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EP0083325B1 - Procédé pour la préparation d'un agent édulcorant à base de lait et un édulcorant préparé selon ce procédé - Google Patents

Procédé pour la préparation d'un agent édulcorant à base de lait et un édulcorant préparé selon ce procédé Download PDF

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Publication number
EP0083325B1
EP0083325B1 EP82850235A EP82850235A EP0083325B1 EP 0083325 B1 EP0083325 B1 EP 0083325B1 EP 82850235 A EP82850235 A EP 82850235A EP 82850235 A EP82850235 A EP 82850235A EP 0083325 B1 EP0083325 B1 EP 0083325B1
Authority
EP
European Patent Office
Prior art keywords
lactose
product
hydrolysis
dry matter
process according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP82850235A
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German (de)
English (en)
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EP0083325A3 (en
EP0083325A2 (fr
Inventor
Henrik Holmberg
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Arla Ekonomisk Forening
Original Assignee
Arla Ekonomisk Forening
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from SE8206009A external-priority patent/SE452337B/sv
Application filed by Arla Ekonomisk Forening filed Critical Arla Ekonomisk Forening
Priority to AT82850235T priority Critical patent/ATE25322T1/de
Publication of EP0083325A2 publication Critical patent/EP0083325A2/fr
Publication of EP0083325A3 publication Critical patent/EP0083325A3/en
Application granted granted Critical
Publication of EP0083325B1 publication Critical patent/EP0083325B1/fr
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00—Sugars not otherwise provided for in this class
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups

