CN1045199C - Method for preparing fuller's olefine C60-C70 by mass production - Google Patents
Method for preparing fuller's olefine C60-C70 by mass production Download PDFInfo
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- CN1045199C CN1045199C CN93104758A CN93104758A CN1045199C CN 1045199 C CN1045199 C CN 1045199C CN 93104758 A CN93104758 A CN 93104758A CN 93104758 A CN93104758 A CN 93104758A CN 1045199 C CN1045199 C CN 1045199C
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- electrode
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- graphite
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Abstract
The present invention relates to a method for preparing Fuller olefin C60/C70 by mass production. The present invention adopts a vacuum consumable-electrode electric-arc furnace to prepare soot (kilogram by weight) containing Fuller olefin C60 /C70. In the production, high-purity graphite bars are arranged in the electric furnace to be used as consumable electrodes, an arc is started in high-pure helium atmosphere, certain voltage and certain current are controlled so that the electric arc between the graphite electrode bars is controlled, and the graphite electrode bars are evaporated to form the fullerene soot. The present invention enhances the preparation scale of the Fuller olefin C60 /C70 to the gram weight from the kilogram weight and utilizes the present industrial equipment so as to have less required investment and make the preparation of the Fuller olefin C60 /C70 enter the industrial production scale, and therefore, a fullerene product with expensive selling price on market has the advantages of cost reduction and rapid output increase so that the present invention has obvious economic benefit; meanwhile, the present invention lay the foundation for impelling the research of the fullerene product and achieving practical application.
Description
The present invention relates to technical scale and prepare soccerballene C
60/ C
70Method.Belong to organic novel material synthesis technical field.
Since nineteen ninety W.Kratschmer etc. and (W.Kratschmer et al., Nature, 34,354,1990 such as R.E.Haufler; Phys, Lett.170,167,1990; R.E.Haufler et al., J.Phys, Chem., 94,8634,1990) successfully synthesized for soccerballene (Fullerene) carbon 60 of research usefulness and the mixture of carbon 70 and (followingly write C respectively by international representation
60, C
70) after, be fullerene synthesis C
60/ C
70Lay a good foundation.The various countries scientist is competitively seeking more effective preparation method always later on, so that obtain a large amount of soccerballene C
60And C
70
Existing preparation method has arc vaporization graphite method, benzene-oxygen-argon mixture gas combustion method (J.B.Howard et al., Nature, 352,139,1991) etc.The mixed gas combustion method is because the concentration of the ratio of pressure, carbon and the oxygen of combustion chamber, argon gas, gas velocity, retention time etc. are difficult to control to an optimum value, and therefore the people of employing is fewer.Using maximum is the arc vaporization graphite method that Kratschmer proposes, and has worldwide set up the different arc vaporization graphite furnace of form since nineteen ninety, and acquisition gram magnitude soccerballene C that can be in various degree
60/ C
70, still, all still being in laboratory scale, the cost height yields poorly, thereby causes soccerballene C
60, C
70Cost an arm and a leg, and high, for further investigation with use this compounds and bring difficulty.For this reason, be necessary to seek a kind of with low cost, mass preparation soccerballene C
60/ C
70Method.
The objective of the invention is: provide a kind of with low cost, be suitable for plant-scale preparation soccerballene C
60/ C
70Method.
Realize that the technical measures that purpose of the present invention is taked are: adopt metallurgical vaccum consumable electrode electric arc furnace (seeing accompanying drawing) preparation to contain C
60/ C
70Soot:
Carbon content is become upper and lower electrode greater than 99.99% machining graphite.With fastening chuck (4) top electrode (7) is linked to each other with the vaccum consumable electrode electric arc furnace negative potential, lower electrode (8) is placed crystallizer (9), be connected with the electric furnace positive electrode with the free way of contact.Closed electric arc furnace vacuumizes, make that vacuum tightness reaches in the stove≤and 10
-3To 10
-6Pa opens and fills the helium valve, charges into helium in stove, make helium pressure reach 〉=10
3To 10
6Pa reduces the graphite top electrode, and it is contacted with the graphite lower electrode, pass to the electric current about 800A, and promote top electrode rapidly, the starting the arc, after the starting the arc with current control about 6000A, voltage control is 〉=30 to 70V, constantly adjust power-on and power-off interpolar distance, make electric arc keep stable, this moment, graphite constantly evaporated, form soot, on the water mold inwall, deposit.After the electrode efficient part evaporated, soot was taken out in blowing out, separates in order to extracting.
