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    11548907-Allulose Crystals-23

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    USO11548907B2 ay United States Patent (10) Patent No. US 11,548,907 B2 Iyer et al. (45) Date of Patent: Jan, 10, 2023 (64) METHOD FOR PRODUCING ALLULOSE Soways 82 102011 Oba al CRYSTALS 8 leceta soaies6 BS Kine (71) Applicant: Tate & Lyte Ingredients Americas toa ae LLG, Holtman Estate, 1 (US) Boisoatons AL Fa01g Woodger st oigoaisess AL 02017 Kimcca (2 Inventors: Krishnan Viswanathan Iyer, Soigonries AL 120K Leet Champaign Ir (US) Sunes Gaddy, doisoate7s Al* "82019 Pak ann orca care rosy re Dc ‘Timothy Pobrte, Si. Charles, IL (US) ey, s01s00001 4 x to2zsoist (73), Assignce: “Tate & Lyle Solutions USA LLC, EP wo anaorasss onan Estates, IL (US) Ee Sno aL ra oszr7000 A (©) Notice: Subject any disclaimer the teem of this JP 2901206084 patent is extended or afjsted under 35 hy pone USC, 154) by 0 days wo zonitiboo4 Az 21) Appl. Nos 17036.995 Wo Dotaonasst ar ee “ Wo tenes? AL (22) Filed: Sep. 29, 2020 WO N6135458 AL 6) Prior Publication Data OTHER PUBLICATIONS, US 20210009619 AL Jan, 14, 2021 ‘ivan Ofie Actin with Souch Report for Tivan Appicaion No 10616, dtl i 23 2031, 9 ge. Related U.S. Application Data Intron Preliminary Rept on Pact fr lean (@) Divison of application No. 1634168, fed as Aton No RCEUSADT O88 sal Ap” 302518" application No. PCT/US2017/088753 on Oct. 27, [aterational Search Report and Writen Opinion for Intemational 2017, now abandoned. Appaton No DCTUSOI7OSN7SS: dod May” 20018 15 (60), Provisional pplication No 62/14.280, ladon Oct. PE ea pesos hry oft. Ap No, 1448.4 28,2016 ‘pri 2015 emis Sth or ProdiingAllose Cal” [epeaons Note of eas or Restn for pense Apion (1) neck NE"Toio.tbnik ded Nov 202 with alton, pase comm aa 2006.01) Innal Office Acon fr Aplction No, 29910, died A & A231. 2750 (o1601) 2a. peas conn Gooeor) Chines tise Action for Chinese Appleton No, 2179166740, 2 Us.cL eda Aug 1, 2002 wih slo, 19 pass. ‘ost Examination Repo for Aran Applicaton No, coe 07H 32 2013.01), 42312733 on 70224 pone, (201608) COT 106 2013015 CO7B etn tana Kept asian Aptian No, 2200713 (2013.01) 91531808 dated Now. 1022, 4 pe (68) Field of Classification Search CPC." COTE 302: COTE 106; A231. 27/38; COT * cited by examiner 220013 src 53612 Primary Examiner — YibHomg Shiao See application fle or complete search history (74) Attorney, Agen. oF Firm — RatwerPresti 66) References Cited “7 ABSTRACT US, PATENT DOCUMENTS SALLS80 A 11982 Edwards ‘$1995 ramos Allulose erysals are efficiently produced from an alllose syrup using seed erst. 25 Claims, 2 Dravsing Sheets U.S. Patent Jan, 10,2023 Sheet 1 of 2 US 11,548,907 B2 FIGURE 1 U.S. Patent Jan, 10,2023 Sheet 2 of 2 US 11,548,907 B2 FIGURE 2 US 11,548,907 B2 1 METHOD FOR PRODUCING ALLULOS CRYSTALS) ‘CROSS-REFERENCE TO RELATED APPLICATIONS, This isa Divisional Application of U.S. application Ser No, 16/341,688, filed Apr. 12, 2019, which is the US. National Phase of Intemational Application No PCT! US2017/058753, fled Oct. 27, 2017, which claims priity {0 United States Provisional Patent Application No, 6241 280, fled Oct. 28,2016, te disclosures ofeach of which are incorporate herein by reference herein in thie envicey for all purposes, FIELD OF THE INVENTION ‘The present invention relates tothe prodaction of crystals of allulose from syrups containing allulos. DISCUSSION OF THE RELATED ART ‘Many food and beverage products contain nutriive sweet feners such as sucrose (generally refered to a “sugar” or “able sugar), elvcone, Iritose, com syrup, high Irvcose com syrp and the like, Although desirable in tems of taste and functional properties, excess intake of mutitivesweel- feners, such as sucrose, hs long been associated with an Increase in diet-clatod health issues, such as obesity, heat disease, metabolic disorders snd dental problems. This wor ying trend has caused consumers to hecome increasingly aware ofthe importance of adopting a healthier lifestyle and rescing the level of nutritive sweeteners in thee diet. In veal years, there has heen # movement towards the development of replacements for nutritive sweeteners, with ‘particule fous da the development of low of zeno-caloric ‘woeteners. One proposed altemative to native sweoteners fs allulose (also Known as D-psicose). Alfulose is known “rare sigae, since t occurs inate in only very smal ‘amounts 3s about 70% as sweet as suerose, but provides ‘only around 5% of the calories of suerose (approximately 10.2 