CN106744814A - A kind of extracting method of embedded metal fullerene - Google Patents
A kind of extracting method of embedded metal fullerene Download PDFInfo
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- CN106744814A CN106744814A CN201611108237.7A CN201611108237A CN106744814A CN 106744814 A CN106744814 A CN 106744814A CN 201611108237 A CN201611108237 A CN 201611108237A CN 106744814 A CN106744814 A CN 106744814A
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- soot
- extracting method
- rare earth
- fullerene
- embedded metal
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Abstract
The invention discloses a kind of extracting method of embedded metal fullerene in fullerene extractive technique field, the extracting method of the embedded metal fullerene is comprised the following steps that：S1：The mixture through pretreated various rare earth oxides and graphite powder is filled in deep hole；S2：Rare earth oxide is set to be changed into Rare Earth Carbides；S3：Electric discharge produces soot；S4：Back discharge makes Carbon deposition rod consume into soot；S5：Thick cigarette ash extraction；S6：Vacuum drying；S7：Collect soot and extract；S8：Remaining soot is removed and dried；S9：It is put into autoclave and extracts；S10：Extract solution suction filtration is simultaneously dried, the present invention is further extracted to the cigarette ash produced in discharge process, cigarette ash can not only made full use of, and in product the content of fullerene high dramatically increase be embedded fullerene further enrichment and separating-purifying open shortcut, be particularly well-suited to fairly large extraction.
Description
Technical field
The present invention relates to fullerene extractive technique field, specially a kind of extracting method of embedded metal fullerene.
Background technology
Fowler body is the address of the solid states of fullerene and its derivative, and Chinese does not typically call this form especially.
Superhard this word of fowler body is generally used to the fowler body that is obtained using high pressure-temperature of statement, it is this under the conditions of common fullerene
Solid can form the nanocrystal of diamond form, and it has at a relatively high mechanical strength and hardness.Embedded fullerene is that some are former
The new embedded fullerene of a class that son is embedded in Fullerene Carbon cage and is formed, such as hydrogen, carbon, scandium, nitrogen, major part is in electric arc legal system
Formed during making fullerene, it is also possible to load some atoms or molecule after fullerene is opened hole by chemical method.
The fullerene purity that current fullerene is extracted in the extraction process of laboratory is not high, causes the significant wastage of material,
And the large-scale production of fullerene is not adapted to, therefore, we have proposed a kind of extracting method input of embedded metal fullerene
Use, to solve the above problems.
The content of the invention
It is an object of the invention to provide a kind of extracting method of embedded metal fullerene, with solving above-mentioned background technology
The fullerene purity that the current fullerene for proposing is extracted in the extraction process of laboratory is not high, causes the significant wastage of material, and
The problem of the large-scale production of fullerene is not adapted to.
To achieve the above object, the present invention provides following technical scheme：A kind of extracting method of embedded metal fullerene, institute
The extracting method for stating embedded metal fullerene is comprised the following steps that：
S1：Spectroscopic graphite rod is got outDeep hole, filled in deep hole through pretreated various
The mixture of rare earth oxide and graphite powder；
S2：The graphite rod that will have been filled 1700~1900 DEG C of 3~4h of high-temperature roasting under vacuum, make rare earth oxide
It is changed into Rare Earth Carbides；
S3：1.1 × 104~1.3 × 104Electric discharge synthesis is carried out under the helium protection of Pa, and is produced during discharging a large amount of
Soot, while cathode end produce Carbon deposition rod；
S4：Electrode, and back discharge are exchanged, Carbon deposition rod is consumed into soot completely；
S5：The thick cigarette ash that graphite rod is produced is well mixed with ortho-xylene, injection extracts in the extractor equipped with filter paper bucket
Take 30~45h；
S6：Extract is vacuum dried through filtering, rotary evaporation removal solvent, extracts soot；
S7：Collect whole soots, and 20~25h of extraction under being put into extractor with toluene as solvent boiling point, until toluene
Untill distillate is colourless；
S8：Remaining soot is taken out, is spontaneously dried；
S9：Soot after natural drying is put into autoclave with extract solution and HTHP extraction 4 under nitrogen protection
~5h；
S10：Extract solution is carried out into suction filtration, after vacuum drying, is obtained rich in metal fullerene powder.
