EP0052541B1 - Process for the manufacture of crystallized lactose and apparatus for carrying out this method - Google Patents

Process for the manufacture of crystallized lactose and apparatus for carrying out this method Download PDF

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Publication number
EP0052541B1
EP0052541B1 EP81401637A EP81401637A EP0052541B1 EP 0052541 B1 EP0052541 B1 EP 0052541B1 EP 81401637 A EP81401637 A EP 81401637A EP 81401637 A EP81401637 A EP 81401637A EP 0052541 B1 EP0052541 B1 EP 0052541B1
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Prior art keywords
crystals
crystallization
process according
unit
mother liquor
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German (de)
French (fr)
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EP0052541A1 (en
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Paul Credoz
Pierre Beuneu
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Fives Cail Babcock SA
Pierre Guerin SA
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Fives Cail Babcock SA
Pierre Guerin SA
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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: raw or technical lactose whose purity varies from 92 to 98% by weight, 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.
  • Such a process is described in US Patent 2,768,912.
  • 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 is carried out in an apparatus for crystallization by continuous evaporation, that the mixture of mother liquor and crystals leaving this apparatus is subjected to a first centrifugal spin in a continuous sieve wringer to separate lactose crystals whose dimensions are greater than a predetermined dimension of between 40 and 90 ⁇ m from the light, than the mother liquor containing the small crystals whose dimensions are smaller than this predetermined dimension is cooled to cause the magnification of these small crystals and that the product obtained is subjected to a second centrifugal spin 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% by weight.
  • the residence time of the product in the apparatus for crystallization by evaporation is chosen so as to obtain at the outlet of 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 rate of dry matter at the outlet of the device is approximately 80% by weight
  • the crystal yield (weight of crystallized lactose / total weight of lactose) 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.
  • the crystallization device is heated by steam, the temperature of which is between 65 ° C and 80 ° C. Part of the heating vapor of the crystallization device can be constituted by the steam produced in this device and recompressed.
  • the cooling of the mixture of mother liquor and crystals may be carried out in a cooling mixer comprising a cylindrical tank, with a vertical axis, and a rotary shaft placed in the axis of the tank and carrying members which ensure mixing and / or cooling the treated product.
  • 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 spins with water and subjecting this mixture to a final spin 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 ⁇ m, are ground to the state of micronized powder (1 to 5 ⁇ m approximately).
  • the installation shown schematically in the drawing consists essentially of an evaporative crystallization device 10, a first centrifugal wringer 12, a mixer-cooler 14 and a second centrifugal wringer 16. All these devices are in continuous operation, that is to say 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 FR-A-2451778. They comprise a frustoconical basket 26, flared upwards and mounted inside 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 ferrule.
  • the solid particles whose dimensions are larger than the openings of the screen are moved upwards on the screen, 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 FR-A-2461754. 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 rotary 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 introduced continuously into the various compartments of the apparatus 10 where it is heated by the steam supplying the tubes of the bundle 20. It is also introduced into the first compartment a concentrated solution containing crystals of small dimensions coming from the wringer 12. Under the action of the heat supplied by the heating steam, part of the water evaporates and the whey is brought to the state of supersaturation.
  • the concentration of whey in the different compartments is hand held at the desired value by controlling the feed rate 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 25 feeds the wringer 12.
  • the lactose crystals the dimensions of which are greater than those of the openings of the sieve, for example greater than 90 ⁇ m, are separated and discharged at 40 to the subsequent stages of the treatment.
  • 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 whey supply flow rate of the apparatus 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 etc to grow larger, therefore, allows additional lactose recovery 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 ⁇ m. These crystals are directed to the later stages of processing. As a variant, these crystals could be dissolved in water and the solution obtained could be introduced with the whey, into the apparatus 10.
  • the crystals separated in the centrifugal dryers 12 and 16 are used for the production of very high purity lactose. These crystals are mixed, in a mixer 46, with washing water coming from a third continuous centrifugal wringer 48 and this mixture is then treated in this wringer where the crystals are first separated from the mother liquor 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)

Description

La présente invention concerne la production de lactose cristallisé sous ses trois formes commerciales: lactose brut ou technique dont la pureté varie de 92 à 98% en poids, lactose édible ou alimentaire dont la pureté est supérieure à 98% et lactose codex ou pharmaceutique dont la pureté est supérieure à 99,85%.The present invention relates to the production of lactose crystallized in its three commercial forms: raw or technical lactose whose purity varies from 92 to 98% by weight, edible or edible lactose whose purity is greater than 98% and lactose codex or pharmaceutical whose purity is greater than 99.85%.