kealig). Ir may therefore essentially be considered tobe 18 “zero calorie’ sweetener. In view of is seacity in nature, production of allulose relies on the epimerization of readily available fructose. Ketow-3-epimerases ean interconvertfniciose and aluose, and various ketose-3-epimerases are known for carrying out this conversion. Such epimerization reactions ae typically conducted using an aqueous medium in whieh fructose is Initially dissolved, wherein the allulose-containing product ‘obtained aa result of the epimerization is inthe fray of ‘olution of allulse in water Purther processing and puri cation of the reaction product may be conducted in acc0e- dance in known procedures, whereby an allulose syrop containing alluse in eiely high concentration and purity is prxluced, Such allulose syrups ae capable of being used in ‘many consumable produes, including foods and heverszes, fs substitutes for conventional “sugar” syrups such as Blt ose syrups, high fructose com syrups and the like. For other applications, however it would be desirable to utilize allulose which isin “dry” foe-oming, erytalline orm, i. form generally resembling that of table sugar, Although some sempts to develop procedes for prodc= ing crystalline allulose have been reported (se, for example, US. Pat, No. 8,524,888 and WO 2016/064087) itis gene erally recognized that allulose is saccharide which is challenging to crystallize in 8 controlled, ficient way such 2 that crystals of suitable shape and size are reliably obtained in high yield. Therefore, improved erystalization methods for allulose sre still of great interes. SUMMARY OF THE INVENTION Various aspects ofthe present invention may be summa ized as follows Aspect I: A. method for produ wherein the method comprises: 2) cooling and agitating a fst admixture comprised of a first portion of allulose syrup and allulose seed erystals and initiating crystallization of alulose dissolved inthe allulose syrip thereby forming a fst massecite com: prising allulose crystals and a frst mother liquor con Taining esidoal dissolved allulose, the cooling and sgitating being continued until a first preselected target Yield of alllose crystals is achieved; optionally, separating the fist massecuite into frst portion (which may be subjected to further proces Sep, sch 38 separating te allulose erystals fom the other liquor portion and washing andlor drying the separated alllose enstals) and a second portion: ©) optionally, combining a second portion of allulose syrup ith the second portion ofthe fist massectite 10 form second admixtire: and 4) optionally, cooling and sgitating the second admixture ‘and initiating crystallization of lliose dissolved in the second portion of sllulose syrup, thereby forming a second massecuite comprising allulose rystals andl a fecond mother liquor conisining residual dissolved allulos, the cooling and agitating being continued until ‘8 sooond preselected target yield of allulose crystal i schieved In various embodiments of Aspect 1, a least steps) and by are performed, atleast steps a)-c) ane performed, or at Feast steps ad) ae performed Aspect 2: The method of Aspect 1, wherein the fist aalmixture is obtained by combining the first portion of allulose syrup and dry allulose crystals Aspoct 3: The method! of Aspect 1, wherein the fist ‘admixtures obtained by combining withthe frst ponion of alluose syrup and a heel comprised of allulose crystals and ‘mother liquor. Aspect 4: The method of any of Aspects 1-3, wherein the first admixture ai second admixture ae agitated in steps 3) and di sep ds performed, espoctvely using an agitator having a tip speed of 0.02 to 2 musec. Aspect 5 The method of any of Aspects 1-4, wherein stop 8) aditionally comprises, following initiation of erytall ‘ation of allulose dissolved in the alluose syrup, combining at Teast one additonal portion of alllose syrup withthe fist ‘aiture. Aspect 6; The method of any of Aspeets 1-5, wherein the cooling in step a) involves lowering the temperature of The fist admixture from within an initial temperature range 19 ‘within a scoond temperature range and holting the tempert- ture of the fist admixture within the second temperature range fora period of time. Aspeet 7: The method of any of Aspects 16, wherein step «is performed and the cooling in sep 4) involves lowering the temperature of the sevond admixture from within an initial temperature range to within a second temperature range and holding the temperature of the second admixture ‘within