EP0017778B1 - Procédé pour la préparation d'un produit anhydre, épandable et cristallin contenant du fructose - Google Patents

Procédé pour la préparation d'un produit anhydre, épandable et cristallin contenant du fructose Download PDF

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Publication number
EP0017778B1
EP0017778B1 EP80101415A EP80101415A EP0017778B1 EP 0017778 B1 EP0017778 B1 EP 0017778B1 EP 80101415 A EP80101415 A EP 80101415A EP 80101415 A EP80101415 A EP 80101415A EP 0017778 B1 EP0017778 B1 EP 0017778B1
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EP
European Patent Office
Prior art keywords
fructose
starting solution
temperature
solution
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
EP80101415A
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German (de)
English (en)
Other versions
EP0017778A1 (fr
Inventor
Basant K. Dwivedi
Subodh Kumar Raniwala
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.)
Chimicasa GmbH
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Chimicasa GmbH
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
Application filed by Chimicasa GmbH filed Critical Chimicasa GmbH
Publication of EP0017778A1 publication Critical patent/EP0017778A1/fr
Application granted granted Critical
Publication of EP0017778B1 publication Critical patent/EP0017778B1/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
    • C13K11/00—Fructose

Definitions

  • the invention relates to a method for producing an anhydrous, free-flowing, crystalline, fructose-containing material.
  • Crystalline fructose is commercially produced through a very complicated and time consuming crystallization process that requires relatively unusual process mechanisms and equipment, as well as careful control of process conditions to ensure the production of a satisfactory crystalline fructose product.
  • anhydrous fructose crystals can be obtained both by crystallization from aqueous solutions and from aqueous, alcoholic solutions, such as, for example, aqueous methanol and aqueous ethanol solutions of fructose.
  • the use of solvents in fructose solutions is undesirable from a health point of view and because the solvent has to be completely removed from the crystals precipitated from the solution before the consumption or use of crystal fructose, and for economic reasons also the solvent from the mother liquor used for the process should regain.
  • US-A-3513023 describes a process starting with a fructose solution containing at least 95% by weight fructose, which is then further concentrated under vacuum to a water content of 2 to 5% and then to a temperature of 60 ° to 80 ° F ( ⁇ 15.6 ° C to 26.7 ° C). (° F means degrees Fahrenheit; ° C means degrees Celsius.) A large amount of the seed crystals are then added to the concentrated, chilled solution and the mixture must then be stirred at a low temperature until it becomes a soft mass. This mass is then solidified and dried at a temperature below 150 ° F ( ⁇ 65.5 ° C). This method is unsatisfactory because the fructose concentration of the starting solution must be at least 95%.
  • the soft mass must be kneaded and only pure crystalline fructose seed crystals may be used.
  • This known method is therefore disadvantageous in terms of the conditions for treating the material, because of the high energy costs and because it is limited to the use of pure fructose syrups.
  • the object of the invention is a method of the type mentioned at the outset in such a way that the disadvantages of the known processes are avoided and water-free, free-flowing, crystalline fructose can be produced with the least possible energy and processing effort.
  • the length of time during which the seeded starting solution has to be left to crystallize also depends on the type and size of the seed crystals used, the relative humidity of the ambient air, the temperature and the moisture content of the starting solution used. You can find the optimal time by trying.
