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US4808270A Expired / Lapsed US ⏱️ 0.0 years remaining

Process and apparatus for the preparation of ether

Assignee: Linde GmbH
•
Filing: 1987-01-21
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Granted: 1989-02-28
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Expires: 2007-01-21
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Abstract

Abstract For the preparation of an ether, e.g., tertiary amyl methyl ether, an olefin-containing feed stream is catalytically etherified with an alcohol, e.g., methyl alcohol. The etherification product is fractionally distilled into an overhead fraction containing essentially unreacted, light hydrocarbons and unreacted alcohol and into a bottoms fraction containing essentially the desired ether. The overhead fraction is condensed and cooled to resultant immiscible phases, of which one contains essentially the alcohol and the other contains essentially the hydrocarbons, are removed separately from each other. Water may be added to the overhead stream to facilitate the formation of the two liquid phases.

Inventors

  • 👤 Hans-Juergen Wernicke
  • 👤 Reinhard Glatthaar
  • 👤 Nikolaus Buckl

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 06:00
CPC Classifications
C; C07; C07C; C07C41/00; C07C41/01; C07C41/34; C07C41/18; C07C41/24; C07C41/40; C07C41/42; Y; Y10; Y10S; Y10S203/00; Y10S203/24

Claims Analysis

Total Claims: 22
Claim 1
Independent Claim 150 words
In a process for the production of tertiary alkyl methyl ether (TAME) comprising etherifying a C 5 olefin-containing hydrocarbon feed stream with methyl alcohol in a reactor; fractionally distilling resultant reaction product formed during the etherifying into an overhead fraction containing essentially unreacted hydrocarbons and unreacted alcohol, and a bottom fraction containing essentially the ether; condensing the overhead fraction; and separating the alcohol from the condensed overhead fraction, the improvement which comprises cooling the condensed overhead fraction to below the single phase saturation temperature to form immiscible liquid phases, one containing essentially the alcohol and the other containing essentially the hydrocarbons, and withdrawing the immiscible phases separately from each other, with the provision that water is not added in said separating step to separate the alcohol from the C 5 hydrocarbon so as to form an aqueous phase containing the alcohol which is thereafter distilled into water and alcohol fractions.
Claim 2
Dependent Claim 150 words
In a process for the production of tertiary alkyl methyl ether (TAME) comprising etherifying a C 5 olefin-containing hydrocarbon feed stream with methyl alcohol in a reactor; fractionally distilling resultant reaction product formed during the etherifying into an overhead fraction containing essentially unreacted hydrocarbons and unreacted alcohol, and a bottom fraction containing essentially the ether; condensing the overhead fraction; and separating the alcohol from the condensed overhead fraction, the improvement which comprises cooling the condensed overhead fraction to below the single phase saturation temperature to form immiscible liquid phases, one containing essentially the alcohol and the other containing essentially the hydrocarbons, and withdrawing the immiscible phases separately from each other, with the provision that water is not added in said separating step to separate the alcohol from the C 5 hydrocarbon so as to form an aqueous phase containing the alcohol which is thereafter distilled into water and alcohol fractions.
Claim 3
Dependent Claim 25 words
A process according to claim 1 further comprising recycling at least part of the withdrawn immiscible phase containing essentially the alcohol into the etherification reactor.
Claim 4
Dependent Claim 29 words
A process according to claim 1 wherein said cooling of the overhead fraction is conducted in indirect heat exchange with a cold stream from a low-temperature gas separation facility.
Claim 5
Dependent Claim 30 words
A process according to claim 1 wherein said cooling of the overhead fraction, prior to separation of the two phases, is conducted to a temperature of -60° to +50° C.
Claim 6
Dependent Claim 60 words
A process according to claim 1 further comprising admixing a minor amount of water to the overhead fraction prior to phase separation in order to increase the separability of the immiscible phases, most of said water being passed into the liquid phase containing essentially alcohols and the remainder of said water passing into said liquid phase containing essentially the hydrocarbons.
Claim 7
Dependent Claim 23 words
A process according to claim 5 wherein the admixed proportion of water is between 0.01 and 2% by weight of the overhead fraction.
Claim 8
Dependent Claim 38 words
A process according to claim 5 further comprising recycling at least part of the withdrawn immiscible phase containing essentially the methyl alcohol into the etherification reactor without removing said water from said immiscible phase in an interventing step.
Claim 9
Dependent Claim 30 words
A process according to claim 5 further comprising passing at least a portion of the immiscible phase containing essentially the hydrocarbons directly into the fractional distillation zone as reflux liquid.
Claim 10
Dependent Claim 31 words
