EP0052541A1 - Verfahren zur Herstellung kristallisierter Laktose und Vorrichtung zur Durchführung dieses Verfahrens - Google Patents

Verfahren zur Herstellung kristallisierter Laktose und Vorrichtung zur Durchführung dieses Verfahrens Download PDF

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Publication number
EP0052541A1
EP0052541A1 EP81401637A EP81401637A EP0052541A1 EP 0052541 A1 EP0052541 A1 EP 0052541A1 EP 81401637 A EP81401637 A EP 81401637A EP 81401637 A EP81401637 A EP 81401637A EP 0052541 A1 EP0052541 A1 EP 0052541A1
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EP
European Patent Office
Prior art keywords
crystals
crystallization
mother liquor
lactose
whey
Prior art date
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Application number
EP81401637A
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English (en)
French (fr)
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EP0052541B1 (de
Inventor
Paul Credoz
Pierre Beuneu
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.)
Fives Cail Babcock SA
Pierre Guerin SA
Original Assignee
Fives Cail Babcock SA
Pierre Guerin SA
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Publication of EP0052541A1 publication Critical patent/EP0052541A1/de
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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
    • C13K5/00—Lactose

Definitions

  • the present invention relates to the production of lactose crystallized in its three commercial forms: crude or technical lactose whose purity varies from 92 to 98%, edible or edible lactose whose purity is greater than 98 / and lactose codex or pharmaceutical whose purity is greater than 99.85%.
  • lactose is obtained from whole, or deproteinized and / or demineralized whey.
  • the whey is concentrated by evaporation, subjected to crystallization, and the crystals obtained are separated and ground and possibly subjected to refining.
  • crystallization is carried out by cooling the concentrated whey and the percentage of crystallized lactose relative to the total lactose is low.
  • the present invention makes it possible to significantly increase the percentage of lactose recovered without appreciable increase in investment costs and energy consumption.
  • the process which is the subject of the invention is characterized in that the first crystallization phase takes place in an apparatus for crystallization by continuous evaporation, that the mixture of mother liquor and crystals produced by this apparatus is subjected to a wringing centrifugal in a continuous sieve wringer to separate the mother liquor lactose crystals whose dimensions are greater than a predetermined dimension between 40 and 90 microns, that the mother liquor containing the small crystals whose dimensions are less than this predetermined dimension is cooled in a double-shell tank or a kneader continuous operation to cause the magnification of these small crystals and the product obtained is subjected to a second spin in a centrifugal continuous operation machine to separate the crystals from the mother liquor.
  • the crystallization phase by evaporation is carried out at the maximum temperature compatible with the thermosensitivity of the products and with a concentration of dry matter such that the supersaturation is always as high as possible: these two conditions make it possible to have a very high crystallization speed, of the order of ten times that obtained in a crystallizer by cooling, and to obtain a good yield of crystallized lactose.
  • its temperature during this crystallization phase is of the order of 50 to 55 ° C; in the case where deproteinized and / or demineralized whey is treated, the temperature is of the order of 65 to 70 ° C.
  • the dry matter concentration of the product subjected to this crystallization phase is of the order of 50-55%.
  • the residence time of the product in the apparatus for crystallization by evaporation is chosen so as to obtain, on leaving the apparatus, a dry matter content as high as possible and compatible with the conditions of transport and subsequent treatment: pumping, spin, etc ...
  • the residence time is between 1 and 3 hours
  • the dry matter content at the outlet of the apparatus is approximately 80%
  • the yield of crystals is 50 to 55%.
  • Part of the mother liquor from the first spin can be returned to the inlet of the crystallization apparatus by evaporation, the small lactose crystals it contains being used as germs of crystallization.
  • the flow of recycled mother liquor will be linked to the nature of the product treated and the quality of the crystals desired.
  • the seed crystals introduced into the crystallization apparatus can be obtained by grinding lactose crystals.
  • the crystals separated from the mother liquor during the first spin are advantageously subjected to washing with water or with water added with hydrochloric acid to increase their purity.
  • an apparatus consisting of a horizontal tank divided by transverse partitions into several compartments which are successively crossed by the mixture of concentrated whey and crystals moving from one end to the other is used.
  • each compartment comprising heating means and an inlet for the product to be treated.
  • the heating means can be constituted by hollow elements (tubes or plates) heated by steam, a fraction of which consists of steam produced in the crystallization apparatus and recompressed by means of a thermocompressor or a motorbike. -compressor.
  • This solution makes it possible to have an energy consumption close to that obtained with conventional methods with a much higher lactose yield.
  • the temperature of the heating steam will be of the order of 65 to 80 ° C.
  • first and second spins we use continuous spin dryers with frustoconical sieve.
  • This type of extractor makes it possible to obtain crystals whose moisture content is much lower than that of the crystals separated by means of the centrifugal decanters usually used and to clearly separate the crystals whose dimensions are greater and less than a predetermined dimension.
  • These extractors will advantageously be provided with a crystal washing system.
  • lactose crystals obtained by the process described above will be refined and for this will be dissolved in water and the solution obtained, optionally purified, will be treated according to the same process.
  • lactose codex very high purity lactose (lactose codex) can be obtained by mixing the lactose crystals from the first and second spin cycles with water and subjecting this mixture to a final spin cycle and then washing in a centrifugal spinner. with continuous operation, the mother liquor separated by spinning being returned to the head of the installation, upstream of the crystallization apparatus by evaporation, and the washing water being used to prepare said mixture.
  • the crystals obtained which have dimensions of between 50 and 250 microns, are ground to the state of micronized powder (1 to 5 microns approximately).
  • FIG. 1 The installation shown diagrammatically in FIG. 1 consists essentially of an evaporative crystallization apparatus 10, a first centrifugal wringer 12, a mixer-cooler 14 and a second centrifugal wringer 16. All of these apparatuses are in continuous operation, that is to say that the supply and the evacuation of the products are done continuously.
