BG97580A - METHOD FOR PREPARING CRYSTAL FRUCTOSIS - Google Patents

Abstract

The process is complex and produces two products, crystalline fructose and a liquid sweetener, e.g. high fructose syrup, from a dextrose-containing feedstock. Part of the dextrose is isomerized to fructose and the resulting solution containing dextrose and fructose is fractionated to produce a high fructose solution. The latter is crystallized to produce fructose and the remaining mother liquor is then mixed with dextrose-containing solutions to produce the liquid sweetener.

Description

Inventory% refers to the production of sugars for nutritional purposes. In particular, it relates to the production of fructose by isomerization of dextrose. In particular, the invention relates to the simultaneous preparation of anhydrous crystalline .. fructose and a syrup containing ractose and dextrose.

Also from the specific. Sachet are a method of crystallization of Fructose from a solution of fructose upon cooling, so that different degrees of saturation are obtained during different periods of crystal growth, as well as a method of obtaining purified and coadentodranium fructose syrup.

Πρεowosxuc cd

Liquid phase of p-ructose products

Fructose is a monosaccharide, highly valued as a nutrient sweetener. Much of ructose is obtained from cereal starch and the main form in which the product is produced is high-syrup syrup. _L. ruktose / SVSF /. Syrups in commercial irea contain from 12 to 96 wt. X fructose sprmao dry solid / mt /. (as used below in the description, including the claims, the notation m in * denotes weight percent by weight of dry solid). the remainder is pre-dextrose. The syrup commonly used as a sucrose substitute in soft drinks Sjb /

Fructose, 41 (dextrose; ι 4) / sacoli saccharide violets / all strands are lean.

in production; ' the process of obtaining C.mb * begins with the enzymatic degradation of purified mud from. pour, the main source of crude ... atherll is the grain of chicken obtained in the process of wet grinding. However, '.ιχ'3 .. <3 ^{1 1 - 1} uses lx-starch of similar purity from other sources.

In the first step, a typical method for the heat-shrinking kappa is jellied by high-temperature cooking. the gelling starch is then decomposed and converted into dextrin by means of a thermostable alpha-α-chylase in a continuous two-step reaction, the product of this reaction being soluble dextran hydrolyzate with dextrose equivalent ZW 6-lb, suitable for subsequent ethane conversion .

After the degradation process to dextrins is carried out and the temperature of 10-lb dd-chlorolysis is adjusted to the saccharification step. At the time of saccharification, the hydrolyzate is further hydrolyzed to dextrose under the enzymatic action of glpamllas. _; . Although sugaring can be done in portions, in most modern sugar factories .... the process is carried out in a continuous process. Eri continuously carrying out the saccharification reaction to 10-1b to -zzrolzlzat after adjusting the appropriate temperature and temperature was added gl; The composition of the typical hydrocarbon fluid, obtained with high-dextrose saccharification, is as follows: 04-9b 7 dextrose, 2-h /, maltose, o-h-b, y, maltotriose and 1-2 / h saccharlides, all percentages are given relative to the dry solid. Typically, the product obtained contains from 20 to 37 / ♦ dry matter. Doses of high-dextrose hydrolyzate are then purified to provide dextrose-containing feedstock for the subsequent lysomerization process.

It is necessary to obtain a starting material, dextrose-containing raw material of very high quality for carrying out the lomerisation, so that the resulting fructose-high syrup (CaCw) can be very weakly colored and have a low ash content. a high purity of feedstock is also required for efficient use of immobilized lysomerase columns.

columns for carrying out enzymatic isomerization containing lmoblated isomerase are used continuously for a period of several months, during which time a very large volume of dextrose vessel passes through the columns; .giving feedstock, extremely small amounts of contaminants such as ash, lethal?; Onl / ll protein, being digested into the feedstock may accumulate l to reduce the enzyme productivity to this very low rate _. the known starting material is purified to a color of i.1 (µl x 160) and to

-1 conductivity from o-IU and i.roroma.

After the solvent is removed, the high-dextrose liquid is evaporated and concentrated to the degree of crystallization, whereby it is prepared for carrying out the rhizocyl. In addition, the feedstock is chemically treated by the preparation of a magnesium horse which, on the one hand, immobilizes the heparase and on the other hand. ^ eral.

the process of fructose is converted to fructose, usually carried out in a stream containing 34-96 7- / s t / dextrose l 4-6 7 / s t / weeds candle, at

- 4 46-00 / dry wax. η the swelling o with pii of 7.6-0.2 l temperature 2b ° and l is subjected to enzyme reaction and lengthens for 1/2 to 4 hours αρ. · ΐ ай— * ао а.

the conversion of glucose to cructose and ooratl. * process with an equilibrium constant of about 1.and at 6a °. lo _r idd this is to be expected that the rd equilibrium with equilibrium yields about 47-16 / .ructose, for example, we use 94-όυ / dextrose / glucose / deacrose on the initial raw material. the extent of the process _; -; a. {zo ^ erlzar, la illo to equilibrium liquid proves that it is loosely the reindex of isomerslacl .. to interrupt the true degree of conversion of about 42 / - * ructose to provide n, antique optimolao it is time for the oeaxone mixture to precipitate in the reactor.

η used zo-column / column with lyloylphenol-aHoZo. «eoase / ', the degree of dextrose (Gdmkoza) injury in <* hand <this proportional to ease activity of .sholiazlian isomerase.This. .with the flow of g ^ is ^ in an approximately exponential way, because the column is new & the activity is high, the flow rate of the feedstock through the column is relatively high, while the shorter time aa resides in the source. in the column ensures a degree of conversion to 42% when the ple as the use of the column increases, the feedstock flow rate through the tray column is reduced proportionally to allow longer time for the lomerization to occur, in accordance with the reduced activity, so as to obtain a constant degree of conversion.

In practice, multiple Jo-columns are used to reduce production fluctuations related to capacity and conversion rate. a * ri such organization and production!

each column can act essentially independently of the others; the variation of the total deoite of the columnar should be kept within a relatively narrow range, because of the need for evaporation to carry out subsequent finishing operations, in practice the flow cannot be precisely controlled at all times so that a flow of 42 / fructose, but this can easily be achieved as a level.

one of the more critical parameters for conducting the method is pli inside the iso-columns. The working pH is usually a compromise value between the pH fatigue at maximum activity (typically about pH 8) and the pH value at maximum; stability (typically about ph from 7.0 to 7.8). This is compounded by the fact that the dextrose feedstock does not have a stable ph at temperatures around 6b ° C. j shows some decomposition channels, which release acidic by-products that cause the pH in the iso-column to drop during the process.

After isomerization, a typical step in the production process is the secondary purification of the resulting 42 / _s high fructose content syrup. but the time of chemical treatment and isomerisation, when the feedstock is held at a higher pH and.temperature for a certain period of time, further coloration of the product is obtained, the product also contains additional. inorganic impurities from chemicals added during of isomerization. These coloring and contaminants are removed by secondary charcoal treatment and through ion exchange systems. The refined 42 (syrup / Sab *) is then usually evaporated to give a 71 Z solid when the product is ready for sale.

- Ο the use of activated carbon for the purification of sugar syrups generally 2 known, η US patent g 1,979,761 describes the mixing of raw sugar syrup / inter alia syrup not mixed with glycose or Art sugar / at 60 ° Bri-x / 60 X dry matter / 1 to 2 X wt. Activated carbon on heating for a short period of change to 134 ° C. US Patent 2,763,580 describes in detail the processing of sugar solutions / e.g. of cane, beet or grain sugars / with a solids content of between 10 and 60 X, in particular 20 to 56 / wt at 125 to 200 ° C with activated charcoal. The patent has described that partial activation of a single concentration or other conditions can be carried out, after which treatment with charcoal may be completed at higher concentrations of the solution (obtained by evaporation) or under other conditions.

and .Micro patents relating to the preparation of sugar syrups from grains containing fructose, inter alia, the treatment of charcoal and the subsequent concentration of aqueous solutions having different concentrations of fructose (w / w) and different amounts of dry matter in patents of. U.S. Patent Nos. 3,883,245 and 3, 9 and 948 describe the treatment of syrups containing ractose with about 20 X / wt / fructose and about 40 X dry solid with activated carbon and subsequent concentration of syrup / e. by evaporation to 70-83 (dry matter).

U.S. Patent No. 3,684,574 discloses a treatment with charcoal syrup containing about 20 (/ wt /) of ruktose in dry matter of about 20 X, and a further concentration of the syrup, in patent Pat Sam -ν 4,395,292 supplying separating columns with charcoal-treated * ect of rructose and dextrose with a solids content of 10 to 7i /, preferably 40 X a / 1, subsequent concentration of the fructose-containing extracts. it is feared that extracts containing over 90 7 fructose may be obtained, and specifically in Example 7 it is stated that when loading fractionating column with a solution containing 40 Z of dry matter, a fraction containing 100 Z / s w / ractose or 9 / dry solid was obtained.

the resulting syrup (CBOI) after isosurfacing usually contains 12 Z of fructose, 52 Z of dextrose and about 6 Z of oligosaccharides. but for the reasons outlined above, this product represents practically the maximum amount of fructose produced by the isomerization process. A selective concentration of fructose is required in order to obtain a higher concentration of fructose. many of the usual separation techniques cannot be used for this purpose, dull as the differences between the two isomers with the same molecular weight are small. However, the fruit preferably forms complexes with different cations, such as calcium. This difference was used to create manufacturing methods for the separation of isomers.