Definitions

  • the present invention relates to a process for the manufacture of a sweetener from milk-sugar or lactose and a sweetener manufactured according to the process.
  • Lactose can be derived from any type of milk product like whole milk, skim milk, butter milk, whey, cottage cheese whey etc. Of particular interest is to make use of lactose from whey which is often considered a non-useful rye side product. Lactose has little sweet taste and for making use of lactose as a sweetener the lactose has to be transformed or split up into glucose and galactose which are sweeter types of sugar. It is known that such transforming of lactose is made by hydrolysis with some acid, some ion exchanger or some enzym. Such a method and other hydrolysing methods are described for instance in Journal of Dairy Science, Vol. 64, pages 1759-17771, "Beta-Galactosidase: Review of Recent Research", M. L. Richmond, J. I. Gray and C. M. Stine.
  • any the transforming speed during the hydrolysis has been low. It has not been considered possible to hydrolyse lactose having a dry matter content of more than about 20-40%, and therefore the degree of hydrolysis or the transforming speed during hydrolysis has been unprofitably low. Due to the low degree of hydrolysis in some previously known processes the sugar solution, in addition to glucose and galactose, also contains some amounts of remaining lactose, which especially during long storage at low temperature tends to separate as crystals.
  • a method for hydrolysing of lactose is also known from the U.S. Patent 4,067,748.
  • the lactose is hydrolysed by means of a strongly acidic cation exchanger preferably a strongly acidic polystyrene ion exchanger resin.
  • the hydrolysing can be made for a dry matter content of 20-40%, for instance 30%, and that the hydrolysing is made by means of an ion exchanger resin having a very low cross linking number, preferably a cross linking number of between 0,5 and 5%.
  • the lactose to be treated has a dry matter content which is of such low magnitude that the hydrolysed lactose for many purposes is not directly useful but has to be subjected to further treatments like evaporization etc.
  • an ion exchanger resin having a very low cross linking degree can be used and can be advisable for the indicated low dry matter contents, but on the contrary it is not practically possible to use such low cross linking degrees for higher dry matter contents since the osmothic pressure at high dry matter contents is so high that there is a risk that the ion exchanger resin balls crack and thereby are destroyed.
  • the lactose transforming into glucose and galactose also is made by stirring the lactose solution together with the ion exchange resin which causes cracking and wear of the ion exchange resin balls.
  • the lactose transformation can be made in that the ion exchange resin is allowed to successively fall to the bottom of a column in counter current to a rising lactose bearing liquid while the ion exchange resin is recirculated to the top of the column.
  • the object of the invention is therefore to solve the problem of providing a new process for the manufacture of a sweetener from lactose, which process allows a practical and economical manufacture of the intended sweetener.
  • the invention also relates to a sweetener manufactured according to the said process.
  • a further object of the invention is to provide such a process, in which the dry matter content in the lactose solution can be kept substantially higher than has so far been possible, and in which the dry matter content of the final product is correspondingly higher than previously considered possible without evaporating or further treating the hydrolysed product.
  • a further object of the invention is to provide a process for the manufacture of sweeteners of lactose, according to which a substantially higher dry matter content is obtained than has previously been usual, at which a higher degree of hydrolysis is obtained than has previously been usual and which process can be proceeded so that the cycle speed is substantially higher than has previously been possible.
  • the starting material in the process according to the invention is lactose in a water solution or permeate having a dry matter content of between 40 and 80% or even more.
  • lactose solution is given a dry matter content of between 50 and 60%. If the lactose is to be dissolved in water the temperature is raised to between 80 and 150°C or preferably between 90 and 120°C. At high temperatures lactose is dissolved more completely and as a consequence a higher dry matter content is obtained than at lower temperatures.
  • the high dry matter content of the lactose solution is advantageous in that a concentrated solution is obtained which need not be evaporated and which gives the process a high capacity.
  • the pH-value of the lactose solution may vary, but normally the pH-value is less than 7 and preferably the pH-value is between 5 and 6.
  • the lactose solution may be filtered for the purpose of purifying the solution, but this is not quite necessary. On the contrary the lactose solution may be further treated for splitting the lactose up to glucose and galactose immediately after having been dissolved in water.
  • This further treatment of the lactose solution is made by an acid heterogeneous catalysis, in this case a hydrolysis, whereby the lactose solution is treated with a strongly acidic cation exchanger for instance polystyrene-sulfonic acid or any other ion exchanger built on a polymer.
  • a strongly acidic cation exchanger for instance polystyrene-sulfonic acid or any other ion exchanger built on a polymer.
  • a cation exchanger for this purpose preferably should have a moderately low cross linking degree, or for instance a cross linking degree of 5,5-10% or preferably 5,5-6%.