Preferably, in the step S1, rare earth oxide is dehydrated 3.5~4.5h by 280~300 DEG C of high temperature dryings, mixes
Compound middle rare earth atom is 1 with the amount ratio of carbon atom material:50.
Preferably, in the step S3, in building-up process of discharging, the electric current that it is passed through is 140~180A, and voltage is 25
~35V.
Preferably, in the step S9, extract solution is trichlorine benzene solvent, and the high pressure under nitrogen protection is 2 × 106~4 ×
106Pa。
Preferably, in the step S10, during the suction filtration of extract solution, filter paper is trimmed to and is slightly less than Buchner funnel,
And distilled water is added dropwise makes filter paper be closely connected with funnel.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is further to the cigarette ash produced in discharge process
Extraction, cigarette ash can not only made full use of, and it is embedded fullerene that the content of fullerene high is dramatically increased in product
Further enrichment and separating-purifying open shortcut, are particularly well-suited to fairly large extraction.
Brief description of the drawings
Fig. 1 is workflow diagram of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment one
A kind of extracting method of embedded metal fullerene, the specific steps of the extracting method of the embedded metal fullerene are such as
Under：
S1：Spectroscopic graphite rod is got outDeep hole, filled in deep hole through pretreated various
The mixture of rare earth oxide and graphite powder, rare earth oxide is dehydrated 3.5h by 280 DEG C of high temperature dryings, and mixture middle rare earth is former
Son is 1 with the amount ratio of carbon atom material:50；
S2：The graphite rod that will have been filled 1700 DEG C of high-temperature roasting 3h under vacuum, make rare earth oxide be changed into rare earth
Carbide；
S3：1.1 × 104Electric discharge synthesis is carried out under the helium protection of Pa, and substantial amounts of soot is produced during discharging, together
When cathode end produce Carbon deposition rod, discharge building-up process in, the electric current that it is passed through be 140A, voltage is 25V；
S4：Electrode, and back discharge are exchanged, Carbon deposition rod is consumed into soot completely；
S5：The thick cigarette ash that graphite rod is produced is well mixed with ortho-xylene, injection extracts in the extractor equipped with filter paper bucket
Take 30h；
S6：Extract is vacuum dried through filtering, rotary evaporation removal solvent, extracts soot；
S7：Collect whole soots, and extract 20h under being put into extractor with toluene as solvent boiling point, until toluene is distillated
Untill liquid is colourless；
S8：Remaining soot is taken out, is spontaneously dried；
S9：Soot after natural drying is put into autoclave with extract solution and HTHP extraction under nitrogen protection
4h, extract solution is trichlorine benzene solvent, and the high pressure under nitrogen protection is 2 × 106Pa；
S10：Extract solution is carried out into suction filtration, after vacuum drying, is obtained rich in metal fullerene powder, in the suction filtration of extract solution
During, filter paper is trimmed to and is slightly less than Buchner funnel, and distilled water is added dropwise makes filter paper be closely connected with funnel.
