CN101597054A - The synthetic method of soccerballene - Google Patents
The synthetic method of soccerballene Download PDFInfo
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- CN101597054A CN101597054A CNA200910112096XA CN200910112096A CN101597054A CN 101597054 A CN101597054 A CN 101597054A CN A200910112096X A CNA200910112096X A CN A200910112096XA CN 200910112096 A CN200910112096 A CN 200910112096A CN 101597054 A CN101597054 A CN 101597054A
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Abstract
The synthetic method of soccerballene relates to the third allotropic substance soccerballene of a kind of carbon.A kind of synthetic method that can improve the soccerballene productive rate is provided.In proportion metal is filled into graphite rod; The graphite rod of filler metal is fixed on the arc discharge device positive terminal, the capping cavity; Open mechanical pump, reaction unit is found time; Charge into He gas in the reaction cavity of having found time, find time, with He gas the entrap bubble of trace in the cavity is replaced, the vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump; In the arc discharge device cavity, charge into He gas; Open water coolant; Open welder power; The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode; After treating that graphite anode has reacted, be cooled to room temperature, close water coolant; In reaction cavity, introduce gas to normal pressure; Collection carbon ash promptly gets target product.
Description
Technical field
The present invention relates to the third allotropic substance soccerballene of a kind of carbon, especially relate to the synthetic C of a kind of high yield
60, C
70Method Deng fullerene-based material.
Background technology
Soccerballene in 20th century the mid-80 by Smally, the Curl of the U.S. and (H.W.Kroto, J.R.Health, S.C.O ' Brien, R.F.Curl, R.E.Smally, the C such as Kroto of Britain
60: Buck minster fullerence.[J], Nature, 1985,318,162-163) form in order to study interplaner space long-chain carbon molecule that mechanism finds in the experimentation of laser pulse evaporation graphite, be the third allotropic substance of carbon except that diamond, graphite, drawn back the prelude of soccerballene chemical research, therefore 3 scientists have also shared Nobel chemistry Prize in 1996.
Soccerballene has attracted each subject scientist extensive interest with its particular structure and electronic property, has formed a brand-new research field based on cross discipline.Based on the particular geometries of soccerballene, the soccerballene lubricating oil additive can prolong lubricant life up to 30%; The compound system that soccerballene and basic metal form is the excellent high-temperature superconducting material, and its superconduction critical temperature is up to 46K.The three-dimensional height nonlocalized electron conjugated structure that exists in the fullerene molecule makes it have good optical and non-linear optical property, uses to some extent at aspects such as photometry calculation, light memory, optical signal processing and controls, at present based on C
60The optoelectronic switch and the opticglass of photoconductive property are succeeded in developing, are that the organic solar batteries photoelectric transformation efficiency of critical material reaches 6.5% with the soccerballene, have broken through to use and have gone up 5% threshold that requires; Aspect life science, because fullerene derivate has the active effect of the HIVP of inhibition, related drugs is near clinical use; Based on the magnetic resonance contrast agent of soccerballene, treatment cancer pharmaceutical preparations is also among the fast development.
Carry out soccerballene research, at first must start the raw material production problem of soccerballene.At present, though soccerballene can be synthetic with several different methods, as classical synthetic method---arc process (
) (
W., LambL.D., Fostiropoulos K.﹠amp; Huffman D.R..Solid C
60: A new form of carbon[J], Nature, 1985,347,354-358), be the main synthetic method of soccerballene always.Regrettably the productive rate of its soccerballene is about 2% only, affects the further investigation of soccerballene and association area thereof.
Therefore, improving the synthetic yield of soccerballene, reduce the preparation cost of soccerballene, is the key link that realizes the fullerene-based material widespread use.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method that can improve the soccerballene productive rate.
