EP0971040B1 - Verfahren zur Herstellung von Kristalfruktose - Google Patents

Verfahren zur Herstellung von Kristalfruktose Download PDF

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Publication number
EP0971040B1
EP0971040B1 EP98202278A EP98202278A EP0971040B1 EP 0971040 B1 EP0971040 B1 EP 0971040B1 EP 98202278 A EP98202278 A EP 98202278A EP 98202278 A EP98202278 A EP 98202278A EP 0971040 B1 EP0971040 B1 EP 0971040B1
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EP
European Patent Office
Prior art keywords
fructose
crystals
syrup
seeding
content
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98202278A
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English (en)
French (fr)
Other versions
EP0971040A1 (de
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Warcoing SA
Original Assignee
Warcoing SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to EP98202278A priority Critical patent/EP0971040B1/de
Application filed by Warcoing SA filed Critical Warcoing SA
Priority to DE69818023T priority patent/DE69818023T2/de
Priority to AT98202278T priority patent/ATE249524T1/de
Priority to ES98202278T priority patent/ES2206826T3/es
Priority to DK98202278T priority patent/DK0971040T3/da
Priority to IL14064099A priority patent/IL140640A/xx
Priority to PCT/EP1999/004732 priority patent/WO2000003040A1/fr
Priority to US09/743,157 priority patent/US6607603B1/en
Priority to JP2000559260A priority patent/JP2002520030A/ja
Publication of EP0971040A1 publication Critical patent/EP0971040A1/de
Priority to ZA200100133A priority patent/ZA200100133B/en
Application granted granted Critical
Publication of EP0971040B1 publication Critical patent/EP0971040B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K11/00—Fructose

Definitions

  • the present invention relates to a process for the manufacture of crystalline fructose by crystallization / solidification of a purified and concentrated fructose syrup.
  • the object of the present invention is to provide a new process for crystallizing fructose, overcoming the problems of the prior art, and thus to offer a form of crystalline fructose which can be used commercially.
  • This new process for the manufacture of crystallized fructose involving the solidification of a hot and concentrated solution of fructose following a seeding of the solution by means of fructose crystals, is characterized by the use of a fructose solution resulting from a pure fructose syrup freshly prepared by melting fructose dihydrate crystals, concentrated by evaporation under vacuum to a dry matter content greater than 96% by weight, and preferably greater than 97% by weight.
  • the fructose solution used for sowing preferably has a preferred temperature of between 50 and 100 ° C, ideally between 80 and 95 ° C.
  • the seeding is preferably done by means of 5 to 30% by weight of crystallized fructose having a particle size less than 500 ⁇ m, preferably less than 250 ⁇ m (for example 50 ⁇ m).
  • the time between the melting of the fructose dihydrate crystals to prepare the initial syrup and the concentration of this syrup with a dry matter content greater than 96% by weight, preferably greater than 97 % by weight, is preferably less than 24 hours, more particularly less than 8 hours, and ideally less than half an hour.
  • the invention relates to crystallized fructose, essentially consisting of beta-D-fructopyranose, having low contents of other tautomers of fructose, as resulting from a process for solidification of a hot and concentrated solution of fructose following sowing.
  • fructose solution used for sowing results from a pure fructose syrup freshly prepared by the melting of crystals of fructose dihydrate, concentrated by evaporation under vacuum until a dry matter content between 96 and 100% by weight
  • the fructose solution used for seeding has a preferred temperature of between 80 and 95 ° C.
  • the seeding is carried out by means of 5 to 30% by weight of crystallized fructose with a particle size of less than 500 ⁇ m, of lower preference at 250 ⁇ m
  • the time between the melting of the fructose dihydrate crystals to prepare the initial syrup and the concentration of this syrup with a dry matter content greater than 96% is less than 8 hours, preferably less than half an hour.
  • Obtaining fructose dihydrate crystals consists of a progressive cooling of an aqueous solution of glucose and fructose, the total sugar content of which is between 45 and 85% and, in the dry matter, the fructose concentration is between 60 and 100%.
  • the temperature of the mass thus grained is gradually lowered and is thus maintained in a zone of supersaturation in fructose such that the crystals present progressively grow, however limiting the appearance of new crystals.
  • the mass of syrup containing the crystals is conveyed to a continuous or discontinuous centrifuge similar to those used in sugar refinery. Any other physical method solid / liquid separation can be considered.
  • the mother liquors of crystallization consisting of water and sugars from the initial solution which have not crystallized, can be subjected to a new crystallization stage as described above.
  • the fructose dihydrate crystals thus separated, can be washed so as to eliminate as much as possible the film of mother liquor surrounding them therefore increasing the purity of the fructose to values between 90% and 100% and preferably between 97.5% and 100 %. They are then melted, preferably at temperatures above 20 ° C. If there is no addition of water during melting, the syrup obtained from properly washed crystals contains 83% sugars and 17% d 'water. The dry matter of such a syrup contains only a few traces of other sugars present in the mother liquors.
  • the 83% dry matter syrup obtained according to Example I is concentrated at temperatures of the order of 65 to 100 ° C. under pressures below 60 mm of mercury, for a period of less than 30 minutes, or even less than 15 minutes. .
  • the dry matter of the concentrated syrup varies between 96.0 and 100.0%.
  • the syrup is relatively viscous and can then be pumped for crystallization / subsequent solidification.
  • the concentrated and viscous syrup obtained in Example II is then kept in a mixer at a temperature between 80 and 95 ° C and seeded using 10 to 25% of crystallized fructose with a very fine particle size ( ⁇ 200 ⁇ m ). This seeding can be done using fructose obtained by the present process, very finely ground.
  • the medium is then agitated so as to ensure optimal dispersion of the germs within it.
  • the medium consisting of a very viscous whitish mass is then poured out of the mixer and stored in an oven whose temperature is fixed between 55 and 75 ° C. depending on the residual water content, the quantity of germs and the state of the mutarotation reaction. The residence time in the oven depends on these same factors.
  • the cistallized mass thus obtained is coarsely crushed by means of a grinder.
  • the particles obtained can then be dried between 50 and 75 ° C (preferably under a flow of dry air) in order to further decrease the water content. Fine grinding can then be carried out. If the initial mass is dry enough to be finely ground, drying subsequent to coarse grinding can be avoided.
  • the product obtained consists of particles (the particle size of which depends on fine grinding), themselves formed from small fructose crystals agglomerated together. In order to remove as much water as possible, final drying at a temperature between 50 and 75 ° C takes place after fine grinding.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)
  • Jellies, Jams, And Syrups (AREA)

