EP0147269B1 - Verfahren und Vorrichtung zur Herstellung von kristallisiertem Dextrosehydrat - Google Patents

Verfahren und Vorrichtung zur Herstellung von kristallisiertem Dextrosehydrat Download PDF

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Publication number
EP0147269B1
EP0147269B1 EP84402321A EP84402321A EP0147269B1 EP 0147269 B1 EP0147269 B1 EP 0147269B1 EP 84402321 A EP84402321 A EP 84402321A EP 84402321 A EP84402321 A EP 84402321A EP 0147269 B1 EP0147269 B1 EP 0147269B1
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European Patent Office
Prior art keywords
crystallization
zone
mass
vicinity
subjected
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EP84402321A
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English (en)
French (fr)
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EP0147269A3 (en
EP0147269A2 (de
Inventor
Gilbert Bodele
Pierrick Duflot
Bernard Valentin
Michel Huchette
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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Application filed by Roquette Freres SA filed Critical Roquette Freres SA
Priority to AT84402321T priority Critical patent/ATE32103T1/de
Publication of EP0147269A2 publication Critical patent/EP0147269A2/de
Publication of EP0147269A3 publication Critical patent/EP0147269A3/fr
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    • 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 production of crystallized dextrose monohydrate.
  • the known methods provide for the simultaneous use of several devices of the mixer type, arranged horizontally or vertically; these devices are equipped with stirring means and with temperature regulation means capable of establishing a decreasing temperature gradient in the mass subjected to crystallization, which includes the syrup and the germs.
  • the invention also relates to other arrangements which are preferably used at the same time and which will be more explicitly discussed below.
  • the single figure of the drawing schematically shows an installation according to the invention.
  • glucose syrups from an acidic and / or enzymatic hydrolysis of starch are used, having a dry matter content of approximately 55 to 85% by weight, with glucose entering at least 60% and, preferably, for a proportion greater than 90% by weight, in the constitution of the syrup with dry raw materials.
  • This concentrated syrup is conveyed to a vertical or inclined crystallization zone, which it runs continuously from top to bottom from a point located near its upper end and inside which it is subjected, in the presence of dextrose crystals playing the role of seeds of crystallization, to kneading and a globally decreasing temperature gradient 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 chosen in the range from 30 to 70 ° C, preferably from 35 to 55 ° C and, in practice, close from 40 to 50 ° C.
  • the temperature gradient established inside the crystallization zone within the mass subjected to crystallization corresponds to a decrease of 0.5 to 5 ° C, preferably from 2 to 4 ° C per linear meter of the area of crystallization 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 within a range of 15 to 40 ° C, preferably 20 to 30 ° C.
  • the fraction taken and recycled represents, by volume, from 10 to 40%, preferably from 25 to 35% of the volume of glucose syrup supplying the crystallization zone.
  • the rate of supply of glucose syrup is chosen such that the average residence time, statistical or theoretical, of a given fraction of the mass subjected to crystallization inside the crystallization zone is from 10 to 40 hours, preferably 20 to 30 hours; the value adopted depends on the heat exchange capacities of the means comprised by the zone and with the help of which is established, inside said zone within the mass subjected to crystallization, the decreasing temperature gradient.
  • the intermediate level at which the withdrawal of the fraction subjected to crystallization which is intended for recycling is carried out is preferably distant from the ends of the crystallization zone by at least a quarter of its total length and, in practice , of the order of at least two fifths of the total length of the said zone.
  • the viscosity of the mass subjected to crystallization which increases as the proportion of dextrose monohydrate crystals increases, that is to say in the downward direction, means that the crystallization zone is preferably equipped with means of delivery or suction suitable for ensuring the movement of the mass inside the zone, gravity alone may be insufficient.
  • the kneading and homogenization means comprised 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 generally of the type turbulent.
  • the product extracted from the crystallization zone and which constitutes, as already indicated, a rich phase baked mass comprises dextrose monohydrate crystals of a particle size spectrum characterized by a small proportion of fine and large crystals and therefore by a strong proportion of crystals of intermediate size, this spectrum does not vary over time, whereby the following treatment step, which consists in separating these crystals from the liquid phase in which they are immersed, does not experience any disturbance.
  • This separation comprises a turbination and possibly a clearing thanks to which the major part of the liquid phase is recovered; this forms hydrols whose dextrose concentration is lower than that of the starting glucose syrup - this concentration generally reaches 70 to 85% - and in which we find almost all of the di-, tri- and polysaccharides contained in the starting glucose syrup.
  • the hydrols collected can be recycled.
  • the XY axis is advantageously arranged vertically but can also be tilted.
  • the heat exchange capacity of 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, c 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 mean temperature difference at a given point in the enclosure between this water and the mass subjected to crystallization, is of the order of 6 at 12 ° C.
  • An installation according to the invention comprising a single cylindrical enclosure with a useful volume of 48 m 3 for a height of 8 meters.
  • the syrup temperature at the entrance to the enclosure is around 50 ° C.
  • a fraction of the mass during crystallization taken from a substantially median level of the enclosure is recycled, with a flow rate of 0.5 m 3 per hour.
  • the average passage time inside the enclosure of a given fraction of the mass subjected to crystallization is approximately 25 hours.
  • the rich phase baked clay extracted at the lower end of the enclosure is at a temperature in the region of 25 ° C, the temperature gradient decreasing overall from top to bottom therefore corresponding to approximately 3.2 ° C per meter .
  • the glucose content of the hydrols recovered after separation of the dextrose monohydrate crystals is 84% on dry matter, the complement to 100 being constituted by the polysaccharides.
  • the crystals collected after turbination and clearing have excellent physical and chemical properties.
  • Example 1 The apparatus and the operating conditions of Example 1 are used.
  • the recycled fraction is no longer taken at an intermediate level but at a point in the enclosure located in the last sixth of the total height.