There are two fundamentally different methods of industrial application that are currently applicable to different cases of fructose purification. in both cases resins are used in a preferred cationic dorm in a filled system cfr united.- from the methods an inorganic resin is used, leading to selective molecular absorption of the fruit / see 1. ^ ensen,%. content of dactose, AOptectl of the Institute of Engineering Hops /, O5th National Meeting, Philadelphia, 1978 /.

in the second of the industrially applied methods organic resins are used / see the article on e. The biomolecule purification, ppm / epo Epo ^ nB -.- 4 _t 6; 37-43, 1982 /. When an aqueous solution of dextrose and fructose is passed through a fractional column / e.g. 42 ("high fructose syrup"), fructose is retained by the resin more than dextrose. deionized and oxygen-liberated water is used as the eluent. the separation is usually carried out with a filler column of fine-grained, low-crosslinked polystyrenesulfonate cation exchange resin, using the calcium salt as the preferred compound. The enriched product containing approximately 90 (fructose is referred to as a very enriched syrup containing Fructose-derived cereal starch AoPS). This fraction can be mixed with 42 (ChCw / starting material) to produce products having a fructose content of between 42 and 90. Nan-typical;

of these products is 55% fructose syrup, which is called enriched fructose bean syrup (b * 6 or 55 bFb). No. 4,395,292 to Patent No. 4,395,292 exemplifies Drscher 1 / for the fractionation of a mixture of fructose a dextrose into various fractions and mixing of the fructose enriched fractions to obtain a fructose-containing syrup of Lb.o. the same example has been described to produce single fractions with a high concentration of .. fructose / e.g. 75.1 /, / with m in // as well as combined fractions with lower fructose concentration / e.g.

64.5 7, / with m in / is combined with 58.2 / / with m in / fructose /.

The treatment of other purification streams in the fractionation process is an important issue to discuss. In general, the dextrose-rich refined streams return to the dextrose feedstock, which feeds the pulmonary column system for subsequent conversion to 42 / SvCF. the purification stream containing dextrose and fructose containing a higher level of

Fructose, compared to that of the feedstock, can be recycled through the fraction column to maintain a high level of solids or reduce the amount of water used. The refined stream rich in oligosaccharide can be recycled into the sugar system.

By using water as an elution medium, this has a major impact on the overall evaporative load of the system. So, the most important parameter for us. The structural design dictating the overall economic process is the optimization of the yield of a solid product with acceptable purity at reduction / reduction to the minimum of the eluent eluent. The efficiency of feeding and using water must be increased to obtain optimum yield. _L obivat is important to reduce the cost of re azomerdzatsiya.

". Approaches suitable for achieving these goals include recycling techniques, more balancing of the resins by appropriately rearranging the group of columns and adding multiple entry and exit points to the columns. 1'this approach can be used to improve the purity and yield of the product.

m a series of fractionating columns - the small, noticeable increase in feedstock fed into the fractionation columns leads to a higher level of fructose produced, which translates into greater benefits from production, by increasing the milk yield and purity of the product . In practice, this results in the maximum optimization of the feed volume ratios relative to the volume of the resin for a given cycle, minimizing the ratio of water not consumed in the columns to the resin volume in the cycle, and careful distribution of the fluid in the columns.

Solid fructose products

- 10 They are known. ”Etodl for crystallization of fructose. 1 E.g. crystalline lactose .. yu _L. is obtained by the addition of absolute alcohol km syrup obtained by acid hydrolysis of inulin / &lt; al., Matt. bu ' ^v , aH .Cirt-.C 44i, 399, 1942 /. Dextrose fructose production is described in U.S. Patent No. 2,354,664, and U.S. Patent No. 2,729,587 describes sucrose (sucrose) fructose production by enzymatic conversion.

Fructose forms orthorhombic ospheroidal prisms from alcohol, which decompose at about 1b3-105 ° C. known aa also hash-hedge ά dhydrate crystalline forms of fruit, but it is preferable to avoid the formation of these forms, since in fact they are more hydroscopic than anhydrous forms and have melting points close to room temperature. These properties of the fruit crystal dorms make it difficult to handle them.

Soluble crystalline fructose (iW) is prepared by a method in which an organic solvent, such as denatured ethyl alcohol, is mixed with a stream containing a high concentration of fructose (95) with m in /. This stream crystallizes upon ohmation, forming pure crystalline ractose. the product is centrifuged to remove from the internal alkali, the solvent is separated and the product is dried.

and Ski Patent No. 4,199,374 discloses a method for the preparation of Fructose crystallized from a solution of <RTI ID = 0.0> OPS </RTI> enriched crude crude / ethanol. The solution is sprinkled with melons of fructose or glucose. The crystals are separated by filtration, centrifugation or other suitable means. The crystals were then washed with alcohol and dried in vacuo. The moisture content of alcohol and syrup in this method must be very carefully controlled so that free-flowing fine crystals of fruit are obtained.

it is also possible to obtain simply dried fructose sweetener / * 1FDD ... etoct to produce shu consists in the drying of fractions obtained from high-content fractionation; Dryers are then rotated, then sorted through sorting sieves and mills, l patent of Cm 4,317, and 21 describes the preparation of such a granular, semi-crystalline solid dactose containing less than 2 wt. / water, the patent indicates that about 60 / wt. of the product is crystalline fructose and less than 35% by weight. / of the product is amorphous' ruktose. an air dryer is used, with an initial temperature of 50-80 ° C. a portion of the solid solid product obtained is recycled and initiates crystallization.

min of the disadvantages of the nFN production method is that the product cannot be called pure fructose as it is a total / common / sugar product and does not meet the criteria for Fructose * in the Food Chemicals Code. Moreover, it is not completely crystalline, which makes it io-hygroscopic and therefore more difficult to handle under conditions of increased humidity than crystalline Fructose,

For the preparation of crystalline fructose, a method with water may also be used. Typically, such a method requires a high-fructose feedstock to be used. cooled to fructose crystallized from solution. Such a method has been described in several publications.

a patent for Om 3,313,023 describes a method for the preparation of crystalline anhydrous fructose from an aqueous solution of fructose (minimum 95 (dry matter)). The pH value of the solution

- 12 must be between Z.b and 8.0. The -fruit solution was concentrated in vacuo to give a water content of α 5 X. The solution was cooled to 60 ° C, sprinkled with crystalline fructose and stirred vigorously while maintaining the temperature in the range of 60-85 ° 0. It is stated in the patent that under these conditions a crystalline mass is obtained which, after slow cooling, the aole ίνΐ cracks or ;; acroo> 1 and after drying, a non-sticky, free-flowing powder. the patent states that the formation of a glassy product is avoided by this method, which usually occurs when a solution of this type of concentrate is concentrated in vacuo and allowed to cool in the usual way.

x patent for CA9. χ 3,883,365 is described crystallized from fructose and glucose crystalline water with 90 X dry matter and containing 9υ-99 X / wt. The solution is saturated (88-65 ° C). - uctose crystallizes from the solution by adding uructose crystals of homogeneous crystal size. The formation of new crystals is minimized by keeping the distances of the crystals that are scattered, causing crystallization from any disadvantage and keeping the degree of glut between 1.1 and 1.2. The volume of the solution was continuously increased in steps as crystallization continued. the optimum pH of the fructose solution is stated to be 5.0, and that the crystals thus obtained have an average size of between 20-600 microns, the crystals are separated from the solution by centrifugation.

in the patent of ... 3,928,062 discloses the preparation of anhydrous crystalline fructose by sprinkling crystals of a solution containing 83-95.5 X · / dry matter / total sugars containing 68-99 X fructose. ... stallation can be carried out by conventional cooling of the solution at atmospheric pressure or by evaporation of the water under reduced pressure. The formation of hemihydrate and dachydrate is crystallized by performing crystallization at a determined concentration of lactose and temperature. These grmxTTs in the saturation region below the point at which crystallization of the hemihydrate begins. It is stated in the foregoing that the material can be reused for crystallization of further quantities of the product at the same time without any further treatment, the sending of crystals which serve as the nucleus of crystallization is effected by suspension ^: wound in solution. of pre-prepared crystals.

A patent for 4,199,373 discloses a process for the preparation of crystalline rructose by the administration of α-15 wt. X crystalline embryos are strucose in _o in fructose syrup at a concentration of 38-96 (w / v), allowing the solution to crystallize at about 5a to 90 ° D at relative humidity below 7U / _s . and the patent states that the crystallization time required is from a to 72 hours. The crystals obtained by this method are in the form of

A.J. Art. No. 4,164,129 discloses a cetode and apparatus for producing crystallization embryos. We use a series of centrifugal separators to select germ crystals from

4XL · treated with embryo syrup having a predetermined size range.

crystallization curves of cooling The cooling of saturated or supersaturated solutions to the distortion of the substance from them is naturally known.

it is also known that the natural cooling of a saturated or saturated solution often leads to germ separation,

- 14 contributing to. obtaining undesirable large differences in the distribution of crystalline product mixtures, iianp. in Chemical Technology Cycle Technology, Volume?, pp. 243-28b / KmK-01i »pgh, publishing house - ^{, χί} '-' - ··. · * · b, pm ^ ork, third edition, 1979 / that when naturally cooled in saturated. the solution occurs at peak rapid crystallization germ formation, the article describes that under controlled cooling conditions a constant level of supersaturation can be maintained to achieve controlled germ formation within certain limits. Figure 5 shows the curves obtained by natural and controlled cooling of the solution, which are published in the article cited above.

