EP2743356B1 - Process for enhancing yield during the manufacture of lactose (i) - Google Patents
Process for enhancing yield during the manufacture of lactose (i) Download PDFInfo
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- 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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- lactose
- solution
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- alpha
- cooled down
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- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 title claims description 58
- 239000008101 lactose Substances 0.000 title claims description 58
- 238000000034 method Methods 0.000 title claims description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 230000002708 enhancing effect Effects 0.000 title 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 78
- 239000013078 crystal Substances 0.000 claims description 28
- 239000012452 mother liquor Substances 0.000 claims description 24
- 229930195727 α-lactose Natural products 0.000 claims description 21
- 239000005862 Whey Substances 0.000 claims description 8
- 102000007544 Whey Proteins Human genes 0.000 claims description 8
- 108010046377 Whey Proteins Proteins 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 238000005115 demineralization Methods 0.000 claims description 6
- 102000004169 proteins and genes Human genes 0.000 claims description 6
- 108090000623 proteins and genes Proteins 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 45
- 238000000108 ultra-filtration Methods 0.000 description 15
- 238000001816 cooling Methods 0.000 description 11
- 239000012466 permeate Substances 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 159000000007 calcium salts Chemical class 0.000 description 5
- 230000002328 demineralizing effect Effects 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001728 nano-filtration Methods 0.000 description 4
- GUBGYTABKSRVRQ-DCSYEGIMSA-N Beta-Lactose Chemical compound OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-DCSYEGIMSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229930195724 β-lactose Natural products 0.000 description 3
- WQZGKKKJIJFFOK-SVZMEOIVSA-N (+)-Galactose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-SVZMEOIVSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000001464 adherent effect Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000012465 retentate Substances 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013611 frozen food Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000008141 laxative Substances 0.000 description 1
- 230000002475 laxative effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Images
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
-
- 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)
Description
Die Erfindung befindet sich auf dem Gebiet der Molkereiindustrie und betrifft ein verbessertes Verfahren zur Herstellung von Lactose.The invention is in the field of the dairy industry and relates to an improved process for the production of lactose.
Lactose gehört zur Gruppe der Disaccharide und besteht aus den beiden Molekülen D-Galactose und D-Glucose, die über eine β-1,4-glycosidische Bindung verbunden sind.
Lactose ist eine kristalline, farblose Substanz mit süßem Geschmack; die Süßkraft liegt je nach Konzentration zwischen 25 und 60 % der von Saccharose. Lactose stellt einen wichtigen Bestandteil der Milch dar und verfügt über eine Vielzahl von ernährungsphysiologischen Vorteilen. So dient es dem Metabolismus als Energiequelle, unterstützt die Calciumresorption, hemmt die Bildung von Fäulnisbakterien im Darm und wirkt zumindest in größeren Mengen eingenommen, abführend. In der Lebensmitteltechnik wird es vor allem zur Herstellung von Milchsäure und als Texturiermittel für Tiefkühlprodukte eingesetzt. Da es Lebensmittel einen cremigen Geschmack verleiht, stellt es ein weit verbreitetes Additiv dar.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 stellt ein Nebenprodukt bei der Herstellung von Proteinpulvern dar. Dabei wird üblicherweise Molke durch Ultrafiltration von Proteinen befreit, die anschließend einer Sprühtrocknung unterworfen werden.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.
Ein heute übliches Verfahren zur Herstellung von Lactose wird beispielsweise in der internationalen Patentanmeldung
Auch das Patent
Üblich nach den Verfahren des Stands der Technik ist, dass die Mutterlauge, die etwa 90 Gew.-% Lactose in der Trockenmasse enthält, nach dem Eindampfer in den Kristallisationstank gefördert wird. Dieser wird zum Befüllen geheizt, um die Lactose in Lösung zu halten. Oberhalb von 93,5 °C liegt reine beta-Lactose vor. Beim Abkühlen wandelt sich diese jedoch quantitativ in alpha-Lactose um. Allerdings handelt es sich hier nicht um einen scharfen Phasenübergang, denn zunächst wird eine metastabile Phase durchlaufen, aus der sich dann die alpha-Lactosekristalle abscheiden. Beim weiteren Abkühlen folgt man in der Regel der Sättigungskurve, damit die Kristalle ausreichend Zeit haben zu wachsen.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.
Nach dem Beginn des Kristallisationsprozesses wird auf eine Temperatur von 30 bis 40 °C abgekühlt, die Lauge für 1 bis 3 h bei dieser Temperatur ruhen gelassen und dann weiter auf 10 °C abgekühlt. Die Gesamte Kühlzeit beträgt etwa 20 h.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.
