Patent EP0331283A1 successfully refreshed from Google Patents.
US5304366A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process and apparatus for producing and separating fullerenes
Assignee: SRI International Inc
•
Filing: 1991-12-24
•
Granted: 1994-04-19
•
Expires: 2011-12-24
Abstract
Abstract A process and apparatus is described for the production of purified fullerenes using a non-reactive gas to collect and transport impure fullerenes from an evaporation zone to a heated filter zone in which solid impurities may be filtered out of the mixture. If one or more condensed fullerenes are present in the gas stream entering the filter zone, such condensed fullerenes may be vaporized in the filter zone and carried to a condensation zone in which one or more vaporized fullerenes may be recovered. When more than one vaporized fullerene is present in the gas entering either the filter zone or the condensation zone, a temperature gradient may be used to permit separation and recovery of purified portions of different fullerenes.
Inventors
- 👤 Donald C. Lorents
- 👤 Ripudaman Malhotra
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 09:38
CPC Classifications
B; B82; B82Y; B82Y30/00; B82Y40/00; C; C01; C01B; C01B32/00; C01B32/15; C01B32/152; C01B32/154; C01B32/156; Y; Y10; Y10S; Y10S977/00; Y10S977/84; Y10S977/842; Y10S977/845
Claims Analysis
Total Claims: 37
Claim 1
Independent Claim
87 words
A process for making fullerenes which comprises: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any unvaporized fullerenes produced in step a); c) purifying said vaporized impure mixture of fullerenes by separating out solid impurities from said fullerenes in a separation zone; and d) recovering one or more of said purified fullerenes from said gas in a condensation zone.
Claim 2
Dependent Claim
87 words
A process for making fullerenes which comprises: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any unvaporized fullerenes produced in step a); c) purifying said vaporized impure mixture of fullerenes by separating out solid impurities from said fullerenes in a separation zone; and d) recovering one or more of said purified fullerenes from said gas in a condensation zone.
Claim 3
Dependent Claim
19 words
The process of claim 1 including the further step of separating and separately recovering individual fullerenes from said gas.
Claim 4
Dependent Claim
30 words
The process of claim 1 wherein said step of producing said impure mixture containing one or more fullerenes in said first zone further comprises evaporating carbon in said first zone.
Claim 5
Dependent Claim
32 words
The process of claim 1 wherein said gas is preheated before being introduced into said first zone to a temperature sufficient to vaporize any fullerenes in condensed form in said first zone.
Claim 6
Dependent Claim
97 words
A process for producing fullerenes which comprises: a) forming a mixture of soot and fullerenes by evaporation of a carbonaceous source in a first zone; b) collecting said mixture by passing a heated flow of a non-reactive gas through said first zone to vaporize and/or entrain said mixture in said gas; c) purifying said fullerenes in said heated gas by separating them from entrained soot in said gas in a filtering zone maintained at a temperature sufficiently high to vaporize any condensed fullerenes in said mixture; and d) then recovering said fullerenes from said gas by condensation.
Claim 7
Dependent Claim
97 words
A process for producing fullerenes which comprises: a) forming a mixture of soot and fullerenes by evaporation of a carbonaceous source in a first zone; b) collecting said mixture by passing a heated flow of a non-reactive gas through said first zone to vaporize and/or entrain said mixture in said gas; c) purifying said fullerenes in said heated gas by separating them from entrained soot in said gas in a filtering zone maintained at a temperature sufficiently high to vaporize any condensed fullerenes in said mixture; and d) then recovering said fullerenes from said gas by condensation.
Claim 8
Dependent Claim
35 words
The process of claim 5 wherein individual fullerenes are produced by the further step of separating and recovering individual fullerenes from said gas by condensation of one or more fullerenes in a temperature graded zone.
Claim 9
Dependent Claim
23 words
The process of claim 6 wherein said nonreactive gas is selected from the group consisting of helium, neon, argon, krypton, xenon, and nitrogen.
Claim 10
Dependent Claim
26 words
The process of claim 5 wherein said nonreactive gas is preheated to a temperature of at least about 500° C. before passing through said first zone.
Claim 11
Dependent Claim
29 words
The process of claim 5 wherein said filtering zone is maintained at a temperature of at least about 700° C. to vaporize any condensed fullerenes in said non-reactive gas.
Claim 12
Dependent Claim
19 words
The process of claim 5 including the further step of separating and separately recovering individual fullerenes from said gas.
Claim 13
Dependent Claim
31 words
The process of claim 10 wherein said step of separating and recovering individual fullerenes from said gas further comprises passing said gas containing said vaporized fullerenes through a temperature graded condenser.