Le lactose commercial est obtenu à partir de lactosérums entiers, ou déprotéinés et/ou déminéralisés. Le lactosérum est concentré par évaporation, soumis à cristallisation, et les cristaux obtenus sont séparés et broyés et éventuellement soumis à un raffinage. Un tel procédé est décrit dans le brevet US 2.768.912. Généralement, la cristallisation est réalisée par refroidissement du lactosérum concentré et le pourcentage de lactose cristallisé par rapport au lactose total est faible. Pour améliorer le taux de récupération du lactose, on a proposé d'effectuer la cristallisation en deux étapes, le lactosérum concentré étant tout d'abord amené à l'état sursaturé dans une chaudière à cuire du type utilisé en sucrerie et ensemencé au moyen de germes cristallins, le contenu de la chaudière étant ensuite transféré dans un cristalliseur classique où il est refroidi pour compléter la cristallisation. Ce procédé a l'inconvénient d'être discontinu, long et coûteux, à cause de l'importante consommation de vapeur de la chaudière à cuire.Commercial 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. Such a process is described in US Patent 2,768,912. Generally, crystallization is carried out by cooling the concentrated whey and the percentage of crystallized lactose relative to the total lactose is low. To improve the lactose recovery rate, it has been proposed to carry out the crystallization in two stages, the concentrated whey being first brought to the supersaturated state in a boiling boiler of the type used in sugar refinery and sown by means of crystalline germs, the contents of the boiler then being transferred to a conventional crystallizer where it is cooled to complete the crystallization. This process has the disadvantage of being discontinuous, long and expensive, because of the large consumption of steam from the boiler to be cooked.

La présente invention permet d'augmenter notablement le pourcentage de lactose récupéré sans augementation sensible des frais d'investissement et de la consommation d'énergie.The present invention makes it possible to significantly increase the percentage of lactose recovered without appreciable increase in investment costs and energy consumption.

Le procédé objet de l'invention est caractérisé en ce que la première phase de cristallisation est effectuée dans un appareil de cristallisation par évaporation à marche continue, que le mélange d'eau-mère et de cristaux sortant de cet appareil est soumis à un premier essorage centrifuge dans une essoreuse à tamis à marche continue pour séparer de l'eaumère les cristaux de lactose dont les dimensions sont supérieures à une dimension prédéterminée comprise entre 40 et 90 pm, que l'eau-mère contenant les petits cristaux dont les dimensions sont inférieures à cette dimension prédéterminée est refroidie pour provoquer le grossissement de ces petits cristaux et que le produit obtenu est soumis à un second essorage centrifuge pour séparer les cristaux de l'eau-mère.The process which is the subject of the invention is characterized in that the first crystallization phase is carried out in an apparatus for crystallization by continuous evaporation, that the mixture of mother liquor and crystals leaving this apparatus is subjected to a first centrifugal spin in a continuous sieve wringer to separate lactose crystals whose dimensions are greater than a predetermined dimension of between 40 and 90 μm from the light, than the mother liquor containing the small crystals whose dimensions are smaller than this predetermined dimension is cooled to cause the magnification of these small crystals and that the product obtained is subjected to a second centrifugal spin to separate the crystals from the mother liquor.