Technical scheme of the present invention is to prepare in the process of soccerballene in arc process, mixes a certain amount of metal in graphite rod, and said metal is common wire or its powder such as silver, nickel.Needn't change soccerballene synthetic reaction unit and reaction conditions in the implementation process of the present invention, only need simply metal to be added in the graphite rod,, promote the formation of soccerballene, improve the synthetic yield of soccerballene to improve the process of growth of soccerballene.
The present invention includes following steps:
1) in proportion metal is filled into graphite rod, stand-by, press atom number ratio, metal: C=1: (10～450);
2) graphite rod with filler metal is fixed on the arc discharge device positive terminal, the capping cavity;
3) open mechanical pump, reaction unit is found time;
4) charge into He gas in the reaction cavity of having found time, find time, with He gas the entrap bubble of trace in the cavity is replaced, the vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump;
5) in the arc discharge device cavity, charge into He gas;
6) open water coolant;
7) open welder power;
8) the precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode;
9) treat that graphite anode has reacted after, be cooled to room temperature, close water coolant;
10) in reaction cavity, introduce gas to normal pressure;
11) collect the carbon ash, promptly get target product.
In step 1), described metal is preferably silver, nickel etc., metallic state is preferably wire or metal-powder, and filling mode wiry is for putting wire into back filled stone ink powder in the carbon-point, and the filling mode of metal-powder is for to be filled in mixed uniformly Graphite Powder 99 and metal mixture in the carbon-point.
In step 3), described find time preferably is evacuated to 10 with the pressure of the reaction cavity of reaction unit
-2MmHg.
In step 4), the described best 0.013～0.053MPa (100～400Torr) of pressure that charges into He gas; Described displacement is preferably replaced 3～5 times, and each displacement preferably charges into the He gas of 50～80Torr.
In step 7), preferably regulate striking electric current to 10～40A after opening welder power.
In step 8), describedly can regulate galvanic current greater than 40A when drawing back graphite anode or graphite cathode, regulate galvanic current and be preferably 60～100A.
The present invention can utilize existing soccerballene synthetic reaction unit by metal is filled into graphite rod, needn't change soccerballene synthetic reaction unit and reaction conditions, improves the productive rate of soccerballene significantly.Through optimizing C
60The productive rate that accounts for original cigarette ash reaches 5.44%, C
70The productive rate that accounts for original cigarette ash reaches 2.73%, than same apparatus, same reaction conditions, does not add the preceding C of metal
60, C
70The productive rate that accounts for original cigarette ash is respectively 1.65%, 0.71%, and its productive rate has improved 2.3 times, 2.8 times respectively.And behind the adding metal, C
60, C
70Account for the proportion that can extract part and reach 45.7%, 20.8% respectively, also have tangible C in addition
76, C
78, C
82, C
84Contour soccerballene can extract weight partly greater than 66.5% so the weight of soccerballene accounts for.
Description of drawings
The total ion current figure that Fig. 1 analyzes for chromatography-mass spectroscopy.In Fig. 1, X-coordinate is time T ime (min), and ordinate zou is intensity I ntens (* 10
7); It is add metal reaction in graphite rod after, to take by weighing a certain amount of cigarette ash that LC-MS analyzes, and after the toluene supersound extraction, carries out the total ion current figure that LC-MS analyzes; 77.8～82.8min is C
60, 98.0～102.7min is C
70It is add metal reaction in graphite rod after, to take by weighing a certain amount of cigarette ash that LC-MS analyzes, and the LC-MS that is carried out after the toluene supersound extraction analyzes.
The 330nm color atlas that Fig. 2 analyzes for chromatography-mass spectroscopy.In Fig. 2, X-coordinate is time T ime (min), and ordinate zou is intensity I ntens (mAU); 77.8～82.8min is C
60, 98.0～102.7min is C
70It is add metal reaction in graphite rod after, to take by weighing a certain amount of cigarette ash that LC-MS analyzes, and the LC-MS that is carried out after the toluene supersound extraction analyzes.