the second temperature range fora period of tim. ng allulose crystals, US 11,548,907 B2 3 Aspect 8: The method oF any of Aspects 1-7, wherein the allulose syrup has a dey solids content of 70% to 95% by ‘weight, 75% to 90% by weight, oF 80% to 85% by weight Aspect 9: The method of any of Aspects 1-8, wherein the lulose syrup tas an alllose purity ofa least 70%, atleast 75%, at Teast 80%, at least 85%, oF at Teast 90%. ‘Aspect 10: The method of any of Aspects 1-9, comprising ‘an additional step of separating allulose crystals from the first mother liquar inthe fist portion of the fist massecuite Aspect 11: The method of Aspect 10, wherein the sepa- rating is carried out atleast in part by one or more paysical ‘Separation methods selected from the group eonsinting of centrifugation iltation, docantation, membrane soparation fd combinations thereat. ‘Aspeet 12: The method of Aspect 10 of 11, wherein allulose eysals separated fiom the fist mother liquor are Subjected to) ashing with t last one of water sn organic Solveat, lend of organic solvents, a blend of water ad ‘onganic solven(s) or an aqueous solution comprised of at feast one carbohydrate (e., alllose) ii) drying: or a combination therof, ‘Aspect 13: The method of any of Aspects 1-12, wherein steps bjed) are performed and repeated at least one. ‘Aspect 14: A metbox! for producing allulose crystals, ‘wherein the method comprises: 4), passing a feed syrupireeyeled masseeuite admixture, comprised of i) 2 feed syrup, comprising water and dissolved allulose, andi a recycled massecuite co Prising allolose crystals and a revycled massocuite other liquor containing dissolved alllose, wherein te feed syrupireeycled massecviteadminture has been cooled to within @ frst eystaliztion temperature range, through a fist stage crystallization zone, while sgitating the fed syrupireeycled massecuite admix ‘ure, maintaining the feed syrupiecyeled massecuite admixture within the fist crystallization temperature range and initiating crystallization of allulose dissolved in the feed syrup and recycled massecuite mother Tiquor, thereby forming a first massecuite comprising alls erystls and a fest mother liguor conning residual dissolved alllose, and withdrawing the fist rmassecuite which has achieved first preselected lange, yield from the first stage crystallization zone: optionally, cooling the fist massecuite withdrawn from the fist stage erystaliztion ‘zone to within a second crystallization temperature range and tansfer- Fing the frst massecite 10 a second stage erystaliza- ©). optionally, passing the frst massecuite through the second stage crystallization zone while agitating the fist massecuite, maintaining the fst massocuite within the second crystallization temperature range and ini ating erystalization of lulose dissolved in the first mother liquor, thereby forming a second massecuite comprising allulose erystals anda second mother Higuor containing esidval dissolved allolose, and withdraw- ing the second massoctite which has achieved a second presclocted target yield from the sco stage erystal= lization zone; and <8 -opsionally. repeating steps band eat leat once yield ‘final massecute comprising allulose crystals and a Final mother Tiguoe. In various embodiments of Aspect 14, at lest steps.) and ) are performed, atleast steps a)-c) are performed, o at least steps a)-) ave performed, Aspoct 15: The method of Aspect 14, wherein steps a)-d) sre performed and comprising an additional step of sep 4 rating the allulose exystals in atleast portion of the final ‘massecuite from the final mother liquor Aspect 16: The method of Aspect 14 or 1S, whersn steps a) ae performed anda portion of the final massecuite is tse as the reeyeled massecite Aspect 17: The method of any of Aspects 14-16, wheecin the feed syruplreeycled massccuite admixture is obtained by ‘mixing in mixing vessel the feed syrup withthe cycled rassecvite comprised of allulose crystals and a rocyeled tmassecuite mother liquor containing dissolved alllose provide the fed syrupireeyeled massecuite admixture ad transferring the feed syruplrecyeled massecuite admixture fom the mixing vessel into the fist stage crystallization Aspect 18: The method of any of Aspects 14-17, wherein the fint admixture and second admixture are agitated in steps a)and cif step es performed, respectively using an agitator having a ip speed of 0.02 to 2 msec, Aspect 19: The method of any of Aspects 14-18, wherein the allulose syrup has. dry solids content of 70% 10 95% by