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1. WO2004096821 - FORME CRISTALLINE AMELIOREE DE SUCRALOSE ET SON PROCEDE DE PRODUCTION

Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique

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CLAIMS:

1. A method of producing stable sucralose crystals from a sucralose solution, the method comprising:

introducing a feed stream of sucralose solution into a system;

causing sucralose crystals to form continuously in the system;

removing an output stream of sucralose solution including sucralose crystals from the system; and

continuously recirculating a part of the output stream to the system, and separating sucralose crystals from the remaining part of the output stream;

wherein the rates of introducing, removing, and recirculating are controlled so that sucralose passing through the system has, on
average, a residence time in the system of at least four hours; and

drying the separated sucralose crystals at a drying temperature of about 85°F or below.

2. The method of claim 1 wherein at least one of the steps of
introducing, recirculating, and removing is performed fully continuously.

3. The method of claim 1 wherein at least one of the steps of introducing and removing is performed intermittently.

4. The method of claim 1 wherein the step of introducing includes introducing at least one of the feed stream and the recirculated part of the output stream into the contents of the system tangentially to produce a swirling motion in the contents.

5. The method of claim 1 further comprising combining the feed stream and the recirculated part of the output stream prior to the step of introducing.

6. The method of claim 1 wherein the residence time is from about 6 hours to about 50 hours.

7. The method of claim 1 wherein the residence time is from about 12 hours to about 24 hours.

8. The method of claim 1 wherein the step of removing the output stream is performed at a rate to provide a turnover time of liquid in the system of from about 2 minutes to about 15 minutes.

9. The method of claim 1 wherein the step of removing the output stream is performed at a rate to provide a turnover time of liquid in the system of from about 4 minutes to about 8 minutes.

10. The method of claim 1 wherein the recirculating comprises subjecting the sucralose crystals to sufficient mechanical disturbance to fracture at least a portion thereof.

11. The method of claim 1 wherein sucralose crystals are caused to form by one of both removing water from the system and cooling the system.

12. The method of claim 1 wherein the step of controlling pressure and temperature comprises selecting the pressure and temperature to vaporize a portion of the water in the system, the method further comprising removing the vaporized water from the system.

13. The method of claim 12 wherein the pressure is between about 0.7 psi and 1.2 psi, and the temperature is between about 75°F and about 110°F.

14. The method of claim 1 wherein the step of controlling pressure and temperature comprises cooling the liquid in the system.

15. The method of claim 1 wherein the step of drying the sucralose crystals is performed at a temperature between about 50°F and about 70°F, and the separated crystals have a moisture content of from about 0.2 wt.% to about 10 wt.%.

16. The method of claim 1 further comprising, after the step of
separating sucralose crystals, drying the crystals at a temperature of about 60°F.

17. A composition comprising stable sucralose crystals, each of at least a portion of the sucralose crystals comprising a plurality of crystalline sucralose domains.

18. The composition of claim 17 having an angle of repose of less than 42 degrees.

19. The composition of claim 17 wherein each of the sucralose crystals has a crystal length, the crystal length being the longest dimension thereof, and a greatest crystal width measured at right angles to the crystal length, wherein the ratio of the crystal length to the greatest crystal width is on average less than 6.

20. The composition of claim 17 wherein each of the sucralose crystals has a crystal length thereof, the crystal length being the longest dimension, and a greatest crystal width measured at right angles to the crystal length, wherein the ratio of the crystal length to the greatest crystal width is on average less than 4.

21. The composition of claim 17 wherein 90 wt.% of the sample has a i particle size less than from about 30 μm to about 150 μm, and 10 wt.% has a particle size less than from about 3 μm to about 40 μm.

22. The composition of claim 17 wherein the sucralose crystals have a moisture content from about 0.2% to about 10%.

23. A composition comprising stable sucralose crystals, wherein the sucralose crystals are generally tapered.

24. The composition of claim 23 wherein each of the sucralose crystals has a crystal length, the crystal length being the longest dimension thereof, and a greatest crystal width measured at right angles to the crystal length, wherein the ratio of the crystal length to the greatest crystal width is on average less than 6.

25. The composition of claim 23 wherein each of the sucralose crystals has a crystal length, the crystal length being the longest dimension thereof, and a greatest crystal width measured at right angles to the crystal length, wherein the ratio of the crystal length to the greatest crystal width is on average less than 4.

26. The composition of claim 23 wherein 90 wt.% of the sample has a particle size less than from about 30 μm to about 150 μm, and 10 wt.% has a particle size less than from about 3 μm to about 40 μm.

27. The composition of claim 23 having an angle of repose of less than 42 degrees.

28. The composition of claim 23 wherein the sucralose crystals have a moisture content from about 0.2% to about 10%.

29. Stable sucralose crystals prepared by the method of claim 1.