  • the starting solution which can preferably also be a cereal syrup solution, advantageously contains 90 to 95 percent by weight, preferably 92 to 94 percent by weight, fructose and / or a mixture of fructose and glucose. If one starts from an aqueous cereal syrup solution, then this is in a lower concentration than that prescribed here for the starting solution. In such a case, the cereal syrup solution is concentrated to the desired concentration and this is preferably done by heating in a vacuum at temperatures of no higher than 200 ° F ( ⁇ 93.3 ° C), since undesirable discolouration can occur in the syrup solution at higher temperatures.
  • the relative humidity of the ambient air is kept below 70%, preferably below 50% and preferably between 35 and 45%, and the temperature of the surroundings should either be between 50 ° F ( ⁇ 10.0 ° C) to 90 ° F ( ⁇ 32.2 ° C) or be reduced to this temperature or a lower temperature during crystallization.
  • the seed crystals should preferably be 50 to 150 microns in size. It was found that seed crystals larger than 250 microns would not crystallize the material from the aqueous syrup solution within an acceptable period of time and would therefore affect the economics of the process. In addition, the amount of seed crystals used is a critical issue in drying the final crystalline material made by the process.
  • the amount of seed crystals and the moisture content of the syrup solution are essential for the duration of the crystallization time if the seed crystals are not of the same content or of the same type as those used in the syrup solution. It has been found that the amount of seed crystals used should be greater than 2 percent by weight based on the total solids content of the starting solution, and should preferably be 5 to 15 percent by weight.
  • the seed crystals used in the process can come from any source, but normally they should be pure fructose crystals, a mixture of glucose and fructose crystals, or they should be a part! of the crystalline end product obtained by the process according to the invention from a previous batch. It is important to use seed crystals of the same general type and the same type of sugar in the starting solution, because variations in the type of seed crystals compared to the solution components of the starting solution impair the crystallization in time.
  • the seed crystals should be added to the starting solution if they have a temperature of 120 ° F ( ⁇ 48.9 ° C) to 160 ° F ( ⁇ 71.1 ° C), preferably 130 ° F ( ⁇ 54.4 ° C) up to 140 ° F ( ⁇ 60.0 ° C).
  • the starting solution can be poured into a mold or other suitable container and then at 50 ° F ( ⁇ 10.0 ° C) to 80 ° F ( ⁇ 26.7 ° C) and a relative humidity of 35% up to 45% of the ambient air for a crystallization time of 6 to 72 hours. Pure fructose syrups only take a short time, e.g.
  • the crystalline material is harvested and dried using drying methods which depend on the moisture content of the end product. Then they are ground to obtain the free-flowing, anhydrous, crystalline fructose and glucose according to the invention. It is desirable and preferred to recycle a small percentage of the harvested material and use it as seed crystals for the same type of starting solution from a later batch.
  • the degree of concentration of the starting solution is critical, since it was found that if this degree is below 88 percent by weight, the solution remains pasty even after the addition of seed crystals and the crystallization product becomes pasty, ie hard. It is then impossible to put it in a dry, free-flowing, water-free powder form. If the starting solution exceeds 96% by weight, it remains a fairly glassy mixture.
  • the starting solution is normally at temperatures from 60 ° ( ⁇ 15.6 ° C) to 85 ° F ( ⁇ 29.4 ° C), for example at temperatures from 70 ° F ( ⁇ 21.1 ° C) to 80 ° F ( ⁇ 26.7 ° C), and a relative humidity of 35% to 45% until the crystallization takes place under physical conditions for the crystalline end product, which are partly dependent on the moisture content of the starting solution.