  • the strongly acidic cation exchanger acts as a heterogeneous catalysor in which the hydrogen ions split the lactose to glucose and galactose.
  • the acid heterogeneous catalysis which can be made without change of the temperature at which the lactose is dissolved in water or to which the lactose permeate is heated proceeds at a temperature of 80-150 0 C or preferably 90-120°C.
  • the process can be proceeded to a hydrolysis degree of between 40% and practically 100%.
  • the hydrolysis is preferably proceeded to a hydrolysation degree of about 70-90%. At a hydrolysation degree of less than 70-80%, there is a risk that lactose and/or galactose will crystallize after long storing time and at low temperatures.
  • the acidity of the lactose solution is successively increased, and the glucose-galactose product leaving the process may have a pH-value of 1.5-2.5. It may be considered advantageous that the glucose-galactose solution is kept at a relatively low pH-value since the microbiological resistance is high at low pH-value.
  • the milk sugar product may be polished for instance by being filtered through activated carbon. Such a polishing step, however, is only necessary for certain products in which a clear non-coloured product is required.
  • the final sugar product may be evaporized, but since the dry matter content is as high as 45 ⁇ 80% or preferably 50 ⁇ 60% evaporizing is generally not necessary.
  • the final hydrolysed product normally has a pH-value of 1.5-2.5. For adapting the sugar product to its intended field of use the pH-value may be raised upon demand.
  • the sugar product manufactured according to the process, is well suited for many different purposes, for instance for use in food stuffs like bakery products of different kinds, beverages such as beer, lemonades etc., or different types of canned products for which some sweetener is desired, for cheese products like cheese dip, spreadable cheeses, cream cheese etc., for sweetening of sweet meats and confiture, for dairy products like condensed milk, acidified culture type of milk, sour cream, yoghurt etc., for dry mix powders such as baking mix powder, pancake mix powder, salad dressings, sausages, hamburgers, soups etc or for sweetening of ice-cream.
  • beverages such as beer, lemonades etc.
  • canned products for which some sweetener is desired
  • cheese products like cheese dip, spreadable cheeses, cream cheese etc.
  • sweetening of sweet meats and confiture for dairy products like condensed milk, acidified culture type of milk, sour cream, yoghurt etc.
  • dry mix powders such as baking mix powder, pancake mix powder, salad dressings
  • the product manufactured according to the process, has a high content of dry matter, and a high lactose to glucose-galactose transforming speed, and it is possible to proceed the process, according to the invention, to a very high degree of hydrolysis for the product.
  • lactose powder obtained from whey was added to 60 I water having a temperature of 80°C. The said temperature was maintained until the greatest part of the lactose powder was dissolved, whereupon the lactose solution was treated with a strongly acidic cation exchanger consisting of polystyrene-sulfonic acid having a cross linking degree of 8%.
  • the hydrolysis was proceeded to a hydrolysing degree of 40%, whereupon the ready hydrolysed product was withdrawn and analysed.
  • the transforming cycle speed corresponded to a bed volume of 0.50 per hour.
  • the product had a brown-yellow colour and a soft caramel taste.
  • lactose obtained from whey was dissolved in 35 I water having a temperature of 97°C.
  • the pH was found to be 5.51.
  • the lactose solution was treated with an ion exchanger mass, which ion exchanger is a strongly acidic cation exchanger having a cross linking degree of 5.5%.
  • the hydrolysis was proceeded as far as a hydrolysing degree of 96%.
  • the pH-value was found to be 1.82.
  • the treated product had a pure sweet taste without any substantial extraneous flavour. The colour was slightly yellow.
  • After the product had been polished over activated carbon the product was clear and completely without any flavour.
  • the transforming cycle speed according to this example corresponded to 1.0 bed volume per hour. Depending on the high degree of hydrolysing no crystallization was observed, not even after long storing at low temperatures.
  • lactose obtained from whey was dissolved in 20 I water of 140°C temperature under a pressure of 3.10 bar.
  • the pH-value of the lactose solution was measured to 5.0.
  • the lactose solution was treated with a strongly acidic ion exchanger, based on a polystyrene-sulfonic acid having a cross-linking degree (DVB-degree) of 6%.
  • the hydrolysis was run to a hydrolysing degree of 92%.
  • the transforming cycle speed corresponded to a bed volume of 1.1 per hour.
  • the ready product was brownish and had a slight caramel taste. Without being polished the product was considered well suited for bakery purposes.
  • lactose obtained from whey of cottage cheese was mixed with 50 I water of 100°C.
  • the pH-value of the lactose solution was measured to 4.5.
  • the lactose solution was treated with a strongly acidic cation exchanger having a cross linking degree of 10% and the hydrolysis was run to a hydrolysis degree to 95%.
  • the transforming speed corresponded to a flow cycle speed of 0,7 bed volumes per hour.
  • the ready product was slightly yellow and had a good sweetness without any flavour. After the product had been polished over activated carbon a clear non-coloured product without any noticable flavour had been obtained.
  • the product was considered well suitable as a sweetener for beverages, i.e. beverages of the brewery industry like beer and lemonades etc.
  • lactose powder obtained from whey was dissolved in 291 water and was mixed at a temperature of 119°C and at a pressure of 1.9 bar.
