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US3769177A Expired / Lapsed US ⏱️ 0.0 years remaining

Purification of carboxylic acids by plural stage distillation with side stream draw-offs

Assignee: BP Chemicals Ltd
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Filing: 1971-11-10
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Granted: 1973-10-30
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Expires: 1991-11-10
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Abstract

Abstract A process for the removal and recovery of halogen components and the drying of aqueous monocarboxylic acids, particularly those produced by the reaction of an alcohol or olefin and carbon monoxide in the presence of a catalytic system comprising a Group VIII metal component and a halogen component containing bromine or iodine and at least a portion of the halogen component being either an alkyl halide or a hydrogen halide. The process comprises introducing a monocarboxylic acid stream containing water and the halogen contaminant into a first distillation column, removing an overhead fraction containing primarily alkyl halide, removing a bottoms fraction from said first distillation column containing the hydrogen halides present in said column, taking a stream from the middle portion of said first distillation column and introducing it into the upper half of a second distillation column, removing an overhead fraction consisting primarily of the water charged thereto, taking a stream from the middle portion of the second distillation column and recycling such stream to the lower half of the first distillation column, said stream containing essentially all of the hydrogen halide present in said second distillation column, and removing a product acid stream at or near the bottom of said second distillation column, the product acid stream being essentially dry and substantially free of the halogen components charged to the first column. The method is particularly applicable to the removal of water and iodine-containing compounds from acetic and propionic acids.

Inventors

  • 👤 L Eubanks
  • 👤 F Rosenberger
  • 👤 Mahon K Mc
  • 👤 J Payne

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 22:19
CPC Classifications
C; C07; C07C; C07C51/00; C07C51/42; C07C51/43; C07C51/44

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 27 words
The process of claim 1 wherein the overhead fraction (b) is separated into a heavy phase of predominantly alkyl halide and a lighter phase of predominantly water.
Claim 2
Dependent Claim 11 words
The process of claim 1 wherein said halogen contaminants comprise iodides.
Claim 3
Dependent Claim 11 words
The process of claim 1 wherein said halogen contaminants comprise bromides.
Claim 4
Dependent Claim 19 words
The process of claim 1 wherein said monocarboxylic acid stream comprises acetic acid and said halogen contaminants comprise iodides.
Claim 5
Dependent Claim 45 words
The process of claim 1 wherein the monocarboxylic acid stream comprises acetic or propionic acid produced by the reaction of an alcohol or olefin and carbon monoxide in the presence of a catalyst system of a Group VIII noble metal component and a halogen component.
Claim 6
Dependent Claim 39 words
The process of claim 1 wherein the monocarboxylic acid stream comprises acetic acid produced by the reaction of methanol and carbon monoxide in the presence of a catalyst system of a Group VIII noble metal component and an iodide.
Claim 7
Dependent Claim 27 words
The process of claim 1 wherein a portion of stream (d) is recycled to said first distillation zone below the point at which stream (d) is removed.
Claim 8
Dependent Claim 29 words
The process of claim 1 wherein the product monocarboxylic acid stream is removed in vapor form from above the liquid level in the bottom of said second distillation zone.
Claim 9
Dependent Claim 21 words
The process of claim 1 wherein the product monocarboxylic acid stream is removed from the bottoms of said second distillation zone.
Claim 10
Dependent Claim 20 words
The process of claim 1 wherein said first distillation zone comprises a distillation column having from 2 to 25 trays.
Claim 11
Dependent Claim 20 words
The process of claim 1 wherein said second distillation zone comprises a distillation column having from 10 to 90 trays.
Claim 12
Dependent Claim 30 words
The process of claim 1 wherein the first and second distillation zones are maintained at pressures of from atmospheric to 100 psig and at temperatures of from 100* to 165*C.
Claim 13
Dependent Claim 45 words
The process of claim 1 wherein the proportion of the total feed stream (a) to said first distillation zone which is removed from said zone as overhead fraction (b) and middle stream (d) is from 80 to 99.5 weight percent of said total feed stream.
Claim 14
Dependent Claim 41 words
The process of claim 1 wherein the proportion of the total feed stream (a) to said first distillation zone which is removed from said zone as bottoms stream (c) is from 0.5 to 6 weight percent of said total feed stream.
Claim 15
Dependent Claim 39 words
The process of claim 1 wherein the proportion of the feed stream (d) to said second distillation zone which is removed from said zone as middle stream (f) is from one to eight weight percent of said feed stream.
Claim 16
Dependent Claim 26 words
The process of claim 1 wherein overhead fractions (b) and (e) and bottoms stream (c) are returned to the process for producing said monocarboxylic acid stream.

References Cited (Backward Citations)

US2384374A Cited
US2147306A Cited
US3084109A Cited
US3210271A Cited
US3490997A Cited
US3507755A Cited
US3518165A Cited
US3700566A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1976-10-29 1977-04-30 1977-10-30 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1980-10-29 1981-04-30 1981-10-30 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1984-10-29 1985-04-30 1985-10-30 $7700.00 Window Closed / Lapsed

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