  • the crystalline product produced by the process forms in large pellets during the crystallization process, for example 3 grams, and that the crystallization pellets so formed are quite sensitive to heat. It has been found that the crystallization pellets no longer lose moisture during drying when a certain moisture content is reached, for example 3 to 5%. For example, hemispherical pellets with a base diameter of 0.75 inches ( ⁇ 19 millimeters) do not lose more than 3% moisture. Attempts to dry such pellets to a lower moisture content by subjecting the pellets to higher drying temperatures and vacuum have been unsuccessful because the surface became dry but the interior of the pellets became soft.
  • the heat sensitive, water soluble crystallization pellets can be dried to the desired moisture content by the process by cooling the pellets to a temperature below 34 ° ( ⁇ 1.1 ° C) and then granulating, for example by grinding to a size of less than 18 mesh. Thereafter, the ground pellets can be at a relative humidity of the environment of, for example, less than 50%, preferably 35% to 45%, at temperatures of, for example, 110 ° F ( ⁇ 43.3 ° C) to 160 ° F ( ⁇ 71.1 ° C) are dried to obtain free-flowing material with a low moisture content of, for example, 0.5 to 2%.
  • the high heat sensitivity of the crystallization pellets makes grinding difficult, since the product tends to melt due to the heat generated in the mill.
  • the pellets can be ground and then dried to a lower moisture content in conventional ovens.
  • the starting solution thus obtained was seeded with 5% (weight percent based on the total weight of the starting solution) at a temperature of 160 ° F ( ⁇ 71.1 ° C).
  • the seed crystals were 177 to 250 microns in size and came from a previous batch using the same starting solution as here. The seed crystals therefore contained the same solids in the same mixture as the starting solution used here.
  • Granular, free-flowing, colorless material of the same solid composition as the starting solution was obtained with a purity of 99% and a yield of 45%.
  • a pure starting solution concentrated to 95% was obtained from pure fructose and water. This starting solution was seeded with 5% (weight percent based on the total weight of the starting solution) seed crystals.
  • the seed crystals consisted of pure fructose and were 74 to 177 in size Micron.
  • the inoculated starting solution was placed in a mold and left at 80 ° F ( ⁇ 26.7 ° C) with a relative humidity of 45% for 72 hours. During this time, crystallization took place. The crystals formed were sieved off and then dried in a vacuum oven at 29 millimeters of mercury. The drying process lasted 4 hours. The drying temperature was initially 70 ° C ( ⁇ 21.1 ° C) and was increased evenly to 200 ° F ( ⁇ 93.3 ° C) during the 4 hours. The dried crystals were then cooled to a temperature a few degrees below 34 ° F ( ⁇ 1.1 ° C) and milled at this temperature to a grain size of less than 18 mesh (1.0 mm).
  • a pure starting solution of 93% was obtained from pure fructose and water. This starting solution was seeded with 10% (weight percent based on the total weight of the starting solution) seed crystals.
  • the seed crystals consisted of pure fructose and had a size of 74 to 174 microns.
  • the inoculated starting solution was placed in a mold and allowed to stand at 85 ° F ( ⁇ 29.4 ° C) with a relative humidity of 45% for 12 hours.
  • the crystals formed were sieved and then dried and ground.
  • 1 kg (kg) of the powder obtained according to Example 1 and ground to 18 mesh (1.0 mm) was dried in a temperature-controlled oven in the presence of circulating air as follows: in a first batch, the drying time was 8 hours at an oven temperature of 110 ° F ( ⁇ 43.3 ° C) and at a circulating air humidity of 35%. The final moisture content of the dried crystals was 2%. A second batch was dried for 4 hours at an oven temperature of 150 ° F F ( ⁇ 65.5 ° C) and a circulating air humidity of 35%. The final moisture content of the dried crystals was 1%.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)

