EP2743356A1 - Process for enhancing yield during the manufacture of lactose (I) - Google Patents

Abstract

Improving the yield during the production of crystalline alpha -lactose, comprises: (a) adjusting an aqueous lactose solution to a temperature of 62-67[deg] C; (b) cooling the solution to 20-30[deg] C; (c) maintaining the solution at this temperature for a period of 0.5-5 hours, (d) subsequently re-heating the solution to 35-40[deg] C; (e) maintaining the solution at this temperature for a period of 0.5-5 hours; (f) subsequently cooling the solution to 10[deg] C; and (g) optionally separating the precipitated alpha -lactose crystals from the mother liquor. Independent claims are also included for: (1) mother liquor comprising 15-20 wt.% alpha -lactose; and (2) producing crystalline alpha -lactose, comprising (i) subjecting whey to a separation process in which a protein-rich and a lactose-rich fraction is obtained, (ii) subjecting the lactose-rich fraction (optionally after concentrating the main flow) to demineralization in which slowly soluble salts are precipitated, (iii) cooling the demineralized residue, optionally after further evaporation, until lactose precipitates are in crystalline form, (iv) separating the lactose crystals from the mother liquor and evaporating, and further adjusting the first mother liquor to a temperature of 62-67[deg] C, cooling the solution to 20-30[deg] C, maintaining the solution at this temperature for a period of 0.5-5 hours, subsequently re-heating the solution to 35-40[deg] C, maintaining the solution at this temperature for a period of 0.5-5 hours, subsequently cooling the solution to 10[deg] C, and optionally separating the precipitated alpha -lactose crystals from the second mother liquor.

Description

Field of the invention

The invention is in the field of the dairy industry and relates to an improved process for the production of lactose.

State of the art

Lactose belongs to the group of disaccharides and consists of the two molecules D-galactose and D-glucose, which are linked by a β-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. In this case, 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). For this purpose, in the first process step, the permeate obtained in the ultrafiltration of the whey is concentrated by reverse osmosis (RO) or nanofiltration (NF). Subsequently, 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. In the second precipitation step, 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.

That too Patent US 4,202,909 describes a process for the production of lactose, in which one initially 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.

It is customary in the processes of the prior art that the mother liquor, which contains about 90% by weight of lactose in the dry mass, 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.

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 problem is that in this cooling process again phases metabstabilen state are passed, where again fresh crystal nuclei can form, but have little time to grow and remain very small. Since the deposition of the alpha-lactose crystals in the decanter, the freshly formed small crystals are not detected with a diameter of less than 80 microns, about 17% of lactose are lost.

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.

It is obvious that any process improvement that results in the residual amount of lactose in the mother liquor being reduced would have a significant impact on the economics of the process. Thus, 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 .-%.

Description of the invention

• (a) eine wässrige Lactoselösung auf eine Temperatur von etwa 62 bis 67 °C einstellt,
• (b) die Lösung dann bis auf etwa 20 bis 30 °C abkühlt,
• (c) die Lösung bei dieser Temperatur für 0,5 bis 5 h hält,
• (d) anschließend die Lösung wieder bis auf etwa 35 bis 40 °C erwärmt,
• (e) die Lösung bei dieser Temperatur für 0,5 bis 5 h hält,
• (f) anschließend die Lösung bis auf etwa 10 °C abkühlt und
• (g) abschließend die ausgefallenen alpha-Lactosekristalle von der Mutterlauge abtrennt.

The invention relates to a process for improving the yield in the production of crystalline alpha-lactose, in which

• (a) adjusting an aqueous lactose solution to a temperature of about 62 to 67 ° C,
• (b) then cooling the solution to about 20 to 30 ° C,
• (c) holding the solution at this temperature for 0.5 to 5 hours,
• (d) subsequently heating the solution again to about 35 to 40 ° C,
• (e) holding the solution at this temperature for 0.5 to 5 hours,
• (f) then cooling the solution to about 10 ° C and
• (G) finally separates the precipitated alpha-lactose crystals from the mother liquor.

Surprisingly, it has been found that by temporarily heating the lactose solution small crystals and crystal abrasion go back into solution and are therefore available again to grow on large crystals. In this way, the loss of lactose due to crystal breakage and poor decanting can be approximately halved, so that the remaining after decanting mother liquor only has a lactose content of at most 20 wt .-%.

lactose solutions

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. For this purpose, 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. Typically, 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.

As an optional but generally preferred step, 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).

The UF permeate has - optionally after concentration - a content of minerals in the order of 1 to 2 wt .-% to. In order to be able to achieve the specification which is below 0.3% by weight, 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. To adjust the pH and to precipitate NaOH, an aqueous preparation of calcium chloride and alkali metal hydroxide or calcium hydroxide is used. In principle, 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, however, has the advantage that the precipitant is inexpensive and the salts have a very low solubility product, ie the precipitation is substantially complete. Even without the addition of precipitants, 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. After precipitation, 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. If desired or necessary, 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.

As a second optional but generally also preferred step, 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 Demineralisierungsstufe. The aqueous lactose solutions thus obtained can now be used in the crystallization stage.

Process implementation

In the first step of the process, 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. This can be plant-specific continuously or batchwise. 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. In the tank, the solution is then cooled to 62-67 and preferably about 63-65 ° C. For this purpose, 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.

Then, 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. In this temperature course 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.

Through these measures, the seeds are brought back into solution and now have the opportunity to grow on the larger crystals. For this purpose, 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.