Claims (8)

  1. Verfahren zur Herstellung von Kristallfructose durch Solidifikation einer warmen und konzentrierten Fructoselösung nach Impfung der Lösung mit Fructosekristallen, dadurch gekennzeichnet, dass die für die Impfung verwendete Fructoselösung aus einem reinen, durch Schmelzen von Fructosedihydratkristallen frisch hergestellten Fruotosesirup gebildet wurde, der durch Verdampfung im Vakuum bis auf einen Gehalt von über 96 Gew.-% in der Trockenmasse konzentriert wird.
  2. Verfahren zur Herstellung von Kristallfructose nach Anspruch 1, dadurch gekennzeichnet, dass die für die Impfung verwendete Fructoselösung eine Temperatur zwischen 50 und 100 °C aufweist.
  3. Verfahren zur Herstellung von Kristallfructose nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass für die Impfung 5 bis 30 Gew.-% Kristallfructose mit einer Granulatgröße unter 500 µm verwendet werden.
  4. Verfahren zur Herstellung von Kristallfructose nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass der Zeitraum zwischen dem Schmelzen der Fructosedihydratkristalle zur Zubereitung des Ausgangssirups und der Konzentration dieses Sirups auf einen Gehalt von über 96 % in der Trockenmasse weniger als 24 Stunden beträgt.
  5. Verfahren zur Herstellung von Kristallfructose nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass der Zeitraum zwischen dem Schmelzen der Fructosedihydratkristalle zur Zubereitung des Ausgangssirups und der Konzentration dieses Sirups auf einen Gehalt von über 96 % in der Trockenmasse weniger als 8 Stunden beträgt.
  6. Verfahren zur Herstellung von Kristallfructose nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass der Zeitraum zwischen dem Schmelzen der Fructosedihydratkristalle zur Zubereitung des Ausgangssirups und der Konzentration dieses Sirups auf einen Gehalt von über 96 % in der Trockenmasse weniger als eine halbe Stunde beträgt.
  7. Verfahren zur Herstellung von Kristallfructose aus einem Sirup, der Fructose und eventuell andere Stoffe enthält, durch Reinigen dieser Fructoselösung und durch Solidifikation derselben durch Impfung mit Fructosekristallen, das durch folgende sukzessive Schritte gekennzeichnet ist:
    Impfen der Fructoselösung mit Fructosedihydratkristallen, wobei die Fructoselösung einen Gesamtgehalt an Zucker zwischen 45 und 85 Gew.-% und einen Fructosegehalt über 60 Gew.-% der Trockenmasse aufweist, bei einer Temperatur zwischen 10 und -10 °C,
    Belassen der Lösung in einem Bereich der Übersättigung an Fructose durch fortschreitendes Absenken der Temperatur bis zum Erhalt von Kristallen der gewünschten Größe, und
    Trennen der aus der Mutterlösung gewonnenen Kristalle in der Weise, dass man Fructosedihydratkristalle erhält, deren Fructosegehalt zwischen 95 und 100 Gew.-% der Trockenmasse liegt;
    Schmelzen der gewonnenen Kristalle zu einem Sirup, der einen Gehalt von etwa 83 Gew.-% Zucker und etwa 17 % Wasser aufweist,
    Konzentrieren des Sirups durch Wasserverdampfung unter vermindertem Druck bis auf einen Gehalt in der Trockenmasse zwischen 96 und 100 Gew.-%;
    Impfen des so gewonnenen Sirups mittels 5 bis 30 Gew.-% Kristallfructose,
    Belassen der gewonnenen Masse bei einer Temperatur zwischen 55 und 75 °C bis zum Erhalt einer nicht klebenden und brüchigen Masse, und
    Brechen, Trocknen und Zerkleinern dieser Masse zu Partikeln, die aus agglomerierten Fructosekristallen bestehen.
  8. Verfahren zur Herstellung von Kristallfructose nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, dass
    die für die Impfung mit Fructosekristallen verwendete Fructoselösung eine Temperatur zwischen 80 und 95 °C aufweist,
    die für die Impfung mit Fructosekristallen verwendete Fructoselösung durch Verdampfung im Vakuum konzentriert wurde,
    die für die Impfung mit Fructosekristallen verwendete Fructoselösung auf einen Gehalt von über 96 Gew.-% in der Trockenmasse konzentriert wurde, und/oder dass die Impfkristalle eine Granulatgröße unter 250 µm aufweisen.
EP98202278A 1998-07-08 1998-07-08 Verfahren zur Herstellung von Kristalfruktose Expired - Lifetime EP0971040B1 (de)