La phase de cristallisation par évaporation est conduite à la température maximale compatible avec la thermosensibilité des produits et avec une concentration en matières sèches telle que la sursaturation soit toujours la plus élevée possible: ces deux conditions permettent d'avoir une vitesse de cristallisation très élevée, de l'ordre de dix fois celle obtenue dans un cristalliseur par refroidissement, et d'obtenir un bon rendement en lactose cristallisé. Lorsqu'on traite du lactosérum entier, sa température au cours de cette phase de cristallisation est de l'ordre de 50° à 55°C; dans le cas où on traite du lactosérum déprotéiné et/ou déminéralisé la température est de l'ordre de 65° à 70°C. La concentration en matières sèches du produit soumis à cette phase de cristallisation est de l'ordre de 50-55% en poids.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. When treating whole whey, 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% by weight.

Le temps de séjour du produit dans l'appareil de cristallisation par évaporation est choisi de manière à obtenir à la sortie de l'appareil une teneur en matières sèches aussi èlevée que possible et compatible avec les conditions de transport et de traitement ultérieures: pompage, essorage, etc.The residence time of the product in the apparatus for crystallization by evaporation is chosen so as to obtain at the outlet of the apparatus a dry matter content as high as possible and compatible with the conditions of transport and subsequent treatment: pumping, spin, etc.

Par exemple, dans le cas où on traite du lactosérum déprotéiné et déminéralisé, le temps de séjour est compris entre 1 et 3 heures, le taux de matières, sèches à la sortie de l'appareil est d'environ 80% en poids et le rendement en cristaux (poids de lactose cristallisé/poids total de lactose) est de 50 à 55%.For example, in the case of deproteinized and demineralized whey, the residence time is between 1 and 3 hours, the rate of dry matter at the outlet of the device is approximately 80% by weight and the crystal yield (weight of crystallized lactose / total weight of lactose) is 50 to 55%.

Une partie de l'eau-mère provenant du premier essorage pourra être ramenée à l'entrée de l'appareil de cristallisation par évaporation, les petits cristaux de lactose qu'elle contient étant utilisés comme germes de cristallisation. Le débit d'eau-mère recyclée sera lié à la nature du produit traité et à la qualité des cristaux désirée. En variante, les germes cristallins introduits dans l'appareil de cristallisation peuvent être obtenus par broyage de cristaux de lactose.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. Alternatively, the seed crystals introduced into the crystallization apparatus can be obtained by grinding lactose crystals.

Les cristaux séparés de l'eau-mère au cours du premier essorage sont avantageusement soumis à un lavage à l'eau ou à l'eau additionnée d'acide chlorhydrique pour aug- menteur leur pureté.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.

L'appareil de cristallisation est chauffé par de la vapeur dont la température est comprise entre 65°C et 80°C. Une partie de la vapeur de chauffage de l'appareil de cristallisation pourra être constituée par de la vapeur produite dans cet appareil et recomprimée.The crystallization device is heated by steam, the temperature of which is between 65 ° C and 80 ° C. Part of the heating vapor of the crystallization device can be constituted by the steam produced in this device and recompressed.

Pour les premier et second essorages on utilise des essoreuses à marche continue à tamis tronconique. Ce type d'essoreuse permet d'obtenir des cristaux dont le taux d'humidité est beaucoup plus faible que celui des cristaux séparés au moyen de décanteurs centrifuges habituellement utilisés et de séparer nettement les cristaux dont les dimensions sont supérieures et inférieures à une dimension prédéterminée. Ces essoreuses seront avantageusement munies d'un système de lavage des cristaux.For the first and second spins we use continuous wringers with frustoconical sieve. This type of wringer makes it possible to obtain crystals whose moisture content is much lower than that of the crystals separated by means of 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 fitted with a crystal washing system.

Le refroidissement du mélange d'eau-mère et de cristaux pourra être effectué dans un malaxeur refroidisseur comportant une cuve cylindrique, à axe vertical, et un arbre rotatif placé dans l'axe de la cuve et portant des organes qui assurent le brassage et/ou le refroidissement du produit traité.The cooling of the mixture of mother liquor and crystals may be carried out in a cooling mixer comprising a cylindrical tank, with a vertical axis, and a rotary shaft placed in the axis of the tank and carrying members which ensure mixing and / or cooling the treated product.

Pour la production de lactose de très haute pureté, les cristaux de lactose obtenus par le procédé décrit ci-dessus seront raffinés et pour cela seront dissous dans de l'eau et la solution obtenue, éventuellement épurée, sera traitée suivant le même procédé.For the production of very high purity lactose, the 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.

