Chromatographic separation using ion-exchange resins

• US 5,221,478 A
• Filed: 09/09/1992
• Issued: 06/22/1993
• Est. Priority Date: 02/05/1988
• Status: Expired due to Term

• Current Assignee: The Dow Chemical Company (Dow, Inc.)
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Pynnonen, Bruce W., Dhingra, Yog R.
• Primary Examiner(s): Therkorn, Ernest G.
• Application Number:
  US07/942,484
• Time in Patent Office: 286 Days
• Field of Search: 210/635, 210/656, 210/659, 210/681, 210/198.2, 210/502.1, 127/46.2, 127/46.3
• US Class Current: 210/635
• CPC Class Codes: B01J 39/20 obtained by reactions only involving unsaturated carbon-to-carbon bonds
• CPC Class Codes: B01J 39/26 Cation exchangers for chromatographic processes
• CPC Class Codes: C13K 11/00 Fructose separation from invert sugar C13K3/00

Abstract

This invention is a process for the chromatographic separation of a fluid mixture in which the mixture is contacted with an ion-exchange resin, eluted through the resin under conditions such that the rate of passage of one component of the mixture through the resin bed is retarded relative to the rate of passage of a second component of the mixture, and a first product stream rich in said first component and a second product stream rich in said second component are recovered. The invention involves the use of an ion-exchange resin made from a copolymer which is prepared in a multi-stage polymerization process. The use of this resin is found to provide fast separation kinetics and increases the overall speed and efficiency of the separation. This invention is particularly suited for fructose/glucose separations in the preparation of high fructose corn syrup.

Claims

1. A process for the chromatographic separation of a fluid mixture which contains at least a first component and a second component into a recoverable stream rich in said first component and another recoverable stream rich in said second component, wherein at least one of said first and second components is a saccharide, comprising

(a) contacting said fluid mixture with a bed of an ion-exchange resin exhibiting an apparent cross-link density of at least about 1.1 times the actual cross-link density and having a water retention capacity, on a fully functionalized basis, of at least about 40 percent, said ion-exchange resin being prepared by functionalizing a gel-type copolymer, the gel-type copolymer being prepared in a multi-stage polymerization process employing seed copolymer particles,

(b) eluting said fluid mixture such that the fluid mixture passes through said resin bed under conditions such that the rate of passage of said first component through the resin bed is retarded relative to the rate of passage of said second component, and

(c) recovering a product stream rich in said first component and another product stream rich in said second component, the first component being recovered at a percent yield which is at least about 20% greater than the percent yield obtained when an ion-exchange resin made from a single step process having an equivalent average particle size and water retention capacity is employed in an otherwise similar process.

2. The process of claim 1 wherein said first component is an organic compound and said second component is an inorganic compound.

3. The process of claim 1 wherein said first component and second component in said fluid mixture are water-soluble or water-miscible organic compounds.

4. The process of claim 3 wherein said ion-exchange resin is a cation-exchange resin.

5. The process of claim 4 wherein said fluid mixture is eluted with water or a polar organic compound.

6. The process of claim 5 wherein said ion-exchange resin contains a plurality of sulfonic acid groups.

7. The process of claim 6 wherein said ion-exchange resin is prepared by functionalizing a gel-type copolymer which is made in a multi-stage polymerization process wherein mixtures of ethylenically unsaturated monomers are polymerized in successive polymerization stages, wherein in a last polymerization stage, a monomer mixture containing substantially no free radical initiator is added under polymerization conditions to a free radical-containing copolymer formed in one or more preceding polymerization stages, imbibed thereby and polymerized therein.

8. The process of claim 7 wherein the seed copolymer particles are prepared from a monomer mixture having about 0.05 to less than about 5 weight percent of a cross-linking monomer.

9. The process of claim 7 wherein said copolymer is a copolymer of styrene and divinylbenzene.

10. The process of claim 7 wherein said fluid mixture comprises at least two saccharides.

11. The process of claim 10 wherein said saccharides comprise fructose and glucose.

12. The process of claim 11 wherein said ion-exchange resin is in the calcium form.

13. The process of claim 12 wherein said ion-exchange resin has an average particle size of about 300-450 μ

m.

14. The process of claim 6 wherein said ion-exchange resin is prepared by functionalizing a copolymer made in a batch-seeded process.

15. The process of claim 14 wherein the seed copolymer particles are prepared from a monomer mixture having about 0.05 to about 5 weight percent of a cross-linking monomer.

16. The process of claim 6 wherein said ion-exchange resin is prepared by functionalizing a copolymer made by swelling the seed copolymer particles with a first monomer mixture, partially polymerizing the first monomer mixture, then cooling said partially polymerized particles below polymerization temperature, swelling said seed particles with a second monomer mixture, and then polymerizing said swollen seed particles.

17. The process of claim 16 wherein the seed copolymer particles are prepared from a monomer mixture having about 0.05 to less than about 5 weight percent of a cross-linking monomer.

18. In a process for the chromatographic separation of a fluid mixture, wherein said mixture is passed through an ion-exchange resin bed under conditions such that the rate of passage of a first component of said mixture is retarded relative to the rate of passage of at least a second component of said mixture, wherein at least one of said first and second components is a saccharide, the improvement comprising employing an ion-exchange resin which is characterized in that it is prepared by a multi-step polymerization process wherein seed copolymer particles are prepared from a monomer mixture containing about 0.05 to less than about 5 weight percent of a cross-linking monomer, the ion-exchange resin exhibiting an apparent cross-link density of at least about 1.1 times the actual cross-link level and a water retention capacity, on a fully functionalized basis, of at least about 40 percent, the first component capable of being recovered at a percent yield which is at least 20% greater than the percent yield obtained when an ion-exchange resin made from a single step process having an equivalent average particle size and water retention capacity is employed in an otherwise similar process.

19. The process of claim 18 wherein said first component and second component in said fluid mixture are water-soluble or water-miscible organic compounds.

20. The process of claim 19 wherein said ion-exchange resin is a cation-exchange resin.

21. The process of claim 20 wherein said fluid mixture is eluted with water or a polar organic compound.

22. The process of claim 21 wherein said ion-exchange resin contains a plurality of sulfonic acid groups and the resin has a dry weight capacity of at least about 4.5 meq/g.

23. The process of claim 22 wherein said fluid mixture comprises at least two saccharides.

24. The process of claim 23 wherein said saccharides comprise fructose and glucose.

25. The process of claim 24 wherein said ion-exchange resin is in the calcium form.

26. The process of claim 18 wherein said first component is an organic compound and said second component is an inorganic compound.