Method for producing D-allulose crystals

Patent metadata

Field	Value
Publication number	US-11945835-B2
Application number	US-201816471753-A
Country	US
Kind code	B2
Filing date	Jan 5, 2018
Priority date	Jan 5, 2017
Publication date	Apr 2, 2024
Grant date	Apr 2, 2024

Abstract

A new method for producing D-allulose crystals that allows for a continuous production process and ensures a high yield. Also, new D-allulose crystals. Further, the use of a nanofiltration unit in a method for producing D-allulose crystals to improve the yield and/or quality of the resulting crystals.

First claim

The invention claimed is:

1. Process for producing D-allulose crystals comprising:
a step of providing a composition rich in D-allulose;
at least one nanofiltration step of said composition rich in D-allulose so as to provide a retentate and a permeate, said nanofiltration step being performed with a membrane having a cut-off threshold of less than 300 Da;
a step of recovering the nanofiltration permeate;
a step of concentrating said permeate so as to form a stock solution to be crystallized;
a step of crystallizing the stock solution so as to form D-allulose crystals and mother liquors.

2. Process according to claim 1 , wherein the stock solution obtained comprises by dry mass:
from 80% to 99% of D-allulose,
from 0% to 20% of D-fructose,
from 0% to 10% of glucose,
from 0% to 1.5% of D-allulose dimers.

3. Process according to claim 1 , wherein the volume concentration factor of the nanofiltration ranges from 5 to 20.

4. Process according to claim 1 , wherein the crystallizing step comprises:
i. an adiabatic evaporative cooling stage, carried out in an adiabatic crystallizer-evaporator under vacuum so as to form a massecuite,
ii. followed by a stage of crystallization by cooling of said massecuite so as to form crystals.

5. Process according to claim 4 , wherein the temperature during the adiabatic evaporative cooling stage ranges from 30 to 40° C.

6. Process according to claim 1 , wherein it is continuous.

7. Process according to claim 1 , wherein it comprises at least one recycling step.

8. Process according to claim 1 , wherein it comprises a step of recycling at least one part of the mother liquors.

9. Process according to claim 1 , wherein it comprises a step of recycling at least one part of the retentate.

10. Process according to claim 1 , wherein the step of providing the composition rich in D-allulose comprises:
a step of providing a composition comprising D-fructose;
an epimerizing step so as to form a composition comprising D-fructose and D-allulose;
a chromatography step so as to provide a composition rich in D-allulose and a composition rich in D-fructose.

11. Process according to claim 10 , wherein it comprises a step of recycling at least one part of the composition rich in D-fructose.

12. Process according to claim 11 , wherein the degree of recycling of the composition rich in D-fructose ranges from 50% to 95%.

13. D-allulose crystals comprising a mass content of D-allulose dimer, determined by gas chromatography (GC), of less than 0.50%, and having a volume mean size D4,3 of greater than 200 μm, and for a given volume particle size D4,3 chosen in the range of from 200 to 400 μm, a Feret min/Feret max ratio greater than 0.60.

14. D-allulose crystals according to claim 13 , wherein they comprise a mass content of D-allulose dimer ranging from 0.01% to 0.48%.

15. D-allulose crystals according to claim 13 , wherein they have this Feret min/Feret max ratio over all of the volume particle sizes D4,3 in the range of from 200 to 400 μm.

Assignees

• Roquette Freres

Inventors

• Boit Baptiste
• Lacroix Geoffrey
• Rossi Laurent

Classifications

• C07H3/02 Primary

  Monosaccharides · CPC title

• A23L27/33 Primary

  containing sugars or derivatives · CPC title

• B01D61/027

  Nanofiltration · CPC title

• B01D61/04

  Feed pretreatment · CPC title

• C07H1/06

  Separation; Purification · CPC title