weight, 75% to 90% by weight, oF 80% to 85% by weight Aspect 20: The method of any of Aspects 14-19, wherein the alulose syrup has an allulose purty ofa least 70%%, at Teast 75%, at Teast 80% atleast R5%, oF a east 90%, Aspoct 21: The method of Aspect 15, wherein the sepa rating is carried out atleast in part by one or more pasical ‘eparation methods selected from the group consisting of centrifugation ition, decantation, membrane separation land combinations theca. Aspect 22: The method of Aspect 15 or 21, wherein allolose crystals separated from the final mother fiquo subjected to i) washing with t last one of water, an organic solvent, blend of onganic solvents, a blend of water and ommanic solvent(s) or an aqueous solution comprised of at Feast one carbohydrate (e2 alllose); fi) drying; or a combination thereof. Aspect 23: The method of any of Aspects 14-22, wherein the feed synuplrecycled massecuite admixture is passe through the frst sage exystallization zone in a plug Bow ‘manner andor if steps b) and e) are performed, the fist ‘asocuite is parsed through the soond stage crystallization one in plug flow manner. Aspect 24: The method of any of Aspects 1-23, wherein the method is performed in a continvous manne. ‘Aspect 25: Allulose crystal, obtained in secordance with the method of any of Aspects 1-24 Aspect 26: A consumable product, comprised of o pro pared using allslose crystals in accordance with Aspoct 25 and at least one additonal ingredient other than allulose enya ‘Aspect 27: A method of making consumable produc, comprising using allulose erytls in accordance with Aspect 3s Aspoct 28: A mother liquor, obtained in aecondance with, the method of any of Aspects 1-24 ‘Aspect 2% The mother liquor of Aspect 28, wherein the ‘mother liguor is suitable fr se a «product consumable by humans oe animals or as an ingredient in. formulate pxluct consumable by humans or animals DESCRIPTION OF THE DRAWINGS FIG, 1 illustrates in schematic form a crystallization system and procets in ascondance with one embodiment of the invention US 11,548,907 B2 5 FIG, 2 isa microscopic image ofa massecuite containing allulose crystals which has been produced in accordance ‘with an embodiment ofthe invention DETAILED DESCRIPTION OF CERTAIN EMBODIMENTS OF THE INVENTION Allulose Syrup The present invention wilizes atleast one allulose syrup 8 staring material fora erystalization process, wherein lulose present in dissolved form in the syrup is converted to crystalline form, Methods of obtaining alloose syras are ‘well knows inthe art ad are described, for example, in the following patent documents, the disclosure of each of which fs incomporated herein by reference in its entity for all pumoses: WO 2016/138458; US 20150210996; US, Pat Nos. $411,880, 8,735,106; and 8,030,035, For example, the allulose syrup may be prepared by a process comprising contacting an aqueous solution of fr: ‘ose with an allulose (D-psicose)epimerase enzyme under conditions effective to eonvert at lest a portion of the fructose t allulse, purifying the reaction product obtained, tnd then concentrating the purified reaction product to a ‘desired dry solids content, The purification steps may involve the removal of impuriesffem the reaction product using ene or more technigues suchas deproeination,decol- brization tesiment with decolorizing agents), desing, jon exchange chromatography (ising one or more ion texchange resins, such as anion exchange resin, cation exchange resin and the lke), column chromatography, fac- oation, and the Fike “Theallulose syrup should have a dry solids content whieh is sulicent to effect crystallization of allulose when the ‘syrup is cooled inthe presence of sed erst, as describe hereafier in more del. For example, in various embodi- ‘ments, he dy solids content ofthe lulose syrup may be at least 50% by weight, atleast 55% by weight at loast 0% by weight, t least 63% by weight, at least 70% by weight, a least 75% by weight or at least 80% by weight, However, it will penerally be prefered that the dey solids content of the allulose be sufficiently low dhat the syrup remains a firse-flowing solation in the absence of seed erytals at the temperature at which the syrup isto be maintained prior to the initiation of erystallization by the introduction of seed ‘exystals, Ths in various embodiments ofthe vention, the allulose syrup basa dry solids content not gree than 909% ‘ormnot greater than 85%, The desired dey solids content my be attained by subjecting a diluted allulose