal fullerene, and be added new liquid solvent 10 continue into
The extraction of row metal fullerene.
Above-mentioned steps 1) in, n,N-Dimethylformamide (DMF) can be used in solvent 10.
Above-mentioned steps 2) in, argon gas is passed through into extractor 4 by pressue device 9, the pressure control in extractor 4 is existed
5atm, the heating and temperature control of the heating device 7 of 4 bottom of extractor under the pressure limit is between 140~160 DEG C.
Above-mentioned steps 4) in, by decompressor 8 by solvent memory 1 pressure control -0.08atm~-
Between 0.09atm, the heating and temperature control of the heating device 7 of 1 bottom of solvent memory under the pressure limit is 100~120
Between DEG C.
The various embodiments described above are merely to illustrate the present invention, wherein the structure of each component, connection type etc. are all can be
Variation, every equivalents carried out based on the technical solution of the present invention and improvement should not be excluded the present invention's
Except protection domain.
Claims (5)
1. a kind of purification process of embedded metal fullerene purification devices comprising following steps：
1) the embedded metal fullerene purification devices include solvent memory, and the top of the solvent memory passes through the first pipeline
It is connect with the top of extractor, the lower part of the extractor is connect by the second pipeline with the solvent memory；Described
It is provided with condensing unit on one pipeline；It is respectively arranged with valve on first pipeline and second pipeline；Described molten
The bottom of agent memory and the extractor is respectively arranged with heating device；
2) object to be extracted is put into extractor, and the solvent of the required liquid of reaction is added into extractor；
3) heating device for starting extractor bottoms, makes the solvent of liquid be reacted with the object to be extracted in extractor, will be to be extracted
Metal fullerene in object extracts；In the process, argon gas is passed through into extractor by pressue device, it will be in extractor
Pressure control in 5atm, the heating and temperature control of the heating devices of extractor bottoms under the pressure limit is at 140~160 DEG C
Between；
4) valve on the second pipeline is opened, the solvent of the liquid dissolved with metal fullerene is flowed into solvent by the second pipeline
In memory；
5) valve on the second pipeline is closed, the heating device of solvent memory bottom is started, opens the valve on the first pipeline,
The solvent of liquid dissolved with metal fullerene gasifies so that the solvent of liquid is flowed into the first pipeline after becoming gaseous solvent
In, and the solute metal fullerene extracted then stays in solvent memory；In the process, solvent is deposited by decompressor
Pressure in reservoir controls between -0.08atm~-0.09atm, and the heating device of solvent memory bottom is in the pressure limit
Under heating and temperature control between 100~120 DEG C；
6) the gaseous solvent being flowed into the first pipeline is flowed into after being condensed into liquid again by condensing unit in extractor
Continuation is reacted with object to be extracted, when the solvent of the liquid in solvent memory is reduced to the 1/10 of the solvent of stoste state, is opened
The solvent of valve on second pipeline, the liquid dissolved with metal fullerene flow back into solvent memory again by the second pipeline
In；
7) by the solvent for the liquid dissolved with metal fullerene flowing back into again in solvent memory by above-mentioned steps 5), step
6) metal fullerene extracted in object to be extracted is continued cycling through, until the solvent of the liquid after being reacted with object to be extracted becomes nothing
Color completes the purifying of metal fullerene.
2. a kind of purification process as described in claim 1, it is characterised in that：In the step 2), solvent uses N, N- diformazans
Base formamide.
3. a kind of purification process as described in claim 1, it is characterised in that：In the step 5), when in solvent memory
When solute metal fullerene content is excessively high, the solvent of liquid is dry after gasifying in order to prevent, by the liquid dissolved with metal fullerene
The solvent of state takes out, and the solvent that new liquid is added continues the extraction of metal fullerene.
4. a kind of purification process as described in claim 1, it is characterised in that：The condensing unit is arranged in first pipeline
Close to one end of the extractor.
5. a kind of purification process as described in claim 1, it is characterised in that：Sample is provided in the extractor to hold
Each wall surface of box, the sample holding box is provided with sieve.
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| CN201610308268.0A CN106006598B (en) | 2016-05-11 | 2016-05-11 | A kind of embedded metal fullerene purification devices and purification process |
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| CN201610308268.0A CN106006598B (en) | 2016-05-11 | 2016-05-11 | A kind of embedded metal fullerene purification devices and purification process |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR907632A (en) * | 1942-04-22 | 1946-03-18 | Extraction device | |
| US4006062A (en) * | 1975-01-09 | 1977-02-01 | Council Of Scientific And Industrial Research | Still extractor with novel stopcock means |
| DE4301343C2 (en) * | 1993-01-20 | 1994-12-01 | Gerhardt Fabrik Und Lager Chem | Method and device for solvent extraction |
| JP2002177702A (en) * | 2000-12-08 | 2002-06-25 | Sony Corp | Ultrasonic reflux system for single step refining of carbon nano structure |
| CN102115074B (en) * | 2009-12-30 | 2013-09-04 | 中国科学院高能物理研究所 | Extraction method of internally-embedded metal fullerene |
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Address after: No. 1001, Longgang Avenue, Longgang District, Shenzhen, Guangdong 518000 Patentee after: Shenzhen Lihe Technology Innovation Co.,Ltd. Address before: 518117 TONGCHAN Lixing science and Technology Industrial Park, 1001 Longgang Avenue (Ping lot), Longgang District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN BEAUTY STAR Co.,Ltd. |