This method is used existing metallurgical vaccum consumable electrode electric arc furnace, only does a small amount of technology repacking, and facility investment is few.The stone black electrode of preparation fullerene soot can according to Capacity design electrode diameter 〉=1/10 of electric furnace to the internal diameter of 1/4 consumable electrode arc furnace crystallizer can reach 〉=30 to 80mm; Electrode length determined by the top electrode mobile range of consumable electroarc furnace, can reach 〉=300 to 800mm, and (10-30 minute) can evaporate in the short period of time, and what once can prepare feather weight contains soccerballene C
60/ C
70The soot of product, as seen this method cost is inefficient high, is soccerballene C
60/ C
70Product moves towards practical application and lays a good foundation.
Description of drawings:
Fig. 1 is for smelting the vaccum consumable electrode electric arc furnace synoptic diagram
Among the figure: 1. current lead; 2. water cooled electrode bar;
3. vacuum chamber; 4. fastening chuck;
5. transition electrode; 6. vacuum system interface;
7. graphite top electrode; 8. graphite lower electrode;
9. crystallizer; 10. crystallizer water-cooled overcoat;
11. cooling water intakeoutfall.
Embodiment:
With the black top electrode that is processed into Φ 40mm * 600mm of the stone of homemade carbon containing more than 99.99%, the lower electrode of d80mm * 300mm places in the 500kg vaccum consumable electrode electric arc furnace, vacuum is evacuated to≤1.33 * 10
-5Pa charges into the homemade helium of helium more than 99.99% that contain then, and air pressure is 〉=1 * 10
4To 5 * 10
5Pa.The post-arc current of having switched on is controlled to about 6000A, the about 40V of voltage, and electrode evaporated blowing out in about 10 minutes.Soot deposit is at the water mold inwall.Soot is taken out through extracting, oven dry, C in the cooling back
60/ C
70Yield be 4-5%.Measure with large-scale mass spectrum (VC ZAB-3F type).C
60With C
70Ratio be about 8: 1.
Claims (3)
1. one kind is adopted vaccum consumable electrode electric arc furnace to produce soccerballene C
60/ C
70Method, it is characterized in that:
With carbon containing be＞99.99% graphite rod as consumable electrode, be divided into upper and lower two electrodes; During preparation, need to vacuumize in the stove with vaccum consumable electrode electric arc furnace, fill helium then; Before the energising, reduce top electrode, it is contacted with lower electrode, during energising, promote top electrode, the starting the arc, sparking voltage is controlled in the 30-70 volt, and electric current is controlled in the 800-6000 peace, produces stable arc, and Graphite Electrodes constantly evaporates, and generates soccerballene C
60/ C
70Soot.
2. by the described method of claim 1, it is characterized in that: upper and lower two graphite rod consumable electrodes, electrode diameter is 30-80mm, electrode length is 300-800mm, and top electrode is connected with the electric arc furnace negative pole with fastening chuck, and lower electrode is connected with the anodal contact of electric arc furnace.
3. it is characterized in that by the described method of claim 1: during preparation, will be evacuated to 10 in the stove
-3-10
-6Pa fills helium then, and making furnace pressure is 10
3-10
6Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93104758A CN1045199C (en) | 1993-04-23 | 1993-04-23 | Method for preparing fuller's olefine C60-C70 by mass production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93104758A CN1045199C (en) | 1993-04-23 | 1993-04-23 | Method for preparing fuller's olefine C60-C70 by mass production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1094389A CN1094389A (en) | 1994-11-02 |
| CN1045199C true CN1045199C (en) | 1999-09-22 |
Family
ID=4985349
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93104758A Expired - Fee Related CN1045199C (en) | 1993-04-23 | 1993-04-23 | Method for preparing fuller's olefine C60-C70 by mass production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045199C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351174C (en) * | 2005-12-12 | 2007-11-28 | 西安交通大学 | Method for producing fullerene by temperature-controlling arc furnace |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114982776A (en) * | 2022-05-17 | 2022-09-02 | 中研瑞科科技(北京)有限公司 | Fullerene functional liquid for preventing and treating root knot nematode disease of crops and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0302771A1 (en) * | 1987-08-07 | 1989-02-08 | Institut Français du Pétrole | Process for the simultaneous removal of arsenic and carbon oxysulfide from a cut of unsaturated hydrocarbons in the liquid phase |
-
1993
- 1993-04-23 CN CN93104758A patent/CN1045199C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0302771A1 (en) * | 1987-08-07 | 1989-02-08 | Institut Français du Pétrole | Process for the simultaneous removal of arsenic and carbon oxysulfide from a cut of unsaturated hydrocarbons in the liquid phase |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351174C (en) * | 2005-12-12 | 2007-11-28 | 西安交通大学 | Method for producing fullerene by temperature-controlling arc furnace |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1094389A (en) | 1994-11-02 |
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