solution to an evaporation or concentration procedure wherein volatiles (eg, water) are removed from the solution, leaving behind ‘more concentrsted syrup. The evaporation/condensation Conditions may advantageously be soleted 80 a3 10 miai- Imize or reduce the extent of alllose degradation for example, relatively low evaporation temperatures: may be employed The purty ofthe allulose syrup may vary. but typically it will be desirable for alilose to sanstitate the majority, by ‘weight ofthe non-volatile substances present inthe allulose syrup. Accordingly, the allulose purity of the syrup my be, in varios embodiments of the invention, at lest GO% By weight, at least 65% by weight at Teast 70% by weigh, at Teast 75% by weight, atleast 80% by weight, a least 854% by weit or at least 90% by weight. The term “allulose purity” as used herein with respect to an allulose syrup ‘cans the perceat by weight of alluose in the syrup, based ‘om the total weight of cry solids in te syrup 6 Seed Crystals of AMulose “The present invention employs seed crystals of allsose to help promote the initiation of crystallization of additional alluose from solution (eg. the formation of solid erystals containing allulose that had previously been in solution in an lulose syrup, mother liquor or the like) In eeain embod iments, the allulose seed crystals are in dry form (for exannple, dry exysals of alllose recovered from a previe ‘ously performed crystallization) andor in the form of ahel, such as a portion of a massccuite comprised of allulose crystals and a mother liquor. The precise amount ofallulose sco erysas is not helieved to be partcully erties, but ‘may, for example, be emplayed in a quantity representing fom about 0.1 to about $9 of the total amount of allulose presen in a enstalization vesel or enysallization zone, a8 will be deveribed in more detail subsequently. Generally speaking, alulose soed crystals of relatively high purity are prefered for us: for example, the alulose seed crystals may have an allulose purity of at least 90%, at least 95% or at least 98% by weight, in various embodiments ofthe inven- tion. The term “alllose purity” as used herein with respect to allulse erystals means the peeent by eight of allulose in the crystals, based onthe total weight of dey’ solids in the cexystals Deseription of Various Exemplary Embodiments of Ces tallization Process Inone embodiment ofthe invention, batch crystallization of allulose may be perfomied ina jacketed vessel equipped ‘vith an agitator by dropping the temperature of the coo medium (eq, water or other heat transfer Figuid) in the jacket to lower the massecute temperature and thereby drive crystallization, The following series of steps may be per- form: 1. The vessel is parally filled with a suitable allulose son. ‘The temperature of the cooling modium is set at @ desired inital temperate The agitator is started and set at an RPM effective to provide a desired tip speed, "The temperature of the allulose syrup inthe vessel i lowered to a desired temperature, by varying the tem perature ofthe cooling medium as appropri 5.,A desired amount of seed erystals (ex, dry seed ‘erystals is add to the vessel (this addition may be perform peor to the time the allulose syrup reaches the temperature referenced in step 2). ‘Mix the seed crystals andthe allulose syrup, using an appropriate agitator tip speed. The agitator tip speed iy be sclected to minimize or avoid breakage ofthe cod crystals os well as the allulose crystals subse quently formed “during crystallization. In cenin ‘embodiments, the agitator ip speeds higher during the initial mixing of the seed erystals with the alllose syrup than i is during the subsequent crystallization step). 7. The lemperture of the allalose syrupseed crystal admixture is then kowered to a desired tempertire Cflectve to achieve enstalization of a portion of the allolose dissolved ia the allulose syrup. This tempera ture will vary, depending upon, for example, the con ‘centration of allulose in the syrp, but typically il be hot greater than about 40° C, and not less than but O° © 8. Coystllization is pemattd to contin, with a suitable degree of agitation, until » desired yield of allulose is achieved (this may’ be checkea by peri US 11,548,907 B2 7 cally withdrawing a sample from the vessel and mea ‘uring the dy solids content of the mother iguo. 9. To achieve the desired yield of allulose crystals, the tempersture of the massecuite may continue 10 be lowers, either continuously or in one oF more stages. 