En variante, on peut obtenir du lactose de très haute pureté (lactose codex) en mélangeant les cristaux de lactose provenant des premier et second essorages à de l'eau et en soumettant ce mélange à un dernier essorage puis à un lavage dans une essoreuse centrifuge à marche continue, l'eau-mère séparée par essorage étant renvoyée en tête de l'installation, en amont de l'appareil de cristallisation par évaporation, et l'eau de lavage étant utilisée pour préparer ledit mélange. Pour la mise en oeuvre de ce procédé on pourra utiliser une installation comportant en plus d'un appareil de cristallisation à marche continue, d'un malaxeur-refroidisseur et de deux essoreuses centrifuges, un malaxeur recevant les cristaux séparés dans les deux essoreuses et une troisième essoreuse centrifuge qui est munie d'une rampe de lavage à l'eau et dont la sortie des eaux du lavage est reliée à l'entrée dudit malaxeur.Alternatively, very high purity lactose (lactose codex) can be obtained by mixing the lactose crystals from the first and second spins with water and subjecting this mixture to a final spin 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. For the implementation of this process, it is possible to use an installation comprising in addition to a continuous crystallization apparatus, a mixer-cooler and two centrifugal dryers, a mixer receiving the crystals separated in the two dryers and a third centrifugal wringer which is provided with a ramp for washing with water and the outlet of the washing water being connected to the inlet of said mixer.

Les cristaux obtenus, qui ont des dimensions comprises entre 50 et 250 µm sont broyés à l'état de poudre micronisée (1 à 5 µm environ).The crystals obtained, which have dimensions of between 50 and 250 μm, are ground to the state of micronized powder (1 to 5 μm approximately).

La description qui suit se réfère au dessin l'accompagnant et dont l'unique figure est le schéma d'une installation pour la mise en oeuvre de l'invention.The following description refers to the accompanying drawing, the only figure of which is the diagram of an installation for implementing the invention.

L'installation représentée schématiquement sur le dessin est constituée essentiellement par un appareil de cristallisation par évaporation 10, une première essoreuse centrifuge 12, un malaxeur-refroidisseur 14 et une seconde essoreuse centrifuge 16. Tous ces appareils sont à marche continue, c'est-à-dire que l'alimentation et l'évacuation des produits se font en continu.The installation shown schematically in the drawing consists essentially of an evaporative crystallization device 10, a first centrifugal wringer 12, a mixer-cooler 14 and a second centrifugal wringer 16. All these devices are in continuous operation, that is to say that is to say that the supply and the evacuation of the products are done continuously.

L'appareil 10 est constitué par une cuve cylindrique fermée disposée horizontalement et divisée en plusieurs compartiments 1 à 5 par des cloisons transversales 18. Ces cloisons sont moins hautes que la cuve de sorte que les différents compartiments communiquent entre eux à leur partie supérieure. Des ouvertures sont percées dans les cloisons 18 pour permettre le passage du produit traité d'un compartiment à l'autre.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.

Un ou plusieurs faisceaux de chauffage 20 formés de tubes horizontaux disposés parallèlement à l'axe de la cuve sont placés dans la partie inférieure de celle-ci. Ces tubes sont alimentés en vapeur par un thermo-compresseur 22 et assurent le chauffage des différents compartiments; ils sont en permanence noyés dans le produit traité remplissant la partie inférieure de la cuve. Le thermo-compresseur 22 sert à recomprimer, au moyen de vapeur vive, une partie de la vapeur produite dans l'appareil 10 et prélevée dans la partie supérieure de la cuve. En variante, on pourrait utiliser un moto-compresseur. Des entrées 24 pour le produit à traiter sont prévues dans chaque compartiment et une sortie reliée à une pompe 25 est prévue dans le dernier compartiment 5.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.