Overall, a time of about 18 to 24 and preferably about 20 hours to set for the entire cooling process. Subsequently, 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.

Industrial Applicability

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.

• (i) Molke einem Trennverfahren unterwirft, bei dem eine proteinreiche und eine lactosereiche Fraktion erhalten wird,
• (ii) die lactosereiche Fraktion gegebenenfalls nach Aufkonzentrierung Hauptstrom) einer Demineralisierung unterwirft, bei der schwerlösliche Salze gefällt werden,
• (ii) den demineralisierten Rückstand gegebenenfalls nach weiterer Aufkonzentrierung abkühlt, bis Lactose kristallin ausfällt,
• (iii) die Lactosekristalle von der Mutterlauge abtrennt und entwässert,
  welches sich dadurch auszeichnet, dass man
  • (a) die erste Mutterlauge auf eine Temperatur von etwa 62 bis 67 °C einstellt,
  • (b) die Lösung dann bis auf etwa 20 bis 30 °C abkühlt,
  • (c) die Lösung bei dieser Temperatur für 0,5 bis 5 h hält,
  • (d) anschließend die Lösung wieder bis auf etwa 35 bis 40 °C erwärmt,
  • (e) die Lösung bei dieser Temperatur für 0,5 bis 5 h hält,
  • (f) anschließend die Lösung bis auf etwa 10 °C abkühlt und
  • (g) abschließend die ausgefallenen alpha-Lactosekristalle von der zweiten Mutterlauge abtrennt.

Also enclosed by the invention is a process for the production of lactose, in which

• (i) subjecting whey to a separation process to obtain a high protein and high lactose fraction,
• (ii) subjecting the lactose-rich fraction, optionally after mainstream concentration), to demineralization precipitating sparingly soluble salts,
• (ii) optionally after further concentration, cooling the demineralized residue until lactose precipitates in crystalline form,
• (iii) separating the lactose crystals from the mother liquor and dehydrating,
  which is characterized by the fact that one
  • (a) adjusting the first mother liquor to a temperature of about 62 to 67 ° C,
  • (b) then cooling the solution to about 20 to 30 ° C,
  • (c) holding the solution at this temperature for 0.5 to 5 hours,
  • (d) subsequently heating the solution again to about 35 to 40 ° C,
  • (e) holding the solution at this temperature for 0.5 to 5 hours,
  • (f) then cooling the solution to about 10 ° C and
  • (G) finally separates the precipitated alpha-lactose crystals from the second mother liquor.

Comparative Example C1

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. With the onset of crystal deposition, 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.

example 1

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. With the onset of crystal deposition, the solution was held at that temperature for about 12 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 18.4 wt .-% lactose. Lactose on. The temperature / time profile is in Figure 2 played.

Claims (13)

Process for improving the yield in the production of crystalline alpha-lactose, in which (a) adjusting an aqueous lactose solution to a temperature of about 62 to 67 ° C, (b) then cooling the solution to about 20 to 30 ° C, (c) holding the solution at this temperature for 0.5 to 5 hours, (d) subsequently heating the solution again to about 35 to 40 ° C, (e) holding the solution at this temperature for 0.5 to 5 hours, (f) then cooling the solution to about 10 ° C and (G) finally separates the precipitated alpha-lactose crystals from the mother liquor. Process according to Claim 1, characterized in that the lactose solution in step (a) is adjusted to 63 to 65 ° C. Process according to claims 1 and / or 2, characterized in that the solution in step (b) is cooled at a rate of about 1 to 5 ° K / h. Process according to at least one of Claims 1 to 3, characterized in that the solution in step (b) is cooled down to 23 to 26 ° C. Process according to at least one of Claims 1 to 4, characterized in that the solution in step (c) is kept at the temperature for about 1 to 3 hours. Process according to at least one of Claims 1 to 5, characterized in that the solution in step (d) is heated to about 36 to 38 ° C. Process according to at least one of Claims 1 to 6, characterized in that the solution in step (d) is kept at this temperature for about 1 to 3 hours. Method according to at least one of claims 1 to 7, characterized in that the solution in step (f) is cooled at a rate of about 1 to 5 ° K / h. Method according to at least one of claims 1 to 8, characterized in that the temperature profile comprising the steps (a) to (g) is passed through within a period of about 18 to 24 hours. Method according to at least one of claims 1 to 9, characterized in that the alpha-lactose crystals are separated by means of a decanter. A method according to claim 10, characterized in that the separated alpha-lactose crystals are dewatered using a belt dryer. A mother liquor containing about 15 to 20% by weight of alpha-lactose obtainable by the process according to claim 1. Process for the preparation of crystalline alpha-lactose, in which (i) subjecting whey to a separation process to obtain a high protein and high lactose fraction, (ii) subjecting the lactose-rich fraction, optionally after mainstream concentration), to demineralization where sparingly soluble salts are precipitated, (ii) optionally cooling the demineralized residue after further concentration until lactose precipitates in crystalline form, (Iii) the lactose crystals separated from the first mother liquor and dehydrated, characterized in that (a) adjusting the first mother liquor to a temperature of about 62 to 67 ° C, (b) then cooling the solution to about 20 to 30 ° C, (c) holding the solution at this temperature for 0.5 to 5 hours, (d) subsequently heating the solution again to about 35 to 40 ° C, (e) holding the solution at this temperature for 0.5 to 5 hours, (f) then cooling the solution to about 10 ° C and (G) finally separates the precipitated alpha-lactose crystals from the second mother liquor.

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