10. Once the desired yield of aluiose erystals is met, the ‘masccuite is combined with an additional portion of allose syrap (illing the vessel, foe example). Steps 749 ae then repeated 11. Once the desired yield of allulose crystals is achieved Tollowing the introduction of the ekitional portion of alllose synup into the vessel, a portion (ex appro nately one-quarter to three-quarters) of the massecuite js removed Irom the vessel, with the remaining portion ofthe massecute being retained in the vesel to serve 28 8 sourve of seed crystals fora subsequent batch of rmassecuite. In this way, amutiple batches oF massecite may be prepared, 12. The portions) of the massecuite withdrawn from the vessel may be subjected to one of more desired pro= esting steps, such os separating the allulose crystals from the mother liguor By one or more physical sepa ration methods selected fiom the group consisting of centrifugation, filtration, decantation, membrane sepa ration and combinations thereof and thea washing andlor drying the separated allulose crystals In another embodiment of the iavention, the erystalliza= don may be conducted in a continuous manner involving a plurality of stages e.,thise o four stages). Such a process fy be cari out using a system as illustrated in schematic oem in FIG. Land as further explained as follows. AAmallulose syrup of suitable purty i introduced though line Iw evaporator 2, wherein the dey solids content of the syrup is increased to the desired level. The alllose syrup is then pumped (ilizing pump 8) through line 4 ino allulose syrup feed hold-up tank 8, Prom tank §, the allulse syrup {is pumped (using pump 6) via fine 7 andinteoducod int heat exchanger 8, wherein the temperature of the allulose syrap is adjusted toa desired value prior to being fed va line 910 ‘mix tank 10. In mix tank 1, the allulosesyeupis combined, using vigorous mixing, with massecuite from erytallization zone 22, which is fed to mix tank 10 using line 28, An admixture of alulose syrup and massecuite (which serves as ‘souroe of seed erste is withdrawn fom mix tank 10 and inroduced into erystallizaton zone 12. Crystallization zone 12 may be within a suitable tank or oiher vessel equipped with an agitator Any agitator of the type Known in the art may be used in particular, the agitator may be any of the types of mechanical devices recognized as being Useil in spiating solution/sed crystal mixtures in a erystallization process may be utilized. In one embodiment, the agitator i the ensallization zone can bring about its agitating elect horizontally but not vertically In order to prevent or reduce turbulent flow and. destrictioavbreakage” of the crystals Tormed during erstallzation the agitation ean be preferably cstried out at low speed. The agitator may be configured tnd operated $0 a 10 prevent enysals of allulose from dering tothe walls) andlor the bottom of a vessel com- Stinting crystallization zone 12. Acconding to one aspect of the invention, the admixture of allulose. syrup and ‘massecnite isnot subjected to concentration within eystal- Tization zone 12, The alulose syrupimassecuite admixture ‘may move through erystallization zone 12 in a plug fow ‘manner, withthe lip speed a the auitator being ajusted appropriate to promote erstallization of alllose dissolved inthe liquid phase ofthe admixture and to generate allulose ferystals ofthe desea size and shape. In ane embodiment, 8 the process parameters are controlled sueh tha the allulose syruplmassecuite admixture is passed, in descending eon Tinuous Mow, through a vessel comprising crystallization zone 12, The flow rte of the admixture through erytalli- ation zone 12 and hs the residence ime of the admixture in erystallization zone 12 are controlled such that the admix ture exiting fom erystllization zone 12 via line 14 has a desired content of alfulose erytals (ie, the desired yield of allulose erystls is achieved by te time the admixture is withdrawn. from exystallization zope 12). In one embodi- rent, the temperature of the allulose syrupimassoctite ‘admixture remains constant or essentially constant a the fdmixture passes through crystallization zone 12. For cxample, the temperamre of the admixture may be con- twoed such that the admixture temperature at the point of introduction into erystallization zone 12 dies by no more than 5°C., no more than 4° C,, no more than 3° C, no more than 2° Cor no more than 1°C, trom the temperate ofthe txlmiscure at the point where it