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Confectionery (AREA)
  • Seasonings (AREA)

Claims (7)

1. Verfahren zur Herstellung von als Monohydrat kristallisierter Dextrose, bei welchem die der Kristallisation unterworfene Masse Kontinuierlich von oben nach unten und unter Maischen eine vertikal ausgerichtete oder geneigte Kristallisationszone durchläuft, in welcher ein Temperaturgradient herrscht, der insgesamt von oben nach unten abnimmt, dadurch gekennzeichnet, daß man
- die Kristallisationszone in der Nähe ihres oberen Endes einerseits mit einem Glucosesirup, der einen Glucosegehalt von mehr als 60 % und einen Gehalt an Trockensubstanz von mehr als 55 % aufweist, und anderseits mit einer der Kristallisation bereits unterworfenen Masse beschickt, welche aus einem mittleren Niveau der Kristallisationszone entnommen und in den Kreislauf rückgeführt wird, wobei dieses mittlere Niveau um eine Distanz von den Enden der Kristallisationszone entfernt ist, welche wenigstens.ein Sechstel der Gesamtlänge der genannten Zone beträgt, und wobei die Menge der der Kristallisation bereits unterworfenen und in den Kreislauf rückgeführten Masse 10 bis 40 Vol.-%, bezogen auf die in die Kristallisationszone eingeführte Menge an Glucosesirup, beträgt, und
- daß man kontinuierlich in der Nähe des unteren Endes der Kristallisationszone ein Produkt abzieht, welches an Dextrose-Monohydratkristallen stark angereichert ist und aus welchem man die genannten Kristalle gewinnt.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Anteil der der Kristallisation bereits unterworfenen Masse, welcher Anteil entnommen und in den Kreislauf rückgeführt wird, 25 bis 35 Vol.-% des in die Kristallisationszone eingebrachten Glucosesirups beträgt.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das mittlere Niveau, bei welchem die Entnahme des bereits der Kristallisation unterworfenen Anteils erfolgt, welcher Anteil für das Rückführen in den Kreislauf bestimmt ist, vorzugsweise von den Enden der Kristallisationszone um eine Distanz entfernt ist, welche wenigstens ein Viertel der Gesamtlänge der Kristallisationszone beträgt, und welche in der Praxis in der Größenordnung von wenigstens zwei Fünfteln der Gesamtlänge der genannten Zone liegt.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß
- die Temperatur des Sirups zum Zeitpunkt seiner Einführung in die Kristallisationszone auf einen Wert gebracht oder auf einem Wert gehalten wird, der in den Bereich von 30 bis 70 °C, vorzugsweise von 35 bis 55°C, fällt, und in der Praxis in der Nähe von 40 bis 50 °C liegt,
- der Temperaturgradient, der im Inneren der Kristallisationszone und inmitten der der Kristallisation unterworfenen Masse herrscht, einem Temperaturabfall von 0,5 bis 5 °C, vorzugsweise von 2 bis 4°C, je Linearmeter der Kristallisationszone entspricht, und