  • the device 10 consists of a closed cylindrical tank arranged horizontally and divided into several compartments 1 to 5 by transverse partitions 18. These partitions are lower than the tank so that the various compartments communicate with each other at their upper part. Openings are drilled in the partitions 18 to allow the passage of the treated product from one compartment to the other.
  • thermo-compressor 22 One or more heating bundles 20 formed of horizontal tubes arranged parallel to the axis of the tank are placed in the lower part thereof. These tubes are supplied with steam by a thermo-compressor 22 and provide heating for the various compartments; they are permanently embedded in the treated product filling the lower part of the tank.
  • the thermo-compressor 22 is used to recompress, by means of live steam, part of the steam produced in the apparatus 10 and taken from the upper part of the tank. Alternatively, a motor compressor could be used.
  • Inlets 24 for the product to be treated are provided in each compartment and an outlet connected to a pump 25 is provided in the last compartment 5.
  • the centrifugal dryers 12 and 16 are of the type described in French patent 79/06829. They include a frustoconical basket 26, flared upward and mounted inside of a tank 28. The basket is mounted on a vertical pivot and is rotated about its axis. The product to be spun is poured into the bottom of the basket. A sieve rests on the interior surface of the basket and the liquid phase of the product to be wrung as well as the solid particles whose dimensions are smaller than the sieve openings are collected in a chamber 30 constituted by a ferrule whose upper end is located near the upper edge of the basket and by a bottom fixed to the shell.
  • Solid particles whose dimensions are larger than the sieve openings are moved upward on the sieve by centrifugal force, and are finally ejected at the upper end of the basket into the tank 28 from where they fall into a hopper 32 connected to the bottom of the tank.
  • Watering ramps 33 placed inside the basket make it possible to wash the solid materials before they are expelled from the basket.
  • the mixer-cooler is of the type described in French patent n ° 79/18325. It consists of a cylindrical tank 34, of circular section and arranged vertically. Ports are provided in the lower part and in the upper part of the tank for the admission and evacuation of products.
  • a vertical shaft 35 is placed in the axis of the tank and carries members ensuring both the stirring and the cooling of the treated products; these organs can, for example, be constituted by tubes wound in a spiral and traversed by a refrigerant. Alternatively, sheets of tubes fixed to the wall of the tank and ensuring the cooling of the products could alternate with blades integral with the shaft and ensuring the mixing of the products.
  • the shaft is rotated by a geared motor group 36 mounted on the tank.
  • the whey previously concentrated in an evaporator is continuously introduced into the various compartments of the apparatus 10 where it is heated by the steam supplying the tubes of the bundle 20.
  • a concentrated solution is also introduced into the first compartment containing crystals of small dimensions coming from the wringer 12.
  • the concentration of the whey in the various compartments is maintained at the desired value by controlling the flow rate of supply of whey or steam, which ensures regular magnification of the crystals introduced into the first compartment throughout their stay in the device. .
  • the mixture of concentrated whey or mother liquor and crystals is continuously extracted from the last compartment by the pump 25.
  • a level regulator controls this pump to maintain the level of the products in the tank substantially at mid-height.
  • the dimensions of the device are chosen, depending on the flow to be treated, so that the residence time has the desired value.
  • thermo-compressor 22 Part of the steam produced in the apparatus 10 is recompressed by means of the thermo-compressor 22, which is moreover supplied with live steam by a pipe 38, and is used for heating the bundle 20.
  • the pump 26 feeds the wringer 12.
  • the lactose crystals whose dimensions are greater than those of the sieve openings, for example greater than 90 microns, are separated and discharged at 40 to the subsequent stages of the treatment: grinding -drying or refining.
  • the crystals are washed with water or with water acidulated with hydrochloric acid at pH 2.5 to 3.5 by means of ramps 33.
  • Most of the mother liquor and the small crystals which have passed through the sieve of the wringer are sent to the mixer-cooler 14.
  • the other part is introduced by means of a pump 42 into the first compartment of the apparatus 10 where the small crystals serve as sprouts; the flow rate of the pump 42 can be controlled as a function of the feed flow rate whey from the device 10.
  • the mixer-cooler 14 the mixture of mother liquor and crystals which had a temperature of 50 to 70 ° C at the outlet of the apparatus 10 is cooled to about 10-15 ° C. This cooling causes the crystals to magnify and, consequently, allows an additional recovery of the lactose and facilitates the separation of the crystals in the wringer 16.
  • the pump 44 ensures both the supply of the wringer 16 and the recycling of a fraction of the water-mother-crystal mixture taken from the bottom of the mixer-cooler 14; this recycling overcomes the rapid settling of the crystals in the mixer.
  • the sieve of the wringer 16 must be very fine to allow almost all of the lactose crystals to be recovered; the dimensions of the screen openings will for example be between 40 and 60 microns.
  • These crystals are directed to the subsequent stages of the treatment: grinding-drying or refining. As a variant, these crystals could be dissolved in water and the solution obtained could be introduced with the whey, into the apparatus 10.
  • FIG. 2 illustrates a process for the production of very high purity lactose from the crystals separated in the centrifugal dryers 12 and 16.
  • These crystals are mixed, in a mixer 46, with washing water coming from a centrifugal wringer at continuous operation 48 and this mixture is then treated in this wringer where the crystals are first separated from the mother liquor and then washed by means of a ramp 50 supplied with water.
  • the wringer 48 is designed to allow the separation of the mother liquor and the washing water. As already mentioned, the latter is sent to the mixer 46 and mixed with the separated crystals in the extractors 12 and 16.
  • the mother liquor is returned, by a pipe 52 to the inlet of the evaporator placed in upstream of the crystallization apparatus 10.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Dairy Products (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
EP81401637A 1980-11-10 1981-10-19 Verfahren zur Herstellung kristallisierter Laktose und Vorrichtung zur Durchführung dieses Verfahrens Expired EP0052541B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8023958 1980-11-10
FR8023958A FR2493869A1 (fr) 1980-11-10 1980-11-10 Procede de production de lactose cristallise et installation pour la mise en oeuvre de ce procede

