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US4277635A Expired / Lapsed US ⏱️ 0.0 years remaining

Process of concentrating ethanol from dilute aqueous solutions thereof

Assignee: Iowa State University Research Foundation Inc
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Filing: 1980-06-24
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Granted: 1981-07-07
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Expires: 2000-06-24
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Abstract

Abstract Relatively dilute aqueous solutions of ethanol are concentrated by passage through a bed of a crystalline silica polymorph, such as silicalite, to adsorb the ethanol with residual dilute feed in contact with the bed, which is displaced by passing concentrated aqueous ethanol through the bed without displacing the adsorbed ethanol. A product concentrate is then obtained by removing the adsorbed ethanol from the bed together with at least a portion of the concentrated aqueous ethanol used as the displacer liquid. This process permits ethanol to be concentrated from dilute fermentation beers, which may contain from 6 to 10% ethanol, to obtain a concentrate product at very low energy cost having an ethanol concentration in excess of 95%, such as a concentration of from 98 to 99.5%.

Inventors

  • 👤 Charles S. Oulman
  • 👤 Colin D. Chriswell

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 01:44
CPC Classifications
C; C12; C12P; C12P7/00; C12P7/02; C12P7/04; C12P7/06; C07; C07C; C07C29/00; C07C29/74; C07C29/76; Y; Y02; Y02E; Y02E50/00; Y02E50/10

Claims Analysis

Total Claims: 13
Claim 1
Independent Claim 188 words
The process of concentrating ethanol from an aqueous solution thereof, comprising: (a) passing a relatively dilute liquid aqueous ethanol feed through a bed composed of graules of a crystalline silica polymorph capable of selectively adsorbing ethanol from an aqueous solution thereof, said feed having an ethanol concentration of less than 70% by weight. (b) discontinuing the passing of said feed through said bed when said granules have become loaded with adsorbed ethanol, said bed containing residual dilute aqueous ethanol feed; (c) passing a displacer liquid through said bed to displace said residual feed without displacing the adsorbed ethanol, said displacer liquid comprising aqueous ethanol containing at least 80% ethanol by weight; (d) continuing said passing of said displacer liquid through said bed until substantially all of said dilute ethanol feed has been displaced from said bed so that it contains said adsorbed ethanol together with said displacer liquid; and (e) thereafter removing said adsorbed ethanol from said bed together with at least a portion of displacer liquid and obtaining a concentrate product consisting of an admixture thereof which has an ethanol concentration of at least 80% by weight.
Claim 2
Dependent Claim 188 words
The process of concentrating ethanol from an aqueous solution thereof, comprising: (a) passing a relatively dilute liquid aqueous ethanol feed through a bed composed of graules of a crystalline silica polymorph capable of selectively adsorbing ethanol from an aqueous solution thereof, said feed having an ethanol concentration of less than 70% by weight. (b) discontinuing the passing of said feed through said bed when said granules have become loaded with adsorbed ethanol, said bed containing residual dilute aqueous ethanol feed; (c) passing a displacer liquid through said bed to displace said residual feed without displacing the adsorbed ethanol, said displacer liquid comprising aqueous ethanol containing at least 80% ethanol by weight; (d) continuing said passing of said displacer liquid through said bed until substantially all of said dilute ethanol feed has been displaced from said bed so that it contains said adsorbed ethanol together with said displacer liquid; and (e) thereafter removing said adsorbed ethanol from said bed together with at least a portion of displacer liquid and obtaining a concentrate product consisting of an admixture thereof which has an ethanol concentration of at least 80% by weight.
Claim 3
Dependent Claim 12 words
The method of claim 1 in which said silica polymorph is silicalite.
Claim 4
Dependent Claim 24 words
The method of claim 1 or claim 2 in which said ethanol feed has an ethanol concentration of from 1 to 15% by weight.
Claim 5
Dependent Claim 27 words
The method of claim 1 or claim 2 in which both said displacer liquid and concentrate product have an ethanol concentration of at least 95% by weight.
Claim 6
Dependent Claim 193 words
The process of concentrating ethanol from a dilute aqueous solution thereof, comprising: (a) passing a dilute liquid aqueous ethanol feed through a column containing a bed composed of granules of silicalite, said feed having an ethanol concentration of from 1 to 15% by weight; (b) discontinuing the passing of said feed through said bed when said granules have become loaded with adsorbed ethanol, said column and said bed therein containing residual dilute aqueous ethanol feed; (c) passing a displacer liquid through said column to displace said residual feed without displacing the adsorbed ethanol in said bed, said displacer liquid comprising aqueous ethanol having an ethanol concentration of at least 95% by weight; (d) continuing said passing of said displacer liquid through said column until substantially all of said dilute ethanol feed has been displaced from said bed and said column so that said bed contains absorbed ethanol together with said displacer liquid; and (e) thereafter removing said adsorbed ethanol from said bed together with at least a portion of said displacer liquid and obtaining a concentrate product consisting of an admixture thereof which has an ethanol concentration of at least 95% by weight.
Claim 7
Dependent Claim 193 words
The process of concentrating ethanol from a dilute aqueous solution thereof, comprising: (a) passing a dilute liquid aqueous ethanol feed through a column containing a bed composed of granules of silicalite, said feed having an ethanol concentration of from 1 to 15% by weight; (b) discontinuing the passing of said feed through said bed when said granules have become loaded with adsorbed ethanol, said column and said bed therein containing residual dilute aqueous ethanol feed; (c) passing a displacer liquid through said column to displace said residual feed without displacing the adsorbed ethanol in said bed, said displacer liquid comprising aqueous ethanol having an ethanol concentration of at least 95% by weight; (d) continuing said passing of said displacer liquid through said column until substantially all of said dilute ethanol feed has been displaced from said bed and said column so that said bed contains absorbed ethanol together with said displacer liquid; and (e) thereafter removing said adsorbed ethanol from said bed together with at least a portion of said displacer liquid and obtaining a concentrate product consisting of an admixture thereof which has an ethanol concentration of at least 95% by weight.
Claim 8
Dependent Claim 24 words
The process of claim 5 in which both said displacer liquid and concentrate product have an ethanol concentration of at least 98% by weight.
Claim 9
Dependent Claim 27 words
The process of claim 5 or claim 6 in which said displacer liquid is passed through said bed with substantially no intermixing thereof with said residual feed.
Claim 10
Dependent Claim 30 words
The method of claim 1 or claim 5 in which said adsorbed ethanol is removed by passing a carrier gas through said bed which is composed essentially of carbon dioxide.
Claim 11
Dependent Claim 32 words
The method of claim 1 or claim 5 in which water is passed through said bed following the removal of said ethanol therefrom to prepare said bed for further adsorption of ethanol.
Claim 12
Dependent Claim 51 words
The method of claim 1 or claim 5 in which said adsorbed ethanol is removed by passing a carrier gas through said bed composed essentially of carbon dioxide, and thereafter water is passed through said bed to remove retained carbon dioxide therefrom in preparing said bed for further adsorption of ethanol.
Claim 13
Dependent Claim 19 words
The process of claim 1 or claim 5 in which said displacer liquid is passed downwardly through said bed.

References Cited (Backward Citations)

US1985204A Cited
US1985205A Cited
US2619497A Cited
US2564717A Cited
US3485879A Cited
US4061724A Cited
US4073865A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-07-06 1985-01-05 1985-07-07 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-07-06 1989-01-05 1989-07-07 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-07-06 1993-01-05 1993-07-07 $7700.00 Window Closed / Lapsed

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