Texwu-WFCXA ua U00EpeT £ WM.eT6

The various aspects of the present invention are discussed in greater detail below.

A complex, versatile method of producing fructose-containing sweeteners In one aspect, the present invention relates to the complex preparation of a plurality of uructose-containing sweetening products. which is the most general aspect.

A. simultaneous preparation of liquid sweetener and crystalline uruitosis

B. In a more particular aspect, the invention relates to a process for the preparation of crystalline fructose and a liquid sweetener containing fructose and dextrose, which comprises: crystallization of fructose from an aqueous solution of fructose, to a mixture containing crystalline fructose and mother liquor ; separation of cryst-: ·? ·· :? . fructose lactose; and mixing dextrose with the mother liquor to obtain a liquid-oasis sweetener containing dextrose and fructose.

In the preparation of crystalline sucrose from an aqueous solution, it is a common practice to reuse the mother liquor for further crystallization, thereby increasing impurities in the lateral alkali, called molasses. This pelvis is generally so polluted that it only has value as an additive

to animal feed or as a phe!) mentation medium, µ patent on SL,. * · 'a described that the ether alkali from crystallization- tion of the Fruit Yao. g to be reused to get- next river < fructose zebrafish. Relatively we- kay yields ya scabies two single-stage fructose crystals · when used of the ordinary crystallization technique

the difficulties associated with the isomerization and fractionation of

syrups obtained from cereal feedstock to obtain starting syrup from Fr.u: a goat with a high enough concentration for

powering the crystal * mash makes the recycling of the mother liquor in the subsequent crystallization of crystalline fructose as desirable as it is, the skin of producing crystalline fructose together with the liquid sweetener by adding dextrose to the mother liquor. once to get two high quality sweeteners. This in turn allows the maximum yield of fructose, which is useful as a sweetener, to maximize the difficulties associated with isomerization. The unit sings to the point of losing its usefulness, dextrose was consumed, and the raw material for scab lysis was obtained, and thus the deaxtrose to ether fluid was at the expense of part of the enriched achieved by Fractionization.

as one specific embodiment of this aspect of the invention, the present invention relates to a process for preparing

extracting crystalline fructose and dextrose-containing and fructose-containing flux containing dextrose, which is an ethodermisation of a portion of dextrose in the feed stream to obtain the first dextrose and fructose-containing stream; separating the first dextrose and fructose containing stream into a first feed stream and a second feed stream; fractionation of the first feed stream to obtain a high fructose stream; crystallization of fructose from the stream with high concentration of fructose to yield ccfc, yielding crystalline fructose and mother liquor; separation of crystalline fructose from the mother fluid; and mixing at least a portion of the mother liquor with the second feed stream to obtain a second fructose and dextrose containing stream having the first fructose content higher in dextrose relative to dextrose and fructose. / as used in the claims the expression dextrose flow and

Fructose means

L is a related stream that contains fructose dextrose / aspect, the invention also relates to a process for the preparation of crystalline fructose and a liquid sweetener, which consists in crystallization of an aqueous solution of Fructose to obtain a mixture of crystalline fructose and mother fluid; separation of crystalline fructose from the mother liquor and stopping subsequent crystallization in the mother liquor to obtain a fructose-containing liquid sweetener.

"The aetheric fluid remaining after crystallization is a saturated solution of. dactose. It is known from the prior art, e.g. from US patent 92b, 0b2 that the mother liquor may be reused to crystallize further quantities of crystals. In order to be used with such a liquid, it is necessary to heat this saturated lateral fluid or concentrate it to a suitable fructose solution, which is suitable for crystallization, to allow crystallization in this mother liquor. The hay is found to be / doodore interrupt the subsequent crystallization and use the mother liquor to produce a liquid sweetener than to create conditions that cause crystallization of the next crop of lateral fluid. as mentioned above, the mother liquor is a saturated solution of fructose. To prevent crystallization and precipitation of fructose crystals from this saturated solution during the subsequent handling, transport and / or storage in storage, steps should be taken to interrupt crystallization in the mother liquor. The '1' aspect of the invention relates to the first embodiment of the invention described above, which avoids recrystallization from the mother liquor. However, this process does not necessarily require the sacrifice of the benefit of> - radiation, since the inhibition of subsequent crystallization need not be carried out by the addition of dextrose, but may be effected by the simple dilution of the mother liquor with water, at which stops crystallization without altering the purity of fructose in the mother liquor.

υ. , '.-. Ultra-sophisticated fractionation of high-practose sweeteners

In one specific embodiment, the present invention relates to a method for producing several fructose-containing sweeteners and at least one containing dextrose and fructose, which method consists in fractionating the feed stream containing dextrose and fructose enriched with dextrose raffinate, low-fructose extract and high extract

- 18 fructose content, in which the fructose concentration is above about 90% (w / w); and the mixing of the low-fructose extract with a composition having a greater amount of t in the concentration of dextrose than the said low-fructose extract to give a liquid sweetener.

this context, the concept lruktozen sweetener includes any sweetener sadardasht fructose oez be taken into account, _including whether type .ruktozata in solution dispergyarana, amorphous or crystalline. For example, a high fructose extract can be used for. the preparation of syrup containing N-fructose, of crystalline 'Fructose or of semi-crystalline fructose, in which at least part of the &lt; RTI ID = 0.0 &gt; fructose is in solid amorphous &lt; / RTI &gt;

fractionation of lomeromerated dextrose syrup, e.g. one that contains both fructose and dextrose, to produce a Fructose sweetener is usually carried out by making a dextrose raffinate and a fructose extract, by recycling the remaining fractionation products. For example, U.S. Patent No. 4,395,292 states that such conditions for carrying out the process are preferably, however, using two extracts, one of which has a higher concentration of Fructose (by weight in), the so-called high- h, ructose extract, and of a second lower concentration (s) in fructose extract, the higher concentration fructose extract can elicit the resulting swelling to magnify the total degradation rate of the parent material during isomerization , as well as any related problems disappear. / So e.g. no capacity reduction required; of fractionation, the higher the load associated with evaporation of the elution mode and / or the harmful pressure drop caused by the increased elution water flow required to increase the spreading /

- 19 The benefit of obtaining a low-fructose extract has a limited scope compared to the benefit of the high-fructose extract. Dova means that using low-fructose extract to produce crystalline -... rutose would be difficult /. The ractose in this extract ..one should not be used to increase the fructose content of sugar syrups obtained from grains that odorate to less fructose, e.g. when mixed with isomerizadal syrup, such as e.g. with 42 X fructose syrup, to obtain an extracellular syrup, e.g. Fm / fructose; syrup.

in one particularly preferred embodiment of this aspect of the invention, the high-octo-ruktosyl extract is used to power crystals. for crystal and set to fructose. Accordingly, in one aspect, the invention relates to a process for the preparation of crystalline. Fructose and a sweetener such as sterling dextrose and fructose, the method of which comprises flow distraction comprising dextrose or fructose, enriched with dextrose, raffinate, iodine-fructose extract and viscose. fructose extract; crystallization of pactose from an aqueous solution obtained from the high-fructose extract; l mixing the low-fructose extract with a dextrose-containing composition, which has a dextrose concentration higher than that of the low-fructose extract to produce a liquid sweetener, seizure dextrose and fructose.

This implementation of the ethics-d. is particularly advantageous, since the concentration of ₄ ruktose (w / w) usually required for crystallization of Fructose from an aqueous solution is so high that the fracture of the flow from the isomerization process containing dextrose l fructose to obtain a single extract bl were impractical. In other words, the rate of decomposition required to produce an extract which

- 2U to go satisfactorily extinguished ^ ructose purity to swell drilloli! as a feedstock source for the crystallizer to feed, it will often reduce the recirculation capacity and / or increase the other difficulties associated with the encapsulation that such a variant of. implementation rather impractical.

possible extract of the method, since two extracts are taken - high-rustzzen, 1 alsko-ruktozen and they are separately used for down-crystalline sweetener and liquid sweetener respectively, in that the amount of kactuctose in π: ΐΰ «ίθ - ·; .ρνκτο39.ιπ extract which is useful for enhancing the content of. tructose in syringe-pap syrup is lower than that given in octo-ractose extract, boot powder / x 2-C. V-Ju.v> decomposition state, this reduces the total amount of fructose (by weight in), which is useful for obtaining a precise sweetener. this disadvantage is reduced by the use of .later fluid from the crystallization of a portion of the fruit in a high-density, lactose extract. In other showers, in a particularly preferred embodiment of the process, a mother liquor containing. Aructose, psxx-arctose extract or lomerised syrup of a grain of raw material is mixed with one another to obtain a liquid sweetener / e.g. t £ /. . _l. lactose syrup / ·

There is a crisis and cooling down. supersaturated solution

... another aspect of the invention relates to a method for the preparation of crystalline uructose from a solution containing arctose, any method of which consists in cooling said solution in the first instance; the turkey has reached its original speed to cool again; with this coolant of the said solution pud. range and intermediate cooling rate, which is slower than the original speed; and - zl - thereafter cooling the solution at a finite temperature range and a cooling rate at a rate greater than the intermediate rate.

