US4508745A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Production of a mannan oligomer hydrolysate
Assignee: Mondelez International Inc
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Filing: 1982-12-30
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Granted: 1985-04-02
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Expires: 2002-12-30
Abstract
Abstract A method of hydrolyzing a coffee extraction residue material to produce a mannan oligomer solution having oligomers from DP 1 to DP 10 is disclosed. The coffee material, preferably spent grounds from a commercial percolation system, is hydrolyzed in a reactor in the presence of an acid catalyst. A tubular plug flow reactor is convenient, although any reactor providing for the relatively high temperature, short time reaction will suffice. Particular acid catalysts include sulphuric acid, phosphoric acid, acetic acid and carbon dioxide gas. Depending on the specific time, temperature and catalyst concentration selected, a mannan oligomer solution having any desired distribution of oligomers between DP 1 and DP 10 is produced.
Inventors
- 👤 Charles V. Fulger
- 👤 Howard D. Stahl
- 👤 Evan J. Turek
- 👤 Renee Bayha
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 22:29
CPC Classifications
C; C13; C13K; C13K13/00; A; A23; A23F; A23F5/00; A23F5/24; A23F5/26; A23F5/36; A23F5/40
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
188 words
A method of hydrolyzing a coffee extraction residue material to produce mannan oligomers from DP 1 to about DP 10 said coffee extraction residue material comprising coffee grounds that have been atmospherically extracted and then thermally hydrolyzed to remove most of the arabinogalactan therefrom, said method comprising: (a) slurrying the coffee extraction residue material in a liquid to between 5% and 60% by weight dry basis, residue material; (b) adding an acid catalyst to the slurry in an amount sufficient to adjust the pH of said slurry to between pH 0.5 and pH 4; (c) feeding the slurry through a reactor at a temperature between 160° C. and 260° C. in from 6 seconds to 60 seconds at a pressure between 6 atmospheres and 35 atmospheres to hydrolyze the mannan; (d) discharging the slurry from the reactor through an orifice so that the pressure is rapidly reduced to atmospheric, quenching the hydrolysis reaction; (e) neutralizing the discharged slurry; and (f) separating hydrolyzed coffee extraction residue material from the mannan oligomers from DP 1 to about DP 10 to produce mannan oligomers of a purity in excess of 80%.
Claim 2
Independent Claim
188 words
A method of hydrolyzing a coffee extraction residue material to produce mannan oligomers from DP 1 to about DP 10 said coffee extraction residue material comprising coffee grounds that have been atmospherically extracted and then thermally hydrolyzed to remove most of the arabinogalactan therefrom, said method comprising: (a) slurrying the coffee extraction residue material in a liquid to between 5% and 60% by weight dry basis, residue material; (b) adding an acid catalyst to the slurry in an amount sufficient to adjust the pH of said slurry to between pH 0.5 and pH 4; (c) feeding the slurry through a reactor at a temperature between 160° C. and 260° C. in from 6 seconds to 60 seconds at a pressure between 6 atmospheres and 35 atmospheres to hydrolyze the mannan; (d) discharging the slurry from the reactor through an orifice so that the pressure is rapidly reduced to atmospheric, quenching the hydrolysis reaction; (e) neutralizing the discharged slurry; and (f) separating hydrolyzed coffee extraction residue material from the mannan oligomers from DP 1 to about DP 10 to produce mannan oligomers of a purity in excess of 80%.
Claim 3
Dependent Claim
32 words
A method as in claim 1 wherein the slurry is between about 5% and 20% by weight dry basis, residue material and the reactor of 1(c) is a plug flow tubular reactor.
Claim 4
Dependent Claim
30 words
A method as in claim 2 wherein the mannan oligomers from DP 1 to about DP 10 are separated from the hydrolyzed coffee extraction residue material as an aqueous solution.
Claim 5
Dependent Claim
40 words
A method as in claim 3 wherein the acid catalyst is selected from the group consisting of sulphuric acid, phosphuric acid, nitric acid, hydrochloric acid, acetic acid, citric acid, tartaric acid, malic acid, adipic acid, fumaric acid and combinations thereof.
Claim 6
Dependent Claim
22 words
A method as in claim 4 wherein the temperature in the plug flow tubular reactor is from 190° C. to 220° C.
Claim 7
Dependent Claim
14 words
A method as in claim 1 wherein the reactor of 1(c) is an extruder.
Claim 8
Dependent Claim
28 words
A method as in claim 1 wherein sulphuric acid is added to the slurry at between 0.05% and 0.5% by weight of said slurry as the acid catalyst.
Claim 9
Independent Claim
170 words
A method of hydrolyzing a coffee extraction residue material to produce mannan oligomers from DP 1 to about DP 10 said coffee extraction residue material comprising coffee grounds that have been atmospherically extracted and then thermally hydrolyzed to remove most of the arabinogalactan therefrom, said method comprising: (a) slurrying the coffee extraction residue material in a liquid to between 5% and 60% by weight dry basis, residue material; (b) reacting the slurry in a reactor at a temperature between 160° C. and 260° C. for from 6 seconds to 60 seconds while simultaneously injecting carbon dioxide into the reactor as an acid catalyst so that the pH is less than about pH 4; (d) discharging the slurry from the reactor through an orifice so that the pressure is rapidly reduced to atmospheric, rapidly quenching the hydrolysis reaction; and (e) separating hydrolyzed coffee extraction residue material from the mannan oligomer solution having oligomers from DP 1 to about DP 10 to produce mannan oligomers of a purity in excess of 80%.
Claim 10
Independent Claim
170 words
A method of hydrolyzing a coffee extraction residue material to produce mannan oligomers from DP 1 to about DP 10 said coffee extraction residue material comprising coffee grounds that have been atmospherically extracted and then thermally hydrolyzed to remove most of the arabinogalactan therefrom, said method comprising: (a) slurrying the coffee extraction residue material in a liquid to between 5% and 60% by weight dry basis, residue material; (b) reacting the slurry in a reactor at a temperature between 160° C. and 260° C. for from 6 seconds to 60 seconds while simultaneously injecting carbon dioxide into the reactor as an acid catalyst so that the pH is less than about pH 4; (d) discharging the slurry from the reactor through an orifice so that the pressure is rapidly reduced to atmospheric, rapidly quenching the hydrolysis reaction; and (e) separating hydrolyzed coffee extraction residue material from the mannan oligomer solution having oligomers from DP 1 to about DP 10 to produce mannan oligomers of a purity in excess of 80%.
Claim 11
Dependent Claim
31 words
A method as in claim 8 wherein the slurry is between 5% and 20% by weight dry basis, residue material and the reactor of 9(b) is a plug flow tubular reactor.
Claim 12
Dependent Claim
14 words
A method as in claim 8 wherein the reactor of 9(b) is an extruder.
Claim 13
Dependent Claim
19 words
A method as in claim 1 or 9 wherein the liquid from which the slurry is made is water.
Claim 14
Dependent Claim
24 words
A method as in claim 3 or 9 which further comprises drying the mannan oligomer solution having oligomers from DP 1 to DP 10.
Claim 15
Dependent Claim
19 words
A method as in claim 12 which further comprises combining the dried mannan oligomer solution with a soluble coffee.
Claim 16
Dependent Claim
33 words
A method as in claim 3 or 9 which further comprises combining the mannan oligomer solution having oligomers from DP 1 to DP 10 with a conventional coffee extract and drying said combination.
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) | 1988-04-01 | 1988-10-01 | 1989-04-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-04-01 | 1992-10-01 | 1993-04-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-04-01 | 1996-10-01 | 1997-04-02 | $7700.00 | Window Closed / Lapsed |