EP2743356B1 - Procédé d'augmentation du rendement pour la fabrication de lactose (i) - Google Patents

Procédé d'augmentation du rendement pour la fabrication de lactose (i) Download PDF

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Publication number
EP2743356B1
EP2743356B1 EP12196712.9A EP12196712A EP2743356B1 EP 2743356 B1 EP2743356 B1 EP 2743356B1 EP 12196712 A EP12196712 A EP 12196712A EP 2743356 B1 EP2743356 B1 EP 2743356B1
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Prior art keywords
lactose
solution
temperature
alpha
cooled down
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EP12196712.9A
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German (de)
English (en)
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EP2743356A1 (fr
Inventor
Sven-Rainer Döring
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DMK Deutsches Milchkontor GmbH
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DMK Deutsches Milchkontor GmbH
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Priority to DK12196712.9T priority Critical patent/DK2743356T3/en
Priority to EP12196712.9A priority patent/EP2743356B1/fr
Priority to CN201310681584.9A priority patent/CN103864857B/zh
Priority to US14/103,967 priority patent/US9476105B2/en
Publication of EP2743356A1 publication Critical patent/EP2743356A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K5/00—Lactose
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/16—Purification of sugar juices by physical means, e.g. osmosis or filtration

Definitions

  • the invention is in the field of the dairy industry and relates to an improved process for the production of lactose.
  • Lactose belongs to the group of disaccharides and consists of the two molecules D-galactose and D-glucose, which are linked by a ⁇ -1,4-glycosidic bond.
  • Lactose is a crystalline, colorless substance with a sweet taste; depending on the concentration, the sweetening power is between 25 and 60% of that of sucrose. Lactose is an important component of milk and has a variety of nutritional benefits. So it serves the metabolism as an energy source, supports calcium absorption, inhibits the formation of putrefactive bacteria in the intestine and is at least taken in large quantities, laxative. In food technology, it is mainly used for the production of lactic acid and as a texturizer for frozen foods. Because it gives food a creamy taste, it is a widely used additive.
  • Lactose is a by-product in the production of protein powders.
  • whey is usually freed by ultrafiltration of proteins, which are then subjected to spray drying.
  • a currently customary process for the production of lactose is described, for example, in the international patent application WO 2002 050089 A1 (Food Science Australia).
  • the permeate obtained in the ultrafiltration of the whey is concentrated by reverse osmosis (RO) or nanofiltration (NF).
  • RO reverse osmosis
  • NF nanofiltration
  • the concentrate thus obtained is demineralized in two steps, ie first mixed with an alkaline earth salt, usually an aqueous calcium chloride solution, wherein the minerals are precipitated as calcium phosphate.
  • an alkaline earth salt usually an aqueous calcium chloride solution
  • the solubility of the calcium salts is further reduced by the addition of lower alcohols and further phosphate precipitated.
  • the separation of the salts is then carried out with the aid of suitable filtration devices, such as membranes, separators or the like. Subsequently, the purified lactose solution is subjected to vacuum distillation and adjusted to a solids content of about 65% by weight.
  • the patent US 4,202,909 describes a process for the production of lactose, in which one first subjects whey to ultrafiltration, subjects the UF permeate to demineralization, concentrates the permeate, and then separates the lactose from the mother liquor. In particular, it is described that the mother liquor can then be demineralized and worked up again in order to obtain a further amount of lactose. Similar content is also the GB 1575089 B in which a process for the production of lactose is described in Example 1, in which first subjected to ultrafiltration of whey, the UF permeate subjected to a demineralization, the permeate concentrated and then separates the lactose from the mother liquor.
  • the mother liquor which contains about 90% by weight of lactose in the dry mass
