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US4029552A Expired / Lapsed US ⏱️ 0.0 years remaining

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
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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 12:56
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)

US2582197A Cited
US2789087A Cited
US2695321A Cited
US3101304A Cited
US3511761A Cited

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

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