exits or is withdrawn from cxjstallization zone 12. "The massecuite obtained from crystallization zone 12 is further cooled using heat exchanger 15 10 & desired fem: perature (hich may be, for example, about 1° C. to about 10° C. lower than the temperature of the massecuite a it exits from enstlization zone 12) and intmduced into txysallization zone 17, via Tine 16, Acconling to one tmbodiment ofthe invention, the massecuite obtains! from crystallization zone 12 is not subjected to conceatration before or alter being introduced int erytallization zone 17 Casstallization zone 17 may be within a suitable tank or other vessel equipped with an agitator. The massecute may ‘move through erystallization zone 17 ina plug Now manner, with the tip speed of the agitator being adjusted as appro- Pate to promote enstalization of ellos stl dissolved in the liguid phase (mother liquor) ofthe massecuite. The Bow rate of the massocvite through enstaliztion zone 17 and ths the residence time of the admixture in crystallization zone 17 are controled such that the admisture exiting from txytallization 2one 17 via line 18 is desired content of allulose crystals (ie, the desired yield of alulose erystals is achieved by the time the massecuite is withdrawn. from crystallization zone 17), withthe desired content of allulose cya being higher than tht of the massccuite withdeswn from erystallization zone 12. The massecuite in erystalliza tion zone 17 is not subjected 0 concentration, according 19 ‘one embodiment of te invention, “The mssecuite obsained from erystallization zone 17 is, further cooled using heat exchanger 20 t0 a desired tex perature (hich may be, for example, about 1° C. to about 10" C. lower than the temperature of the mussecuite a it exits from enystliztion zone 17) and introduced into crystallization zone 22, via line 21. Acconding to one embodiment ofthe invention, the massecuite obtained from exystallization zone 17 is not subjected to concentration before or after being introduced into crystallization zone 22 Cstallization zone 22 may be within a suitable tank or other vessel equipped with an agitator. The massecuite may ‘move through erysallization zane 22 ina plug flow manner, vith the tip sposd of the agitator being adjusted as appro= priate promote crystallization of aulse stl dissolved in the figuid phase (mother liquor) ofthe massecuite, The ow Fate of the massecuite through erysalization zone 22 and thus the residence time ofthe admixture in crystallization one 22 are controlled sich that the admixture exiting from ceystilliztion zone 22 via line 23 has a desired content of allulose crystals (Le, the desired yield of allulose crystals is fchieved by the time the massecuite is withdrawn from US 11,548,907 B2 9 xytallization zone 22), with the desired content oF allulose texystals being higher than that of the massecuite withdrawn trom erystllization zone 17, The massecuite in erstliza ion zone 22 is not subjected to concentration, according to fone embodiment of the invention, so desired, ane oF more addtional erstalization zones (oot illustrated) may be induced, which is or are operated ‘na manne similar otha of erystallization zones 12,17 and 22, wherein the massecuite exiting crystallization zone 22 is ‘subjected to further cooling and crystallization. According to cerain embodiments ofthe invention, such further process ing is cared) out without any concentration of the ‘Once a massecite having the desired final target yield of alfulose crystals has boon produced, 2 portion of it may be tecyeled and utilized a a source of seed erystals as previ ‘ously mentioned (being conveyed via Tine 25 to mix tank 18) tnd the remaining portion may be pussed through heat texehanger 27 and fed via line 28 wo massecnite hold-up tank 29, The masteeite fom messocuite holdp tank 29 may be Subjected to a separation of the aulose crystals from the ‘mother liqo using centrifuge 30, wth the resulting cake of allulose crystals then being washed before being dried in rotary diyee 31 Generally speaking, it will be desiable to contol the cejtallization conditions such tat the final masseuite (.e the massecute fom which allulose erstals will be reo0V ered, involving separation from the mother liquor compo: ‘eat ofthe massecuite) does not have an overly high content tf allulose crystals, since a high allulose crystal concentra tion may tend to result in a massecuite which has a high Viscosity and which is consequently

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