US4366060A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process and equipment for chromatographic separation of fructose/dextrose solutions
Assignee: Staley Continental Inc
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Filing: 1978-12-26
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Granted: 1982-12-28
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Expires: 1998-12-26
Abstract
Abstract Large-scale apparatus and process for chromatographic separation of fructose/dextrose sugar solutions employing large diameter beds of a strongly cationic salt of an ion exchange resin. The cationic ion exchange resin is densely and uniformly packed in a separation column by means of a resin loading method which includes washing the resin with a salt selected from the group of calcium, barium, strontium or silver salts of the resin. The shrunken resin is then placed in the column to completely fill the column. After sealing the column, excess salt is washed away to thereby expand the resin inside the confined separation column chamber. The uniformly dense packing of the resin in the separation column chamber eliminates the need for mechanical baffles which were formerly required to insure regular and uniform flow throughout the entire cross sectional area of the separation columns. Large diameter separation columns without baffles are made possible by the column packing method of the invention because undesirable channeling or irregular flow in the densely packed resin bed is virtually eliminated. A liquid feed stream containing fructose and dextrose and a second stream of elution water are fed through a series of separation columns in alternate, cyclic pulses. The liquid streams are further redistributed between the successive columns of the series to further increase the degree of separation of the output stream into a portion rich in fructose, and another output stream rich in dextrose.
Inventors
- 👤 Roger S. Leiser
- 👤 Gin C. Liaw
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 04:34
CPC Classifications
B; B01; B01D; B01D15/00; B01D15/08; B01D15/10; B01D15/20; B01D15/206; B01D15/26; B01D15/36; B01D15/361; B01D15/362; C; C13; C13K; C13K3/00
Claims Analysis
Total Claims: 43
Claim 1
Independent Claim
221 words
In a chromatographic separation process wherein the chromatographic separation column is densely packed with an adsorbent to permit the separation of a fluid feed stream containing a mixture of substances into a plurality of streams richer in one or more of said substances by alternately passing said mixed fluid feed stream and an elution fluid stream through a chromatographic separation column to obtain an effluent stream in which the adsorbent has a selective affinity for one of said substances in said fluid feed stream so that portions of said effluent stream have higher concentrations of one of the substances, and thereafter separately collecting successive portions of the effluent stream having higher concentrations of at least one of the substances, the improvement which comprises: (a) selecting an adsorbent which will contract to a reduced volume when exposed to a concentrated solution of a selected reagent and swells to an expanded volume by removing the concentrated solution from said adsorbent; (b) confining the adsorbent in its contracted and reduced volume condition within the chromatographic separation column; and (c) thereafter removing a sufficient amount of the concentrated solution from the confined adsorbent to cause the adsorbent to swell so as to completely and uniformly pack the adsorbent throughout the column and thereby eliminate channeling within said column when said fluid stream is passed therethrough.
Claim 2
Dependent Claim
221 words
In a chromatographic separation process wherein the chromatographic separation column is densely packed with an adsorbent to permit the separation of a fluid feed stream containing a mixture of substances into a plurality of streams richer in one or more of said substances by alternately passing said mixed fluid feed stream and an elution fluid stream through a chromatographic separation column to obtain an effluent stream in which the adsorbent has a selective affinity for one of said substances in said fluid feed stream so that portions of said effluent stream have higher concentrations of one of the substances, and thereafter separately collecting successive portions of the effluent stream having higher concentrations of at least one of the substances, the improvement which comprises: (a) selecting an adsorbent which will contract to a reduced volume when exposed to a concentrated solution of a selected reagent and swells to an expanded volume by removing the concentrated solution from said adsorbent; (b) confining the adsorbent in its contracted and reduced volume condition within the chromatographic separation column; and (c) thereafter removing a sufficient amount of the concentrated solution from the confined adsorbent to cause the adsorbent to swell so as to completely and uniformly pack the adsorbent throughout the column and thereby eliminate channeling within said column when said fluid stream is passed therethrough.
Claim 3
Dependent Claim
17 words
The method of claim 1 in which the column chamber is at least seven feet in height.
Claim 4
Dependent Claim
26 words
The method of claim 1 in which the mixed substances to be separated include monosaccharides, and at least one of the fluid streams is a liquid.
Claim 5
Dependent Claim
26 words
The method of claim 3 in which the substances to be separated include fructose and dextrose, and the mixed fluid feed stream is an aqueous solution.
Claim 6
Dependent Claim
17 words
The method of claim 4 in which the adsorbent is a crosslinked, nuclearly sulfonated polystyrene cationic resin.
Claim 7
Dependent Claim
14 words
The method of claim 5 in which the resin is crosslinked with 3-8% divinylbenzene.
Claim 8
Dependent Claim
20 words
The method of claim 6 in which the initial particle size of the resin is from 200-500 microns (30-50 mesh).