  • the mother liquor is conveyed downstream of the evaporator into the crystallization tank. This is heated to fill to keep the lactose in solution. Above 93.5 ° C pure beta-lactose is present. Upon cooling, however, this converts quantitatively into alpha-lactose. However, this is not a sharp phase transition, because initially a metastable phase is run through, from which then precipitate the alpha-lactose crystals. On further cooling, the saturation curve is usually followed so that the crystals have sufficient time to grow.
  • the liquor After the start of the crystallization process is cooled to a temperature of 30 to 40 ° C, the liquor for 1 to 3 h at this temperature and then allowed to continue to 10 ° C cooled.
  • the total cooling time is about 20 h.
  • the stirring also leads to crystal breakage in the decanter, which in turn produces material that can not be separated due to its small particle diameter. In this way, a further 20% of the lactose are lost, so that the mother race finally contains 35 to 40% lactose, which must be worked up again at great expense in order to arrive at an acceptable yield in the overall consideration of the process.
  • the object of the present invention was to improve existing processes for lactose production to this effect and to limit the residual amount of alpha-lactose, which is lost after crystallization with the mother liquor, to a maximum of 20 wt .-%.
  • Lactose solutions which come into consideration for the purposes of the process according to the invention as starting materials for the recovery of the alpha-lactose crystals, are generally obtained starting from whey.
  • whey is first split into a protein-rich and a lactose-rich fraction.
  • the preferred separation method for this purpose is ultrafiltration (UF), in which the UF retentate is further processed to obtain proteins and the UF permeate is used for the recovery of the lactose.
  • UF ultrafiltration
  • the UF retentate contains about 20% by weight of dry matter and about 2% by weight of lactose, and the ash content is about 1% by weight.
  • the UF permeate which is further processed to produce the lactose, however, has a dry matter content of about 4.5 to 5.5 wt .-%, wherein the content of lactose at about 4.1 to 4.6 and the ash content at is about 0.3 to 0.5.
  • the UF permeate is concentrated to provide a dry matter content of about 10 to 30% by weight, corresponding to 10 to 30 ° Brix. This is preferably done either by reverse osmosis (RO) or nanofiltration (NF).
  • RO reverse osmosis
  • NF nanofiltration
  • the UF permeate has - optionally after concentration - a content of minerals in the order of 1 to 2 wt .-% to.
  • the solutions are first adjusted to an approximately neutral pH in the range from 6 to 8 by the addition of bases, and the minerals which are essentially soluble Phosphates are added with such an amount of a solution of a water-soluble calcium salt that low-soluble calcium salts are precipitated.
  • an aqueous preparation of calcium chloride and alkali metal hydroxide or calcium hydroxide is used.
  • other alkali or alkaline earth bases, such as KOH may be used to adjust the pH.
  • the nature of the precipitation salt is not critical in itself, it can be, for example, barium precipitate.
  • the use of calcium salts has the advantage that the precipitant is inexpensive and the salts have a very low solubility product, ie the precipitation is substantially complete.
  • the demineralization is carried out in stirred tanks, wherein it has proved to be advantageous to set a temperature in the range of about 50 to 90 and preferably of about 80 ° C.
  • the precipitation time is typically about 20 to 120, and preferably about 30 to 45 minutes, which are only indicative, since lower temperatures require longer reaction times and vice versa.
  • the salts are separated, for example in separators, which exploit the greater specific gravity of the precipitated particles. But it is also possible to carry out the separation, for example by membrane filter in the context of a further ultrafiltration in the range 5 to 150 kDa, preferably 10 to 50 kDa.
  • the purified stream now typically contains about 15 to 20, preferably about 17.5 weight percent lactose, while the ash content has already been reduced to about 0.8.
  • a second demineralization stage can now follow, in which the amount of lower alcohols, in particular of ethanol, is added to the prepurified stream in order to further reduce the solubility product of the calcium salts still present. In this way, if necessary, a further amount of salts can be precipitated and separated as described above.