Figure b shows typical cooling curves used in the crystallization process, curve A is the natural cooling curve and curve b is a controlled cooling curve designed to achieve a constant level of 'saturation'. 4a shows the cooling curve for different saturation solutions according to the invention. When comparing the two figures, one can see the big difference between the cooling curves of the conventional method and the cooling curves obtained according to the present invention.

the use of a certain cooling rate in the intermediate cooling period, which is lower than the cooling rate in the initial and final periods, allows one to reduce to a minimum both spontaneous nucleation of crystals in the solution l heat-induced decay of ructose in solution, especially during the initial cooling period, · the reduction of the ability to form crystalline nuclei results in a crystalline product having a more uniform ionic particle size distribution. to reduce the damage caused by heating, to increase the yield of crystalline fructose liters of mother liquor and reduces the level of • impurities from the degradation products in the mother liquor, thus improving the soft value as a source of "rruktoza for preparing a liquid sweetener.

III Purification of high fructose syrups by treatment with low carbon content of solids and solution in charcoal

B. Another aspect, the present application relates to a method for preparing a concentrated fructose solution, which consists of preparing a fructose solution having a concentration higher than about 75 (w / w) and a concentration of cyxi substances less from 4o Z; treating this solution with activated charcoal to obtain a purified ractose solution; and evaporation of this purified solution to a solids concentration greater than 40 [mu] m. .

As the treatment of activated carbon sugar syrups for the purification of such syrups is well known, it has now been established that fructose syrup having a high fructose concentration (w / w) should have a relatively low dry matter concentration in the presence of activated charcoal to reduce the formation of di-products, e.g. of daroctose, which may reduce the available fructose in the syrup, inhibit the crystallization of the fructose from the syrup and / or affect the organoleptic properties of the syrup or sweetener prepared therefrom. Tables XIl III show the effect of the concentration of solids on the formation of dlfructose at high fructose concentration in syrup / 95 + / wt / for a certain time in contact with activated carbon.

In one such aspect, the present invention relates to a process for the preparation of crystalline fructose, which consists in fractionating a stream containing dextrose and fructose to obtain a stream having a high fructose content of more than 90% (w / w) ; treating this high-fructose activated carbon stream to obtain a purified stream containing / ructose; then subjecting this purified fructose vapor to evaporation to obtain a fructose solution; and crystallization of fructose from this aqueous fructose solution.

The sequence of treatment with activated charcoal after the subsequent evaporation of the high fructose stream ensures that the treatment is carried out at a relatively low solids content, since high-fructose extracts usually have a low solids content when obtained by elution on a fractional column.

B) another specific embodiment, the present invention relates to a process for the preparation of crystalline fructose, which consists in crystallizing fructose from a solution of Fructose, to obtain a mixture of crystalline fructose and a mother liquor containing fructose; separation of crystalline fructose from the mother fluid; mixing at least a portion of the fructose from this mother liquor with a liquid containing water to obtain a low solids fructose solution / e.g. less than about 70 (dry solids); treatment of this fructose solution containing a low content of activated carbon solids; and evaporation of this solution of low-solids fructose to obtain a higher solids of fructose.

in one particularly preferred embodiment of the method, the mother liquor obtained from the crystallization of fructose is mixed with a liquid containing water / e.g. tap water, fresh water, saccharide syrups, such as 42 /. fructose syrup and the like / to reduce the solids content before treatment with activated charcoal and then evaporate to obtain a higher solids content, the resulting solution with a higher solids content can be used in various ways, e.g. to feed the crystallizer, to a high-fructose syrup sweetener or to obtain a feed stream, all of which benefit from

- 24 advantages mentioned above which result from the reduction of the concentration of solids in the mother liquor, before being treated with activated charcoal and subsequent evaporation.

pa Figure 1 shows the various steps of the conventional method for the preparation of 42 (high fructose syrup / Cx *) and 55% enriched fructose syrup (OPS) from starch.

I-ia Figure 2 is a proven combined method for the preparation of two starch-based products, namely crystalline fructose and enriched fructose syrup.

11a Figure 3 shows in more detail the implementation of the method illustrated in Figure 2.

Pa. Figure 4 shows a graph of the temperature of the sugar mass as a function of time after the introduction of the crystalline embryos in a conventional cooling program of the supersaturated solution according to the invention.

Figure 5 shows the time-dependent graft of temperature variation in a series of crystallizers, curve a showing temperature variation under natural cooling and curve L for constant-saturation cooling

An important feature of the present invention is the co-occurring effect of producing both anhydrous crystalline fructose and enriched fructose syrup. The yield of crystalline fructose from the sugar mass is generally in the order of 40-55 Z, e.g. 45 /. . longer crystallization time would increase the yield, but at the expense of a more costly process due to a reduction in the throughput of the installation. Thus, a significant advantage of the method is that it combines the crystallization of fructose with a process that not only provides the raw material for the crystallization process, but can also be considered as a lossless process

- 2b of non-crystallized fructose.

In some of the prior art methods for the preparation of crystalline ractose, the non-crystallized portions are recycled back to the crystallization process. The drawback to this approach is that unwanted by-products, such as diffructose, L- (hydroxidyl) -2-hydrofluoro-Aβ, and no higher saccharide are accumulated in the recycle stream, while fructose crystallization is essentially selective. as a result, the recycling stream is contaminated with by-products and needs to be purified, which is accompanied by the loss of certain quantities of fruit.

The present invention solves the problem of accumulation of co-products by incorporating the liquid phase which remains after crystallization (the mother liquor) in the process of producing high-fructose liquid sweeteners. However, in this way, the unwanted by-products are not concentrated in the step of producing crystalline fructose, but are continually removed from the system, bry such combination eliminates the need to purify the fructose-containing streams while maintaining the dactose in an economically advantageous product.

ha Figure 1 shows that the preparation of b5% enriched fructose syrup involves a step of separation (fractionation) of the reaction stream, which is generally required to produce a syrup with a ractose concentration higher than about 48 / . For crystallisation purposes, the syrup should preferably be at a concentration higher than 9b% of fructose (w / w), although it is possible to obtain crystalline Fructose and from solutions with a lower fructose content, such a method. would be economically disadvantageous because of the low yields that would result.

The technique of fractionation, which is to provide a stream of Fructose at a concentration of 95+ (from a feedstock containing 42 (/ wt. In (fructose), the usually obtained product by dextrose azoisomerization) is known. Thus, it is possible to obtain the feed stream to obtain anhydrous crystalline fructose from enriched fructose syrup (IFS) with little change or no change at all in the prior art, preferably, the fractionation system is chromatographic, of the type imitating rolling layers that is well known to those skilled in the art.

Figure 2 shows details of the combined method. As shown in the block, entitled primary conversion / dilution, the starch was initially converted to dextrose using an enzyme-based method as described above.

isomerization

The Cree isomerization process for the conversion of dextrose to Fructose uses an enzyme, the enzyme is fixed on a carrier and is housed in a column (called the above iso-column) until it is displaced after depletion. an advantage of the present invention is that it allows efficient use of the increasing amount of isomerase in the λ-columns. With seasonal fluctuations in the demand for enrichment of fructose syrup / 55 / fructose /, a producer who invests in additional amounts of isomerase to meet the period of peak market demand must pay for this increased level of isomerization capacity throughout the year, even when the production of enriched Fructose syrup is at a relatively low level, selective application of the combined method described herein, the manufacturer can effectively utilize the increased level of isomerization by targeting a larger m high flux content of fractionation from fractionation to produce enriched chromosome syrup when demand for such a product is high and use the greater part of that flow respectively to produce anhydrous crystalline fructose, in case the demand for enriched fructose syrup has decreased. however, this way the investment of increased iso-sherrization capabilities of the installation can be used effectively throughout the year.

Fractionation

Fractionation is carried out in a series or group of resin-containing reactors that sequentially act to separate fructose from dextrose in the feed stream, feed stream and eluent stream flow into the reactor system to produce one or more product streams with high fructose content, one high-dextrose raffinate stream and / or one or more high-oligosaccharide containing rarinate. as seen in Figure 3, the high dextrose flow is recycled to re-isomerize to fructose, while the high fructose flows are used to produce crystalline Fructose or mixed to produce enriched fructose syrup.

The fractionation capacity is determined by the feed rate, the percentage of fructose in the stream, and the utilization of fructose in the stream, at a given fructose content (by t in), the higher the fractionation capacity, the sharper the conversion of fructose in need of isomerization. Therefore, in order to reduce the cost of isomerase, it is preferable to operate continuously, with maximum fractionation capacity.

in order to obtain a practical yield of the crystalline product in the process of obtaining anhydrous crystalline fructose, the product refractory must contain more than about 90 X / wt / fructose, preferably more than 95 D fructose. As the product usually receiving the Fructose syrup content is higher than 90 7 / wt / in the process of obtaining enriched fructose syrup, special working conditions must be used in the conventional fractionation system in order to obtain reduce the fractionation capacity. These conditions are: slowing the flow rate of the feed stream without altering the ratio of the elution water to increase the solubility and / or increasing the amount of the elution water to increase the solubility. These operating conditions have the disadvantage that they reduce the throughput of the installation and / or the completion of the water demanding further and removal, which at least leads to additional energy costs. Either way, this is the preferred alternative.