Problematisch ist, dass bei diesem Kühlverlauf immer wieder Phasen metabstabilen Zustandes durchschritten werden, bei denen sich erneut frische Kristallkeime bilden können, die jedoch wenig Zeit zum Wachsen haben und sehr klein bleiben. Da bei der Abscheidung der alpha-Lactose Kristalle im Dekanter die frisch gebildeten kleinen Kristalle mit einem Durchmesser von weniger als 80 µm nicht erfasst werden, gehen etwa 17 % der Lactose verloren.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.
Durch das Rühren kommt es im Dekanter zudem zu Kristallbruch, wobei wiederum Material entsteht, dass wegen seines zu geringen Teilchendurchmessers nicht abgeschieden werden kann. Auf diese Weise gehen weitere 20 % der Lactose verloren, so dass die Mutterlaufe schließlich noch 35 bis 40 % Lactose enthält, die mit hohem Aufwand wieder aufgearbeitet werden muss, um in der Gesamtbetrachtung des Verfahrens zu einer akzeptablen Ausbeute zu gelangen.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.
Es liegt auf der Hand, dass jede Verfahrensverbesserung, die dazu führt, dass sich die Restmenge an Lactose in der Mutterlauge verringert, einen erheblichen Einfluss auf die Ökonomie des Verfahrens hätte. Somit hat die Aufgabe der vorliegenden Erfindung darin bestanden, bestehende Verfahren zur Lactoseherstellung dahingehend zu verbessern und die Restmenge an alpha-Lactose, die nach der Kristallisation mit der Mutterlauge verloren geht, auf maximal 20 Gew.-% zu begrenzen.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 .-%.
Gegenstand der Erfindung ist ein Verfahren zur Verbesserung der Ausbeute bei der Herstellung von kristalliner alpha-Lactose, bei dem man
- (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.
- (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.
Überraschenderweise wurde gefunden, dass durch zwischenzeitliches Aufheizen der Lactoselösung kleine Kristalle und Kristallabrieb wieder in Lösung gehen und damit wieder zur Verfügung stehen, um auf großen Kristallen aufzuwachsen. Auf diese Weise kann der Verlust an Lactose durch Kristallbruch und mangelhaftes Dekantieren etwa halbiert werden, so dass die nach dem Dekantieren zurückbleibende Mutterlauge nur noch einen Lactosegehalt von maximal 20 Gew.-% aufweist.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 .-%.
Lactoselösungen, die im Sinne des erfindungsgemäßen Verfahrens als Ausgangsstoffe für die Gewinnung der alpha-Lactosekristalle in Betracht kommen, werden in der Regel ausgehend von Molke gewonnen. Dazu wird Molke zunächst in eine proteinreiche und eine lactosereiche Fraktion aufgespalten. Das bevorzugte Trennverfahren stellt hierfür die Ultrafiltration (UF) dar, bei der das UF Retentat zur Gewinnung von Proteinen weiterverarbeitet und das UF Permeat für die Gewinnung der Lactose verwendet wird. Typischerweise enthält das UF Retentat etwa 20 Gew.-% Trockenmasse und davon etwa 2 Gew.-% Lactose, der Aschegehalt liegt bei etwa 1 Gew.-%. Das UF Permeat, das zur Herstellung der Lactose weiterverarbeitet wird, weist hingegen eine Trockenmasse von etwa 4,5 bis 5,5 Gew.-% auf, wobei der Gehalt an Lactose bei ca. 4,1 bis 4,6 und der Aschegehalt bei etwa 0,3 bis 0,5 liegt.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.
Als optionaler, jedoch im Allgemeinen bevorzugter Schritt, wird das UF Permeat aufkonzentriert, wobei man eine Trockenmasse von etwa 10 bis 30 Gew.-% - entsprechend 10 bis 30 °Brix - einstellt. Dies erfolgt vorzugsweise entweder durch Umkehrosmose (RO) oder Nanofiltration (NF).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).