  • the pH-value of the lactose solution was measured to be 1.8.
  • the lactose solution was treated with a strongly acidic cation exchanger having a cross linking degree of 5.5%.
  • the hydrolysis was run to a hydrolysis degree of 93%.
  • the transforming speed corresponded to flow cycle speed of 1.9 bed volumes per hour.
  • the ready product was slightly yellowish and had a pure sweet taste without any noticable flavour.
  • the hydrolysis could be carried out with a flow cycle speed of 1.9 bed volume per hour corresponding to a period for transforming lactose into glucose and galactose of not more than about half an hour. No substantial crack formation or any other damage of the ion exchange resin could be noticed.
  • lactose powder from whey was dissolved in 40 I water of 100°C temperature.
  • the lactose mixture was treated with a strongly acidic cation exchanger which was a mixture of 50% of a strongly acidic cation exchanger having a cross linking degree of 5.5% and the remaining a cation exchanger having a cross linking degree of 8%.
  • the hydrolysis was run to a hydrolysing degree of 98% at a transforming speed cycle of 1.5 bed volumes per hour.
  • the product thereby manufactured was practically completely clear and non-coloured and had a strong sweet taste.
  • lactose powder 50 kg lactose powder was solved in 50 I water at a temperature of 97°C.
  • the lactose solution was hydrolysed as far as to 96% by means of a strong acidic cation exchanger having a cross linking degree of 5.5%.
  • the hydrolysed lactose had a relatively sweet taste.
  • To the hydrolysed lactose was thereafter added 15% of non-hydrolysed lactose, and a taste panel considered the sweetness of the product substantially higher than the sweetness of the hydrolysed lactose without the addition of non-hydrolysed lactose.
  • BV/h bed volume per hour
  • DM dry matter content of starting material
  • a strongly acidic cation exchanger having a low cross linking degree within the above mentioned interval makes the hydrolysis run more easily, so that a higher flow speed can be maintained without the risk that the hydrolysis degree decreases.
  • the product is so stable that there is practically no crystallizing, not even at long time of storing.
  • Cation exchangers having a low cross linking degree are rather sensitive to pressure or are brittle, and as mentioned above the osmotic pressure at high dry matter contents becomes so high that there is a risk that the cation exchanger is damaged.
  • high dry matter contents it is therefore often considered necessary to use cation exchangers having a higher cross linking degree than the above indicated cross linking degree interval of 5.5-10% than should have been desired, depending on operating technical viewpoints.
  • the apparatus illustrated in Figure 1 comprises a closed container 1 having a top dome 2 and a bottom dome 3 and an intermediate bottom 4 adjacent the bottom dome 3.
  • a bed 5 of a cation exchanger On the intermediate bottom 4 and up to about half the height of the container has been applied a bed 5 of a cation exchanger, and on a level slightly above the upper surface 6 of the cation exchanger bed there is an inlet 7 for lactose.
  • the inlet 7 is connected to a spreading device having several nozzles (not illustrated) which spread the lactose evenly over the surface of the ion exchanger bed.
  • the acid inlet 12 and the air inlet 14 are closed and the lactose solution is pumped into the container in a predetermined amount per unit of time, preferably by means of a positive pump.
  • the lactose is spread over the surface 6 of the ion exchanger bed 5 by means of the spreading device 8.
  • the lactose successively passes through the ion exchanger bed at a certain speed, but if the lactose is pumped into the container with a higher speed than can pass through the ion exchanger bed 5 a layer 15 of lactose solution appears on top of the surface 6 of the ion exchanger bed.
  • the lactose solution which is pumped into the container through the inlet 7 always meets the strongest part of the acid at or adjacent the outlet, even if the acid of the ion exchanger resin is partly consumed, what is advantageous in order to maintain the highest possible degree of hydrolysis.
  • the acid content of the ion exchanger resin successively is reduced during the hydrolysing process, and at a certain stage it is necessary to regenerate the ion exchanger resin.
  • the ion exchanger bed 5 is thereafter forced down to its original level, acid, for instance hydrochloric acid, of about 5% concentration is pumped into the container through the acid inlet 12 and the spreading device 13 and is allowed to pass through the ion exchanger bed 5 from above until the ion exchanger mass is saturated. Excess of acid is removed by flushing water through the bed, and thereafter the equipment is ready for once again being taken into use for hydrolysing lactose into glucose and galactose.
  • acid for instance hydrochloric acid
  • FIG 2 there is shown a diagram of suitable handling temperatures. Along the vertical axis is plotted the dry matter content in percent and along the horizontal axis is plotted the solution temperature for lactose or permeate respectively in water. It is evident that the temperature for completely solving lactose of for instance 40% dry matter content in water is about 92°C and that the temperature becomes higher corresponding to a higher dry matter content to about 140°C for a dry matter content of 90%. The above temperatures relate to the lactose curve L. Corresponding temperatures for permeate P are about 55°C for a permeate having a dry matter content of about 40% and about 100°C for a permeate of 90% dry matter content.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Seasonings (AREA)
  • Saccharide Compounds (AREA)
  • Dairy Products (AREA)