Les essoreuses centrifuges 12 et 16 sont du type décrit dans le brevet français FR-A-2451778. Elles comportent un panier tronconique 26, évasé vers le haut et monté à l'intérieur d'une cuve 28. Le panier est monté sur un pivot vertical et est entrainé en rotation autour de son axe. Le produit à essorer est déversé au fond du panier. Un tamis repose sur la surface intérieure du panier et la phase liquide du produit à essorer ainsi que les particules solides dont les dimensions sont inférieures aux ouvertures du tamis sont recueillies dans une chambre 30 constituée par une virole dont l'extrémité supérieure se trouve près du bord supérieur du panier et par un fond fixé à la virole. Les particules solides dont les dimensions sont supérieures aux ouvertures du tamis sont déplacées vers le haut sur le tamis, par la force centrifuge, et sont finalement éjectées à l'extrémité supérieure du panier dans la cuve 28 d'où elles tombent dans une trémie 32 raccordée au bas de la cuve. Des rampes d'arrosage 33 placées à l'intérieur du panier permettent de laver les matières solides avant qu'elles soient expulsées du panier.The centrifugal dryers 12 and 16 are of the type described in French patent FR-A-2451778. They comprise a frustoconical basket 26, flared upwards and mounted inside 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 ferrule. The solid particles whose dimensions are larger than the openings of the screen are moved upwards on the screen, 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.

Le malaxeur-refroidisseur est du type décrit dans le brevet français FR-A-2461754. Il est constitué par un cuve cylindrique 34, à section circulaire et disposée verticalement. Des orifices sont prévus à la partie inférieure et à la partie supérieure de la cuve pour l'admission et l'évacuation des produits. Un arbre rotatif 35 est placé dans l'axe de la cuve et porte des organes assurant à ta fois le brassage et le refroidissement des produits traités; ces organes peuvent, par exemple, être constitués par des tubes enroulés en spirale et parcourus par un fluide réfrigérant. En variante, des nappes de tubes fixées à la paroi de la cuve et assurant le refroidissement des produits pourraient alterner avec des pales solidaires de l'arbre et assurant le brassage des produits. L'arbre est entrainé en rotation par un groupe moto-réducteur 36 monté sur la cuve.The mixer-cooler is of the type described in French patent FR-A-2461754. 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 rotary 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.

En fonctionnement, le lactosérum préalablement concentré dans un évaporateur, non représenté sur le dessin, est introduit en continu dans les différents compartiments de l'appareil 10 où il est chauffé par la vapeur alimentant les tubes du faisceau 20. On introduit également dans le premier compartiment une solution concentrée contenant des cristaux de petites dimensions provenant de l'essoreuse 12. Sous l'action de la chaleur fournie par la vapeur de chauffage, une partie de l'eau s'évapore et le lactosérum est amené à l'état de sursaturation. La concentration du lactosérum dans les différents compartiments est maintenue à la valeur voulue par contrôle du débit d'alimentation en lactosérum ou en vapeur ce qui permet d'assurer un grossissement régulier des cristaux introduits dans le premier compartiment pendant tout leur séjour dans l'appareil. Le mélange de lactosérum concentré ou eau-mère et de cristaux est extrait en continu du dernier compartiment par la pompe 25. Un régulateur de niveau commande cette pompe pour maintenir le niveau des produits dans la cuve sensiblement à mi-hauteur. Les dimensions de l'appareil sont choisies, en fonction du dèbit à traiter, pour que le temps de séjour ait la valeur voulue.In operation, the whey previously concentrated in an evaporator, not shown in the drawing, is introduced continuously into the various compartments of the apparatus 10 where it is heated by the steam supplying the tubes of the bundle 20. It is also introduced into the first compartment a concentrated solution containing crystals of small dimensions coming from the wringer 12. Under the action of the heat supplied by the heating steam, part of the water evaporates and the whey is brought to the state of supersaturation. The concentration of whey in the different compartments is hand held at the desired value by controlling the feed rate 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.

Une partie de la vapeur produite dans l'appareil 10 est recomprimée au moyen du thermo-compresseur 22, qui est par ailleurs alimenté en vapeur vive par une tuyauterie 38, et est utilisée pour le chauffage du faisceau 20.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.

