Patent US4029552A successfully refreshed from Google Patents.
US4029552A
Expired / Lapsed
US
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Process for obtaining high purity perfluoro-n-heptane
Assignee: Phillips Petroleum Co
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Filing: 1975-10-24
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Granted: 1977-06-14
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Expires: 1995-10-24
Abstract
Abstract A process is disclosed for obtaining a high purity perfluoro-n-heptane from an electrochemical fluorination product which comprises perfluoro-n-heptane, n-heptane, partially fluorinated heptanes, and water soluble acidic components such as hydrofluoric acid and is derived from the electrochemical fluorination of n-heptane.
Inventors
- 👤 George B. Fozzard
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 17:28
CPC Classifications
C; C07; C07C; C07C17/00; C07C17/38; C07C19/00; C07C19/08
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
178 words
The process for obtaining a high purity perfluoro-n-heptane from an electrochemical fluorination product stream derived from the electrochemical fluorination of n-heptane, wherein said product stream comprises perfluoro-n-heptane, n-heptane, partially fluorinated heptanes, and water soluble acidic components comprising hydrofluoric acid, which process comprises: a. water-washing said electrochemical fluorination product stream, thereby removing substantially water soluble acidic components and producing a water-washed stream, b. fractionating said water-washed stream, thereby producing a first overhead fraction rich in perfluoro-n-heptane and n-heptane, a second higher boiling fraction, and a bottoms fraction, c. washing said first overhead perfluoro-n-heptane rich fraction with toluene, thereby substantially extracting said n-heptane as an n-heptane-toluene admixture and leaving a raffinate admixture comprising perfluoro-n-heptane and toluene, d. distilling said raffinate, thereby producing a toluene fraction and a toluene/perfluoro-n-heptane azeotrope, e. effecting phase separation between said toluene and said perfluoro-n-heptane from said perfluoro-n-heptane/toluene azeotrope, thereby resulting in a substantially toluene rich phase and a substantially rich perfluoro-n-heptane rich phase, f. drawing off said toluene rich phase from said perfluoro-n-heptane rich phase, and g. recovering said perfluoro-n-heptane as a substantially pure material.
Claim 2
Dependent Claim
178 words
The process for obtaining a high purity perfluoro-n-heptane from an electrochemical fluorination product stream derived from the electrochemical fluorination of n-heptane, wherein said product stream comprises perfluoro-n-heptane, n-heptane, partially fluorinated heptanes, and water soluble acidic components comprising hydrofluoric acid, which process comprises: a. water-washing said electrochemical fluorination product stream, thereby removing substantially water soluble acidic components and producing a water-washed stream, b. fractionating said water-washed stream, thereby producing a first overhead fraction rich in perfluoro-n-heptane and n-heptane, a second higher boiling fraction, and a bottoms fraction, c. washing said first overhead perfluoro-n-heptane rich fraction with toluene, thereby substantially extracting said n-heptane as an n-heptane-toluene admixture and leaving a raffinate admixture comprising perfluoro-n-heptane and toluene, d. distilling said raffinate, thereby producing a toluene fraction and a toluene/perfluoro-n-heptane azeotrope, e. effecting phase separation between said toluene and said perfluoro-n-heptane from said perfluoro-n-heptane/toluene azeotrope, thereby resulting in a substantially toluene rich phase and a substantially rich perfluoro-n-heptane rich phase, f. drawing off said toluene rich phase from said perfluoro-n-heptane rich phase, and g. recovering said perfluoro-n-heptane as a substantially pure material.
Claim 3
Dependent Claim
21 words
The process of claim 1 wherein said phase separation is accompanied by cooling said azeotrope to at least about -10° C.
Claim 4
Dependent Claim
36 words
The process according to claim 1 wherein said step (g) comprises distilling said layer enriched in perfluoro-n-heptane overhead until the kettle product is depleted of residual toluene, and recovering said kettle product as substantially pure perfluoro-n-heptane.
Claim 5
Dependent Claim
26 words
The process of claim 1 wherein said n-heptane-toluene admixture is fractionated into n-heptane and toluene, and said so-separated toluene is recycled to said washing step (c).
Claim 6
Dependent Claim
36 words
The process of claim 1 further comprising fractionating said n-heptane/toluene admixture from said step (c) to produce a toluene stream and an n-heptane stream, and wherein said toluene stream is recycled to said washing step (c).
Claim 7
Dependent Claim
36 words
The process of claim 1 further comprising fractionating said n-heptane/toluene admixture from said stop (c) to produce a toluene stream and an n-heptane stream, and wherein said toluene stream is recycled to said distilling step (d).
Claim 8
Dependent Claim
14 words
The process of claim 1 wherein said distilling step (d) further employs added toluene.
Claim 9
Dependent Claim
20 words
The process of claim 1 further comprising recycling said drawn off toluene from step (f) to said washing step (c).
Claim 10
Dependent Claim
21 words
The process of claim 1 further comprising recycling said drawn off toluene from step (b) to step (d) as added toluene.
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) | 1980-06-13 | 1980-12-13 | 1981-06-14 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-06-13 | 1984-12-13 | 1985-06-14 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-06-13 | 1988-12-13 | 1989-06-14 | $7700.00 | Window Closed / Lapsed |