Das UF Permeat weist - gegebenenfalls nach Aufkonzentrieren - einen Gehalt an Mineralien in der Größenordnung von 1 bis 2 Gew.-% auf. Um die Spezifikation, die bei unter 0,3 Gew.-% liegt, erreichen zu können, werden die Lösungen durch Zugabe von Basen zunächst auf einen annähernd neutralen pH-Wert im Bereich von 6 bis 8 eingestellt und die Mineralien, die im Wesentlichen lösliche Phosphate darstellen mit einer solchen Menge einer Lösung eines wasserlöslichen Calciumsalzes versetzt, dass schwerlösliche Calciumsalze gefällt werden. Zur Einstellung des pH-Wertes und zur Fällung werden NaOH, eine wässrige Zubereitung aus Calciumchlorid und Alkalihydroxid oder Calciumhydroxid einsetzt. Grundsätzlich können zur Einstellung des pH-Wertes auch andere Alkali- oder Erdalkalibasen, wie z.B.-KOH eingesetzt werden. Auch die Natur des Fällungssalzes ist an sich unkritisch, es lassen sich beispielsweise Bariumsalze fällen. Die Verwendung von Calciumsalzen hat indes den Vorteil, dass das Fällungsmittel kostengünstig und die Salze ein sehr niedriges Löslichkeitsprodukt haben, die Fällung also im Wesentlichen vollständig ist. Auch ohne Zugabe von Fällungsmitteln erfolgt die Demineralisierung in Rührkesseln, wobei es sich als vorteilhaft erwiesen hat, eine Temperatur im Bereich von etwa 50 bis 90 und vorzugsweise von etwa 80 °C einzustellen. Die Fällungszeit liegt typischerweise bei etwa 20 bis 120 und vorzugsweise etwa 30 bis 45 min, wobei diese Angaben nur als Anhaltspunkte zu verstehen sind, da niedrigere Temperaturen längere Reaktionszeiten erfordern und umgekehrt. Nach der Fällung werden die Salze abgetrennt, beispielsweise in Separatoren, welche das größere spezifische Gewicht der gefällten Partikel ausnutzen. Es ist aber ebenso möglich, die Abtrennung beispielsweise durch Membranfilter im Rahmen einer weiteren Ultrafiltration im Bereich 5 bis 150 kDa, vorzugsweise 10 bis 50 kDa vorzunehmen.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
Der gereinigte Strom enthält jetzt typischerweise etwa 15 bis 20, vorzugsweise etwa 17,5 Gew.-% Lactose, während der Aschegehalt bereits auf etwa 0,8 vermindert worden ist. Falls gewünscht oder erforderlich, kann sich nun eine zweite Demineralisierungsstufe anschließen, bei der man dem vorgereinigten Strom eine Menge an niederen Alkoholen, insbesondere an Ethanol zusetzt, um das Löslichkeitsprodukt der noch enthaltenen Calciumsalze weiter herabzusetzen. Auf diese Weise kann im Bedarfsfall eine weitere Menge an Salzen gefällt und wie oben beschrieben abgetrennt werden.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.
Als zweiter optionaler, jedoch im Allgemeinen ebenfalls bevorzugter Schritt, wird der demineralisierte lactosereiche Strom nach Verlassen der Separatoren ein weiteres Mal aufkonzentriert, wobei man einen Feststoffgehalt - im Wesentlichen identisch mit dem Gehalt an Lactose - von etwa 50 bis 70 Gew.-% - entsprechend 40 bis 50 °Brix - einstellt. Dies erfolgt vorzugsweise durch eine Vakuumeindampfung, bei der das Produkt auf vorzugsweise etwa 65 Gew.-% entwässert und gegebenenfalls auch Alkohol aus der Demineralisierungsstufe abgetrennt wird. Die so erhaltenen wässrigen Lactoselösungen können nun in die Kristallisationsstufe eingesetzt werden.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
Im ersten Schritt des Verfahrens wird eine Lactoselösung, die wie oben beschrieben erhältlich ist und etwa 60 bis 95 und vorzugsweise etwa 85 bis 90 Gew.-% Lactose in der Trockenmasse aufweist, in einen vorgeheizten Kristallisationstank gepumpt. Dies kann anlagenspezifisch kontinuierlich oder batchweise erfolgen. Die Mutterlauge kann vor dem Befüllen des Tanks auf eine Temperatur oberhalb von 93,5 °C eingestellt werden, um die Bildung von alpha-Lactose zu verhindern; dies ist jedoch nicht zwingend. Es können auch Mutterlaugen eingesetzt werden, bei denen die Umwandlung von beta- in alpha-Lactose schon begonnen hat. Im Tank wird die Lösung dann auf 62 bis 67 und vorzugsweise etwa 63 bis 65 °C. abgekühlt. Dazu reicht es aus, die heiße Lactoselösung sich einfach an die Starttemperatur des Kristallisationstanks anpassen zu lassen, was innerhalb von 1 bis 2 h üblicherweise der Fall ist.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 at 62 to 67 and preferably about 63 to 65 ° C. cooled. 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.