The C that Fig. 3 analyzes for chromatography-mass spectroscopy
76, C
78, C
80, C
82, C
84, C
86Selectivity ion flow graph.In Fig. 3, X-coordinate is time T ime (min), and ordinate zou is that (x 10 for intensity I ntens
5); 118.1～122.4min is C
76, 122.8～129.8min is C
78, 134.8～138.2min is C
80, 139.1～144.7min is C
82, 143.6～152.4min is C
84, 128.0～163.5min is C
86It is add metal reaction in graphite rod after, to take by weighing a certain amount of cigarette ash that LC-MS analyzes, and the LC-MS that is carried out after the toluene supersound extraction analyzes.
Fig. 4 is C for the chromatogram enlarged view of chromatography-mass spectroscopy analysis
76, C
78, C
82, C
84Tangible absorption peak figure on the 330nm UV spectrum.In Fig. 4,118.1～122.4min is C
76, 122.8～129.8min is C
78, 139.1～144.7min is C
82, 143.6～152.4min is C
84It is add metal reaction in graphite rod after, to take by weighing a certain amount of cigarette ash that LC-MS analyzes, and the LC-MS that is carried out after the toluene supersound extraction analyzes.
Embodiment
The invention will be further described by embodiment below.
The nickel wire diameter is 1mm, and purity is 99.9%.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ni: C=1: 10, nickel wire is mixed rod, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling nickel wire, the capping cavity.Open mechanical pump, reaction unit is found time, the pressure of reaction cavity is evacuated to 10
-2MmHg.In the reaction cavity of having found time, charge into 50Torr He gas, find time again.With He gas the entrap bubble of trace in the reaction cavity is replaced, replace 5 times.The metathetical principle is on a small quantity repeatedly.Vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump.In the arc discharge device cavity, charge into 280Torr He gas.Open water coolant.Open welder power, regulate the striking electric current to 10A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
With product behind methylbenzene extraction, carry out chromatography-mass spectroscopy (LC-MS) coupling analysis, can get total ion current figure that chromatography-mass spectroscopy (LC-MS) coupling analyzes as shown in Figure 1, the color atlas that chromatography-mass spectroscopy (LC-MS) coupling is analyzed as shown in Figure 2, the C that chromatography-mass spectroscopy (LC-MS) coupling is analyzed
76, C
78, C
80, C
82, C
84, C
86Selectivity ion flow graph as shown in Figure 3, the color atlas enlarged view that chromatography-mass spectroscopy (LC-MS) coupling is analyzed is C
76, C
78, C
82, C
84Tangible absorption peak figure on the 330nm UV spectrum.
Nickel powder is that purity is 99.9%.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ni: C=1: 20, insert in the graphite rod after nickel powder and Graphite Powder 99 mixed, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling nickel powder, the capping cavity.Open mechanical pump, reaction unit is found time, the pressure of reaction cavity is evacuated to 10
-2MmHg.In the reaction cavity of having found time, charge into 60Torr He gas, find time again.With He gas the entrap bubble of trace in the reaction cavity is replaced, replace 4 times.Vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump.In the arc discharge device cavity, charge into 280Torr He gas.Open water coolant.Open welder power, regulate the striking electric current to 15A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
The filamentary silver diameter is 0.2mm, and purity is 99.9%.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ag: C=1: 80, filamentary silver is mixed rod, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling filamentary silver, the capping cavity.Open mechanical pump, reaction unit is found time, the pressure of reaction chamber is evacuated to 10
-2MmHg.In the reaction cavity of having found time, charge into 70Torr He gas, find time again.With He gas the entrap bubble of trace in the cavity is replaced, replace 3 times.The metathetical principle is on a small quantity repeatedly.Close the vacuum valve between cavity and the mechanical pump after displacement finishes, close vacuum pump.In the arc discharge device cavity, charge into 280Torr He gas.Open water coolant.Open welder power, regulate the striking electric current to 20A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
The filamentary silver diameter is 0.2mm, and purity is 99.9%.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ag: C=1: 140, filamentary silver is mixed rod, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling filamentary silver, the capping cavity.Open mechanical pump,, the pressure of reaction cavity is evacuated to 10 system pump down