  • the demineralized lactose-rich stream is concentrated once more after leaving the separators, corresponding to a solids content substantially identical to the lactose content of about 50 to 70% by weight 40 to 50 ° Brix - sets.
  • This is preferably done by a vacuum evaporation in which the product is dehydrated to preferably about 65 wt .-% and, if appropriate, alcohol is separated from the Demineralmaschineseck.
  • the aqueous lactose solutions thus obtained can now be used in the crystallization stage.
  • a lactose solution which is obtainable as described above and has about 60 to 95 and preferably about 85 to 90% by weight of lactose in dry matter, is pumped into a preheated crystallization tank.
  • the mother liquor may be adjusted to a temperature above 93.5 ° C prior to filling the tank to prevent the formation of alpha-lactose; however, this is not mandatory. It can also be mother liquors where the conversion of beta-alpha-lactose has already begun.
  • the solution is then at 62 to 67 and preferably about 63 to 65 ° C. cooled.
  • it is sufficient to have the hot lactose solution simply adapted to the starting temperature of the crystallization tank, which is usually the case within 1 to 2 hours.
  • the lactose solution is continuously cooled at a rate of about 1 to 5 ° K / h to 20 to 30 and preferably about 23 to 26 ° C and held there for about 0.5 to 5 and preferably about 1 to 3 hours.
  • metastable phases are repeatedly passed, in which also beta-lactose is stable or alpha-lactose is converted back into beta-lactose.
  • New crystal nuclei are formed again, which on further cooling hardly have any chances to reach a sufficient size to be separated in the decanter. Therefore, in the next step, the solution is again gently heated, namely to about 35 to 40 and preferably about 36 to 38 ° C. At this temperature, the solution is again left for about 0.5 to 5 hours and especially for about 1 to 3 hours. The heating takes place again at a speed of about 1 to 5 ° K / h.
  • the seeds are brought back into solution and now have the opportunity to grow on the larger crystals.
  • the solution is then cooled at a rate of about 1 to 3 ° K / h to about 10 ° C, preferably 5 to 10 ° C and held at this temperature for about 12 to 15 hours, so that the alpha-lactose crystals sufficient time have to leave.
  • the lactose crystals are separated from the mother liquor, which is preferably carried out by means of decanters work according to the centrifugal principle. In principle, however, any other component with the aid of which solid / liquid separation is possible is also suitable for this step. These include, for example, separators that work with membranes.
  • the lactose crystals, to which mother liquor still adheres, are subsequently gently dried, for which band dryers, in particular, have proved suitable.
  • a further subject of the present patent application relates to a mother liquor with an alpha-lactose content of about 15 to 20 wt .-%, which is obtainable by the process according to the invention.
  • a lactose mother liquor having a content of 89.5% by weight in the dry mass was placed at a temperature of about 95 ° C. in a preheated crystallization tank, there at a rate of about 3 ° K / h within about 1 h Cooled to 65 ° C and held for one hour before the solution was again cooled at a rate of about 3 ° K / h in about 1 h at 25 ° C. There, the solution was kept at the temperature for a further 3 h and then cooled at a rate of 1 ° K / h within 1 h to 10 ° C.
  • the solution was held at this temperature for about 15 hours, the precipitated alpha-lactose crystals separated in a decanter and freed of adherent moisture on a belt dryer.
  • the remaining mother liquor had a residual content of 34.7 wt .-% lactose.
  • the temperature / time profile is in illustration 1 played.
  • the lactose mother liquor from Comparative Example C1 was added at a temperature of about 95 ° C in a preheated crystallization tank, where it cooled at a rate of about 3 ° K / h within about 1 h to 65 ° C held there for about an hour, before the solution was again cooled at a rate of about 3 ° K / h to 25 ° C within about 1 h. There the solution was kept at the temperature for a further 3 hours and then reheated to 37 ° C. at a rate of about 3 ° K / h. The solution was kept at this temperature for a further 3 hours and then cooled at a rate of 1 ° K / h within 1 h to 10 ° C.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Saccharide Compounds (AREA)
  • Dairy Products (AREA)

