EP0052541B1 - Procédé de production de lactose cristallisé et installation pour la mise en oeuvre de ce procédé - Google Patents

Procédé de production de lactose cristallisé et installation pour la mise en oeuvre de ce procédé 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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EP
European Patent Office
Prior art keywords
crystals
crystallization
process according
unit
mother liquor
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.)
Expired
Application number
EP81401637A
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German (de)
English (en)
French (fr)
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EP0052541A1 (fr
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
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.)
Filing date
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Application filed by Fives Cail Babcock SA, Pierre Guerin SA filed Critical Fives Cail Babcock SA
Publication of EP0052541A1 publication Critical patent/EP0052541A1/fr
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Publication of EP0052541B1 publication Critical patent/EP0052541B1/fr
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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
    • 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.

Landscapes

  • 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 Procédé de production de lactose cristallisé et installation pour la mise en oeuvre de ce procédé Expired EP0052541B1 (fr)

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 EP0052541A1 (fr) 1982-05-26
EP0052541B1 true EP0052541B1 (fr) 1985-02-13

Family

ID=9247849

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81401637A Expired EP0052541B1 (fr) 1980-11-10 1981-10-19 Procédé de production de lactose cristallisé et installation pour la mise en oeuvre de ce procédé

Country Status (4)

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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9365905B2 (en) 2005-02-10 2016-06-14 Dmv-Fonterra Excipients Technology Gmbh Processes for making lactose utilizing pre-classification techniques and pharmaceutical formulations formed therefrom

Families Citing this family (12)

* 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
FI78504C (fi) * 1987-10-14 1989-08-10 Valio Meijerien Foerfarande foer tillvaratagande av laktos ur vassla.
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
LT2629623T (lt) 2010-10-07 2018-08-27 Fonterra Co-Operative Group Limited Laktozės gamyba
SI2570689T1 (sl) † 2011-09-14 2015-12-31 Knorr-Bremse Systeme Fuer Nutzfahrzeuge Gmbh Kolutna zavora motornega vozila in zavorna obloga
DK2757162T5 (da) * 2013-01-22 2016-02-15 Dmk Deutsches Milchkontor Gmbh Fremgangsmåde til at øge udbyttet i fremstillingen af laktose (II)
DK2767596T3 (en) 2013-02-16 2016-05-23 Dmk Deutsches Milchkontor Gmbh A process for increasing the yield in the production of lactose (III)
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
EP3302080B1 (en) * 2015-05-29 2019-01-09 Spx Flow Technology Danmark A/S Second pass lactose crystallization
IT201900023046A1 (it) * 2019-12-05 2021-06-05 Vomm Impianti E Processi S P A Prodotto in forma di polvere comprendente lattosio e suo procedimento di produzione

Family Cites Families (16)

* 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
US2768912A (en) * 1952-03-10 1956-10-30 Western Condensing Co Separation of crystallized lactose from whey solids
US2778750A (en) * 1953-03-24 1957-01-22 Armour & Co Ion exchange purification of whey in the preparation of lactose
US3447930A (en) * 1966-04-14 1969-06-03 Foremost Mckesson Process of treating whey
DE1642536A1 (de) * 1966-10-28 1971-05-06 Struthers Scient And Internat Verfahren zur kontinuierlichen Kristallisierung von Dextrose
FR1581088A (en)van) * 1968-07-17 1969-09-12
NL6908590A (en)van) * 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
US3721585A (en) * 1971-01-28 1973-03-20 Foremost Mckesson Method for manufacture of lactose
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
DE2930282A1 (de) * 1979-07-26 1981-02-19 Helmut Dipl Ing Hayer Lactoseherstellungsverfahren

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9365905B2 (en) 2005-02-10 2016-06-14 Dmv-Fonterra Excipients Technology Gmbh Processes for making lactose utilizing pre-classification techniques and pharmaceutical formulations formed therefrom

Also Published As

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

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