Claim 14
Dependent Claim
56 words
The process of claim 5 which further comprises maintaining said filtering zone at a temperature which will condense all fullerenes in said gas except C 60 fullerenes and then recovering said C 60 fullerenes from said gas by condensation in a condensation zone maintained at a temperature below the vaporization temperature of said C 60 fullerenes.
Claim 15
Dependent Claim
83 words
The process of claim 12 which further comprises recovering other fullerenes from said mixture by the steps of: a) stopping said evaporation of said carbonaceous source in said first zone; b) continuing to flow heated gas into said filtering zone; c) raising the temperature in said filtering zone until one or more condensed fullerenes in said filtering zone vaporizes; and d) recovering said one or more vaporized fullerenes from said gas by passing said gas containing said vaporized fullerenes through said condensation zone.
Claim 16
Dependent Claim
45 words
The process of claim 13 which further includes the step of separating and recovering individual fullerenes from said gas by passing said gas containing said vaporized fullerenes through a temperature graded filter to condense one or more fullerenes before said gas reaches said condensation zone.
Claim 17
Dependent Claim
36 words
The process of claim 13 which further includes the step of separating and recovering individual fullerenes from said gas by passing said gas containing said vaporized fullerenes through a temperature graded condenser in said condensation zone.
Claim 18
Dependent Claim
133 words
A process for producing fullerenes which comprises: a) forming a mixture of soot and one or more fullerenes by evaporation of graphite in a first zone; b) collecting said mixture by passing through said first zone a heated flow of a non-reactive gas selected from the group consisting of helium, neon, argon, krypton, xenon, and nitrogen to vaporize and/or entrain said mixture in said gas; c) purifying said one or more fullerenes in said heated gas by separating them from said entrained soot in said gas in a filtering zone maintained at a temperature sufficiently high to vaporize and condensed fullerenes in said mixture; and d) recovering said one or more vaporized fullerenes from said gas by passing said gas containing said one or more vaporized fullerenes through a temperature graded condensation zone.
Claim 19
Dependent Claim
133 words
A process for producing fullerenes which comprises: a) forming a mixture of soot and one or more fullerenes by evaporation of graphite in a first zone; b) collecting said mixture by passing through said first zone a heated flow of a non-reactive gas selected from the group consisting of helium, neon, argon, krypton, xenon, and nitrogen to vaporize and/or entrain said mixture in said gas; c) purifying said one or more fullerenes in said heated gas by separating them from said entrained soot in said gas in a filtering zone maintained at a temperature sufficiently high to vaporize and condensed fullerenes in said mixture; and d) recovering said one or more vaporized fullerenes from said gas by passing said gas containing said one or more vaporized fullerenes through a temperature graded condensation zone.
Claim 20
Dependent Claim
86 words
Apparatus for making and recovering fullerenes which comprises: a) means for producing an impure mixture containing one or more fullerenes in a first zone; b) means for collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone; c) filter means for purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes; d) means for heating said filter means; and e) means for recovering one or more of said purified fullerenes from said gas.
Claim 21
Dependent Claim
86 words
Apparatus for making and recovering fullerenes which comprises: a) means for producing an impure mixture containing one or more fullerenes in a first zone; b) means for collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone; c) filter means for purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes; d) means for heating said filter means; and e) means for recovering one or more of said purified fullerenes from said gas.
Claim 22
Dependent Claim
30 words
The apparatus of claim 17 wherein said means for producing an impure mixture containing one or more fullerenes in a first zone comprises carbonaceous rods spaced in an evaporation chamber.
Claim 23
Dependent Claim
41 words
The apparatus of claim 18 wherein said means for collecting said impure mixture of fullerenes from said first zone further comprises a source of non-reactive gas connected to said evaporation chamber to thereby flow said non-reactive gas through said evaporation chamber.
Claim 24
Dependent Claim
22 words
The apparatus of claim 17 wherein said heated filter means further comprise means for maintaining a temperature gradient in said filter means.
Claim 25
Dependent Claim
24 words
The apparatus of claim 18 wherein conduit means, with means for heating said conduit means, connect said evaporation chamber with said heated filter means.
Claim 26
Dependent Claim
19 words
The apparatus of claim 17 wherein said means for recovering said fullerenes from said gas further comprise condenser means.
Claim 27
Dependent Claim
21 words
The apparatus of claim 22 wherein said condenser means further comprise means for maintaining a temperature gradient in said condenser means.
Claim 28
Dependent Claim
31 words
The apparatus of claim 22 wherein a conduit means, with means for heating said conduit means, connects said filter means with said condenser means for recovering said fullerenes from said gas.