Embodiment two
A kind of extracting method of embedded metal fullerene, the specific steps of the extracting method of the embedded metal fullerene are such as
Under：
S1：Spectroscopic graphite rod is got outDeep hole, filled in deep hole through pretreated various
The mixture of rare earth oxide and graphite powder, rare earth oxide is dehydrated 4.5h by 300 DEG C of high temperature dryings, and mixture middle rare earth is former
Son is 1 with the amount ratio of carbon atom material:50；
S2：The graphite rod that will have been filled 1900 DEG C of high-temperature roasting 4h under vacuum, make rare earth oxide be changed into rare earth
Carbide；
S3：1.3 × 104Electric discharge synthesis is carried out under the helium protection of Pa, and substantial amounts of soot is produced during discharging, together
When cathode end produce Carbon deposition rod, discharge building-up process in, the electric current that it is passed through be 180A, voltage is 35V；
S4：Electrode, and back discharge are exchanged, Carbon deposition rod is consumed into soot completely；
S5：The thick cigarette ash that graphite rod is produced is well mixed with ortho-xylene, injection extracts in the extractor equipped with filter paper bucket
Take 45h；
S6：Extract is vacuum dried through filtering, rotary evaporation removal solvent, extracts soot；
S7：Collect whole soots, and extract 25h under being put into extractor with toluene as solvent boiling point, until toluene is distillated
Untill liquid is colourless；
S8：Remaining soot is taken out, is spontaneously dried；
S9：Soot after natural drying is put into autoclave with extract solution and HTHP extraction under nitrogen protection
5h, extract solution is trichlorine benzene solvent, and the high pressure under nitrogen protection is 4 × 106Pa；
S10：Extract solution is carried out into suction filtration, after vacuum drying, is obtained rich in metal fullerene powder, in the suction filtration of extract solution
During, filter paper is trimmed to and is slightly less than Buchner funnel, and distilled water is added dropwise makes filter paper be closely connected with funnel.
Embodiment three
A kind of extracting method of embedded metal fullerene, the specific steps of the extracting method of the embedded metal fullerene are such as
Under：
S1：Spectroscopic graphite rod is got outDeep hole, filled in deep hole through pretreated various
The mixture of rare earth oxide and graphite powder, rare earth oxide is dehydrated 4h, mixture middle rare earth atom by 290 DEG C of high temperature dryings
It is 1 with the amount ratio of carbon atom material:50；
S2：The graphite rod that will have been filled 1800 DEG C of high-temperature roasting 3.5h under vacuum, make rare earth oxide be changed into dilute
Native carbide；
S3：1.2 × 104Electric discharge synthesis is carried out under the helium protection of Pa, and substantial amounts of soot is produced during discharging, together
When cathode end produce Carbon deposition rod, discharge building-up process in, the electric current that it is passed through be 160A, voltage is 30V；
S4：Electrode, and back discharge are exchanged, Carbon deposition rod is consumed into soot completely；
S5：The thick cigarette ash that graphite rod is produced is well mixed with ortho-xylene, injection extracts in the extractor equipped with filter paper bucket
Take 40h；
S6：Extract is vacuum dried through filtering, rotary evaporation removal solvent, extracts soot；
S7：Collect whole soots, and extract 23h under being put into extractor with toluene as solvent boiling point, until toluene is distillated
Untill liquid is colourless；
S8：Remaining soot is taken out, is spontaneously dried；
S9：Soot after natural drying is put into autoclave with extract solution and HTHP extraction under nitrogen protection
4.5h, extract solution is trichlorine benzene solvent, and the high pressure under nitrogen protection is 3 × 106Pa；
S10：Extract solution is carried out into suction filtration, after vacuum drying, is obtained rich in metal fullerene powder, in the suction filtration of extract solution
During, filter paper is trimmed to and is slightly less than Buchner funnel, and distilled water is added dropwise makes filter paper be closely connected with funnel.
In sum, highly preferred embodiment of the present invention is embodiment three.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (5)
1. a kind of extracting method of embedded metal fullerene, it is characterised in that：The extracting method of the embedded metal fullerene
Comprise the following steps that：
S1：Spectroscopic graphite rod is got outDeep hole, filled in deep hole through pretreated various rare earths
The mixture of oxide and graphite powder；
S2：The graphite rod that will have been filled 1700~1900 DEG C of 3~4h of high-temperature roasting under vacuum, are changed into rare earth oxide
Rare Earth Carbides；
S3：1.1 × 104~1.3 × 104Electric discharge synthesis is carried out under the helium protection of Pa, and substantial amounts of cigarette is produced during discharging
Soot, while producing Carbon deposition rod in cathode end；
S4：Electrode, and back discharge are exchanged, Carbon deposition rod is consumed into soot completely；
S5：The thick cigarette ash that graphite rod is produced is well mixed with ortho-xylene, injection extracts 30 in the extractor equipped with filter paper bucket
~45h；
S6：Extract is vacuum dried through filtering, rotary evaporation removal solvent, extracts soot；
S7：Collect whole soots, and 20~25h of extraction under being put into extractor with toluene as solvent boiling point, until toluene is distillated
Untill liquid is colourless；
S8：Remaining soot is taken out, is spontaneously dried；
S9：By the soot after natural drying be put into autoclave with extract solution and under nitrogen protection HTHP extract 4~5h；
S10：Extract solution is carried out into suction filtration, after vacuum drying, is obtained rich in metal fullerene powder.