It will be appreciated by those skilled in the art that when an aqueous solution containing fructose and dextrose passes through suitable chromatographic columns, at least a partial separation of the two species is obtained. In order to ensure fractionation, the column effluent must be appropriately discharged so that separate fractions are isolated. The various portions that are separated are called fractions. The narrow fractions represent portions of the wastewater flowing through the column of smaller volume than the broad fractions. Thus, for the purity of the product, the separation can be optimized by appropriately separating the narrower fractions containing the individual substances. Usually, the trade-off made in collecting narrow fractions of wastewater is that the total utilization of the released substance is adversely affected!

It has now been found that fructose flux with a fructose content / wt / above 95 /···, which is the preferred starting material for the preparation of crystalline fructose by the process according to the invention, can be obtained by separating suitably narrow fractions of the reaction stream exiting the digestive system of the conventional method for the preparation of enriched fructose syrup. Such a fractionation system, which is also particularly preferred, is described in the publicly available patent application in CAF, Serial No. 861,026, filed on 5/8/1986, which is entitled * Chromatographic Separator Apparatus. The methods of work contained in this publication are suitable for use in this method.

a preferred method of using the aforementioned chromatographic separation apparatus, when used for fractionation, by the method according to the present invention, involves increasing the eluent-feed stream ratio by about

1.7 to about 2.0. This feed stream preferably contains about 60 /. dry substance (by weight) and kept at a temperature of about 140 ° D.

The purified stream exiting the fractionation system is separated into fractions in a manner similar to that used in separating the extraction stream, so that the stream, which is relatively rich in oligosaccharides, can be isolated and returned to the saccharification system, to be split in order to return to the saccharification system or to withdraw from the system.

lipia absence of purification or recycling of oligosaccharides to the saccharification system, the only way out of the oligosaccharides from the system is the extraction flow, since

- 30 usual isomerisacsl hs affect oligosaccharide. Thus, the oligosaccharides in the refining stream that are recycled to the isomerization system are simply passed through this system without being altered and returned to the feedstock to the fractionation system.

Oligosaccharides are unwanted in the extraction stream since at least a portion of this stream is used to feed the fructose crystallization process, which is preferably carried out from a solution containing at least other sugars. In the same way, oligosaccharides are undesirable in the liquid sweetener produced by the process of the invention, therefore only limited quantities of such oligosaccharides can be withdrawn from the system by the resulting liquid product.

an additional advantage is the possibility of recycling the oligomer-rich stream from the fractionation system to the saccharification system. such a flow is usually relatively low in dry matter, most commonly about 10 X, which means that the current contains about 90 wt. X water. The starch slurry obtained in the liquefaction and decomposition stage of dextrin should be diluted before saccharification. Its water flow containing oligosaccharides can be used, at least in part, as a starch thinner, using the water and reducing the digestion capacity required by the system as a whole.

Mixing in the conventional methods for the preparation of enriched fructose syrups, the highly ractose fractionation fraction is mixed with the isomerization product (usually containing 42-48 (/ wt / yaructose) to obtain a gelatin content of fruit.

- 31 tons in the final product / 85 / / wt / enriched fructose syrup /. In the combined method according to the invention, the mother liquor obtained in the centrifugation attachment aaed carrying out the crystallization contains about 68-92 (.· / with m in (fructose, preferably 99-92 ') / is m in / fructose, such as approximately 88 /.

a dry substance containing a mother liquor is also suitable for mixing. 1''s gives additional possibilities for process variation, since different streams may be mixed, from the ion exchange process, from the treatment with charcoal and then concentrated to a dry matter content of 77 X, as part of the method for producing enriched fructose syrup . The dashed line in Figure 3 shows some mixing cases. The choice of flows to be mixed depends, of course, on the mass balance of the system as a whole.

As no chemicals are added to the stream with high fructose content in the step of producing anhydrous crystalline fructose except for very small amounts of hydrochloric acid and sodium carbonate to adjust the appropriate pH, no appreciable amounts are accumulated in the method for producing crystalline fructose. from new contaminants. Coloring agents, hydroxymethylfurfural and dl-fructose can be obtained during the charcoal treatment or during the evaporation steps of the crystallizer feedstock. as such, these compounds can be removed in the final coal or ion exchange resin treatment at the stage of preparation of enriched fructose syrup.

1 As more steps in the general process are carried out at high dry solids level, the microbial calc.

it is also inhibited and should not be of great importance, as a result, the level of acetaldehyde should not be increased appreciably, and if necessary, the ion exchange resin or the final evaporation steps may decrease.

Fructose flow for the mold

Adjusting pj ^!

It has been found that the aqueous fructose solution from which fructose crystals are to be obtained is preferably between about pb 3.7 l and about 4.3, although the literature describes the opposite (see patent for. . Accurate control of the pp of the crystalline feed stream is required to minimize the formation of diffractodic anhydrides. The presence of dysructose anhydride in the crystallizer has been found to lead to lower yields of crystalline pro-

you become fructose-forming. It is considered.

that the rate of anhydride formation is minimal at pp within

3.7 to 4.3. both higher and lower pH values than those indicated here cause an increase in the amount of porous anhydrides. u> v> htu also indicates that at higher pH values the tendency to form coloring products increases.

An example of the effect of -pli values on the solubility of ructose a on the accumulation of impurities in syrup with an approximate fructose content of 93 7 as a dry solid was investigated as described below, the syrups tested being representative for use as a feedstock to be used in the crystallization step according to the method according to the invention.

Adding crystalline fructose to the usual very enriched fructose syrup (/. And / or FS) with a solids content of 90 X yields a fructose-containing syrup of about 95 X / wt /. This solution is then treated with granular activated carbon as described above in the section dealing with activated carbon, but in this way, the syrup is subjected to the same treatments as the feedstock to feed the crystallizer.

a sample of the above-described syrup was treated to obtain pH 3.94 and evaporated at 73 ° C to obtain a higher solids content, two liters, of the concentrated syrup so transferred to a closed flask with a stirrer immersed in a constant temperature bath maintained at bark 55 ° C. This solution, called a pH 4 sample, was stirred continuously at a constant bath temperature (approximately 5 hours), during which time a second sample was prepared.

The second sample of 95 Z fructose syrup was treated to pH 5.48 and concentrated at 77 ° C by evaporation. Evaporation was slower than that obtained to obtain pH 4 millet, two liters of the new sample obtained. ph 5.5 / were transferred to a sealed flask and the flask was placed in the same constant temperature bath containing the sample ph 4.

After adjusting the bath temperature to 55.5 ° C, 56 grams of crystalline fructose were introduced into both flasks. Stirring was continued for bi hours at a constant temperature. This is the approximate residence time of the syrup in the mold according to the invention.

The resulting sugar mass is tested, centrifuged and the mother liquor is analyzed in parallel with the feeder syrup begs, the data obtained from this experiment are summarized in Table I below:

- 34 1 MILITARY 1

Welcome Equilibrium ph 4 ph b.b pH 4 pii b.b Fructose / HST / 90.31 90.80 00.33 90.24 Fructose / Xst / after hydrolysis 00.33 96.10 90.33 90.72 it-achadrldi / dst / 0.27 0.24 * 0.40 Solids / wt. // 39.79 8C13 08.90 88.00 HDF / ppv-c, CTv / 0.71 4.03 20.9 6.08 Acetaldehyde / total PPO / 104 48 58 06 * URFU RUB / pp <*. st / 2 and 0.29 0.44 Coloring / RnU-one- NICE / 14.0 39.6 00.7 163.1

Solubility / o Fruck-

toza / with water / -. - 7.64 7.60 flushing - - 1.0 1.0 '

h - means that the values of mono-anhydrides found are calculated as a difference from the data in the analysis of fructose before and after hydrolysis of the sample. The solubility was calculated from the analysis of the fruit precursor hydrolysis and the solids content of the millet, so that the equilibrium value was allowed to allow a little fructose to crystallize out of the samples.

the increase in staining in the sample with ph 0.0 is significantly greater than that observed with the proo-o pp. 1. stronger staining will result in a lower yield on crystallization, ie: requiring more operations by washing the mass after centrifugation, the need for purification of the mother liquor ** * 3 'j will also increase.

both samples showed a significant increase in mono-anhydride during feedstock preparation (compare 0.27 Z cm at pH 4 with 0.24). at ph. However, results from liquid chromatography studies (not shown above) indicate that more diffractive dianchigy should be obtained with pii 5.5.

Summary of the results, it is seen that the sample is ph 4 has less staining, demonstrates a decrease in the total acetaldehyde content and has a solubility not significantly different from that of the sample with pH 5.5. The feed syrup for the crystallization process with pii 4 ish benefits over the syrup of pv 5.5, since a product with a higher yield of better qualities of the mother liquor is obtained due to the lower content of coloring agents, the lower pH visibly decreases to a minimum the coloration as well as the formation of di- fructose and have a negligible effect on solubility.

As shown in Figure 3, the pp adjustment is conveniently carried out after the fractionation step prior to the charcoal treatment, at this stage of the method the viscosity of the fructose solution is relatively low and therefore the pH adjustment can be carried out relatively easily by mixing the solution with an acid or base. Those skilled in the art are aware of the acids and bases suitable for this purpose. Particularly preferred are hydrochloric acid (ICl) for lowering pii and anhydrous sodium carbonate / Kla2COy for increasing pii.

