CN100351174C - Method for producing fullerene by temperature-controlling arc furnace - Google Patents
Method for producing fullerene by temperature-controlling arc furnace Download PDFInfo
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- CN100351174C CN100351174C CNB2005101245257A CN200510124525A CN100351174C CN 100351174 C CN100351174 C CN 100351174C CN B2005101245257 A CNB2005101245257 A CN B2005101245257A CN 200510124525 A CN200510124525 A CN 200510124525A CN 100351174 C CN100351174 C CN 100351174C
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- arc
- soccerballene
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Abstract
The present invention discloses a method for producing fullerene in a temperature control arc furnace. A temperature control arc generating furnace is used, and pure graphite rods are used as an anode and a cathode to carry out arc discharge in an atmosphere of helium gas. The temperature of an arc discharge chamber is from 100 to 350 DEG C through the adjustment of a temperature controller, and high purity fullerene is generated on the inner wall of the temperature control arc furnace. Since the present invention uses the temperature control arc furnace with a patent technique, the arc discharge can be carried out at higher environmental temperature to prepare the fullerene and the yield of the fullerene is increased. The method can be used for large scale industrial production.
Description
One, technical field
The invention belongs to the preparation field of soccerballene, particularly a kind of method of in temperature-controlling arc furnace, producing soccerballene.
Two, background technology
In time-of-flight mass spectrometer, detect C behind the human laser evaporation graphite such as kroto in 1985 and Smalley
60, C
70And other soccerballenes.At present, the preparation soccerballene mainly contains three kinds of methods: benzene combustion method, laser evaporation graphite method, arc discharge method.Nineteen ninety Kratschmer at first adopts arc discharge method to prepare the C of maroscopic quantity
60, this method proves effective means, though C in the carbon ash that Kratschmer obtains
60Content only is 1%, but its foot makes the countless researchist in the whole world enter this research field.Employing resistive heating graphite such as Tayloy obtain 8% productive rate, and people such as Ajie adopts the resistive heating graphite rod equally subsequently, and the soccerballene productive rate reaches 14% in the carbon ash that obtains.
Haufler etc. obtain 12% productive rate with arc discharge method, Hare etc. find that the type of graphite rod is bigger to the productive rate influence, dissimilar graphite rods, productive rate changes .Saito etc. and has studied the influence of helium pressure to the soccerballene productive rate between 5～10%, under 2.6KPa helium pressure and 220～250A direct current arc discharging condition, they have obtained 13% productive rate.Simultaneously, discovery soccerballene productive rates such as Huczko are subjected to the influence of discharging current and two interelectrode distances, have obtained 20% productive rate under 13.3Kpa helium and 65A current condition.Mieno manages to increase carbon ash output to improve productive rate when discharge.Srivastava etc. have studied the influence of different designs parameter to productive rate, find that the different resulting productive rates of vacuum reaction chamber size changes between 4～20%.
People such as Sugai prepare soccerballene with pulse arc discharge evaporation graphite in a heated silica tube, the soccerballene productive rate prolongs with the pulse duration and increases.Dubrovsky and Beznelnitsyn feed the mobile helium increasing the speed of cooling of carbon vapor to positive and negative interpolar arc region, and when the helium that feeds is 3 liters/timesharing, the soccerballene productive rate reaches 17.3%.Recently
In 5 liters of stainless-steel vacuum chambers, insert the carbon tube of a long 200mm diameter 20mm and feed the mobile helium Deng the people and carry out arc-over, obtain the soccerballene productive rate up to 32%.
At present, the productive rate that the arc discharge method of bibliographical information prepares soccerballene is 5～20%, and the soccerballene productive rate only is about 5% in the industrial production.Therefore, each method of system of invention high yield soccerballene is significant with application to the research of soccerballene.
Three, summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of method of using temperature-controlling arc furnace to produce soccerballene is provided, can improve the productive rate of soccerballene.
To achieve these goals, the technical solution used in the present invention is: a kind of method of producing soccerballene in temperature-controlling arc furnace, use temperature-controlling arc furnace, this temperature-controlling arc furnace comprises arc discharge chamber 5, disposes anode 1 and negative electrode 2 in the arc discharge chamber 5, and is arranged at the temperature control unit 3 on the temperature-controlling arc furnace inwall 4, it is characterized in that, as anode 1 and negative electrode 2, the spacing between negative electrode 1 and the anode 2 is 1～4mm with pure graphite rod, makes the vacuum tightness of arc discharge chamber 5 reach 10
-3Pa charges into helium to predetermined pressure 3～13Kpa, regulates the interior temperature range of stove at 100～350 ℃ with temperature control unit 3, discharging current is between 30～200A, voltage 5～30 minutes discharge times, promptly generates the carbon ash that contains soccerballene on temperature-controlling arc furnace inwall 4 between 20～100V.
