EP0202999A1 - Verfahren und Vorrichtung zur Herstellung von kristalliner wasserfreier Dextrose - Google Patents

Verfahren und Vorrichtung zur Herstellung von kristalliner wasserfreier Dextrose Download PDF

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Publication number
EP0202999A1
EP0202999A1 EP86401015A EP86401015A EP0202999A1 EP 0202999 A1 EP0202999 A1 EP 0202999A1 EP 86401015 A EP86401015 A EP 86401015A EP 86401015 A EP86401015 A EP 86401015A EP 0202999 A1 EP0202999 A1 EP 0202999A1
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EP
European Patent Office
Prior art keywords
crystallization
zone
enclosure
temperature
mass
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Granted
Application number
EP86401015A
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English (en)
French (fr)
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EP0202999B1 (de
Inventor
Jean Bernard Leleu
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.)
Roquette Freres SA
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Roquette Freres SA
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Publication date
Application filed by Roquette Freres SA filed Critical Roquette Freres SA
Priority to AT86401015T priority Critical patent/ATE42572T1/de
Publication of EP0202999A1 publication Critical patent/EP0202999A1/de
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Publication of EP0202999B1 publication Critical patent/EP0202999B1/de
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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
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/10—Crystallisation

Definitions

  • the subject of the invention is a process and an installation for the preparation of anhydrous crystallized dextrose.
  • the hydrolyzate of a dry matter greater than 92% is stirred, firstly, preferably in the presence of seeds of crystallization; the crushed dextrose thus obtained is ground, conditioned on a fluidized bed and cooled.
  • the invention also relates to other arrangements which are preferably used at the same time and which will be more explicitly discussed below.
  • FIGS 1 and 2 of this drawing schematically show two variants of an installation according to the invention.
  • the starting material used is a syrup rich in glucose, preferably free of crystals and of nuclei and originating for example from a starch hydrolyzate; this syrup has a dry matter content greater than 80%, preferably from 82 to 90% and more preferentially still from 85 to 88% by weight, the glucose entering for at least 92% and, preferably, for a proportion greater than 94% by weight on dry matter in its constitution.
  • This syrup is conveyed to a crystallization zone of preferably substantially vertical axis, which it travels continuously from top to bottom from a point located near its upper end and inside which it is subjected , in the presence of anhydrous dextrose crystals playing the role of seeds of crystallization, to a kneading and to a temperature gradient generally decreasing from top to bottom.
  • the temperature of the syrup is brought or maintained, at the time of its introduction into the crystallization zone, at a value greater than 60 ° C., preferably chosen in the range from 80 to 90 ° C. and, in practice, close to 85 ° C.
  • the temperature gradient established inside the crystallization zone within the mass subjected to crystallization corresponds to a decrease of 0.2 to 2 ° C, preferably from 0.5 to 0.75 ° C per hour of treatment and is such that at the exit from said zone, at a point located near the lower end thereof, the mass subjected to crystallization which includes the syrup, the crystals initially present and those formed by the phenomenon crystallization, is brought to a temperature above 55 ° C and preferably within a range of 58 to 65 ° C.
  • the decreasing temperature gradient extends only over a part of the crystallization zone and is then followed and / or preceded by two or a single part of the zone inside which the temperature is substantially constant at all points.
  • the fraction taken and recycled represents, by volume, from 10 to 120%, preferably from 40 to 110% and more preferably still from 80 to 100% of the volume of the glucose syrup supplying the crystallization zone.
  • the glucose syrup feed rate is chosen such that the average residence time of a given fraction of the mass subjected to crystallization inside the crystallization zone is 12 to 120 hours, preferably 30 to 50 hours; the value adopted depends on the composition of the supply syrup and on the heat exchange capacities of the means comprised by the zone using which is established, inside said zone within the mass subjected to crystallization, the decreasing temperature gradient.
  • the viscosity of the mass subjected to crystallization which increases as the proportion of crystals of anhydrous dextrose increases, that is to say in the downward direction, makes that the zone of crystallization is, of preferably equipped with discharge or suction means capable of facilitating the movement of the mass inside the zone.
  • the kneading and homogenization means provided by the crystallization zone must be arranged in such a way that dead zones are avoided and that the heat exchange between the mass subjected to crystallization and the cooling means is the most effective. possible.
  • the above-mentioned crystallization zone is preceded, upstream, by a crystallization initiation zone, preferably with a substantially vertical axis.
  • the dextrose syrup preferably substantially free of crystals and of nucleus, which is the raw material and which is then brought to pass through this priming zone, is routed. subject to continuous agitation; inside this zone, the syrup is maintained at a substantially constant temperature, 2 to 5 "C lower than the saturation temperature, thanks to which the initiation of crystallization which results in the formation of '' a mixture of glucose syrup and anhydrous dextrose crystals.
  • the average residence time of a given fraction of mixture inside this first zone is 8 to 24 hours and more preferably 10 to 16 hours.
  • the mixture leaving the priming zone is then brought to pass always from top to bottom, under kneading, the above-mentioned crystallization zone.
  • the axes of the two zones are arranged in the extension of one another.
  • the temperature of the syrup is brought or maintained, at the time of its introduction into the second crystallization zone, at a value substantially equal to that of the syrup leaving the first zone.
  • the mixture leaving the second zone is in the form of a crystallized mass rich in anhydrous dextrose crystals, from which these are recovered.
  • the initiation of crystallization at the first zone is favored by recycling preferably at the upper end thereof of the fraction of the mixture passing through the second zone which, in the case where the invention does not provide that a zone is recycled towards the upper end of this single zone; this recycled fraction always representing from 10 to 120%, preferably from 40 to 110% and more preferably still from 80 to 100% of the syrup introduced into the first zone; it is taken at a variable level and determined as a function of the respective importance of the initiation and crystallization zones, this level preferably being located in the upper third when the initiation zone represents approximately one third of the crystallization zone.
