Method for producing allulose crystals
Allulose crystals are efficiently produced from an allulose syrup using seed crystals.
1 . A method for producing allulose crystals, wherein the method comprises:
a) evaporating a feed allulose syrup at a first sub-ambient pressure and a first temperature to produce a first supersaturated allulose syrup having an allulose syrup target saturation;
b) introducing seed crystals to the first supersaturated allulose syrup and allowing the allulose to crystallize to produce a first massecuite comprising first allulose crystals and a first supersaturated mother liquor having a first target mother liquor saturation higher than the allulose syrup target saturation;
c) evaporating the first massecuite at the first sub-ambient pressure and the first temperature to produce a second massecuite comprising second allulose crystals and a second supersaturated mother liquor having a second mother liquor target saturation lower than the first mother liquor target saturation;
d) increasing the first sub-ambient pressure to a second sub-ambient pressure and cooling the second massecuite to a second temperature to produce a third massecuite comprising third allulose crystals and a third supersaturated mother liquor having a third mother liquor target saturation;
e) holding the third massecuite at the second sub-ambient pressure and the second temperature for a period of time to produce a fourth massecuite comprising fourth allulose crystals and a fourth mother liquor having a fourth target mother liquor saturation;
f) increasing the pressure to ambient and cooling the fourth massecuite to a third temperature at a cooling rate to produce a fifth massecuite comprising fifth allulose crystals and a fifth supersaturated mother liquor having a fifth target mother liquor saturation;
g) allowing the fifth massecuite to crystallize for a crystallization time to produce a product massecuite comprising product allulose crystals at a target yield and a product mother liquor, the product mother liquor having a target product mother liquor supersaturation; and
h) separating the product allulose crystals from the product supersaturated mother liquor to provide the product allulose crystals at the target yield, wherein temperatures for the evaporating and cooling are effectively controlled to reliably obtain the target yield.
2 . The method of claim 1 , wherein the target yield of the product allulose crystals is 40% or more of the feed allulose syrup.
3 . The method of claim 1 , wherein the feed allulose syrup has a total dry solids content of from 50% to 80% by weight.
4 . The method of claim 1 , wherein the allulose in the feed allulose syrup is at least 80% pure on a dry solids basis by weight.
5 . The method of claim 1 , wherein the pH of the feed allulose syrup is from 2.5 to 6.0.
6 . The method of claim 1 , wherein the feed allulose syrup is at least 95% pure on a dry solids basis by weight.
7 . The method of claim 1 , wherein the feed allulose syrup is at least 98% pure on a dry solids basis by weight.
8 . The method of claim 1 , wherein the seed crystals comprise from 0.0001% to 5% by weight of the feed allulose syrup.
9 . The method of claim 1 , wherein the seed crystals have an average particle size of 75 microns or less.
10 . The method of claim 1 , wherein the seed crystals have an average particle size of from 5 to 250 microns.
11 . The method of claim 1 , wherein the first temperature is from 35 to 50° C.
12 . The method of claim 1 , wherein the first target mother liquor saturation is from 1.10 to 1.15.
13 . The method of claim 1 , wherein the first supersaturated mother liquor comprises from 85-90 wt % allulose on a dry solids basis.
14 . The method of claim 1 , wherein the second temperature is from 22 to 35° C.
15 . The method of claim 1 , wherein the second target mother liquor saturation is 1.05 supersaturated or less.
16 . The method of claim 1 , wherein the second supersaturated mother liquor comprises from 80 to 95 wt % allulose on a dry solids basis.
17 . The method of claim 1 , wherein the third temperature is from 20 to 25° C.
18 . The method of claim 1 , wherein the fourth target mother liquor saturation is from 1.1 to 1.2 supersaturated.
19 . The method of claim 1 , wherein the fifth target mother liquor saturation is from 1.05 to 1.2 supersaturated.
20 . The method of claim 1 , wherein the separating is carried out at least in part by one or more physical separation methods selected from the group consisting of centrifugation, filtration, decantation, membrane separation and combinations of distinct separation methods thereof.
21 . The method of claim 1 , wherein the product allulose crystals separated from the product mother liquor are further subjected to i) washing with at least one of water, an organic solvent, a blend of organic solvents, a blend of water and organic solvent(s) or an aqueous solution containing at least one carbohydrate; ii) drying; or a combination thereof.
22 . Product allulose crystals, obtained in accordance with the method of claim 1 .
23 . A consumable product, comprising the product allulose crystals in accordance with claim 1 and at least one additional ingredient other than allulose crystals.
24 . A method of making a consumable product, comprising combining the product allulose crystals prepared in accordance with claim 1 and at least one additional ingredient other than the product allulose crystals.
25 . A mother liquor, comprising the product supersaturated mother liquor obtained in accordance with the method of claim 1 .
26 . A mother liquor, comprising the product supersaturated mother liquor obtained in accordance with the method of claim 1 , wherein the mother liquor is suitable for use as a product consumable by humans or animals or as an ingredient in a formulated product consumable by humans or animals.