Claims (8)

1. Procédé pour la préparation d'un agent édulcorant, caractérisé en ce que du lactose ayant une valeur de pH inférieure à 7 est dissous dans l'eau ayant une température comprise entre 80―150°C ou de préférence 90-120°C pour obtenir une teneur en extrait sec de 40 à 80%, ou de préférence 50 à 60%, ou un perméat de lactose ayant la même teneur en extrait sec est chauffé à la même température, après quoi la solution de lactose ainsi obtenue est hydrolysée en la traitant par un échangeur cationique fortement acide ayant un degré de réticulation de 5,5-10%, ce qui transforme le lactose en glucose et galactose, et l'hydrolyse est poussée jusqu'à un degré d'hydrolyse de 40-100% ou de préférence 70-90% pour une vitesse de cycle d'écoulement de 2,0-0,5 volumes de lit par heure correspondant à une durée de transformation du lactose en glucose et galactose de 0,5-2,0 heures, après quoi le produit de glucose-galactose ainsi obtenu est redroidi à une température de 10-20°C et est soutiré pour usage direct, pour stockage intermédiaire ou pour traitement ultérieur.
2. Procédé selon la revendication 1, caractérisé en ce que l'hydrolyse est réalisée sans changer la température à laquelle le lactose est dissous dans l'eau ou à laquelle le perméat de lactose est chauffé.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que la solution de lactose est purifiée avant le traitement d'hydrolyse.
4. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la solution de lactose en un écoulement parallèle est forcée de passer à travers un lit fixe d'échangeur cationique fortement acide.
5. Procédé selon la revendication 4, dans lequel l'échangeur cationique fortement acide est un acide polystyrène-sulfonique ou tout autre polymère à base d'échangeur d'ion acide ayant un degré de réticulation compris de préférence entre 5,5 et 6%.
6. Procédé selon la revendication 1, dans lequel le produit de glucose-galactose obtenu par hydrolyse est filtré sur du charbon actif pour purifier le produit et enlever le goût éventuel de caramel.
7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le produit qui vient d'être hydrolysé est soumis à un ou plusieurs des traitements suivants: filtration sur charbon activé, évaporation jusqu'à n'importe quelle teneur requise en extrait sec, réglage de la valeur du pH selon le produit pour lequel est prévu l'agent édulcorant.
8. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce qu'on donne à la solution de lactose une valeur de pH de 5―6 avant le traitement catalytique, et en ce que le produit qui vient d'être hydrolysé est conservé à une valeur de pH de 1,5-2,5.
EP82850235A 1981-12-28 1982-11-18 Procédé pour la préparation d'un agent édulcorant à base de lait et un édulcorant préparé selon ce procédé Expired EP0083325B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82850235T ATE25322T1 (de) 1981-12-28 1982-11-18 Verfahren zur herstellung eines suessstoffes auf basis von milch und ein suessstoff hergestellt nach diesem verfahren.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US33452481A 1981-12-28 1981-12-28
US334524 1981-12-28
SE8206009 1982-10-22
SE8206009A SE452337B (sv) 1981-12-28 1982-10-22 Forfarande for framstellning av ett sotningsmedel genom hydrolys av en laktoslosning

Publications (3)

Publication Number Publication Date
EP0083325A2 EP0083325A2 (fr) 1983-07-06
EP0083325A3 EP0083325A3 (en) 1984-11-28
EP0083325B1 true EP0083325B1 (fr) 1987-02-04

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Family Applications (1)

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EP82850235A Expired EP0083325B1 (fr) 1981-12-28 1982-11-18 Procédé pour la préparation d'un agent édulcorant à base de lait et un édulcorant préparé selon ce procédé

Country Status (10)

Country Link
EP (1) EP0083325B1 (fr)
AU (1) AU550326B2 (fr)
CA (1) CA1203115A (fr)
DE (1) DE3275349D1 (fr)
ES (1) ES517877A0 (fr)
FI (1) FI72147C (fr)
IE (1) IE53762B1 (fr)
NO (1) NO157507C (fr)
NZ (1) NZ202634A (fr)
PT (1) PT75963B (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PT1958514E (pt) 2007-02-07 2013-07-04 Kraft Foods R & D Inc Soro de leite em pó modificado e processo para o produzir

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2592509A (en) * 1950-07-13 1952-04-08 Borden Co Noncrystallizing lactose sirup and method of making
GB1539278A (en) * 1977-11-17 1979-01-31 Express Dairy Foods Co Ltd Production of hydrolysed lactose from whey lactose and its use in brewing or other fermentation process
US4266027A (en) * 1980-03-12 1981-05-05 National Distillers And Chemical Corp. Process for the hydrolysis of starch and fermentable hydrolysates obtained therefrom

Also Published As

Publication number Publication date
EP0083325A3 (en) 1984-11-28
DE3275349D1 (en) 1987-03-12
ES8307900A1 (es) 1983-08-16
IE822776L (en) 1983-06-22
FI824400A0 (fi) 1982-12-21
NO824301L (no) 1983-06-23
EP0083325A2 (fr) 1983-07-06
FI72147B (fi) 1986-12-31
IE53762B1 (en) 1989-02-01
NZ202634A (en) 1986-02-21
PT75963B (en) 1985-10-04
NO157507B (no) 1987-12-21
FI824400L (fi) 1983-06-29
FI72147C (fi) 1987-04-13
AU550326B2 (en) 1986-03-20
AU9181882A (en) 1983-06-30
PT75963A (en) 1983-01-01
NO157507C (no) 1988-04-06
CA1203115A (fr) 1986-04-15
ES517877A0 (es) 1983-08-16

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