  • the average residence time of a given fraction of the mass subjected to crystallization inside the second zone is 12 to 120 hours, preferably 30 to 50 hours; the value adopted depends on the composition of the supply syrup and on the heat exchange capacities of the means comprised by this second zone with the help of which is established within the mass subjected to crystallization, the decreasing temperature gradient which it was discussed above.
  • the crystallization zone is preferably equipped with means suitable for facilitating the passage of the mass to the inside the area.
  • this second crystallization zone are arranged as in the case of a single zone, so that the dead zones are avoided and the heat exchange between the mass subjected to crystallization and the cooling means is as efficient as possible.
  • the crystals collected at the exit of the last zone have a sufficiently limited particle size spectrum and a sufficiently large average particle size to allow great ease of work in the subsequent stages of spinning and washing the crystals; however, the particle size spectrum is narrower and the average particle size higher in the two-zone system.
  • the mother liquors collected can be partially recycled.
  • this installation comprises, as shown in FIG. 1, a single enclosure having the shape of a cylinder of revolution of axis XY.
  • the XY axis is preferably substantially vertical.
  • the heat exchange capacity, the temperature regulation system, the speed of rotation of the kneading means and the speed with which, under the influence of the suction means not shown, the mass subjected to crystallization traverses the enclosure, that is to say the average duration of stay of a given fraction of this mass inside the enclosure, are chosen in such a way that is established, within the whole of the mass subjected to crystallization, the temperature gradient provided in accordance with the invention.
  • the cooling fluid is water and that the average temperature difference at a given point of the enclosure between this water and the mass subjected to crystallization, is of the order of 2 at 10'C.
  • this installation essentially comprises two enclosures 1a and 1b advantageously arranged one (1a) above the other (1b); these enclosures advantageously have the shape of cylinders of revolution of axes X 1 , Y 1 and X 2 , Y 2 preferably substantially vertical and preferably located in the extension of one another.
  • the enclosure 1b corresponds to the single enclosure of the first variant.
  • the mixture consisting of glucose syrup and anhydrous dextrose crystals which has formed inside the enclosure 1a flows from the latter at a point 17 located in the vicinity of the lower end of this enclosure; at this location the enclosure may include a pipe 18 through which the mixture is conveyed to the enclosure 1b; one can also provide that the outlet orifice of the enclosure 1a is disposed opposite the inlet orifice of the enclosure 1b, the two enclosures then being juxtaposed.
  • the enclosure 1b is equipped with a continuous extraction system at the lower end of the enclosure and schematically represented by a pipe 20, this system being specific to recover the mass rich in crystals of anhydrous dextrose obtained at the outlet of the enclosure 1b.
  • the temperature regulation system is arranged in such a way that it makes it possible to establish, inside the enclosure 1b, a globally decreasing temperature gradient downwards of the kind already provided in the case of the single enclosure of the first variant.
  • the enclosure can be arranged in such a way that the overall decreasing temperature gradient extends only over a first part of the latter, the second part then being such that the temperature is substantially equal there in all points.
  • the line 23 may include fragmentation means 27, for example a grinder, capable of disintegrating the largest crystals of anhydrous dextrose contained in the recycled fraction.
  • the cooling fluid is water and the average temperature difference at a given point in the enclosure between this water and the mass subjected to crystallization is of the order of 2 to 10 * C.
  • the installation incorporates the constituent elements of the second variant, with the difference that the second part of the second enclosure is embodied in the form of an enclosure independent of the two others and situated in their extension, this third enclosure comprising temperature regulation means capable of imposing a temperature which is substantially constant at all points.
  • the temperature of the syrup at the entrance to enclosure 1a is approximately 82 . vs.
  • the average duration of passage inside the about a given fraction of the mass subjected to crystallization is about 40 hours.
  • the mass rich in anhydrous dextrose crystals extracted at the lower end of the enclosure is at a temperature close to 62 ° C, the temperature gradient generally decreasing from top to bottom therefore corresponding to about 0.5 ° C per hour.
  • the glucose content of the mother liquors recovered after separation and washing of the anhydrous dextrose crystals is 96.3% on dry matter, the complement to 100 being constituted by di- and polysaccharides.
  • the crystals collected after spinning and washing have excellent physical and chemical properties.
  • the recycled fraction is sampled at a level located outside the domain in accordance with the invention.
  • the syrup temperature at the entrance of the enclosure is about 86 * C.
  • This enclosure 1a is provided with an agitator and is kept at a constant temperature of 82 ° C.
  • the average passage time inside the enclosure 1a of a given fraction of the mixture of syrup and dextrose crystals is approximately 12 hours.
  • the mixture leaving the enclosure 1a is brought by the pipe 18 at a point 19 of the enclosure 1b located in the vicinity of the upper end thereof.
  • this mixture is subjected to an overall decreasing temperature gradient; the upper temperature of this gradient is 81 * C and the lower temperature of 61 * C.
  • This gradient generally decreasing from top to bottom, therefore corresponds to approximately 0.5 ° C. per hour.
  • the recycled fraction corresponds to 80% of the quantity of syrup introduced through line 12.
  • Mass rich in crystals of anhydrous dextrose extracted at the lower end of the chamber 1b through line 20 is at a temperature of 61 ° C and to separate an amount of crystals corresponding to 32 weight% of mixed.
  • the separation of the anhydrous dextrose crystals is carried out by wringing, then the crystals are washed.
  • the glucose content of the mother liquors thus recovered is 96.3% on dry matter, the complement to 100 being constituted by di- and polysaccharides.
  • the crystals collected after spinning and washing have excellent physical and chemical properties.
  • the recycled fraction is withdrawn at a level situated outside the domain in accordance with the invention.

