Process for purifying fullerenes

Details Process for purifying fullerenes Process for purifying fullerenes

1997-04-16

1999-05-18

Therkorn, Ernest G.

Liquid purification or separation

Processes

Liquid/liquid solvent or colloidal extraction or diffusing...

210656, 2101982, 423445B, B01D15/08

Patent

active

059048522

ABSTRACT:
A process for separating C.sub.60, C.sub.70, and higher fullerenes above C.sub.70 is provided. The process employs a chromatographic column utilizing a functionalized aromatic-containing resin as the stationary phase, an organic solvent as the mobile phase, and a mixture of fullerenes dissolved in the mobile phase.

REFERENCES:
patent: 5308481 (1994-05-01), Stalling et al.
patent: 5310532 (1994-05-01), Tour et al.
patent: 5487831 (1996-01-01), Pirkle
patent: 5698174 (1997-12-01), Muller
Whetten et al., "Spectroscopic and Photophysical Properties of the Soluble C.sub.n Molecules, n=60, 70, 76/78, 84," pp. 639-651, Materials Research Society Symp. Proc. vol. 206, 1991.
Heath et al., "C.sub.60 Research at the University of California at Berkeley," pp. 667-671, Materials Research Society Sump. Proc. vol. 206, 1991.
A. V. Kiselev, "Adsorbents in Gas Chromatography," pp. 127-143, Advances in Chromatography, vol. 4, 1967.
J. V. Dawkins, "Gel Permeation Chromatography," pp. 337-366, Techniques in Liquid Chromatography, 1982.
Scrivens et al., "Chemical Communications," pp. 1207-1209, J. Chem. Soc., Chemical Communications, Issue 15, 1993.
Scrivens et al., "Single Column Purification of Gram Quantities of C70," pp. 6939-6940, Journal of the American Chemical Society, 116, 1994.
Bhyrappa et al., "Improved Chromatographic Separation and Purification of C.sub.60 and C.sub.70 Fullerenes," pp. 936-937, J. Chem. Soc., Chem. Commun., 1992.
Ruoff et al., "Solubility of C.sub.60 in a Variety of Solvents," pp. 3379-3383, J. Phys. Chem. 98, 1993.
Scrivens et al., "Single Column Purification of Gram Quantities of C.sub.70," pp. 6939-6940, J. Am. Chem. Soc. 116, 1994.
McKean et al., "Synthesis of Functionalized Styrenes via Palladium-Catalyzed Coupling of Aryl Bromides with Vinyl Tin Reagents," pp. 422-424, J. Org. Chem. 52, 1987.
Sivaraman et al., "Solubility of C.sub.60 in Organic Solvents," pp. 6077-6079, J. Org. Chem. 57, 1992.
Trost et al., "Sulfur-Substituted Dienes and the Silylene Protecting Group in Systhesis, Deoxypillaromycinone," pp. 3253-3265, J. Org. Chem. 48, 1983.
Tour et al., "A Zirconium-Promoted Methylenation of Aldehydes, Ketones, and Enones," pp. 2937-2930, Tetrahedron Letters, vol. 30, No. 30, 1989.
Gugel et al., "Separation of C.sub.60 and C.sub.70 on polystyrene gel with toluene as mobile phase," pp. 23-29, Journal of Chromatography, 628, 1993.
Scrivens et al. "Potent Solvents for C.sub.60 and Their Utility for the Rapid Acquisition of .sup.13 C NMR Data for Fullerenes," pp. 1207-1209, J. Chem. Soc., Chem. Commun., 1993.
Baum, "Flood of Fullerene Discoveries Continues Unabated," pp. 25-31, Chemical and Engineering News, Jun. 1, 1992.
Pradeep et al., "Preparation of Buckminsterfullerene, C.sub.60," pp. 1101-1105, Mat. Res. Bull., vol. 26, 1991.
Kratschmer et al., "The infrared and ultraviolet absorption spectra of laboratory-produced carbon dust: evidence for the presence of the C.sub.60 molecule," pp. 167-170, Chemical Physics Letters, vol. 170, No. 2,3, Jul. 6, 1990.
Hare et al., "Preparation and UV/visible spectra of fullerenes C.sub.60 and C70," pp. 394-398, Chemical Physics Letters, vol. 177, No. 4,5, Mar. 1, 1991.
Vassallo et al., "Improved Separation of Fullerene-60 and-70," pp. 60-61, J. Chem. Soc., Chem. Commun. 1992.
Taylor et al., "Isolation, Separation and Characterisation of the Fullerenes C.sub.60 and C.sub.7 : The Third Form of Carbon," pp. 1423-1425, J. Chem. Soc., Chem. Commun., 1990.
Peters et al., "A New Fullerene Synthesis," pp. 223-224, Angew. Chem. Int. Ed. Engl. 31, No. 2, 1992.
Still et al., "Rapid Chromatographic Technique for Preparative Separations with Moderate Resolution," pp. 2923-2925, J. Org. Chem., vol. 43, No. 14, 1978.
Meier et al., "Efficient Preparative Separation of C.sub.60 and C.sub.70 Gel Permeation Chromatography of Fullerenes Using 100% Toluene as Mobile Phases," pp. 1924-1926, J. Org. Chem., 57, 1992.
Chatterjee et al., "Fast One-Step Separation and Purification of Buckminsterfullerene, C.sub.60 from Carbon Soot," pp. 3253-3254, J. Org. Chem., 57, 1992.