Charcoal treatment

The fructose feed stream for the crystallization step has a concentration above 9b Z / wt / and it is preferable to treat the tone with charcoal before concentrating it by evaporation.

- 36 One of the purposes of charcoal treatment is to remove impurities that may inhibit crystallization, another aim is to remove impurities as colorants, hydroxymethyl Uyd-Urals. FURFUrol and acetaldehyde, which adversely affect the properties of the mother liquor and significantly reduce its use as a component of liquid sweeteners. The treatment is charcoal is preferably carried out on granular charcoal, in an amount of 1-3 7 dry matter, or with powdered charcoal, usually in an amount less than when using granular charcoal. The temperature of the syrup is preferably about 160 DEG, and typically 1b-3O, the syrup is preferably about 20 to 25 wt. X dry matter.

It is most appropriate that the charcoal treatment is carried out immediately after fractionation before evaporation of thia syrup. Low-carbon charcoal treatment keeps Fructose from diffractose in quantities below 0.5 X. If the charcoal treatment is carried out after evaporation, fructose losses greater than 2.5 X are observed. The temperature of the syrup should be approximately 160 ° D (as compared to 140 ° D) to prevent microbial development in the carbon adsorber and also to reduce the viscosity of the aa syrup in order to obtain a better, diffusion around carbon particles.

Example

The amount of diffructose formed in water jellies with the highest thirst is burned 35 /. fructose content, by change in the amount of dry solids, in the first two experiments the aqueous solutions were mixed in a flask with 2.7 X granular charcoal / dry matter of granular charcoal by weight of the dry matter in aqueous solutions / and is stirred at 16 ° C for 24 hours, zero, sixth, four ......... l.

- 3? in the twenty-fourth hour, samples were taken and the content of Δαfructose <= measured in them. The results of the measurements are given in the following Table II:

Table II diffructose / X cm / in:

π strap / hour / Solids: 25 / dry in 50 / dry in 0 3.25 0.47 6 and 32 0.85 14 0.38 1.82 24 0.78 1.94

The above data indicate that diffructose is formed much faster (up to 4 times faster) in the solution containing 50 (dry matter) than in the solution with 25). dry substance.

The following four experiments are intended to reproduce the operation of the coal treatment under production conditions in a column at a structural flow in a stream so as to allow the measurement of the resulting diffructose in a dynamic flow system, as compared with the results obtained in a static system with stirring in flask.

two, 5 cm glass columns are used in series to provide a residence time of the feed stream in the column for about 20 hours, the tubes and short coil of clean tubes used to heat the feed stream are immersed in an adjustable water bath.

To mimic the steady-state counter current of coal, the columns are initially used to a state of partial carbon depletion and the second column is then loaded with unused fresh granular activated carbon, placing about 5 ci of fresh coal at the point of removal from this column.

This apparatus was used under four different conditions for the study to be carried out, provided that each of these happened to use fresh / new / granular charcoal, the following conditions are used; 70 / dry matter at 1.4b ° D, / e dry matter at 1 ° C ° 1,% dry matter at 1'60 ° D and

X dry substance at 16 ° C.

if all of the above conditions are carried out under continuous feed without recycling for 36 hours and the amounts of diffructose present in the effluent at 0, 6, 1.4, 24 and 36 hours are shown below in Table 111:

Table III Diffructose / X dry solids

1temperature; 140 ° D 166 ° D Dry substance: 70X 2b X 56 / ? '' /. time / hour / and 0.32 o.o2 6.35 a.32 6 'J · O ·. j - - 1.3 14 6. 26 0.92 0.95 - 24 0.33 9.t »l 1.35 1.03 36 v.71 0. -34 1.72 fO · * c4

That being, at 140 ° F at 76% dry matter, the formation of diffructose is not a problem, as the table shows, lower temperatures would increase the risk of developing germs and increase the viscosity of the syrup, so both of the high content attempts

- o9 solids (b3) and 76 χ / at show levels of dl, | .. the substantially increasing fructose is over time ^ even though the fib time j is not the effect of heating l on carbon is the same for all presses, if you wish to be associated with some fecal theory, a possible explanation for the formation of lidructose is to catalyze or / and co-cadadislation from a substance that is released from the aqueous solution upon entering, thus increasing this substance increases by increasing the substance. the extent of the conversion of fructose to di- fructose over the course of the use of carbon, there is a significant increase in diffructose.

A carbon filter can be used to separate the carbon from the syrup leaving the charcoal column, which traps the finer particles of the stream. Effective filtration is very sculpted, since any insoluble matter that passes through the crystallizer is trapped after crystallization. .ructose and will directly affect the purity of the product.

Dumb as, _am .rukt.: .. STA, which is not dakrlotadchzlrala mixed to obtain a revered podsladated, then treatment with charcoal podaor.ava quality i fu liquid product. Typically, the processing of enriched coal carbonate syrups is done by. King of the process (after mixing), the lateral centrifugation fluid is purified by two carbon treatments, which enriches the end product.

Evaporation of the starting material for crystallization

The driving force for crystallization is the super-saturation of a high-concentration Fructose solution, which is obtained by cooling the saturated solution at a temperature of. J. ci '.lei I.; ; C1X - ', - t H'Ji. ΓΧΟΖ Fructose / co-concentration / saturation is saturated. to achieve

40 theoretical yield of crystallization in the range 40-65 /, e.g. 40-48 X it is necessary to cool the outlet feed of the crystallizer fructose syrup within 45-55 ° D, such as e.g. 47 ° D.

During the evaporation step of the feed syrup, water is evaporated so that the solution is concentrated to a degree that allows the fructose to crystallize upon cooling. Evaporators shall be designed and operated in such a way as to provide a concentration; wound the solution with minimal damage to the syrup. Prefers! a way to effectively evaporate it is to carry it out in two stages. Initially, the starting syrup was concentrated in a vacuum evaporator, a 6-step drop, which had multiple erections and mechanical recompression. the compost stream having a concentration greater than 95 (/ wt /) exiting the coal stripping step is introduced into the evaporator with a dry matter content of about 20 to 25 wt. Λ at a tessellation about 190 ° D and a pH of about 3.7 to about 4.3. The resulting syrup from this evaporation step contains from about 55 to about 65 wt. /. dry substance.

In the second evaporation step, the product obtained in the first stage is charged into a plate type evaporator with a rising layer and a single effect, operating at 584.2 to about 639.6. But. From the second step, a product is obtained at a temperature of 165 to about 175 DEG which has a dry matter content of 88 to about 90 wt. Λ * Preferably, the second evaporation step is carried out in vacuo at about 660.4 mm but so that the product temperature is about 140 to 150 ° D, thus minimizing fructose losses.

The main task in the operation of the evaporator is to concentrate the syrup with minimal loss of syrup. The most troublesome loss of syrup on heating is caused by the conversion of fructose to di-fru

- 41 tons, which reduces the yield during crystallization. The formation of diffructose is favored by the high concentration, the high concentration and the longer residence time in the evaporator. Since the concentration is fully oxidized, the operating conditions of the evaporator must be chosen in such a way as to minimize the temperature and the residence time of the syrup in the evaporator.

The suitable evaporators mentioned above are well known to those skilled in the art.

Crystallization

Crystallization - it can be carried out in discontinuous operation in crystallizers with continuous action, in both cases there are advantages and disadvantages, in intermittent operation there is more flexibility for obtaining crystals with different crystal size distribution and at this way of working the change of crystallization conditions becomes faster l easier. However, the intermittent mode of operation has lower productivity, since it takes time to load and empty the crystallizer, as well as to import crystalline nuclei. In this case, it is difficult to maintain a constant crystal size distribution in each subsequent batch, and more tanks are needed to store the feedstock and the sugar mass so as to ensure a minimum stay in the mold. Individual cooling systems for each crystallizer are also required. Continuous operation has the opposite advantages and disadvantages, respectively.

Crystallization can be accomplished by single passage or multiple passage, the first of these methods being preferred. It has been determined that in one run only 88 / of the milk can be obtained and the crystallization time at

- 42 second pass would be 37 / longer. Moreover, the mother fluid at the second transition was more viscous, due to the higher level of higher sugars and the density of the slurry (the weight of the crystals relative to the weight of the mass) was lower at the second transition. These two actors reduce the productivity of the centrifuge.

The usefulness of the mother liquor as a raw material for mixing in obtaining a liquid sweetener depends largely on its purity. The quality of the mother liquor depends on various factors and care must be taken to minimize the side products that are formed during the crystallization stage, as the quantities of by-products that can be admitted into it are determined accurately and, if necessary. their surpluses must be effectively eliminated. Because crystallization is specifically fructose selective, it tends to accumulate by-products in the mother liquor each time it passes through the crystallizer. Thus, this problem is exacerbated in cases of multiple crystallization and the level of contaminants in the mother liquor often imposes an upper limit on the number of passes through the crystallizer that can be used in the combined method.

It has been found that crystallization with multiple leakage does not tend to increase the amount of ash, coloring matter, as well as hydroxymethylfurfural, furfural and acetaldehyde. Of these, the amount of coloring matter increases most rapidly, and therefore the usual determining factor for the number of passes through the mold that can be effectively used is the coloring of the mother liquor.