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  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Ink Jet (AREA)
  • Liquid Crystal Substances (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Seasonings (AREA)
EP86401015A 1985-05-15 1986-05-13 Verfahren und Vorrichtung zur Herstellung von kristalliner wasserfreier Dextrose Expired EP0202999B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86401015T ATE42572T1 (de) 1985-05-15 1986-05-13 Verfahren und vorrichtung zur herstellung von kristalliner wasserfreier dextrose.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8507429A FR2582015B1 (fr) 1985-05-15 1985-05-15 Procede et installation de preparation de dextrose cristallise anhydre
FR8507429 1985-05-15

Publications (2)

Publication Number Publication Date
EP0202999A1 true EP0202999A1 (de) 1986-11-26
EP0202999B1 EP0202999B1 (de) 1989-04-26

Family

ID=9319335

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86401015A Expired EP0202999B1 (de) 1985-05-15 1986-05-13 Verfahren und Vorrichtung zur Herstellung von kristalliner wasserfreier Dextrose

Country Status (7)

Country Link
US (2) US4931101A (de)
EP (1) EP0202999B1 (de)
JP (1) JPS61280300A (de)
AT (1) ATE42572T1 (de)
DE (1) DE3663035D1 (de)
FI (1) FI84081C (de)
FR (1) FR2582015B1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1652938A1 (de) * 2004-10-29 2006-05-03 Roquette FrÀ¨res Nicht im Bereich Lebensmittel oder Pharmazie liegende Verwendung auf Basis von gewählter wasserfreier Dextrosezusammensetzungen

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2582015B1 (fr) * 1985-05-15 1987-09-18 Roquette Freres Procede et installation de preparation de dextrose cristallise anhydre
US5549757A (en) * 1994-06-10 1996-08-27 Ingredient Technology Corporation Process for recrystallizing sugar and product thereof
FI97625C (fi) * 1995-03-01 1997-01-27 Xyrofin Oy Menetelmä ksyloosin kiteyttämiseksi vesiliuoksista
FI952065A0 (fi) * 1995-03-01 1995-04-28 Xyrofin Oy Foerfarande foer tillvaratagande av en kristalliserbar organisk foerening
GB0022522D0 (en) * 2000-09-13 2000-11-01 Cerestar Holding Bv Use of dehydrated dextrose monohydrate for heterogeneous chemical reactions