Als dann wird die Lactoselösung kontinuierlich mit einer Geschwindigkeit von etwa 1 bis 5 °K/h bis auf 20 bis 30 und vorzugsweise etwa 23 bis 26 °C abgekühlt und dort für etwa 0,5 bis 5 und vorzugsweise etwa 1 bis 3 h gehalten. Bei diesem Temperaturverlauf werden immer wieder metastabile Phasen durchschritten, in denen auch beta-Lactose stabil ist bzw. alpha-Lactose wieder in beta-Lactose umgewandelt wird. Es entstehen damit wieder neue Kristallkeime die bei weiterer Abkühlung kaum Chancen haben eine hinreichende Größe zu erreichen, um im Dekanter abgetrennt werden zu können. Deshalb wird die Lösung im nächsten Schritt wieder leicht erwärmt, nämlich bis auf etwa 35 bis 40 und vorzugsweise etwa 36 bis 38°C. Bei dieser Temperatur wird die Lösung wiederum etwa 0,5 bis 5 und insbesondere etwa 1 bis 3 h belassen. Die Erwärmung erfolgt wieder mit einer Geschwindigkeit von etwa 1 bis 5 °K/h.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.
Durch diese Maßnahmen werden die Kristallkeime wieder in Lösung gebracht und haben nun die Möglichkeit auf den größeren Kristallen aufzuwachsen. Dazu wird die Lösung nun mit einer Geschwindigkeit von etwa 1 bis 3 °K/h auf etwa 10 °C, vorzugsweise 5 bis 10 °C abgekühlt und bei dieser Temperatur für etwa 12 bis 15 h gehalten, so dass die alpha-Lactosekristalle hinreichend Zeit haben sich abzuscheiden.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.
Insgesamt ist für das Durchlaufen des gesamten Kühlprozesses eine Zeit von etwa 18 bis 24 und vorzugsweise etwa 20 h anzusetzen. Anschließend werden die Lactosekristalle von der Mutterlauge getrennt, was vorzugsweise mit Hilfe von Dekantern die nach dem Zentrifugalprinzip arbeiten erfolgt. Grundsätzlich ist aber auch jedes andere Bauteil, mit dessen Hilfe eine Fest/Flüssig-Trennung möglich ist, für diesen Schritt geeignet. Dazu gehören beispielsweise auch Separatoren, die mit Membranen arbeiten. Die Lactosekristalle, an denen noch Mutterlauge anhaftet, werden im Anschluss schonend getrocknet, wozu sich insbesondere Bandtrockner als geeignet erwiesen haben.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.
Ein weiterer Gegenstand der vorliegenden Patentanmeldung betrifft eine Mutterlauge mit einem Gehalt an alpha-Lactose von etwa 15 bis 20 Gew.-%, die nach dem erfindungsgemäßen Verfahren erhältlich ist.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.
Ebenfalls von der Erfindung umschlossen ist ein Verfahren zur Herstellung von Lactose, bei dem man
- (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.
- (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.