Appropriate measurements to maintain the purity of the mother liquor include careful control of the conditions under which the evaporation, charcoal treatment and crystallization, and in particular the pH, temperature and duration of the operations, are carried out. Preferred conditions are discussed in the separate sections of the present specification for the various steps of the method.

the crystallizer feed syrup is preferably cooled to about 140 DEG before being introduced into the crystallizer. In order to obtain a theoretical (theoretical) yield of 40-48½ of crystalline fructose, the solution must contain a minimum of 95 / - / wt / and a solids content by weight of 88.3-89.7 X.- / nominal 39 X / s t in //.

Seed crystals are introduced into the specified portions and thoroughly stirred at a temperature of about 135 ° 1 ', which is calculated according to the percentages of dry matter and fructose in the portion. After the syrup is well mixed with the imported crystals, a sample is taken to determine the exact saturation temperature. The crystallizer cooling system is adjusted to provide syrup saturation in the range 1.06-1.65 (relative to fructose concentration). if the sugar is already gone. below these limits, but no crystallization process is occurring, cooling must continue crystallization is a process in which crystals are formed from liquid, drainage solutions / gels / or saturated vapors / clouds /, the crystals are generated on insignificant traces of by-substances acting as a droplet. the impurities are often used for this purpose, and the crystals formed initially in small areas of the maternal dose are then propagated and enlarged. but the method according to the present invention is the origin. - 44 of crystals is thus undesirable, since the resulting crystals are of a very small size, control over the size distribution of crystals is more frequently controlled, preferably using crystal nuclei imported into the solution.

The crystallization progress can be indirectly controlled by the cooling value of the sugar moose, keeping the temperature of the cooling water in accordance with a predetermined cooling curve, such that the level of supersaturation is from 1.0 to 1.35, e.g. 1.0 to 1.3.

preferably, saturation is measured by a direct κοι troll of crystallization development. unsaturation can be calculated from the percentage of dry matter in the mother liquor and the percentage of fructose. use the data of the solution transfer bed aa to decide whether to continue cooling along the predetermined cooling curve or to modify the cooling rate so as to maintain the desired transfer rate.

preferred is the method of effective crystallization, which involves the introduction of crystalline embryos into a syrup with a fructose concentration greater than 95 / which has a dry matter content of about 38 to 99 wt. /, ph from about 3.7 to 4.3 and temperatures from about 130 to 138 ° C, with the crystalline nuclei being about 7 to 10 wt. Z and have an average particle size of about 150 to 250 micrometers. After the embryos are introduced, the syrup is subjected to controlled cooling to cause fructose crystallization.

Cooling may deem to be held like this: by the temperature of the syrup about 138 to about 11b ° D cooling is carried out with about 0.5 storost ^o 1 '/ h; from about 115 to about 86 DEG

- 4b the syrup is cooled at a rate of 1.and up to about 1.5 ° D / h. it is advisable to keep the saturation level below about 1.17 when the syrup temperature is more than about 115 ° F and to keep below about 1.25 if the syrup temperature is below about 115¾. the maximum temperature difference between the temperatures of the cooler a and the sugar mass is about 19 ° D. Uo high temperature difference can cause crystallization to occur.

aa preferably, however, the cooling is controlled in several varying degrees over at least three periods. Thus, for example, during the first period when the temperature of the syrup is between about and about

138 to 125 ° D, cooling is carried out at a speed _of r / h

1.0 and 1.5 D and the browning is kept below about 1.29. During the second critical period, when the syrup is at a temperature between about 125 and 119¾, the cooling is preferably carried out at a rate of about 9.5 to 1.0 ° / hour and the saturation level is kept below about 1.17. And during the third period, the cooling period, the cooling rate when the temperature of the syrup is between about 110 and about 36¾. is preferably about 1.5 to 2.5 DEG / hour and the saturation is kept below about 1.25.

It has been found that a preferred way of conducting the cooling is to include a continuously operating saturation level monitor in the automatic control of the cooling water temperature, and one particularly preferred way is that the data from the continuously obtained information from the temperature measurements of the the syrup, the temperature of the cooling water and the degree of saturation are introduced into the processor. The processor is programmed to use this data to control the temperature of the cooling water and thus

- 46 syrup cooling mode and rate, the processor is programmed to first cool the syrup from the seed germination temperature (T-) to a predetermined critical temperature / T · / at a rate of 2.5 ° D / time. (The critical temperature is calculated from / on fr-uctose and on the dry matter in the syrup feeder and from the temperature at which the transfer will become 1.17 /. The program provides a cooling rate of sugar mass of 1 ° D / hour at cooling from T · to 115 ° P and a cooling rate of 1.5 ° P / hour at cooling from 115 ° D to the final temperature (most often 86 ° D). However, the program is designed to prevent any excessive embryo production. In the first place, the program ensures in all cases that the temperature difference between the sugar mass and the coolant is maintained so that this difference does not exceed the predetermined values (most often about 14 ° C) throughout the cooling time. Secondly, the program ensures that in any case the level of refinement does not exceed the predetermined value (usually 1.28) throughout the cooling period, the specific temperatures and values described above can be optimized, as well as the curve of crystallization dependence without undue experimentation. The most important factor affecting temperatures is the total level of dry matter (dry matter) and the total surface area in which the germ crystals are imported. For example, raising the dry matter level would shift the critical period to an earlier stage of the cooling curve and vice versa. Reduction of the total surface on which crystalline embryos are deposited, e.g. reducing them will lead to an extension of the critical period and vice versa.

- 47 Crystallization Kinetics, Irradiation

In crystallization kinetics, the growth rate of crystals is a function of the driving force. concentration - the instantaneous concentration in the mother liquor, depending on the concentration that must be available at steady state for a given temperature.

Non-saturation is a measure of the driving force, the concentration force, several ways of determining the saturation, for the crystallization of fructose it has been found that the most reliable for the purpose of continuous control of the development of processes in a batch is to determine the saturation on the basis of the available water. Thus, transfusion is defined as the ratio of grams of fructose per gram of water in supersaturated syrup that has stopped this ratio corresponding to the equilibrium state;

Arctose / Water / ^^ d _{In your} irrigation ------ Lactose / iodine / equilibrium

Ideally, the degree of cooling of the batch should be adjusted to control the level of overgrowth of the mother liquor. It has been found that for crystallization of fructose in acceptable yields and with crystalline sizes within the desired range, the transfer is required to go in the range 1.6 to 1.30. The level of irrigation below these limits manifests itself during the cooling time, while a greater irrigation of 1.35 results in interruption of embryo formation.

Formation of embryos

Iip-l saturation setpoint saturation conditions · must be agreed, Fructose does not appear to have established unstable zones, e.g. saturation limits at which no embryo formation occurs. The rise of

- 48 existing crystals, always accompanied by the formation of new crystals. As the level of overgrowth increases, so does the growth rate of crystals, but the same goes with the degree of crystal germ formation, the aim is to find such a level of saturation that the desired crystal size is obtained at one economically viable process time.

The formation of the crystalline embryos referred to above is of the type of poison or shock, as mentioned above, the crystallization of fructose is always accompanied by. new crystallization, shock crystal formation may occur at the beginning of loading of the batch when the crystal embryos are introduced. It is expected to be caused by low temperatures when introduced. If crystallization starts so early, it is preferable to warm the sugar mass to remove the embryos. Once the crystalline embryos have dissolved in the syrup, it can be restarted.

a preferred method of avoiding shock formation of crystals is to maintain the saturation level below 1.30 after the introduction of the crystalline nuclei. Massive crystallization would cause a large increase in the viscosity of the sugar mass, making it very difficult to spin and significantly increase the purification time. The fine crystals separated from the sugar mass create much greater difficulty in drying and tend to agglomerate faster. Ori massive crystallization results in a product having undesirably small average crystal sizes.

It has been found that a portion of 345.58 ί syrup loaded into a 378.5 i crystallizer will require a cooling cycle of 30 to 80 hours, typically about 35 to 40

- 49 hours for crystallization of fructose. During this period, the syrup is usually preferably cooled in several stages, preferably in three stages at different cooling rates, the requirement for different cooling rates in the individual steps is due to the non-linear dependence of Fructose crystallization on temperature, the different speeds correspond to the the different periods of growth of crystals created during cooling.

initial cooling covers temperatures below about 120 ° D. The planned cooling rate is about 1 to 4 ° D / h; the normal speed is 2 ° D per hour, which requires four to six hours to perform at this stage, preferably about eight hours. During this time, the growth almost exclusively of the introduced germ crystals has cooled and the density of the sugar mass increases slowly, most of the heat load of the cooling water comes from the noticeable heat.

The formation of crystalline embryos may occur at this stage, however, only if the embryonic temperature of the embryos is too low or when the saturation exceeds 1.8.

In the critical period, the rate of increase aa increases by a factor of 2 to 4. The density of the hair increases rapidly and the emerging new crystals increase to the desired size. Both competing processes of crystal growth and nucleation are accelerated.

The limits of this wound. are not clearly defined. The best place is at 120 to 110 ° 1 '. caution is needed in this area as the process of crystal formation can be easily increased and controlled, while maintaining a moderate level of saturation (from 1.05 to 1.20) it has been found that the formation of crystalline nuclei can be retained in prm.m1I would be boundaries. equal cooling speed is the preferred way to control the degree of saturation. The cooling rate in this zone is about o.b to 3. and ° P / hour, and a cooling rate of 0.5 to 1.5 ° 1 / hour is usually recommended. The transmitted time for the critical period at this speed is about 10 to 4 (hours, preferably 13-22 hours).