A process according to claim 8, wherein said cooling of the overhead fraction, prior to separation of the two immiscible phases, ranges to temperatures of about -43 ° to -60° C.
Claim 11
Dependent Claim 21 words
A process according to claim 1 wherein the distillation and the phase separation are conducted under a pressure of 1-20 bar.
Claim 12
Dependent Claim 30 words
A process according to claim 1 further comprising combining at least a portion of the immiscible phase containing essentially the hydrocarbons with withdrawn bottoms fraction from the fractional distillation step.
Claim 13
Dependent Claim 30 words
A process according to claim 1 further comprising passing at least a portion of the immiscible phase containing essentially the hydrocarbons directly into the fractional distillation zone as reflux liquid.
Claim 14
Dependent Claim 22 words
A process according to claim 1 wherein the feed stream is a light gasoline fraction from a thermal or catalytic cracking stage.
Claim 15
Dependent Claim 27 words
A process according to claim 1, wherein the bottoms fraction of the distillation column contains the ether in a mixture with a portion of the unreacted hydrocarbons.
Claim 16
Dependent Claim 27 words
A process according to claim 1 wherein the etherification is conducted at a temperature of +40° to -120° C. and under an absolute pressure of 1.2-20 bar.
Claim 17
Dependent Claim 30 words
A process according to claim 1, wherein said cooling of the overhead fraction, prior to separation of the two immiscible phases, ranges to temperatures of about -43° to -60° C.
Claim 18
Dependent Claim 20 words
A process according to claim 1, wherein distillation and phase separation are conducted under a pressure of about 1.5-3 bar.
Claim 19
Dependent Claim 18 words
A process according to claim 1, further comprising separating the ether from the bottoms fraction of the distillation.
Claim 20
Dependent Claim 35 words
A process according to claim 1, wherein at least part of the heat reaction liberated during etherification is employed to heat up at least a portion of the hydrocarbon feed stream passed into the reactor.
Claim 21
Dependent Claim 185 words
In a process for the production of tertiary amyl methyl ether (TAME) comprising etherifying an olefin-containing, essentially C 5 hydrocarbon feed stream with methyl alcohol in a reactor; fractionally distilling resultant reaction product formed during the etherifying into an overhead fraction containing essentially unreacted hydrocarbons and unreacted methyl alcohol and a bottom fraction containing essentially the ether; condensing the overhead fraction; and separating the methyl alcohol from the condensed overhead fraction, the improvement which comprises cooling the condensed overhead fraction to below the single phase saturation temperature to form only two immiscible liquid phases, one containing essentially the methyl alcohol and the other containing essentially the hydrocarbons, and withdrawing the immiscible phases separately from each other with the provision that water in a proportion of between 0.01 and 2% by weight of the overhead fraction is admixed to the overhead fraction prior to phase separation, said water providing increased separability of the two immiscible phases and most of the water transferring into the methanol phase upon condensation, said water being present in said methanol phase in a substantially smaller weight proportion compared to the methanol.
Claim 22
Dependent Claim 185 words
In a process for the production of tertiary amyl methyl ether (TAME) comprising etherifying an olefin-containing, essentially C 5 hydrocarbon feed stream with methyl alcohol in a reactor; fractionally distilling resultant reaction product formed during the etherifying into an overhead fraction containing essentially unreacted hydrocarbons and unreacted methyl alcohol and a bottom fraction containing essentially the ether; condensing the overhead fraction; and separating the methyl alcohol from the condensed overhead fraction, the improvement which comprises cooling the condensed overhead fraction to below the single phase saturation temperature to form only two immiscible liquid phases, one containing essentially the methyl alcohol and the other containing essentially the hydrocarbons, and withdrawing the immiscible phases separately from each other with the provision that water in a proportion of between 0.01 and 2% by weight of the overhead fraction is admixed to the overhead fraction prior to phase separation, said water providing increased separability of the two immiscible phases and most of the water transferring into the methanol phase upon condensation, said water being present in said methanol phase in a substantially smaller weight proportion compared to the methanol.

References Cited (Backward Citations)

GB1473263A Cited
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US4299999A Cited
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EP0075136B1 Cited
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GB2134905A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-02-28 1992-08-29 1993-02-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-02-28 1996-08-29 1997-02-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-02-28 2000-08-29 2001-02-28 $7700.00 Window Closed / Lapsed

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