The conventional arc electric discharge prepares the temperature that soccerballene can not be controlled arc discharge chamber, and temperature is the important factor that influences soccerballene preparation, so that the conventional arc electric discharge prepares the productive rate of soccerballene is very low.The present invention adopts temperature control type electric arc furnace, carries out arc-over under the temperature and prepare soccerballene in higher stove, and the soccerballene productive rate can reach this method of 20～30%. usefulness can carry out large-scale industrial production.
The equipment that the present invention adopts can be utility model patent CNT (carbon nano-tube) electric arc producer (ZL01240373.3 contriver: Liu Yongning, Song Xiaolong).The characteristics of this equipment are that the temperature that a heating unit is controlled the stainless steel reaction internal tank is installed on carbon nanotube reaction vessel inwall, and reaction vessel interior has anode rotating disk and the negative electrode that 1～6 consumable anode rod can be installed simultaneously.
Four, description of drawings
Accompanying drawing is a temperature-controlling arc furnace device synoptic diagram used in the present invention.
Five, specific embodiment
Referring to accompanying drawing, the temperature-controlling arc furnace that the present invention uses comprises an arc discharge chamber 5, dispose graphite anode rod 1 in the arc discharge chamber 5, negative electrode graphite rod 2, and the temperature control unit 3 that is arranged at temperature-controlling arc furnace inwall 4, distance is 1～4mm between graphite anode rod 1 and the negative electrode graphite rod 2, and temperature control unit 3 can be controlled the interior temperature of stove at 100～350 ℃, can generate the carbon ash that contains soccerballene on temperature-controlling arc furnace inwall 4.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
Referring to accompanying drawing, graphite anode rod 1 diameter 6mm, negative electrode graphite rod 2 diameter 15mm charge into the 10KPa helium in the electric arc furnace, and temperature regulating device is controlled to be 300 ℃ with temperature in the stove, and concrete steps are as follows:
(1) installs negative electrode and anode, close the arc discharge chamber door, vacuumize, make the vacuum tightness of arc discharge chamber reach 10
-3Pa;
(2) charge into helium to predetermined pressure 10KPa;
(3) open temperature regulating device 3, furnace temperature is raised to 300 ℃ of predetermined temperature;
(4) carry out arc-over, electric current I=90A, voltage V=25V, the spacing between graphite anode rod 1 and the negative electrode graphite rod 2 is 2mm, 10 minutes discharge times, on temperature-controlling arc furnace inwall 4, can obtain to contain about 5 grams of carbon ash of 20～30% (mass percent) soccerballene.
Referring to accompanying drawing, graphite anode rod 1 diameter 6mm, negative electrode graphite rod 2 diameter 15mm pour the 10KPa helium in the electric arc furnace, and temperature regulating device is controlled to be 200 ℃ with temperature in the stove, and concrete steps are as follows:
(1) installs negative electrode and anode, close the arc discharge chamber door, vacuumize, make the vacuum tightness of arc discharge chamber reach 10
-3Pa;
(2) charge into helium to predetermined pressure 10KPa;
(3) open temperature regulating device 3, furnace temperature is raised to 200 ℃ of predetermined temperature;
(4) carry out arc-over, electric current I=90A, voltage V=25V, the spacing between anode 1 and the negative electrode 2 is 2mm, 10 minutes discharge times, can obtain to contain about 5 grams of carbon ash of 20～30% (mass percent) soccerballene on temperature-controlling arc furnace inwall 4.
Embodiment 3
Referring to accompanying drawing, graphite anode rod 1 diameter 10mm, negative electrode graphite rod 2 diameter 18mm pour the 8KPa helium in the electric arc furnace, and temperature is 250 ℃ in the control process furnace, and concrete steps are as follows:
(1) installs negative electrode and anode, close the arc discharge chamber door, vacuumize, make the vacuum tightness of arc discharge chamber reach 10
-3Pa;
(2) charge into helium to predetermined pressure 8KPa;
(3) open temperature regulating device 3, furnace temperature is raised to 250 ℃ of predetermined temperature;
(4) carry out arc-over, electric current I=150A, voltage V=25V, the spacing between anode 1 and the negative electrode 2 is 2mm, 10 minutes discharge times, can obtain to contain about 10 grams of carbon ash of 20～30% (mass percent) soccerballene on temperature-controlling arc furnace inwall 4.