-2MmHg.In the reaction cavity of having found time, charge into 80TorrHe gas, find time again.With He gas the entrap bubble of trace in the reaction cavity is replaced, replace 5 times.Vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump.In the arc discharge device cavity, charge into 280Torr He gas.Open water coolant.Open welder power, regulate the striking electric current to 25A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
Embodiment 5
The filamentary silver diameter is 0.2mm, and purity is 99.9%.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ag: C=1: 220, filamentary silver is mixed rod, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling filamentary silver, the capping cavity.Open mechanical pump, reaction unit is found time, the pressure of reaction cavity is evacuated to 10
-2MmHg.In the reaction cavity of having found time, charge into 50Torr He gas, find time again.With He gas the entrap bubble of trace in the cavity is replaced, replace 5 times.Vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump.In the arc discharge device reaction cavity, charge into 280TorrHe gas.Open water coolant.Open welder power, regulate the striking electric current to 10A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
The filamentary silver diameter is 0.2mm, and purity is 99.9%.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ag: C=1: 450, filamentary silver is mixed rod, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling filamentary silver, the capping cavity.Open mechanical pump, reaction unit is found time, the pressure of reaction cavity is evacuated to 10
-2MmHg.In the reaction cavity of having found time, charge into 60Torr He gas, find time again.With He gas the entrap bubble of trace in the reaction cavity is replaced, replace 4 times.Vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump.In the arc discharge device reaction cavity, charge into 280Torr He gas.Open water coolant.Open welder power, regulate the striking electric current to 10A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
Embodiment 7
Silver powder purity is 99.9%, 200 order.Graphite Powder 99 purity is 99.9%, 250 order.
During fullerene synthesis, press the atom number than Ag: C=1: 80, silver powder is mixed rod, stand-by.Install device, the resistance to air loss of check reaction unit is fixed on the arc discharge device positive terminal to the carbon-point of filling silver powder, the capping cavity.Open mechanical pump, reaction unit is found time, the pressure of reaction cavity is evacuated to 10
-2MmHg.In the reaction cavity of having found time, charge into 70Torr He gas, find time again.With He gas the entrap bubble of trace in the reaction cavity is replaced, replace 5 times.Vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump.In the arc discharge device reaction cavity, charge into 280Torr He gas.Open water coolant.Open welder power, regulate the striking electric current to 20A.The precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode, regulates electric current to 80A.After treating that graphite anode has reacted, be cooled to room temperature, close water coolant.In reaction cavity, introduce gas to normal pressure.Collection carbon ash promptly gets target product.
Claims (10)
1. the synthetic method of soccerballene is characterized in that may further comprise the steps:
1) in proportion metal is filled into graphite rod, stand-by, press atom number ratio, metal: C=1: (10～450);
2) graphite rod with filler metal is fixed on the arc discharge device positive terminal, the capping cavity;
3) open mechanical pump, reaction unit is found time;
4) charge into He gas in the reaction cavity of having found time, find time, with He gas the entrap bubble of trace in the cavity is replaced, the vacuum valve after displacement finishes between off-response cavity and the mechanical pump cuts out vacuum pump;
5) in the arc discharge device cavity, charge into He gas;
6) open water coolant;
7) open welder power;
8) the precession graphite anode when observing dazzling arc light, draws back graphite anode or graphite cathode near graphite cathode;
9) treat that graphite anode has reacted after, be cooled to room temperature, close water coolant;
10) in reaction cavity, introduce gas to normal pressure;
11) collect the carbon ash, promptly get target product.
2. the synthetic method of soccerballene as claimed in claim 1 is characterized in that in step 1), and described metal is silver or nickel.