Claim 9
Dependent Claim
27 words
The method of claim 7 in which the cation bound to the resin is selected from the group consisting of alkali metals, alkaline earth metals, and silver.
Claim 10
Dependent Claim
24 words
The method of claim 8 in which the cation of the resin is selected from the group consisting of calcium, barium, strontium and silver.
Claim 11
Dependent Claim
30 words
The method of claim 8 in which the cation in the concentrated salt solution employed to shrink the resin comprises the same cation as the cation bound to the resin.
Claim 12
Dependent Claim
23 words
The method of claim 10 in which the cation bound to the resin and the cation of the concentrated salt solution are calcium.
Claim 13
Dependent Claim
86 words
In an improved process for separating a plurality of saccharides from a solution by liquid chromatography, the steps comprising: (a) alternately passing a feed stream and an elution water stream through a large capacity separation column having a chamber therein containing a densely packed bed of a crosslinked nuclearly sulfonated polystyrene resin in a cationic form, said resin having been packed in the chamber by the process of claim 1; and (b) separately collecting portions of the effluent streams having higher concentrations of the respective saccharides.
Claim 14
Dependent Claim
26 words
The process of claim 12 in which the cation of the resin is selected from the group consisting of alkali metals, alkaline earth metals, and silver.
Claim 15
Dependent Claim
24 words
The process of claim 13 in which the cation of the resin is selected from the group consisting of calcium, barium, strontium and silver.
Claim 16
Dependent Claim
35 words
The process of claim 12 in which the cation of the resin is calcium, and the concentrated selected reagent used to initially reduce the volume of the said resin contains 10-35% by weight calcium chloride.
Claim 17
Dependent Claim
56 words
The method of claim 15 in which the initial particle size of the resin is about 200-500 microns and the final void volume of the densely packed resin is about 10% less than the initial void volume of the resin when in the sodium salt form prior to contracting the resin with concentrated calcium chloride solution.
Claim 18
Dependent Claim
65 words
The method of claim 5 including the step of passing the mixed fluid feed stream through a series of at least three of said separation columns, and the feed stream contains about 42% fructose, 50% dextrose and 8% higher saccharides, and a portion of the effluent stream contains about 55-65% by weight fructose, 38-50% dextrose, and no more than about 8% by weight higher saccharides.
Claim 19
Dependent Claim
46 words
The method of claim 5 in which a portion of the initial effluent stream rich in fructose is recycled, and the effluent stream including said recycled portion is collected to obtain a product containing at least 90% fructose, about 5-10% dextrose and about 1-3% higher sugars.
Claim 20
Dependent Claim
26 words
The method of claim 5 in which the fluid flow rate through the separation column is about 0.3 to 2.0 gallons per minute per square foot.
Claim 21
Dependent Claim
16 words
The method of claim 18 in which the flow rate is about 0.4-0.7 gpm/ft. 2 .
Claim 22
Dependent Claim
22 words
The method of claim 5 in which the complete cycle of effluent stream collection, including product and by-product, is about 330 minutes.
Claim 23
Dependent Claim
261 words
In an improved method for separating a fluid feed stream containing a mixture of substances into a plurality of streams richer in one or more of said substances by alternately passing said mixed fluid feed stream and an elution fluid stream through a chromatographic separation column to obtain an effluent stream, said column having a chamber at least 6 to 30 feet wide, said chamber containing an adsorbent which has a selective affinity for one of said substances in said fluid feed stream so that portions of said effluent stream have a higher concentrations of one of the substances, and thereafter separately collecting successive portions of the effluent stream having higher concentration of at least one of the substances, the method including first densely packing the adsorbent in the chamber of said separation column, said chamber being devoid of any internal flow distributing structure, the steps comprising: (a) selecting an adsorbent which contracts to a reduced volume condition in the presence of a selected reagent, and which swells when the excess concentrated reagent is removed; (b) disposing said adsorbent in said separation column chamber in its reduced volume condition; (c) effectively confining said adsorbent in said chamber of the separation column; and (d) thereafter removing the excess of said concentrated reagent from said confined adsorbent, whereby said adsorbent is caused to swell to completely and uniformly pack the adsorbent throughout the separation column chamber to eliminate channeling and turbulent flow, and to improve the uniformity of the cross-sectional flow rate across the column chamber when a fluid stream is passed therethrough.