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2398802A1 (fr) * 1977-07-27 1979-02-23 Staley Mfg Co A E Dextrose anhydre solide
BE877839A (fr) * 1979-07-23 1980-01-23 Zurita Hilda G Perfectionnements relatifs a des echangeurs de chaleur en continu et a contre-courant sous agitation pour la cristallisation de suspensions cristallisables en mouvement
DE3246494A1 (de) * 1982-12-16 1984-06-20 Bayer Ag, 5090 Leverkusen Diskontinuierliches verfahren zur kristallisation einer substanz aus einer homogenen loesung
EP0147269A2 (de) * 1983-11-17 1985-07-03 Roquette Frˬres Verfahren und Vorrichtung zur Herstellung von kristallisiertem Dextrosehydrat

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3513023A (en) * 1966-04-29 1970-05-19 Boehringer Mannheim Gmbh Process for the production of crystalline fructose
CH483272A (fr) * 1967-05-02 1969-12-31 Belge Atel Reunies Appareil de cuisson pour la cristallisation en continu
US3607392A (en) * 1967-12-21 1971-09-21 Boehringer Mannheim Gmbh Process and apparatus for the recovery of crystalline fructose from methanolic solution
JPS502017B1 (de) * 1969-06-27 1975-01-23
JPS5239901B2 (de) * 1973-02-12 1977-10-07
US3981739A (en) * 1974-08-30 1976-09-21 Amstar Corporation Continuous crystallization
US4059460A (en) * 1975-11-07 1977-11-22 A. E. Staley Manufacturing Company Solid anhydrous dextrose
GB2053019B (en) * 1979-07-06 1983-10-26 Zurita H G Heat exchangers for crystallization of crystallizable suspension whilst in motion
US4537637A (en) * 1980-08-19 1985-08-27 The Coca-Cola Company Hydration drying process
JPS60118200A (ja) * 1983-11-29 1985-06-25 加藤化学株式会社 無水結晶果糖の連続結晶化方法及び装置
FR2582015B1 (fr) * 1985-05-15 1987-09-18 Roquette Freres Procede et installation de preparation de dextrose cristallise anhydre

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2398802A1 (fr) * 1977-07-27 1979-02-23 Staley Mfg Co A E Dextrose anhydre solide
BE877839A (fr) * 1979-07-23 1980-01-23 Zurita Hilda G Perfectionnements relatifs a des echangeurs de chaleur en continu et a contre-courant sous agitation pour la cristallisation de suspensions cristallisables en mouvement
DE3246494A1 (de) * 1982-12-16 1984-06-20 Bayer Ag, 5090 Leverkusen Diskontinuierliches verfahren zur kristallisation einer substanz aus einer homogenen loesung
EP0147269A2 (de) * 1983-11-17 1985-07-03 Roquette Frˬres Verfahren und Vorrichtung zur Herstellung von kristallisiertem Dextrosehydrat

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 97, 1982, page 86, résumé no. 111551c, Columbus, Ohio, US; & CS - A - 209 130 (S. KUCERA) 30-11-1981 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1652938A1 (de) * 2004-10-29 2006-05-03 Roquette FrÀ¨res Nicht im Bereich Lebensmittel oder Pharmazie liegende Verwendung auf Basis von gewählter wasserfreier Dextrosezusammensetzungen
FR2877186A1 (fr) * 2004-10-29 2006-05-05 Roquette Freres Utilisation non alimentaire et non pharmaceutique d'une composition de dextrose anhydre selectionnee
US7731991B2 (en) 2004-10-29 2010-06-08 Roquette Freres Non-food and non-pharmaceutical use of a selected anhydrous dextrose composition

Also Published As

Publication number Publication date
FI862024A (fi) 1986-11-16
FR2582015B1 (fr) 1987-09-18
FI84081B (fi) 1991-06-28
US4931101A (en) 1990-06-05
JPS61280300A (ja) 1986-12-10
FR2582015A1 (fr) 1986-11-21
DE3663035D1 (en) 1989-06-01
EP0202999B1 (de) 1989-04-26
FI84081C (fi) 1991-10-10
ATE42572T1 (de) 1989-05-15
FI862024A0 (fi) 1986-05-14
US5076853A (en) 1991-12-31

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