2. the extracting method of a kind of embedded metal fullerene according to claim 1, it is characterised in that：The step S1
In, rare earth oxide is dehydrated 3.5~4.5h, mixture middle rare earth atom and carbon atom material by 280~300 DEG C of high temperature dryings
Amount ratio be 1:50.
3. the extracting method of a kind of embedded metal fullerene according to claim 1, it is characterised in that：The step S3
In, in building-up process of discharging, the electric current that it is passed through is 140~180A, and voltage is 25~35V.
4. the extracting method of a kind of embedded metal fullerene according to claim 1, it is characterised in that：The step S9
In, extract solution is trichlorine benzene solvent, and the high pressure under nitrogen protection is 2 × 106~4 × 106Pa。
5. the extracting method of a kind of embedded metal fullerene according to claim 1, it is characterised in that：The step S10
In, during the suction filtration of extract solution, filter paper is trimmed to and is slightly less than Buchner funnel, and distilled water is added dropwise makes filter paper tight with funnel
Close connection.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107492595A (en) * | 2017-08-23 | 2017-12-19 | 中国科学院化学研究所 | A kind of stable compound of embedded metal fullerene and ring penylene and preparation method thereof |
| CN109650378A (en) * | 2017-10-12 | 2019-04-19 | 北京福纳康生物技术有限公司 | A kind of separation metal fullerene M@C82And its method of isomers |
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| CN1671620A (en) * | 2002-07-22 | 2005-09-21 | 德累斯顿协会莱布尼茨固体材料研究所 | Method for the production of endohedral fullerenes |
| CN102115074A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院高能物理研究所 | Extraction method of internally-embedded metal fullerene |
| CN103754857A (en) * | 2013-12-31 | 2014-04-30 | 厦门福纳新材料科技有限公司 | Method for efficiently extracting monometallic endohedral fullerene M@C82 |
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2016
- 2016-12-06 CN CN201611108237.7A patent/CN106744814A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671620A (en) * | 2002-07-22 | 2005-09-21 | 德累斯顿协会莱布尼茨固体材料研究所 | Method for the production of endohedral fullerenes |
| CN102115074A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院高能物理研究所 | Extraction method of internally-embedded metal fullerene |
| CN103754857A (en) * | 2013-12-31 | 2014-04-30 | 厦门福纳新材料科技有限公司 | Method for efficiently extracting monometallic endohedral fullerene M@C82 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107492595A (en) * | 2017-08-23 | 2017-12-19 | 中国科学院化学研究所 | A kind of stable compound of embedded metal fullerene and ring penylene and preparation method thereof |
| CN107492595B (en) * | 2017-08-23 | 2019-10-25 | 中国科学院化学研究所 | A kind of stable compound and preparation method thereof of embedded metal fullerene and ring penylene |
| CN109650378A (en) * | 2017-10-12 | 2019-04-19 | 北京福纳康生物技术有限公司 | A kind of separation metal fullerene M@C82And its method of isomers |
| CN109650378B (en) * | 2017-10-12 | 2020-09-04 | 北京福纳康生物技术有限公司 | Separation metal fullerene M @ C82And isomers thereof |
| US11352257B2 (en) | 2017-10-12 | 2022-06-07 | Beijing Fullcan Biotechnology Co., Ltd. | Method for separating metallofullerene M@C82 and isomers thereof |
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Application publication date: 20170531 |