Claims (13)

  1. Procédé d'amélioration du rendement lors de la fabrication d'alpha-lactose cristallin, selon lequel
    (a) une solution aqueuse de lactose est ajustée à une température d'environ 62 à 67 °C, puis
    (b) la solution est refroidie à une température d'environ 20 à 30 °C,
    (c) la solution est maintenue à cette température pendant 0,5 à 5 h, puis
    (d) la solution est de nouveau portée à une température d'environ 35 à 40 °C,
    (e) la solution est maintenue à cette température pendant 0,5 à 5 h, puis
    (f) la solution est refroidie à environ 10 °C, et enfin
    (g) les cristaux d'alpha-lactose précipités sont séparés de la liqueur mère.
  2. Procédé selon la revendication 1, caractérisé en ce que la solution de lactose est ajustée à une température de 63 à 65 °C à l'étape (a).
  3. Procédé selon les revendications 1 et/ou 2, caractérisé en ce que la solution est refroidie à une vitesse d'environ 1 à 5 °K/h à l'étape (b).
  4. Procédé selon au moins l'une quelconque des revendications 1 à 3, caractérisé en ce que la solution est refroidie à une température de 23 à 26 °C à l'étape (b).
  5. Procédé selon au moins l'une quelconque des revendications 1 à 4, caractérisé en ce que la solution est maintenue à la température pendant environ 1 à 3 h à l'étape (c).
  6. Procédé selon au moins l'une quelconque des revendications 1 à 5, caractérisé en ce que la solution est portée à une température d'environ 36 à 38 °C à l'étape (d).
  7. Procédé selon au moins l'une quelconque des revendications 1 à 6, caractérisé en ce que la solution est maintenue à cette température pendant environ 1 à 3 h à l'étape (d).
  8. Procédé selon au moins l'une quelconque des revendications 1 à 7, caractérisé en ce que la solution est refroidie à une vitesse d'environ 1 à 5 °K/h à l'étape (f).
  9. Procédé selon au moins l'une quelconque des revendications 1 à 8, caractérisé en ce que le profil de température comprenant les étapes (a) à (g) est traversé en une durée d'environ 18 à 24 h.
  10. Procédé selon au moins l'une quelconque des revendications 1 à 9, caractérisé en ce que les cristaux d'alpha-lactose sont séparés à l'aide d'un décanteur.
  11. Procédé selon la revendication 10, caractérisé en ce que les cristaux d'alpha-lactose séparés sont déshydratés à l'aide d'un séchoir à bande.
  12. Liqueur mère ayant une teneur en alpha-lactose d'environ 15 à 20 % en poids, pouvant être obtenue par le procédé selon la revendication 1.
  13. Procédé de fabrication d'alpha-lactose cristallin, selon lequel
    (i) du lactosérum est soumis à un procédé de séparation, lors duquel une fraction riche en protéines et une fraction riche en lactose sont obtenues,
    (ii) la fraction riche en lactose est soumise, éventuellement après une concentration du courant principal, à une déminéralisation lors de laquelle des sels difficilement solubles sont précipités,
    (iii) le résidu déminéralisé est refroidi, éventuellement après une concentration supplémentaire, jusqu'à la précipitation de lactose cristallin,
    (iv) les cristaux de lactose sont séparés de la première liqueur mère et déshydratés, caractérisé en ce que
    (a) la première liqueur mère est ajustée à une température d'environ 62 à 67 °C, puis
    (b) la solution est refroidie à une température d'environ 20 à 30 °C,
    (c) la solution est maintenue à cette température pendant 0,5 à 5 h, puis
    (d) la solution est de nouveau portée à une température d'environ 35 à 40 °C,
    (e) la solution est maintenue à cette température pendant 0,5 à 5 h, puis
    (f) la solution est refroidie à environ 10 °C, et enfin
    (g) les cristaux d'alpha-lactose précipités sont séparés de la seconde liqueur mère.
EP12196712.9A 2012-12-12 2012-12-12 Procédé d'augmentation du rendement pour la fabrication de lactose (i) Active EP2743356B1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
DK12196712.9T DK2743356T3 (en) 2012-12-12 2012-12-12 Method for improving yield in the manufacture of lactose (I)
EP12196712.9A EP2743356B1 (fr) 2012-12-12 2012-12-12 Procédé d'augmentation du rendement pour la fabrication de lactose (i)
CN201310681584.9A CN103864857B (zh) 2012-12-12 2013-12-12 提高乳糖生产的产量的方法
US14/103,967 US9476105B2 (en) 2012-12-12 2013-12-12 Method for increasing the yield in lactose production (I)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP12196712.9A EP2743356B1 (fr) 2012-12-12 2012-12-12 Procédé d'augmentation du rendement pour la fabrication de lactose (i)

Publications (2)

Publication Number Publication Date
EP2743356A1 EP2743356A1 (fr) 2014-06-18
EP2743356B1 true EP2743356B1 (fr) 2016-03-09

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US (1) US9476105B2 (fr)
EP (1) EP2743356B1 (fr)
CN (1) CN103864857B (fr)
DK (1) DK2743356T3 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180249726A1 (en) * 2017-03-03 2018-09-06 Dmk Deutsches Milchkontor Gmbh Process for producing a milk product free of lactose

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1483190A (en) * 1973-11-02 1977-08-17 Shell Int Research Purification of diphenylolpropane
US4202909A (en) 1976-11-22 1980-05-13 Patent Technology, Inc. Treatment of whey
GB1575089A (en) 1976-11-22 1980-09-17 Patent Technology Process for the treatment of whey and whey permeate and products resulting therefrom
US4316749A (en) * 1980-10-07 1982-02-23 Stauffer Chemical Company Production of USP quality lactose
FI78504C (fi) * 1987-10-14 1989-08-10 Valio Meijerien Foerfarande foer tillvaratagande av laktos ur vassla.
DE4113836A1 (de) * 1990-07-04 1992-01-09 Kali Chemie Ag Verfahren zur suessmolkenpermeataufarbeitung
AUPR217700A0 (en) 2000-12-19 2001-01-25 Food Science Australia Methods for purification of lactose
CN101239996B (zh) * 2008-01-04 2010-10-27 华南理工大学 一种高剪切力微晶乳糖制备方法
PL2629623T3 (pl) * 2010-10-07 2018-12-31 Fonterra Co-Operative Group Limited Wytwarzanie laktozy
DK2767596T3 (en) * 2013-02-16 2016-05-23 Dmk Deutsches Milchkontor Gmbh A process for increasing the yield in the production of lactose (III)

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Publication number Publication date
CN103864857A (zh) 2014-06-18
EP2743356A1 (fr) 2014-06-18
DK2743356T3 (en) 2016-06-20
US20140174434A1 (en) 2014-06-26
CN103864857B (zh) 2018-10-19
US9476105B2 (en) 2016-10-25

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