Claim 29
Dependent Claim
114 words
A process for making fullerenes which comprises: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any condensed fullerenes in said impure mixture of fullerenes; c) purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes by passing said mixture through filter means maintained at a temperature sufficiently high to vaporize any fullerenes not already vaporized to thereby purify said mixture by filtering out non-vaporized portions of said impure gas mixture; and d) recovering said fullerenes from said gas in a condensation zone.
Claim 30
Dependent Claim
114 words
A process for making fullerenes which comprises: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any condensed fullerenes in said impure mixture of fullerenes; c) purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes by passing said mixture through filter means maintained at a temperature sufficiently high to vaporize any fullerenes not already vaporized to thereby purify said mixture by filtering out non-vaporized portions of said impure gas mixture; and d) recovering said fullerenes from said gas in a condensation zone.
Claim 31
Dependent Claim
32 words
The process of claim 25 wherein said step of separating and recovering individual fullerenes from said gas further comprises passing said gas containing said vaporized fullerenes through a temperature graded condensation zone.
Claim 32
Dependent Claim
134 words
A process for making fullerenes which comprise: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any condensed fullerenes in said impure mixture of fullerenes; c) purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes by passing said mixture through filter means maintained at a temperature sufficiently low to condense all of said fullerenes in said mixture except the lowest molecular weight fullerene in said mixture while permitting said lowest molecular weight vaporized fullerene to pass through said filter means for subsequent condensation and recovery in a condensation zone; and d) recovering said vaporized fullerene from said gas in a condensation zone.
Claim 33
Dependent Claim
134 words
A process for making fullerenes which comprise: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any condensed fullerenes in said impure mixture of fullerenes; c) purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes by passing said mixture through filter means maintained at a temperature sufficiently low to condense all of said fullerenes in said mixture except the lowest molecular weight fullerene in said mixture while permitting said lowest molecular weight vaporized fullerene to pass through said filter means for subsequent condensation and recovery in a condensation zone; and d) recovering said vaporized fullerene from said gas in a condensation zone.
Claim 34
Dependent Claim
104 words
A process for making fullerenes which comprises: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any condensed fullerenes in said impure mixture of fullerenes; c) purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes by passing said mixture through filter means maintained at a temperature gradient to thereby condense one or more fullerenes in said filter means; and d) recovering the remaining uncondensed fullerenes from said gas in a condensation zone.
Claim 35
Dependent Claim
104 words
A process for making fullerenes which comprises: a) producing an impure mixture containing one or more fullerenes in a first zone; b) collecting said impure mixture of fullerenes from said first zone by flowing a non-reactive gas through said first zone to vaporize any condensed fullerenes in said impure mixture of fullerenes; c) purifying said impure mixture of fullerenes by separating out solid impurities from said fullerenes by passing said mixture through filter means maintained at a temperature gradient to thereby condense one or more fullerenes in said filter means; and d) recovering the remaining uncondensed fullerenes from said gas in a condensation zone.
Claim 36
Dependent Claim
121 words
A process for making fullerenes which comprises: a) producing an impure mixture comprising one or more fullerenes and solid impurities in a first zone; b) collecting and removing said impure mixture of fullerenes and solid impurities from said first zone by flowing anon-reactive carrier gas through said first zone to vaporize and/or entrain said mixture in said non-reactive gas; c) vaporizing any unvaporized fullerenes in said impure mixture entrained in said non-reactive carrier gas; d) purifying said impure mixture of fullerenes by separating out said solid impurities still entrained in said non-reactive carrier gas from said vaporized fullerenes in a separation zone; and e) recovering one or more of said purified fullerenes from said non-reactive carrier gas in a condensation zone.
Claim 37
Dependent Claim
121 words
A process for making fullerenes which comprises: a) producing an impure mixture comprising one or more fullerenes and solid impurities in a first zone; b) collecting and removing said impure mixture of fullerenes and solid impurities from said first zone by flowing anon-reactive carrier gas through said first zone to vaporize and/or entrain said mixture in said non-reactive gas; c) vaporizing any unvaporized fullerenes in said impure mixture entrained in said non-reactive carrier gas; d) purifying said impure mixture of fullerenes by separating out said solid impurities still entrained in said non-reactive carrier gas from said vaporized fullerenes in a separation zone; and e) recovering one or more of said purified fullerenes from said non-reactive carrier gas in a condensation zone.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1997-04-18 | 1997-10-18 | 1998-04-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2001-04-18 | 2001-10-18 | 2002-04-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2005-04-18 | 2005-10-18 | 2006-04-19 | $7700.00 | Window Closed / Lapsed |