Eine Lactose-Mutterlauge mit einem Gehalt von 89,5 Gew.-% in der Trockenmasse wurde mit einer Temperatur von etwa 95 °C in einen vorgeheizten Kristallisationstank gegeben, dort mit einer Geschwindigkeit von etwa 3 °K/h innerhalb von etwa 1 h auf 65 °C abgekühlt und für eine knappe Stunde gehalten, ehe die Lösung wiederum mit einer Geschwindigkeit von etwa 3 °K/h innerhalb von etwa 1 h auf 25 °C abgekühlt wurde. Dort wurde die Lösung weitere 3 h bei der Temperatur gehalten und dann mit einer Geschwindigkeit von 1 °K/h innerhalb 1 h bis auf 10 °C abgekühlt. Mit dem Beginn der Kristallabscheidung wurde die Lösung etwa 15 h bei dieser Temperatur gehalten, die ausgefallenen alpha-Lactosekristalle in einem Dekanter abgetrennt und auf einem Bandtrockner von anhaftender Feuchtigkeit befreit. Die zurückbleibende Mutterlauge wies einen Restgehalt von 34,7 Gew.-% Lactose auf. Das Temperatur/Zeit-Profil ist in
Die Lactose-Mutterlauge aus Vergleichsbeispiel V1 wurde mit einer Temperatur von etwa 95 °C in einen vorgeheizten Kristallisationstank gegeben, dort mit einer Geschwindigkeit von etwa 3 °K/h innerhalb von etwa 1 h auf 65 °C abgekühlt dort für eine knappe Stunde gehalten, ehe die Lösung wiederum mit einer Geschwindigkeit von etwa 3 °K/h innerhalb von etwa 1 h auf 25 °C abgekühlt wurde. Dort wurde die Lösung weitere 3 h bei der Temperatur gehalten und dann mit einer Geschwindigkeit von etwa 3 °K/h wieder auf 37 °C erwärmt. Die Lösung wurde weitere 3 h bei dieser Temperatur gehalten und dann mit einer Geschwindigkeit von 1 °K/h innerhalb 1 h bis auf 10 °C abgekühlt. Mit dem Beginn der Kristallabscheidung wurde die Lösung etwa 12 h bei dieser Temperatur gehalten, die ausgefallenen alpha-Lactosekristalle in einem Dekanter abgetrennt und auf einem Bandtrockner von anhaftender Feuchtigkeit befreit. Die zurückbleibende Mutterlauge wies einen Restgehalt von 18,4 Gew.-% Lactose auf. Lactose auf. Das Temperatur/Zeit-Profil ist in
Claims (13)
- A method for improving the yield during the production of crystalline alpha lactose, characterized in that(a) an aqueous lactose solution is adjusted to a temperature of between about 62 and 67 °C,(b) the solution is then cooled down to between 20 and 30 °C,(c) the solution is held at this temperature for a period of from 0.5 to 5 h,(d) subsequently, the solution is re-heated to between 35 and 40 °C,(e) the solution is held at this temperature for a period of from 0.5 to 5 h,(f) subsequently, the solution is cooled down to about 10 °C, and(g) the precipitated alpha-lactose crystals are separated from the mother liquor.
- The method of Claim 1, characterized in that the lactose solution under step (a) is adjusted to between 63 °C and 65 °C.
- The method of Claim 1 and/or 2, characterized in that the solution under step (b) is cooled down at a rate of from about 1 to 5 °K/h.
- The method of at least one of Claims 1 to 3, characterized in that the solution under step (b) is cooled down to between 23 and 26 °C.
- The method of at least one of Claims 1 to 4, characterized in that the solution under step (c) is held at this temperature for a period of about 1 to 3 h.
- The method of at least one of Claims 1 to 5, characterized in that the solution under step (d) is heated to between about 36 and 38 °C.
- The method of at least one of Claims 1 to 6, characterized in that the solution under step (d) is held at this temperature for a period of about 1 to 3 h.
- The method of at least one of Claims 1 to 7, characterized in that the solution under step (f) is cooled down at a rate of about 1 to 5 °K/h.
- The method of at least one of Claims 1 to 8, characterized in that the temperature profile comprising steps (a) to (g) is passed through within a period of about 18 to 24 h.
- The method of at least one of Claims 1 to 9, characterized in that the alpha lactose crystals are separated by means of a decanter.
- The method of Claim 10, characterized in that the separated alpha lactose crystals are dehydrated by means of a belt dryer.
- Mother liquor with a content in alpha-lactose of from about 15 to 20 % b.w., obtainable by the method of Claim 1.
- A method for the production of crystalline alpha-lactose, characterized in that(i) Whey is subjected to a separation process in which a protein-rich and a lactose-rich fraction is obtained,(ii) The lactose-rich fraction is optionally after concentrating the main flow subjected to demineralisation in which slowly soluble salts are precipitated,(iii) The demineralised residue is cooled down until lactose precipitates in crystalline form,(iv) The lactose crystals are separated from the mother liquor and evaporated, characterized in that(a) The first mother liquor is adjusted to a temperature of between about 62 and 67 °C,(b) The solution is then cooled down to between about 20 and 30 °C,(c) The solution is held at this temperature for a period of from 0.5 to 5 h,(d) Subsequently, the solution is re-heated to between about 35 and 40 °C,(e) The solution is held at this temperature for a period of from 0.5 to 5 h,(f) Subsequently, the solution is cooled down to about 10 °C, and(g) The precipitated alpha-lactose crystals are separated from the second mother liquor.
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US4202909A (en) | 1976-11-22 | 1980-05-13 | Patent Technology, Inc. | Treatment of whey |
US4316749A (en) * | 1980-10-07 | 1982-02-23 | Stauffer Chemical Company | Production of USP quality lactose |
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