Claims (11)

1. Procédé de fabrication d'une matière anhydre, cristalline, fine et sèche au point de couler comme de l'eau qui ruisselle, à savoir une matière contenant du fructose, caractérisé par
a) la préparation d'une solution aquese de départ contenant du fructose ou un mélange de fructose et de glucose en quantité variant de 88 à 96% en poids environ, laquelle solution est pratiquement exempte de décolorations,
b) l'ensemencement de cette solution de départ au moyen de cristaux germes essentiellement de la même substance que celle qui a été dissoute dans la solution de départ, le poids de ces cristaux germes représentant 2 & 15% du poids total de ladite solution, la dimension de ces cristaux germes en fines particules étant comprise entre 50 et 250 microns et la température de la solution de départ se situant entre 120° F (48,9° C) et 160° F (71,1 °C),
c) la cristallisation complète de la solution de départ ensemencée, cette cristallisation étant obtenue en laissant ladite solution en repos dans un milieu ambiant d'une humidité relative inférieure à 70%, pendant 2 à 72 heures et à une température comprise entre 50° F (10,0° C) et 120° F (48,9° C),
d) la séparation, le séchage et le cas échéant, la fragmentation (en morceaux minuscules) des cristaux ainsi formés.
2. Procédé conforme à la revendication 1, caractérisé par le fait que dans la zone de 50° F (10,0°C) à 120°F (48,9°C), la cristallisation débute à une température élevée et qu'elle se poursuit à des températures plus basses lorsqu'elles est en cours.
3. Procédé, conforme à la revendication 1, caractérisé par la fait que la cristallisation s'effectue à une température de la solution ensemencée de départ, se situant dans la zone comprise entre 50° F (10,0° C) et 90° F (32,2° C).
4. Procédé, conforme à la revendication 1, caractérisé par le fait que la solution de départ est une solution de sirop de céréales, à haute teneur en fructose.
5. Procédé, conforme à la revendication 1, caractérisé par le fait que la solution de départ est une solution de sucre et de fructose contenant du fructose ou un mélange de fructose et de glucose en quantité comprise entre 92 et 94% en poids.
6. Procédé, conforme à la revendication 1, caractérisé par le fait que la cristallisation s'effectue pendant que la solution de départ ensemencée se repose pendant 2 à 72 heures, dans un milieu où !'air ambiant a une humidité relative inférieure à 50%, la solution de départ étant à une température comprise entre 50°F (10,0°C) et 120°F (48,9°C), laquelle température est maintenue constante ou est abaissée dans cette zone de températures, pendant la cristallisation.
7. Procédé, conforme à la revendication 1, caractérisé par le fait que les cristaux germes proviennent d'une solution de départ de la même composition que celle à traiter mais qu'ils ont été obtenus par un procédé appliqué à un moment antérieur.
8. Procédé de fabrication d'une matière anhydre, cristalline, fine et sèche au point de couler comme de l'eau qui ruisselle, à savoir une matière contenant du fructose, à savoir un procédé conforme à la revendication 1, caractérisé par:
a) la préparation d'une solution aqueuse de départ, contenant du fructose ou un mélange de fructose et de glucose en quantité variant de 90 à 95% en poids environ;
b) l'ensemencement au moyen de cristaux germes en particules d'une dimension de 50 à 200 microns;
c) la cristallisation complète de la solution de départ ensemencée, cette cristallisation s'effectuant en laissant ladite solution au repos dans un milieu ambiant d'une humidité relative inférieure à 70% pendant 6 à 72 heures et à une température comprise entre 60° F (15,6° C) et 85° F (29,4° C).
9. Procédé, conforme à la revendication 1 ou 8, caractérisé par le fait que les cristaux séparés sont moulus à une température inférieure à 34°F F (1,1°C) et qu'ils sont ensuite séchés à une teneur en humidité non supérieure à 2%.
10. Procédé, conforme à la revendication 9, caractérisé par le fait que les cristaux moulus sont séchés à une teneur en humidité comprise entre 0,5% et 2% en poids, l'air ambiant étant d'une humidité relative inférieure à 50% et à une température comprise entre 110° F (43,3° C) et 160° F (71,1 ° C).
EP80101415A 1979-04-13 1980-03-18 Procédé pour la préparation d'un produit anhydre, épandable et cristallin contenant du fructose Expired EP0017778B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/029,699 US4199373A (en) 1979-04-13 1979-04-13 Process for the manufacture of crystalline fructose
US29699 1979-04-13

Publications (2)

Publication Number Publication Date
EP0017778A1 EP0017778A1 (fr) 1980-10-29
EP0017778B1 true EP0017778B1 (fr) 1981-11-25

Family

ID=21850400

Family Applications (1)

Application Number Title Priority Date Filing Date
EP80101415A Expired EP0017778B1 (fr) 1979-04-13 1980-03-18 Procédé pour la préparation d'un produit anhydre, épandable et cristallin contenant du fructose

Country Status (6)

Country Link
US (1) US4199373A (fr)
EP (1) EP0017778B1 (fr)
CA (1) CA1095904A (fr)
DE (1) DE3060092D1 (fr)
DK (1) DK155080A (fr)
PT (1) PT71086A (fr)

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Also Published As

Publication number Publication date
DK155080A (da) 1980-10-14
PT71086A (de) 1980-05-01
CA1095904A (fr) 1981-02-17
DE3060092D1 (en) 1982-01-28
EP0017778A1 (fr) 1980-10-29
US4199373A (en) 1980-04-22

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