Priority Applications (10)

Application Number Priority Date Filing Date Title
DE69818023T DE69818023T2 (de) 1998-07-08 1998-07-08 Verfahren zur Herstellung von Kristalfruktose
AT98202278T ATE249524T1 (de) 1998-07-08 1998-07-08 Verfahren zur herstellung von kristalfruktose
ES98202278T ES2206826T3 (es) 1998-07-08 1998-07-08 Procedimiento de fabricacion de fructosa cristalizada.
DK98202278T DK0971040T3 (da) 1998-07-08 1998-07-08 Fremgangsmåde til fremstilling af krystalliseret fructose
EP98202278A EP0971040B1 (de) 1998-07-08 1998-07-08 Verfahren zur Herstellung von Kristalfruktose
PCT/EP1999/004732 WO2000003040A1 (fr) 1998-07-08 1999-07-05 Procede de fabrication de fructose cristallise
IL14064099A IL140640A (en) 1998-07-08 1999-07-05 Method for making crystallized fructose
US09/743,157 US6607603B1 (en) 1998-07-08 1999-07-05 Method for making crystallized fructose
JP2000559260A JP2002520030A (ja) 1998-07-08 1999-07-05 結晶フルクトースの製造方法
ZA200100133A ZA200100133B (en) 1998-07-08 2001-01-05 Method for making crystallised fructose.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP98202278A EP0971040B1 (de) 1998-07-08 1998-07-08 Verfahren zur Herstellung von Kristalfruktose

Publications (2)

Publication Number Publication Date
EP0971040A1 EP0971040A1 (de) 2000-01-12
EP0971040B1 true EP0971040B1 (de) 2003-09-10

Family

ID=8233899

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98202278A Expired - Lifetime EP0971040B1 (de) 1998-07-08 1998-07-08 Verfahren zur Herstellung von Kristalfruktose

Country Status (10)

Country Link
US (1) US6607603B1 (de)
EP (1) EP0971040B1 (de)
JP (1) JP2002520030A (de)
AT (1) ATE249524T1 (de)
DE (1) DE69818023T2 (de)
DK (1) DK0971040T3 (de)
ES (1) ES2206826T3 (de)
IL (1) IL140640A (de)
WO (1) WO2000003040A1 (de)
ZA (1) ZA200100133B (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2292803B1 (de) 2009-07-07 2013-02-13 DuPont Nutrition Biosciences ApS Trennungsverfahren
WO2013049424A1 (en) * 2011-09-28 2013-04-04 Wisconsin Alumni Research Foundation Catalytic conversion of cellulose to fuels and chemicals using boronic acids

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2588449A (en) * 1950-03-03 1952-03-11 Us Agriculture Levulose dihydrate
US3513023A (en) * 1966-04-29 1970-05-19 Boehringer Mannheim Gmbh Process for the production of crystalline fructose
US3607392A (en) * 1967-12-21 1971-09-21 Boehringer Mannheim Gmbh Process and apparatus for the recovery of crystalline fructose from methanolic solution
US3883365A (en) * 1972-01-04 1975-05-13 Suomen Sokeri Oy PH adjustment in fructose crystallization for increased yield
US4199373A (en) * 1979-04-13 1980-04-22 Chimicasa Gmbh Process for the manufacture of crystalline fructose
GB8506482D0 (en) * 1985-03-13 1985-04-17 Tate & Lyle Plc Sugar process
US5047088A (en) * 1989-06-30 1991-09-10 A. E. Staley Manufacturing Company Method for crystallization of fructose

Also Published As

Publication number Publication date
ZA200100133B (en) 2001-07-23
DE69818023T2 (de) 2004-07-08
JP2002520030A (ja) 2002-07-09
ES2206826T3 (es) 2004-05-16
WO2000003040A1 (fr) 2000-01-20
IL140640A (en) 2005-11-20
EP0971040A1 (de) 2000-01-12
US6607603B1 (en) 2003-08-19
IL140640A0 (en) 2002-02-10
DE69818023D1 (de) 2003-10-16
ATE249524T1 (de) 2003-09-15
DK0971040T3 (da) 2003-12-08

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