Khemani et al., "A Simple Soxhlet Chromatographic Method for the Isolation of Pure C.sub.60 and C.sub.70," pp. 3254-3256, J. Org. Chem., 57, 1992.
Koch et al., "Preparation of Fullerenes with a Simple Benchtop Reactor," pp. 4543-4545, J. Org. Chem., 56, 1991.
Ajie et al., "Characterization of the Soluble All-Carbon Molecules C.sub.60 and C.sub.70," pp. 8630-8633, J. Phys. Chem., 94, 1990.
Haufler et al., "Efficient Production of C.sub.60 (Buckminsterfullerene), C.sub.60 H.sub.36, and the Solvated Buckide Ion," pp. 8634-8636, J. Phys. Chem., 94, 1990.
Shinohara et al., "Formation and Extraction of Very Large All-Carbon Fullerenes," pp. 8449-8451, J. Phys. Chem., 95, 1991.
Zhennan et al., "Buckminsterfullerene C.sub.60 : Synthesis, Spectroscopic Characterization, and Structure Analysis," pp. 9615-1918, The Journal of Physical Chemistry, vol. 95, No. 24, Nov. 28, 1991.
Parker et al., "High-Yield Synthesis, Separation, and Mass-Spectrometic Characterization of Fullerenes C.sub.60 to C.sub.266," pp. 7499-7503, J. Am. Chem. Soc., 113, 1991.
Pradeep et al., "A Novel FeC.sub.60 Adduct in the Solid State," pp. 2272-2273, J. Am. Chem. Soc., 114, 1992.
Diederich et al., "The Higher Fullerenes: Isolation and Characterization of C.sub.76, C.sub.84, C.sub.90, C.sub.94, and C.sub.70 O, an Oxide of D.sub.5h -C.sub.70," pp. 548-551, Science, vol. 252, Apr. 26, 1991.
Diederich et al., "Fullerenes Isomerism: Isolation of C.sub.2v -C.sub.78 and D.sub.3 -C.sub.78," pp. 1768-1770, Science Vo. 254, Dec. 20, 1991.
Kroto et al., "C.sub.60 : Buckminsterfullerene," pp. 162-163, Nature Vo. 318, Nov. 14, 1985.
Kratschmer et al., "Solid C.sub.60 : a new form of carbon," pp. 354-358, Nature Vo. 347, Sep. 27, 1990.
Howard et al., "Fullerenes C.sub.60 and C.sub.70 in flames," pp. 139-141, Nature Vo. 352, Jul. 11, 1991.
Jinno et al., "Liquid chromatographic separation of all-carbon molecules C.sub.60 and C.sub.70 with multi-legged phenyl group bonded silica phases," pp. 105-109, Journal of Chromatography, 594, 1992.
Wudl, "The Chemical Properties of Buckminsterfullerene (C.sub.60) and the Birth of Infancy of Fulleroids," pp. 157-161, Acc. Chem. Res., 25, 1992.
Johnson et al., "Fullerene Structure and Dynamics: A Magnetic Resonance Potpourri," pp. 169-175, Acc. Chem. Res., 25, 1992.
McElvany et al., "Characterization of Fullerenes by Mass Spectrometry," pp. 162-168, Acc. Chem. Res., 25, 1992.
Hawkins, "Osmylation of C.sub.60 : Proof and Characterization of the Soccer-Ball Framework," pp. 150-156, Acc. Chem. Res., 25, 1992.
Weaver, "Fullerenes and Fullerides: Photoemission of Scanning Tunneling Microscopy Studies," pp. 143,149, Acc. Chem. Res., 25, 1992.
Fagan et al., "Metal Complexes of Buckminsterfullerene (C.sub.60)," pp. 134-142, Acc. Chem. Res., 25, 1992.
Haddon, "Electronic Structure, Conductivity, and Superconductivity of Alkali Metal Doped C.sub.60," pp. 127-133, Acc. Chem. Res., 25, 1992.
Diederich et al., "Beyond C.sub.60 : The Higher Fullerenes," pp. 119-126, Acc. Chem. Res., 25, 1992.
Hare et al., "A Postbuckminsterfullerene View of Carbon in the Galaxy," pp. 106-112, Acc. Chem. Res., 25, 1992.
Fischer et al., "Solid-State Chemistry of Fullerene-Based Materials," pp. 112-118, Acc. Chem. Res., vol. 25, No. 3, 1992.
Smalley, "Self-Assembly of the Fullerenes," pp. 98-105, Acc. Chem. Res., vol. 25, 1992.
Scrivens et al., "Purification of Gram Quantities of C.sub.60. A New Inexpensive and Facile Method," pp. 7917-7919, J. Am. Chem. Soc., vol. 114, Sep. 23, 1992.
Walling et al., "Substituted Styrenes: I. The Decarboxylation of Substituted Cinnamic Acids," pp. 852-854, J. Am. Chem. Soc., vol. 69, Apr. 1947.
J. Gong et al., "New method for highly efficient separation and purification of C.sub.60," Chemical Abstracts, p. 1093, vol. 122, No. 6, abstract No. 70419e, Feb. 6, 1995.
Kirk and Othmer, "Preparation of Active Carbons" and "Nature of the Active Carbon Surface," Encyclopedia of Chemical Technology, vol. 2, pp. 886-890, 1948.
Hodge et al., "Polymer-Supported Reactions in Organic Synthesis," Polymer Supports, pp.

Affiliated with

Also associated with

Rating

Process for purifying fullerenes does not yet have a rating. At this time, there are no reviews or comments for this patent.

If you have personal experience with Process for purifying fullerenes, we encourage you to share that experience with our LandOfFree.com community. Your opinion is very important and Process for purifying fullerenes will most certainly appreciate the feedback.

Rate now

Comments { 0 }

Profile ID: LFUS-PAI-O-1758075