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Process for preparing Fuller-ene

A fullerene and raw material technology, applied in the field of fullerene preparation, can solve the problems of high cost of raw materials and preparation equipment, low yield, and inability to synthesize in large quantities at low cost

Inactive Publication Date: 2003-09-10
CANON KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, in the above-mentioned conventional methods for producing fullerenes, there is a problem that they cannot be synthesized in large quantities at low cost due to the high cost of raw materials and production equipment and the low yield.

Method used

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  • Process for preparing Fuller-ene
  • Process for preparing Fuller-ene
  • Process for preparing Fuller-ene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] like figure 2 As shown, a pressure-resistant reaction vessel 202 equipped with a pressure gauge 203, a heater 204, and a safety valve 205 is used.

[0054] Add 2g of naphthalene (critical temperature 475°C, critical pressure 4.11MPa) as raw material 200, ferric chloride FeCl 3 0.2g, ethanol (critical temperature 243 ℃, critical pressure 6.38MPa) 2g as the solvent of ferric chloride, dry ice CO as the reaction medium forming substance 201 2 (Critical temperature 31° C., critical pressure 7.38 MPa) 80 g, and airtight, reacted at a temperature of 300° C. and a pressure of 12 MPa for 6 hours to obtain a reaction product. After extracting the obtained reaction product with toluene, use methanol / toluene=51 / 41 high-performance liquid chromatographic analysis when the toluene solution that the extracted reaction product is diluted to 200 times with toluene, in addition to unreacted naphthalene, with A peak was observed at the same retention time as previously measured with a...

Embodiment 2

[0056] In Example 1, 0.2 g of ferrocene was added to ferric chloride, and the same operation as in Example 1 was used to obtain a reaction product. Next, the obtained reaction product was dissolved in toluene and analyzed by the same high-performance liquid chromatography as in Example 1. As a result, in addition to unreacted toluene, a peak was observed at a retention time corresponding to the peak position of fullerene .

Embodiment 3

[0058] In Example 1, no ferric chloride catalyst was added, the reaction temperature was raised to 400° C., and the reaction product was obtained by the same operation as in Example 1. Next, the obtained reaction product was dissolved in toluene and analyzed by the same high performance liquid chromatography as in Example 1. As a result, in addition to unreacted naphthalene, a peak was observed at a retention time corresponding to the peak position of fullerene .

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Abstract

A method for producing fullerenes, characterized in that said method includes a step (a) of contacting an aromatic compound-containing starting material with a supercritical fluid or a subcritical fluid at a temperature in a range of from 31 DEG C to 500 DEG C and at a pressure in a range of from 3.8 MPa to 60 MPa. Said supercritical fluid or said subcritical fluid is formed from one or more kinds of materials selected from the group consisting of an aromatic compound as said starting material, a solvent capable of dissolving said aromatic compound, water, dinitrogen monoxide, and ammonia.

Description

technical field [0001] The present invention relates to the preparation method of fullerene. More specifically, it relates to a production method capable of mass-producing fullerenes from inexpensive raw materials. Background technique [0002] In 1985 by H.W.Kroto, R.E.Smallry, R.F.Curl discovered the fullerene C containing 60 carbon atoms football-shaped polyhedral molecules 60 Afterwards, C with 70 carbon atoms was discovered successively. 70 , C of 76 carbon atoms 76 , C of 78 carbon atoms 78 , C of 82 carbon atoms 82 , C of 84 carbon atoms 84 , C of 86 carbon atoms 86 , C of 88 carbon atoms 88 , 90 carbon atoms of C 90 , 94 carbon atoms of C 94 , 96 carbon atoms of C 96 etc., and fullerenes containing metal elements have also been discovered, and various applications such as functional devices and pharmaceuticals are being actively researched. [0003] Previously, as a method for producing fullerenes, it has been developed to extract fullerenes from soot obta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J3/00C01B31/02
CPCC01B31/0206C01B31/0213B01J2219/00065B01J3/008B01J2219/0286Y10S977/842B82Y30/00B01J2219/0027B01J2219/0277B01J2219/00087B82Y40/00C01B32/15C01B32/154Y02P20/54C01B32/05
Inventor 川上综一郎山本智也佐野瞳
Owner CANON KK
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