La pompe 25 alimente l'essoreuse 12. Dans celle-ci les cristaux de lactose dont les dimensions sont supérieures à celles des ouvertures du tamis, par exemple supérieures à 90 pm, sont séparés et évacués en 40 vers les étapes ultérieures du traitement. Avant leur sortie du panier les cristaux sont lavés à l'eau ou à l'eau acidulée par de l'acide chlorhydrique à pH 2,5 à 3,5 au moyen des rampes 33. La plus grosse partie de l'eau-mère et les cristaux de petites dimensions qui ont traversé le tamis de l'essoreuse est envoyée dans le malaxeur-refroidisseur 14. L'autre partie est introduite au moyen d'une pompe 42 dans le premier compartiment de l'appareil 10 où les petits cristaux servent de germes; le débit de la pompe 42 peut être contrôlé en fonction du débit d'alimentation en lactosérum de l'appareil 10.The pump 25 feeds the wringer 12. In the latter, the lactose crystals, the dimensions of which are greater than those of the openings of the sieve, for example greater than 90 μm, are separated and discharged at 40 to the subsequent stages of the treatment. Before leaving the basket, 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 whey supply flow rate of the apparatus 10.

Dans le malaxeur-refroidisseur 14, le mélange d'eau-mère et de cristaux qui avait une température de 50° à 70°C à la sortie de l'appareil 10 est refroidi jusqu'à 10°-15°C environ. Ce refroidissement provoque le grossissement des cristaux etc, par conséquent, permet une récupération supplémentaire du lactose et facilite la séparation des cristaux dans l'essoreuse 16.In 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 etc to grow larger, therefore, allows additional lactose recovery and facilitates the separation of the crystals in the wringer 16.

La pompe 44 assure à la fois l'alimentation de l'essoreuse 16 et le recyclage d'une fraction du mélange eau-mère-cristaux prélevé au bas du malaxeur-refroidisseur 14; ce recyclage permet de pallier la décantation rapide des cristaux dans le malaxeur.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.

Le tamis de l'essoreuse 16 doit être très fin pour permettre de récupérer la presque totalité des cristaux de lactose; les dimensions des ouvertures du tamis seront par exemple comprises entre 40 et 60µm. Ces cristaux sont dirigés vers les étapes ultérieures du traitement. En variante, ces cristaux pourraient être dissous dans de l'eau et la solution obtenue pourrait être introduite avec le lactosérum, dans l'appareil 10.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 μm. These crystals are directed to the later stages of processing. As a variant, these crystals could be dissolved in water and the solution obtained could be introduced with the whey, into the apparatus 10.

Dans l'exemple illustré, les cristaux séparés dans les essoreuses centrifuges 12 et 16 sont utilisés pour la production de lactose à très haute pureté. Ces cristaux sont mélangés, dans un malaxeur 46, à une eau de lavage provenant d'une troisième essoreuse centrifuge à marche continue 48 et ce mélange est ensuite traité dans cette essoreuse où les cristaux sont tout d'abord séparés de l'eau-mère puis lavés au moyen d'un rampe 50 alimentée en eau. L'essoreuse 48 est conçue permettre la séparation de l'eau-mère et de l'eau de lavage. Comme on l'a déjà dit, cette dernière est envoyée dans le malaxeur 46 et mélangée aux cristaux séparés dans les essoreuses 12 et 16. L'eau-mère est renvoyée, par une tuyauterie 52 à l'entrée de l'évaporateur placé en amont de l'appareil de cristallisation 10.In the example illustrated, the crystals separated in the centrifugal dryers 12 and 16 are used for the production of very high purity lactose. These crystals are mixed, in a mixer 46, with washing water coming from a third continuous centrifugal wringer 48 and this mixture is then treated in this wringer where the crystals are first separated from the mother liquor 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.