Publications (2)

Publication Number Publication Date
EP0052541A1 true EP0052541A1 (de) 1982-05-26
EP0052541B1 EP0052541B1 (de) 1985-02-13

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EP81401637A Expired EP0052541B1 (de) 1980-11-10 1981-10-19 Verfahren zur Herstellung kristallisierter Laktose und Vorrichtung zur Durchführung dieses Verfahrens

Country Status (4)

Country Link
US (1) US4404038A (de)
EP (1) EP0052541B1 (de)
DE (1) DE3168938D1 (de)
FR (1) FR2493869A1 (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0311977A2 (de) * 1987-10-14 1989-04-19 Valio Meijerien Keskusosuusliike Verfahren zur Ausscheidung der Laktose aus Molke
EP2757162A1 (de) * 2013-01-22 2014-07-23 DMK Deutsches Milchkontor GmbH Verfahren zur Steigerung der Ausbeute bei der Lactoseherstellung (II)
EP2767596A1 (de) * 2013-02-16 2014-08-20 DMK Deutsches Milchkontor GmbH Verfahren zur Steigerung der Ausbeute bei der Lactoseherstellung (III)
EP2756206B2 (de) † 2011-09-14 2020-10-21 KNORR-BREMSE Systeme für Nutzfahrzeuge GmbH Scheibenbremse eines kraftfahrzeugs und bremsbelag

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2555201B1 (fr) * 1983-11-17 1986-10-31 Roquette Freres Procede et installation de production de dextrose cristallise monohydrate
US6548099B1 (en) * 2000-11-28 2003-04-15 Hershey Foods Corporation Process for crystallizing amorphous lactose in milk powder
AUPR217700A0 (en) * 2000-12-19 2001-01-25 Food Science Australia Methods for purification of lactose
US20060096525A1 (en) * 2004-11-08 2006-05-11 Sirkar Kamalesh K Solid hollow fiber cooling crystallization systems and methods
CN101155590A (zh) 2005-02-10 2008-04-02 葛兰素集团有限公司 使用预分选技术制备乳糖的方法以及由此形成的药物制剂
LT2629623T (lt) 2010-10-07 2018-08-27 Fonterra Co-Operative Group Limited Laktozės gamyba
JP6186193B2 (ja) * 2013-07-08 2017-08-23 株式会社ササクラ 水溶液の蒸発処理方法
WO2016193138A1 (en) * 2015-05-29 2016-12-08 Spx Flow Technology Danmark A/S Second pass lactose crystallization