3. the synthetic method of soccerballene as claimed in claim 1 or 2, it is characterized in that in step 1), the state of described metal is wire or metal-powder, filling mode wiry is for putting wire into back filled stone ink powder in the carbon-point, and the filling mode of metal-powder is for to be filled in mixed uniformly Graphite Powder 99 and metal mixture in the carbon-point.
4. the synthetic method of soccerballene as claimed in claim 1 is characterized in that in step 3), and described finding time is that pressure with the reaction cavity of reaction unit is evacuated to 10
-2MmHg.
5. the synthetic method of soccerballene as claimed in claim 1 is characterized in that in step 4), and the pressure of the described He of charging into gas is 0.013～0.053MPa.
6. the synthetic method of soccerballene as claimed in claim 1 is characterized in that in step 4), described being replaced into 3～5 times.
7. as the synthetic method of claim 1 or 6 described soccerballenes, it is characterized in that in step 4) that each displacement charges into the He gas of 50～80Torr.
8. the synthetic method of soccerballene as claimed in claim 1 is characterized in that in step 7), and described opening regulated striking electric current to 10～40A behind the welder power.
9. the synthetic method of soccerballene as claimed in claim 1 is characterized in that in step 8), and is described when drawing back graphite anode or graphite cathode, regulates galvanic current greater than 40A.
10. the synthetic method of soccerballene as claimed in claim 9 is characterized in that described adjusting galvanic current is 60～100A.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219209A (en) * | 2011-05-26 | 2011-10-19 | 中国科学院化学研究所 | Method for preparing high fullerene and special anode thereof |
| CN102139871B (en) * | 2010-01-29 | 2013-03-06 | 沈阳科友真空技术有限公司 | Vacuum equipment for continuously preparing fullerene |
| CN108483424A (en) * | 2018-04-28 | 2018-09-04 | 厦门大学 | A kind of fullerene electrical heating synthesizer |
| CN110294468A (en) * | 2019-08-05 | 2019-10-01 | 广州领泰纳米材料科技有限公司 | The device and method of fullerene is prepared using compression arc |
| CN112978712A (en) * | 2019-12-13 | 2021-06-18 | 北京三弧创科技术有限公司 | Method for preparing fullerene by using plasma torch |
| CN115947338A (en) * | 2023-02-24 | 2023-04-11 | 厦门大学 | Preparation method of fullerene and hydrogenated fullerene |
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2009
- 2009-06-28 CN CNA200910112096XA patent/CN101597054A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139871B (en) * | 2010-01-29 | 2013-03-06 | 沈阳科友真空技术有限公司 | Vacuum equipment for continuously preparing fullerene |
| CN102219209A (en) * | 2011-05-26 | 2011-10-19 | 中国科学院化学研究所 | Method for preparing high fullerene and special anode thereof |
| CN102219209B (en) * | 2011-05-26 | 2012-11-07 | 中国科学院化学研究所 | Method for preparing high fullerene and special anode thereof |
| CN108483424A (en) * | 2018-04-28 | 2018-09-04 | 厦门大学 | A kind of fullerene electrical heating synthesizer |
| CN110294468A (en) * | 2019-08-05 | 2019-10-01 | 广州领泰纳米材料科技有限公司 | The device and method of fullerene is prepared using compression arc |
| CN110294468B (en) * | 2019-08-05 | 2024-05-17 | 北京三弧创科技术有限公司 | Device and method for preparing fullerene by using compressed arc |
| CN112978712A (en) * | 2019-12-13 | 2021-06-18 | 北京三弧创科技术有限公司 | Method for preparing fullerene by using plasma torch |
| CN115947338A (en) * | 2023-02-24 | 2023-04-11 | 厦门大学 | Preparation method of fullerene and hydrogenated fullerene |
| CN115947338B (en) * | 2023-02-24 | 2024-06-04 | 厦门大学 | Fullerene and preparation method of hydrogenated fullerene |
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