Claims (1)
1. method that adopts temperature-controlling arc furnace to produce soccerballene, use temperature-controlling arc furnace, this temperature-controlling arc furnace comprises arc discharge chamber (5), arc discharge chamber disposes anode and negative electrode in (5), and be arranged at temperature control unit (3) on the temperature-controlling arc furnace inwall (4), it is characterized in that, with pure graphite rod as anode (1) and negative electrode (2), spacing between anode (1) and the negative electrode (2) is 1～4mm, makes the vacuum tightness of arc discharge chamber (5) reach 10
-3Pa, charge into helium to predetermined pressure 3～13Kpa, regulate the interior temperature range of stove at 100～350 ℃ with temperature control unit (3), carry out arc-over, 5～30 minutes discharge times, discharging current is 30～200A, and voltage is 20～100V, promptly generates at temperature-controlling arc furnace inwall (4) and contains soccerballene carbon ash.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101245257A CN100351174C (en) | 2005-12-12 | 2005-12-12 | Method for producing fullerene by temperature-controlling arc furnace |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101245257A CN100351174C (en) | 2005-12-12 | 2005-12-12 | Method for producing fullerene by temperature-controlling arc furnace |
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| CN1800008A CN1800008A (en) | 2006-07-12 |
| CN100351174C true CN100351174C (en) | 2007-11-28 |
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| CNB2005101245257A Expired - Fee Related CN100351174C (en) | 2005-12-12 | 2005-12-12 | Method for producing fullerene by temperature-controlling arc furnace |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9452410B2 (en) | 2013-11-12 | 2016-09-27 | Xiamen Funano New Material Technology Company. Ltd | Fullerene arc source and fullerene production apparatus comprising the same |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453457C (en) * | 2007-02-08 | 2009-01-21 | 厦门大学 | Production of doped aggregate cluster |
| CN102098821B (en) * | 2010-12-16 | 2013-02-13 | 中国科学院高能物理研究所 | Electrode device and reaction atmosphere control system and method using electrode device |
| CN102231925B (en) * | 2011-05-20 | 2013-05-01 | 中国科学院化学研究所 | Method for improving yield of C60/C70 fullerene prepared by arc discharge method |
| CN107226465A (en) * | 2017-07-25 | 2017-10-03 | 无锡远稳烯科技有限公司 | A kind of graphene production equipment |
Citations (6)
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|---|---|---|---|---|
| JPH07223807A (en) * | 1994-02-08 | 1995-08-22 | Tokai Carbon Co Ltd | Method and device for continuously producing fullerene |
| JPH07257916A (en) * | 1994-03-22 | 1995-10-09 | Tokai Carbon Co Ltd | Production of fullerenes and device therefor |
| CN1045199C (en) * | 1993-04-23 | 1999-09-22 | 武汉大学 | Method for preparing fuller's olefine C60-C70 by mass production |
| CN2475983Y (en) * | 2001-04-30 | 2002-02-06 | 西安交通大学 | Electric arc producer furnace with nanometre carbon tube |
| CN1579931A (en) * | 2004-05-17 | 2005-02-16 | 西安交通大学 | Method for batch type production of single-wall nano carbon tube suing temperature-controlled electric arc furnace |
| CN1583554A (en) * | 2004-05-27 | 2005-02-23 | 西安交通大学 | Temperature controlled arc method for mass preparing amorphous carbon nanometer tubes |
-
2005
- 2005-12-12 CN CNB2005101245257A patent/CN100351174C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045199C (en) * | 1993-04-23 | 1999-09-22 | 武汉大学 | Method for preparing fuller's olefine C60-C70 by mass production |
| JPH07223807A (en) * | 1994-02-08 | 1995-08-22 | Tokai Carbon Co Ltd | Method and device for continuously producing fullerene |
| JPH07257916A (en) * | 1994-03-22 | 1995-10-09 | Tokai Carbon Co Ltd | Production of fullerenes and device therefor |
| CN2475983Y (en) * | 2001-04-30 | 2002-02-06 | 西安交通大学 | Electric arc producer furnace with nanometre carbon tube |
| CN1579931A (en) * | 2004-05-17 | 2005-02-16 | 西安交通大学 | Method for batch type production of single-wall nano carbon tube suing temperature-controlled electric arc furnace |
| CN1583554A (en) * | 2004-05-27 | 2005-02-23 | 西安交通大学 | Temperature controlled arc method for mass preparing amorphous carbon nanometer tubes |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9452410B2 (en) | 2013-11-12 | 2016-09-27 | Xiamen Funano New Material Technology Company. Ltd | Fullerene arc source and fullerene production apparatus comprising the same |
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| CN1800008A (en) | 2006-07-12 |
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