Claims (13)

1. Process for the production of crystallized lactose from lactoserum; consisting in concentrating the lactoserum, bringing the concentrated lactoserum to the supersaturated state, and maintaining it so by evaporation after addition of crystallization germs to provoke a crystallization start, then continuing the crystallization by cooling the mother liquor/crystals mixture obtained during the first crystallization phase, and separating the crystals from the mother liquor by centrifugal drying, characterized in that the first crystallization phase is performed in a continuously operating unit for crystallization by evaporation (10), that the mother liquor and crystals mixture coming out of that unit is submitted to a first centrifugal drying in a continuously-operating, screen type dryer (12) to separate from the mother liquor the lactose crystals, the size of which exceeds a preset size ranging between 40 and 90 lum, that the mother fiquor containing the small crystals the size of which lies under the above preset size is cooled to provoke an increase in the size of these small crystals, and that the product obtained is submitted to a second centrifugal drying to separate the crystals from the mother liquor.
2. Process according to Claim 1, characterized in that a part of the mother liquor proceeding from the first drying is brought back to the inlet of the crystallization unit (10), the small lactose crystals it contains being used as crystallization germs in that unit.
3. Process according to Claim 1 or 2, for the production of lactose from whole lactoserum, characterized in that the concentrated lactoserum is brought to a temperature of 50° to 55°C in the crystallization unit (10).
4. Process according to Claim 1 or 2, for the production of lactose from de-proteinated and/or de-mineralized lactoserum, characterized in that the concentrated lactoserum is brought to a temperature of 65° to 70°C in the crystallization unit (10).
5. Process according to Claim 1, 2 or 4, characterized in that the residence time of the solution in the crystallization unit (10) is comprised between one and three hours.
6. Process according to any one of the above claims, characterized in that the dry matter concentration of the solution at the inlet of the crystallization unit (10) is about 50% to 55% in weight, and the dry matter concentration of the product coming out of the crystallization unit is about 80% in weight.
7. Process according to any one of the preceding claims, characterized in that the crystallization unit (10) is heated by steam, the temperature of which is between 65° and 80°C.
8. Process according to Claim 7, characterized in that part of the crystallization unit (10) heating steam is constituted by steam produced in that unit and re-compressed.
9. Process according to any one of the preceding claims, characterized in that the crystals separated from the mother liquor during the first drying are submitted to a washing with water, or with water to which acid has been added.
10. Process according to any one of Claims 1 to 8, characterized in that the crystals proceeding from first and second dryings (12 and 16) are mixed with water, and that the mixture obtained is submitted to a new drying, then to washing in a continuously operating centrifugal dryer (48), the mother liquor separated by this last drying being returned upstream of the unit for crystallization by evaporation (10) and the wash water being used to prepare the said mixture.
11. Process according to any one of Claims 1 to 10, characterized in that the first, and possibly the second drying, are performed in a dryer (12) with a frusto-conical screen fitted with a crystals sprinkling pipe (33) located inside the basket (26).
12. Process according to any one of Claims 1 to 10, characterized in that the cooling of the mother liquor/crystals mixture is performed in a mixer-cooler (14) consisting of a vertical, cylindrical tank (34) with a revolving shaft (35) located in the centreline of the tank and carrying elements required for the stirring and/or cooling of the product processed.
13. Installation for the implementation of the process according to Claim 10, including a continuously, operating unit for crystallization by evaporation (10), a first continuously operating centrifugal dryer (12), a mixer-cooler (14), and a second centrifugal dryer (16), characterized in that it also includes a mixer (46) receiving the crystals separated in the first and second centrifugal dryers (12, 16) and a third centrifugal dryer (48) fitted with a water washing perforated pipe (50) and the wash water outlet of which is connected to the inlet of the said mixer (46).
EP81401637A 1980-11-10 1981-10-19 Process for the manufacture of crystallized lactose and apparatus for carrying out this method Expired EP0052541B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8023958A FR2493869A1 (en) 1980-11-10 1980-11-10 PROCESS FOR PRODUCING CRYSTALLIZED LACTOSE AND INSTALLATION FOR CARRYING OUT SAID METHOD
FR8023958 1980-11-10

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EP0052541B1 true EP0052541B1 (en) 1985-02-13

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FR2493869B1 (en) 1983-12-23
EP0052541A1 (en) 1982-05-26
FR2493869A1 (en) 1982-05-14
US4404038A (en) 1983-09-13
DE3168938D1 (en) 1985-03-28

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