- daß am Ausgang der genannten Zone, und zwar an einem Punkt, der sich in der Nähe des unteren Endes dieser Zone befindet, die der Kristallisation unterworfene Masse, welche den Sirup, die anfänglich bereits vorhandenen Kristalle und die auf Grund des Kristallisationsvorganges gebildeten Kristalle umfaßt, auf eine Temperatur gebracht worden ist, welche in einem Bereich von 15 bis 40 °C, vorzugsweise von 20 bis 30 °C fällt.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die statistische oder theoretische mittlere Verweilzeit eines gegebenen Anteils der der Kristallisation im Inneren der Kristallisationszone unterworfenen Masse 10 bis 40 Stunden, vorzugsweise 20 bis 30 Stunden, beträgt.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß der als Ausgangsmaterial eingesetzte Glucosesirup einen Gehalt an Trockensubstanz von etwa 55 bis 85 Gew.-% aufweist, wobei die Glucose wenigstens 60 % und vorzugsweise einen höheren Anteil als 90 Gew.-% der Zusammensetzung der Trockensubstanz des Sirups ausmacht.
7. Vorrichtung zur Herstellung von kristallisierter Dextrose, welche Vorrichtung im wesentlichen aus einem Kristallisator (1) mit vertikaler oder geneigter Achse besteht, welcher Kristallisator (1) ausgestattet ist mit :
- einem Beschickungssystem (2) für Glucosesirup in der Nähe seines oberen Endes ;
- einem Maischsystem (4, 5) und einem Temperaturregelungssystem (6), welche geeignet sind, im Inneren des Kristallisators und inmitten der im Kristallisator enthaltenen, der Kristallisation unterworfenen Masse einen insgesamt von oben nach unten abnehmenden Temperaturgradienten aufzubauen, und
- mit einem System (3) zum kontinuierlichen Abziehen, in der Nähe des unteren Endes des Kristallisators, eines Produktes, welches dann durch geeignete Mittel zu einem System befördert wird, welches für die Gewinnung der Kristalle aus diesem Produkt geeignet ist,

dadurch gekennzeichnet, daß der Kristallisator (1) Einrichtungen (7) enthält, welche für die Entnahme einer Menge der der kristallisation unterworfenen Masse, welche Menge 10 bis 40 Vol.-% der in der Nähe des oberen Endes des Kristallisators (1) eingeführten Menge an Glucosesirup entspricht, geeignet sind, und zwar für die Entnahme aus einem mittleren Niveau (8) des Kristallisators (1), welches mittlere Niveau (8) von den Enden des Kristallisators um eine Distanz entfernt ist, welche wenigstens einem Sechstel der Gesamtlänge des Kristallisators (1) entspricht, wobei die genannten Einrichtungen (7) außerdem für die Rückführung dieser Masse in den Kreislauf und in den Kristallisator auf einem Niveau (9), welches sich in der Nähe des oberen Endes des Kristallisators (1) befindet, geeignet sind.
EP84402321A 1983-11-17 1984-11-14 Verfahren und Vorrichtung zur Herstellung von kristallisiertem Dextrosehydrat Expired EP0147269B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT84402321T ATE32103T1 (de) 1983-11-17 1984-11-14 Verfahren und vorrichtung zur herstellung von kristallisiertem dextrosehydrat.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8318318 1983-11-17
FR8318318A FR2555201B1 (fr) 1983-11-17 1983-11-17 Procede et installation de production de dextrose cristallise monohydrate

Publications (3)

Publication Number Publication Date
EP0147269A2 EP0147269A2 (de) 1985-07-03
EP0147269A3 EP0147269A3 (en) 1986-04-02
EP0147269B1 true EP0147269B1 (de) 1988-01-20

