Method for producing D-allulose crystals

Patent metadata

Field	Value
Publication number	US-12534491-B2
Application number	US-202418593522-A
Country	US
Kind code	B2
Filing date	Mar 1, 2024
Priority date	Jan 5, 2017
Publication date	Jan 27, 2026
Grant date	Jan 27, 2026

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 . D-allulose crystals having a volume mean size D4,3 of greater than 200 μm, the crystals having, for a given volume particle size D4,3 present in a range of from 200 to 400 μm, a Feret min/Feret max diameter ratio of greater than 0.60.

2 . D-Allulose crystals according to claim 1 , having a volume mean size D4,3 ranging from 210 to 800 μm.

3 . D-Allulose crystals according to claim 2 , having a volume mean size D4,3 ranging from 220 to 350 μm.

4 . D-Allulose crystals according to claim 2 , having a Feret min/Feret max diameter ratio ranging from 0.62 to 0.90.

5 . D-Allulose crystals according to 2, having a Feret min/Feret max diameter ratio ranging 0.63 to 0.80.

6 . D-allulose crystals according to claim 1 , having, for all the volume particle size D4,3 in the range of from 200 to 400 μm, a Feret min/Feret max diameter ratio of greater than 0.60.

7 . D-allulose crystals according to claim 6 , having a mass content of D-allulose greater than or equal to 99.00%.

8 . D-allulose crystals according to claim 6 , having a mass content of D-allulose greater than or equal to 99.50%.

9 . D-allulose crystals according to claim 6 , having a mass content of D-allulose greater than or equal to 99.70%.

10 . D-allulose crystals according to claim 1 , which are non-agglomerated as determined by observation by optical microscopy.

11 . A process for producing D-allulose crystals according to claim 1 , comprising:
a step of providing a composition rich in D-allulose; a step of concentrating said composition 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; and at least one nanofiltration step, said step taking place in a step prior to the step of concentrating the composition rich in D-allulose.

12 . The Process according to claim 11 , wherein the nanofiltration step is carried out with a membrane having a cut-off threshold of less than 300 Da.

13 . The Process according to claim 11 , wherein the nanofiltration step is carried out with a membrane having a cut-off threshold ranging from 150 to 250 Da.

14 . The Process according to claim 11 , 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.

15 . The Process according to claim 11 , wherein the stock solution obtained comprises by dry mass:
from 85% to 98% of D-allulose; from 0.5% to 15% of D-fructose; from 0% to 5% of glucose; from 0.4% to 1.1% of D-allulose dimers.

16 . The Process according to claim 11 , wherein a volume concentration factor of the nanofiltration ranges from 5 to 20.

17 . The Process according to claim 11 , 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.

18 . The Process according to claim 17 , adiabatic evaporative cooling stage is carried out at a temperature ranging from 30 to 40° C.

19 . The Process according to claim 11 , wherein the step of providing the stock solution of D-allulose comprises:
a step of providing a composition rich in D-allulose; a step of nanofiltration of said composition rich in D-allulose so as to provide a retentate and a permeate; a step of recovering the nanofiltration permeate; a step of concentrating this permeate so as to provide the stock solution of D-allulose.

20 . A process of preparation of a food or pharmaceutical product comprising including the D-allulose crystals of claim 1 in the preparation.

21 . The process according to claim 20 , wherein the D-allulose crystals are used as a sweetener agent.

22 . The process according to claim 21 , wherein the sweetener agent is an alternative sweetener to sucrose.

23 . The process according to claim 21 , wherein the sweetener agent is an alternative sweetener to table sugar.

24 . A process of preparation of any of chewing gums in the form of sticks or dragees, candies and tablets to be sucked, biscuits, cookies, muffins, cakes, gelatin-based cakes, chewing pastes, icings, or of powdered drinks comprising including the D-allulose crystals of claim 1 in the preparation.

25 . A food or pharmaceutical product comprising the D-allulose crystals of claim 1 .

26 . The food or pharmaceutical product of claim 25 , wherein the product is selected from allulose sweetener, chewing gums in the form of sticks or dragees, candies and tablets to be sucked, biscuits, cookies, muffins, cakes, gelatin-based cakes, chewing pastes, icings, and powdered drinks.

Assignees

• Roquette Freres

Inventors

• Boit Baptiste
• Lacroix Geoffrey
• Rossi Laurent

Classifications

• B01D2311/2676

  Centrifugal separation · CPC title

• B01D2311/04

  Specific process operations in the feed stream; Feed pretreatment · CPC title

• C07H1/06

  Separation; Purification · CPC title

• B01D61/04

  Feed pretreatment · CPC title

• B01D61/027

  Nanofiltration · CPC title