EP0147269A2 - 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
EP0147269A2
EP0147269A2 EP84402321A EP84402321A EP0147269A2 EP 0147269 A2 EP0147269 A2 EP 0147269A2 EP 84402321 A EP84402321 A EP 84402321A EP 84402321 A EP84402321 A EP 84402321A EP 0147269 A2 EP0147269 A2 EP 0147269A2
Authority
EP
European Patent Office
Prior art keywords
crystallization
zone
mass
enclosure
subjected
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.)
Granted
Application number
EP84402321A
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English (en)
French (fr)
Other versions
EP0147269A3 (en
EP0147269B1 (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
Original Assignee
Roquette Freres 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.)
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Publication date
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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
Application granted granted Critical
Publication of EP0147269B1 publication Critical patent/EP0147269B1/de
Expired 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
    • 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 originating from an acidic and / or enzymatic hydrolysis of starch, having a dry matter content of approximately 55 to 85% by weight, the glucose entering for at least 60%, are used as raw material, preferably for a higher proportion less than 90 ⁇ by weight, in the dry matter composition of the syrup.
  • This concentrated syrup is conveyed to a vertical or inclined crystallization zone, 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 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 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 reduction of 0.5 to 5 ° C, preferably from 2 to 4 ° C per linear meter of the zone 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 crystals of dextrose monohydrate increases, that is to say in the descending direction, means that the zone of crystallization tion is preferably equipped with delivery or suction means suitable for ensuring the movement of the mass inside the area, gravity alone may be insufficient.
  • 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 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 from 7L 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 control system, the speed of rotation of the mixing means and the speed with which, under the influence 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 to such that the temperature gradient provided for in accordance with the invention is established within the whole of the mass subjected to crystallization.
  • 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 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 approximately 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 dextrose monohydrate crystals is 84% on dry matter, the complement to 100 being constituted by 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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Confectionery (AREA)
  • Seasonings (AREA)
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
FR8318318A FR2555201B1 (fr) 1983-11-17 1983-11-17 Procede et installation de production de dextrose cristallise monohydrate
FR8318318 1983-11-17

Publications (3)

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

Family

ID=9294231

Family Applications (1)

Application Number Title Priority Date Filing Date
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)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202999A1 (de) * 1985-05-15 1986-11-26 Roquette Frˬres Verfahren und Vorrichtung zur Herstellung von kristalliner wasserfreier Dextrose
EP0203844A1 (de) * 1985-05-15 1986-12-03 Roquette Frˬres Verfahren und Vorrichtung zur Herstellung von wasserfreier kristalliner Fruktose

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
BE727378A (de) * 1967-07-13 1969-07-24
DE1642536A1 (de) * 1966-10-28 1971-05-06 Struthers Scient And Internat Verfahren zur kontinuierlichen Kristallisierung von Dextrose

Family Cites Families (8)

* 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
GB1210512A (en) * 1967-03-07 1970-10-28 Tate & Lyle Ltd Method of, and apparatus for, continuously producing crystals from a solution
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
BE727378A (de) * 1967-07-13 1969-07-24

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 97, no. 14, octobre 1982, page 86, abrégé no. 111551c, Columbus, Ohio, US; S. KUCERA: "Apparatus for sugar crystallization", & CS - A - 209 130 (S. KUCERA) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202999A1 (de) * 1985-05-15 1986-11-26 Roquette Frˬres Verfahren und Vorrichtung zur Herstellung von kristalliner wasserfreier Dextrose
EP0203844A1 (de) * 1985-05-15 1986-12-03 Roquette Frˬres Verfahren und Vorrichtung zur Herstellung von wasserfreier kristalliner Fruktose

Also Published As

Publication number Publication date
US4620880A (en) 1986-11-04
CA1242712A (en) 1988-10-04
FI78927C (fi) 1989-10-10
JPH052319B2 (de) 1993-01-12
EP0147269A3 (en) 1986-04-02
ES537579A0 (es) 1985-10-16
KR850003737A (ko) 1985-06-26
FI844490L (fi) 1985-05-18
ES8600405A1 (es) 1985-10-16
JPS60123493A (ja) 1985-07-02
FI78927B (fi) 1989-06-30
SU1452485A3 (ru) 1989-01-15
DE3468905D1 (en) 1988-02-25
AU564900B2 (en) 1987-08-27
ATE32103T1 (de) 1988-02-15
FR2555201A1 (fr) 1985-05-24
EP0147269B1 (de) 1988-01-20
FR2555201B1 (fr) 1986-10-31
KR920006867B1 (ko) 1992-08-21
AU3563284A (en) 1985-05-23
FI844490A0 (fi) 1984-11-15

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