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ID=9294231

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EP84402321A Expired EP0147269B1 (de) 1983-11-17 1984-11-14 Verfahren und Vorrichtung zur Herstellung von kristallisiertem Dextrosehydrat

Country Status (12)

Country Link
US (1) US4620880A (de)
EP (1) EP0147269B1 (de)
JP (1) JPS60123493A (de)
KR (1) KR920006867B1 (de)
AT (1) ATE32103T1 (de)
AU (1) AU564900B2 (de)
CA (1) CA1242712A (de)
DE (1) DE3468905D1 (de)
ES (1) ES8600405A1 (de)
FI (1) FI78927C (de)
FR (1) FR2555201B1 (de)
SU (1) SU1452485A3 (de)

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
FR2582016B1 (fr) * 1985-05-15 1987-09-18 Roquette Freres Procede et installation de production de fructose cristallise anhydre
DE3541576A1 (de) * 1985-11-25 1987-05-27 Krupp Gmbh Verfahren zur dextrose-monohydrat-kristallisation
IT1313586B1 (it) * 1999-07-30 2002-09-09 Vomm Chemipharma Srl Metodo di cristallizzazione di sorbitolo e sorbitolo cristallizzatocosi' ottenuto.
CN101381384B (zh) * 2008-09-11 2012-09-26 西王集团有限公司 一种一水葡萄糖的结晶工艺

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1021173A (en) * 1912-01-09 1912-03-26 Hermann Wiese Process of refining sugar.
US2823242A (en) * 1953-09-08 1958-02-11 Phillips Petroleum Co Process and apparatus for crystal purification and separation
US2800411A (en) * 1954-03-31 1957-07-23 Phillips Petroleum Co Crystal purification apparatus and process
FR1154584A (fr) * 1955-07-02 1958-04-11 Buckau Wolf Maschf R Procédé de cristallisation en continu de glucose concentré
FR1295543A (fr) * 1961-04-28 1962-06-08 Aquitaine Petrole Procédé et appareil de cristallisation
DE1642536A1 (de) * 1966-10-28 1971-05-06 Struthers Scient And Internat Verfahren zur kontinuierlichen Kristallisierung von Dextrose
GB1210512A (en) * 1967-03-07 1970-10-28 Tate & Lyle Ltd Method of, and apparatus for, continuously producing crystals from a solution
BE727378A (de) * 1967-07-13 1969-07-24
US3617382A (en) * 1968-07-17 1971-11-02 Christos B Natsis Mixing apparatus as used in mass and heat transfer processes
DK147287C (da) * 1977-01-13 1984-11-05 Danske Sukkerfab Koeler til blandinger af krystaller og krystalliserende vaeske i produktionen af sukker og beslaegtede produkter
FR2493869A1 (fr) * 1980-11-10 1982-05-14 Fives Cail Babcock Procede de production de lactose cristallise et installation pour la mise en oeuvre de ce procede
US4357172A (en) * 1980-12-17 1982-11-02 Cpc International Inc. Process for continuous crystallization of alpha monohydrate dextrose utilizing high agitation

Also Published As

Publication number Publication date
EP0147269A3 (en) 1986-04-02
FI844490L (fi) 1985-05-18
SU1452485A3 (ru) 1989-01-15
ES537579A0 (es) 1985-10-16
ATE32103T1 (de) 1988-02-15
FI844490A0 (fi) 1984-11-15
FI78927B (fi) 1989-06-30
KR850003737A (ko) 1985-06-26
AU564900B2 (en) 1987-08-27
JPH052319B2 (de) 1993-01-12
FR2555201B1 (fr) 1986-10-31
ES8600405A1 (es) 1985-10-16
DE3468905D1 (en) 1988-02-25
US4620880A (en) 1986-11-04
FI78927C (fi) 1989-10-10
EP0147269A2 (de) 1985-07-03
JPS60123493A (ja) 1985-07-02
CA1242712A (en) 1988-10-04
AU3563284A (en) 1985-05-23
FR2555201A1 (fr) 1985-05-24
KR920006867B1 (ko) 1992-08-21

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