Method for preparing D-psicose crystal

Patent metadata

Field	Value
Publication number	US-10246476-B2
Application number	US-201515520786-A
Country	US
Kind code	B2
Filing date	Aug 9, 2015
Priority date	Oct 20, 2014
Publication date	Apr 2, 2019
Grant date	Apr 2, 2019

Abstract

A method for producing high purity D-psicose crystals having a purity of 98% (w/w) or more and a grain size of MA200 or more. The method includes: removing impurities from a D-psicose solution to obtain a purified D-psicose solution; concentrating the purified D-psicose solution; cooling the concentrated D-psicose solution to 30° C. to 40° C. through a heat exchanger; seed crystallizing the D-psicose solution at 30° C. to 40° C. to obtain a seed crystallized massecuite; and full-scale crystallizing the seed crystallized massecuite. The method can produce pure D-psicose crystals in a suitable form for industrial application through an economical crystallization process from the D-psicose solution without using organic solvents.

First claim

What is claimed is:

1. A method for producing D-psicose crystals having a grain size of MA200 μm or larger, comprising:
removing impurities from a D-psicose solution to obtain a purified D-psicose solution;
concentrating the purified D-psicose solution to provide a concentrated D-psicose solution having a concentration of 80 Brix (%) to 85 Brix (%);
performing rapid cooling of the concentrated D-psicose solution to 30° C. to 40° C. in a heat exchanger to provide a copied D-psicose solution having a temperature between 3° C. and 4° C., wherein the rapid cooling is performed at a cooling rate of 5° C. to 20° C. per hour;
placing the cooled D-psicose solution at a temperature between 30° C. and 40° C. to a crystallizer and adding D-psicose seed crystals to the crystallizer;
performing seeded crystallization of D-psicose in the crystallizer while controlling temperature to stay between 30° C. and 40° C., which provides a D-psicose massecuite having a temperature between 30° C. and 40° C.; and
performing full-scale crystallization of D-psicose using the D-psicose massecuite while controlling temperature to stay between 30° C. and 40° C., which provides D-psicose crystals having a grain size of MA200 μm or larger.

2. The method according to claim 1 , wherein the step of removing impurities from a D-psicose solution to obtain a purified D-psicose solution comprises:
decoloring the D-psicose solution by passing through a column packed with a decoloring agent;
desalting the decolored D-psicose solution via ion exchange resin chromatography; and
passing the desalted D-psicose solution through a continuous chromatography column packed with an ion exchange resin to which calcium activating groups are attached.

3. The method according to claim 2 , wherein the ion exchange resin used in the ion exchange resin chromatography is a 100% weak basic anion resin.

4. The method according to claim 2 , wherein the step of passing through a continuous chromatography column is a simulated moving bed (SMB) process.

5. The method according to claim 2 , wherein the D-psicose solution purified through the continuous chromatography column has a purity of 95% (w/w) or more.

6. The method for producing high purity D-psicose crystals according to claim 1 , wherein performing seeded crystallization comprises
adding seeds of D-psicose to the cooled D-psicose solution at a temperature between 30° C. and 40° C.; and
adding additional D-psicose solutions to the seeds-added D-psicose solution.

7. The method according to claim 6 , wherein the concentration of the additional D-psicose solutions is in a range of 80 Brix (%) to 85 Brix (%).

8. The method according to claim 6 , wherein the volume of the additional D-psicose solutions is in a range of 5 (v/v) % to 20 (v/v) % based on the volume of the seed-added D-psicose solution.

9. The method according to claim 1 , wherein the full-scale crystallization comprises:
adding another D-psicose solution having a purity of 95% (w/w) or higher and a concentration of 80 Brix (%) to 85 Brix (%) to the seed crystallized massecuite, and
subsequently, repeating heating and cooling the resulting solution within the range of 30° C. to 40° C.

10. The method according to claim 9 , wherein repeating heating and cooling the resulting solution comprises adding, to the resulting solution, an additional D-psicose solution at a temperature of 30° C. to 40° C. two times or more an interval of 10 hours to 20 hours.

11. The method according to claim 10 , wherein the additional D-psicose solution is added each time in an amount of 5 (v/v) % to 20 (v/v) % based on the volume of the resulting solution to which the additional D-psicose solution is added.

12. A method of crystallizing D-psicose, the method comprising:
concentrating a D-psicose solution to provide a concentrated D-psicose solution having a concentration of 80 Brix (%) to 85 Brix (%);
performing rapid cooling of the concentrated D-psicose solution to 30° C. to 40° C. to provide a cooled D-psicose solution having a temperature between 30° C. and 40° C., wherein the rapid cooling is performed by heat exchange at a cooling rate of 5° C. to 20° C. per hour;
placing, in a first crystallizer, the cooled D-psicose solution having a temperature between 30° C. and 40° C. and adding D-psicose crystal seeds to the first crystallizer;
performing seeded crystallization of D-psicose in the first crystallizer while controlling a temperature of the D-psicose solution in the first crystallizer to stay between 30° C. and 40° C., which provides a D-psicose massecuite;
placing the D-psicose massecuite to a second crystallizer and adding thereto a processed D-psicose solution to provide a crystallization mixture in the second crystallizer, wherein the processed D-psicose has a concentration between 80 Brix (%) and 85 Brix (%) and a temperature between 30° C. and 40°; and
performing crystallization of D-psicose in the second crystallizer while controlling a temperature of the crystallization mixture in the crystallizer to stay between 30° C. and 40° C., which provides D-psicose crystals having a grain size of MA200 μm or larger.

13. The method of claim 12 , wherein performing seeded crystallization in the first crystallizer comprises adding an additional D-psicose solution to the first crystallizer at least once, wherein the additional D-psicose solution is at a temperature between 30° C. and 40° C. when added.

14. The method of claim 12 , wherein performing crystallization in the second crystallizer comprises adding an additional D-psicose solution to the second crystallizer at least once, wherein the additional D-psicose solution is at a temperature between 30° C. and 40° C. when added.

Assignees

• Cj Cheiljedang Corp

Inventors

• Kim Seong Bo
• Park Seung Won
• An Jun Gap
• Lee Joo Hang

Classifications

• B01D9/0036

  Crystallisation on to a bed of product crystals; Seeding · CPC title

• B01D9/0013

  by indirect heat exchange · CPC title

• C07H3/02

  Monosaccharides · CPC title

• C07H1/06 Primary

  Separation; Purification · CPC title

• B01D15/363

  Anion-exchange · CPC title