Claim 24
Dependent Claim
261 words
In an improved method for separating a fluid feed stream containing a mixture of substances into a plurality of streams richer in one or more of said substances by alternately passing said mixed fluid feed stream and an elution fluid stream through a chromatographic separation column to obtain an effluent stream, said column having a chamber at least 6 to 30 feet wide, said chamber containing an adsorbent which has a selective affinity for one of said substances in said fluid feed stream so that portions of said effluent stream have a higher concentrations of one of the substances, and thereafter separately collecting successive portions of the effluent stream having higher concentration of at least one of the substances, the method including first densely packing the adsorbent in the chamber of said separation column, said chamber being devoid of any internal flow distributing structure, the steps comprising: (a) selecting an adsorbent which contracts to a reduced volume condition in the presence of a selected reagent, and which swells when the excess concentrated reagent is removed; (b) disposing said adsorbent in said separation column chamber in its reduced volume condition; (c) effectively confining said adsorbent in said chamber of the separation column; and (d) thereafter removing the excess of said concentrated reagent from said confined adsorbent, whereby said adsorbent is caused to swell to completely and uniformly pack the adsorbent throughout the separation column chamber to eliminate channeling and turbulent flow, and to improve the uniformity of the cross-sectional flow rate across the column chamber when a fluid stream is passed therethrough.
Claim 25
Dependent Claim
31 words
The method according to claim 22 in which the feed stream containing a mixture of saccharide to be separated include monosaccharides, and at least one of the fluid streams is liquid.
Claim 26
Dependent Claim
30 words
The method according to claim 23 in which the feed stream mixture substances to be separated include fructose and dextrose and the mixed fluid feed stream is an aqueous solution.
Claim 27
Dependent Claim
18 words
The method according to claim 24 in which the adsorbent is a crosslinked, nuclearly sulfonated polystyrene cationic resin.
Claim 28
Dependent Claim
15 words
The method according to claim 25 in which the resin is crosslinked with 3-8% divinylbenzene.
Claim 29
Dependent Claim
21 words
The method according to claim 26 in which the initial particle size of the resin is from 200-500 microns (30-50 mesh).
Claim 30
Dependent Claim
28 words
The method according to claim 27 in which the cation bound to the resin is selected from the group consisting of alkali metals, alkaline earth metals, and silver.
Claim 31
Dependent Claim
25 words
The method according to claim 28 in which the cation of the resin is selected from the group consisting of calcium, barium, strontium and silver.
Claim 32
Dependent Claim
30 words
The method according to claim 28 in which the cation in concentrated salt solution employed to shrink the resin comprises the same cation as the cation bound to the resin.
Claim 33
Dependent Claim
24 words
The method according to claim 30 in which the cation bound to the resin and the cation of the concentrated salt solution are calcium.
Claim 34
Dependent Claim
87 words
The method of claim 22 for separating a plurality of saccharides from a solution by liquid chromatography the steps comprising: (a) alternately passing a feed stream and an elution water stream through a large capacity separation column, having a chamber therein containing a densely packed bed of a crosslinked nuclearly sulfonated polystyrene resin in a cationic form, said resin having been packed in the chamber by the method of claim 22; and (b) separately collecting portions of the effluent streams having higher concentrations of the respective saccharides.
Claim 35
Dependent Claim
27 words
The method according to claim 32 in which the cation of the resin is selected from the group consisting of alkali metals, alkaline earth metals, and silver.
Claim 36
Dependent Claim
25 words
The method according to claim 33 in which the cation of the resin is selected from the group consisting of calcium, barium, strontium and silver.
Claim 37
Dependent Claim
35 words
The method according to claim 32 in which the cation of the resin is calcium, and the concentrated selected reagent used to initially reduce the volume of said resin contains 10-35% by weight calcium chloride.
Claim 38
Dependent Claim
54 words
The method according to claim 35 in which the initial particle size of the resin is 200-500 microns and the final void volume of the densely packed resin is less than the initial void volume of the resin when in the sodium salt form prior to contacting the resin with concentrated calcium chloride solution.
Claim 39
Dependent Claim
61 words
The method according to claim 25 in which at least three of said separation columns are disposed in series, and the feed stream containing about 42% fructose, 50% dextrose and 8% higher saccharides, and the effluent stream is collected to yield a product containing about 55-65% by weight fructose, 38-50% dextrose, and no more than about 8% by weight higher saccharides.
Claim 40
Dependent Claim
47 words
The method according to claim 25 in which a portion of the initial effluent stream rich in fructose is recycled, and the effluent stream including said recycled portion is collected to obtain a product containing at least 90% fructose, about 5-10% dextrose and about 1-3% higher sugars.
Claim 41
Dependent Claim
29 words
The method according to claim 25 in which the fluid flow rate through the separation columns is at least about 0.3 to 2.0 gallons per minute per square foot.
Claim 42
Dependent Claim
22 words
The method according to claim 38 in which the flow rate is at least about 0.4-0.7 gallons per minute per square foot.
Claim 43
Dependent Claim
23 words
The method according to claim 25 in which the complete cycle of effluent stream collection, including product and by-product, is about 330 minutes.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-12-27 | 1986-06-28 | 1986-12-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-12-27 | 1990-06-28 | 1990-12-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-12-27 | 1994-06-28 | 1994-12-28 | $7700.00 | Window Closed / Lapsed |