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2768912A (en) * 1952-03-10 1956-10-30 Western Condensing Co Separation of crystallized lactose from whey solids
FR1519209A (fr) * 1966-04-14 1968-03-29 Foremost Dairies Procédé de traitement de petit lait liquide
FR1581088A (de) * 1968-07-17 1969-09-12
DE1642536A1 (de) * 1966-10-28 1971-05-06 Struthers Scient And Internat Verfahren zur kontinuierlichen Kristallisierung von Dextrose
US3721585A (en) * 1971-01-28 1973-03-20 Foremost Mckesson Method for manufacture of lactose
DE2930282A1 (de) * 1979-07-26 1981-02-19 Helmut Dipl Ing Hayer Lactoseherstellungsverfahren

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1715049A (en) * 1926-09-04 1929-05-28 Bernard H Varnau Process for manufacture of extra fine soft granulated sugar
US2569357A (en) * 1947-06-05 1951-09-25 Werkspoor Nv Process for crystallizing solutions
US2555212A (en) * 1947-06-20 1951-05-29 M & R Dietetic Lab Inc Method of making lactose
US2778750A (en) * 1953-03-24 1957-01-22 Armour & Co Ion exchange purification of whey in the preparation of lactose
NL6908590A (de) * 1969-06-05 1970-12-08
DE2014527A1 (de) * 1970-03-25 1971-10-21 Schneider, Prof Dr Ferdinand, 3300 Braunschweig Verfahren zur kontinuierlichen Kn stalhsation von Saccharose
FI46631C (fi) * 1971-03-11 1973-05-08 Suomen Sokeri Oy Menetelmä fruktoosin kiteyttämiseksi väkevöidystä vesiliuoksesta
US3981739A (en) * 1974-08-30 1976-09-21 Amstar Corporation Continuous crystallization
FR2374067A1 (fr) * 1976-12-14 1978-07-13 Fives Cail Babcock Procede et installation de production de germes de cristallisation selectionnes, applicables aux appareils cristalliseurs discontinus ou continus, particulierement pour bas produit de sucrerie
US4099983A (en) * 1977-05-31 1978-07-11 Wittenberg Lester H Process for preparing high purity lactose

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2768912A (en) * 1952-03-10 1956-10-30 Western Condensing Co Separation of crystallized lactose from whey solids
FR1519209A (fr) * 1966-04-14 1968-03-29 Foremost Dairies Procédé de traitement de petit lait liquide
DE1642536A1 (de) * 1966-10-28 1971-05-06 Struthers Scient And Internat Verfahren zur kontinuierlichen Kristallisierung von Dextrose
FR1581088A (de) * 1968-07-17 1969-09-12
US3721585A (en) * 1971-01-28 1973-03-20 Foremost Mckesson Method for manufacture of lactose
DE2930282A1 (de) * 1979-07-26 1981-02-19 Helmut Dipl Ing Hayer Lactoseherstellungsverfahren

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0311977A2 (de) * 1987-10-14 1989-04-19 Valio Meijerien Keskusosuusliike Verfahren zur Ausscheidung der Laktose aus Molke
EP0311977A3 (en) * 1987-10-14 1990-12-27 Valio Meijerien Keskusosuusliike A process of recovering lactose from whey
EP2756206B2 (de) † 2011-09-14 2020-10-21 KNORR-BREMSE Systeme für Nutzfahrzeuge GmbH Scheibenbremse eines kraftfahrzeugs und bremsbelag
EP2757162A1 (de) * 2013-01-22 2014-07-23 DMK Deutsches Milchkontor GmbH Verfahren zur Steigerung der Ausbeute bei der Lactoseherstellung (II)
US9540703B2 (en) 2013-01-22 2017-01-10 Dmk Deutsches Milchkontor Gmbh Method for increasing the yield in lactose production (II)
EP2767596A1 (de) * 2013-02-16 2014-08-20 DMK Deutsches Milchkontor GmbH Verfahren zur Steigerung der Ausbeute bei der Lactoseherstellung (III)
US9079932B2 (en) 2013-02-16 2015-07-14 Dmk Deutsches Milchkontor Gmbh Method for increasing the yield in lactose production (III)

Also Published As

Publication number Publication date
FR2493869B1 (de) 1983-12-23
FR2493869A1 (fr) 1982-05-14
EP0052541B1 (de) 1985-02-13
US4404038A (en) 1983-09-13
DE3168938D1 (en) 1985-03-28

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