In some cases, high levels of overgrowth may not cause the formation of crystalline embryos; in such cases, further cooling may lead to the formation of fruit hemihydrate. 1'is a type of ama needle crystals that cause a very high viscosity of the lass /> 800,000 Wed /. Pe is practically suitable for spinning this pelvis. It can even overload the mold. Hemihydrate crystals can be detected during routine product inspection and completely removed during the cooling period.

At the end of the critical period * the density of the mass is high enough to provide a faster cooling rate without the formation of a crystalline nucleus. 2 this cooling zone can be lowered rapidly by the cooling water temperature. The rate of cooling of the sugar moose is about 1 to 7 ° D / h, preferably a speed of 1 to 4 ° D / h. Cooling from 110 ° to a final temperature of about 1ύΟ-75 ° Γ takes about 3 to 12 hours, typically 8 to 12 hours, faster cooling without crystalline nucleation can take place, but then the crystalline growth process will be slowed down and the batch will remain at a higher level of supersaturation at the end of the process, part of the residual saturation may be reduced by moving the sugar mass into a mixer or mixing tank for a certain period of time.

Since cooling can be performed more quickly during the rapid cooling period. Than at an earlier stage of the process, there is a certain limit to how much temperature difference can be between the cooling water and the sugar mass that can be will allow. This difference is not precisely determined, but when cooling does not cause a temperature difference between the sugar mass or the cooling surface greater than about 15 ° D to be obtained. A temperature difference greater than that indicated may cause crystallization of dirt and contamination of the cooling surface.

introduction of crystalline embryos

The temperature of introduction of the crystalline embryos may differ from the saturation temperature of the mother liquor in the feedstock filled crystallizer. to obtain this information, a liquid chromatogram of the feed syrup can be made and the refractive index measured. These data are used to calculate the concentration of the fruit, the percentage of Fructose and the dry matter in the feed syrup, the introduction of crystalline embryos may not be made within the limits. a saturation of the lemma of 0.96, e.g. from 1.0 ds 1.10.

oa preferably the crystalline fructose imported has an average crystal size of about 100-400 (lycrons. It is recommended that the amount of crystals imported is from 1 to 20 20 / wt /). This amount is determined by the desired crystal size in the final product. The crystalline embryos are introduced into the feedstock of the crystallizer, doing everything possible to distribute the crystals imported in the crystallization evenly, as mentioned above, US Patent No. 6,164,429 discloses a method and apparatus for producing crystalline embryos.

- b2 The introduction of crystals is preferably carried out at the first mixing of the crystal embryos with the feed fructose syrup to form a liquid mass for introduction into the crystallizer. This has the effect of conditioning the surface of the crystalline embryos. Such pre-introduction of crystalline embryos into the syrup minimizes the formation of blisters in the crystallizer, due to the introduction of crystalline embryos, blisters are a place where unwanted crystallization may begin.

Continuous introduction of crystal embryos is of great importance to provide the surface area for the growth of fructose crystals. Since the surface / volume ratio of the germ crystals generally decreases with increasing particle size, if the size of the germ crystals is larger, a larger weight of the germ crystals is required to obtain the desired surface.

Alternatively, the lower portion of from 5 to 30 / preferably about 10 to 20 Z of the product may be left in the crystallizer to be used to initiate crystallization. This procedure is much easier to perform than using dry crystalline embryos, but it results in a larger crystal size distribution, dull as the residue used to provide crystalline embryos contains fine particles that would otherwise have been removed in the centrifugation and drying steps, thereby producing a product with a wider crystal size range, which can then be saturated to provide the standard crystal size of the final product.

One preferred way is to add hot syrup to the residue to raise the sugar mass to a saturation temperature (approximately 133 ° G) / while the feed syrup is cooled j-ί, ϋ T-Ji W A p </ G J p < -1'GC ia import aa crystalline nucleus. AST of crystalline .lua - probably guoi in this process

- despite the mosquito repetition _{# the} steady-state density of K.ELS tl X Ct Preferably, the superhuman is in the range from 2 to 10 (/ wt /), the critical part of; ΡΛ '<

this operation is divided by the final temperature reached by the feed syrup and the sugar mass, which should provide a saturation in the range of 1.0 · ο to 1.10, which will result in a mishmash l production of the embryos will be small.

Sprinkle Pic?> A USr ^ AlctTMue IA U60BPfT € MUtTc yarimzr <

Crystallization of naphthructose was carried out in an experimental variant of a conventional cropletizer, using a feed of 5.82 L / w / w 89.66 7, a syrup with a fruit content of 35 it dry matter, crystals were provided with a central shaft stirrer. cooling is facilitated by internal fins attached by filling 386.1 to the camshaft *. D-.X i, -s

C / p-Ο · * · *, φ 1 -> 4 / conducted for about 40 hours with BixM C, -JiG, and crumbled $ ng embryos. However, it remains significant at the end of the oversaturation period /1.17/4 the batch is controlled

CilTO. <· Τχ 1.

and the change in saturation is grasped by sieving the crystalline product through

ΟΘ X1 ^ / OSi £ 1> µ1 iiDt / 3 C * 1Tc1 Ο has an average particle size of 161 nuclides ii iviOuitlj THlCii embryos are added directly to the crude Table Itf shows the actual cooling program used during the crystallization

Overgrowth increases in the first 18 hours to a maximum of 1.26. It then lowered to about 1.17 and remained so and grasped.

Faulitsa 1'U The period after the embryo has been introduced? H / h / Starting temp. ⁰ ! Extreme temp. ⁰ ]? Cooling speed 2.0 - 10.3 1oD · 5 1.0.0 1.25 10.8 - 26.8 L22.5 111.7 6.98 20.8 - 30.3 111.? lOv.u 1.11 30.3 - 40.8 ΙΟυ.ό 00.6 1.45 Crystals in the resulting product have a medium size of 268

microns. the yield of crystalline product is 46%, based on the Fructose content of the syrup.

Separation

A preferred method of separating fructose crystals from the mother liquor is centrifugation .in a basket centrifuge. It was found that in 14 x 6 centrifuges can be separated 15.14 With a sugar mass of about 10-15 units. This period includes one to three hot water washes, (126-206 ° D), for the front '-U1T and not two. Higher flow temperature of the pouring water can cause severe dissolution of fructose and loss of yield. It is recommended that the amount of flushing water be from 1 to 5 U ·. in relation to the sugar meat, deionized water is used since hell, preferably the pH of the breakthrough water is in the range of about 3 to 5.

Preferred operating conditions for the aa centrifuge used to separate fructose crystals from the mother liquor are the following: force k-a gravity about 1460, sludge thickness from about 5 to 7.5 cm, sludge moisture about 0.7 to 1 »

1.5 / water, product purity about 99.5 Y, preferably above about 99.8 Y. sludge moisture and its purity are important factors for obtaining a non-agglomerating and stable product.

The product was rinsed in a spinning centrifuge to remove. It is preferable to wash with water at a temperature between about 150 and 180 ° P in an amount of about 1 to 1.5 wt. X relative to the sugar precipitate. When used in this way, the flushing losses of the product are usually about 5 to 10 t. The fructose-containing wash water can be recycled at the coal treatment stage to remove impurities and then concentrated.

Drying

Different types of dryers can be used to dry the resulting product. fluidized bed dryers, vibrating fluidized bed, shelf and drum dryers are suitable. Preferably, the wet centrifuge sludge is dispensed into a continuously operated mixer via a screw conveyor at different speeds. The dry recycled material is dosed in a closed conveyor (to avoid air mixing) at a nominal ratio of up to 4; 1 above the wet sludge. The action of the mixer must be sufficient to ensure that the wet material is mixed with the dry material. The mixed precipitate was then transferred to the oven.

aa preferably the precipitate is co-dried to avoid product overheating, the room air must be pre-purified by passing through an ultrafine borosilicate filter designed to remove 95 / of particles with a size of 0.5 microns. The air is then heated to <a temperature so that after mixing with the air from the cooler it reaches 160 DEG, at which time it is introduced into the oven.

The product leaves the oven at about 130 ° D and is transported to the cooler, a controlled quantity of the product is recycled without cooling to be introduced into the dryer for wet treatment

- 56 centrifuge sludge. The most critical indicator of a drying operation is the humidity of the incoming sludge. If the humidity is too high, pellets and agglomerates are produced upon drying. Humidity can be controlled by the ratio of dry crystals that are recycled to the fiber precipitate. although a 2: 1 ratio of dry repellant to the lime precipitate is generally sufficient to obtain well o / crystals.

to ensure good spin

f * T Q and '9 · 1 to avoid agglomeration requires the ratio to be t ^ · · du · The centrifugation sediment is preferably sucked in PDG ^ GP ' its dryer to reduce the humidity of the crystals OT J r ? uctose below about 0.1 wt. / »· It is found that if the moisture-

bone nz utikatg. of the non-roughening is more than approximately 1.5 wt. 7 is burned to form lumps from the product. as well

it was above, the humidity of the centrifuge precipitate- is adjusted by adding a dry product. For Recommendation well yes the product temperature is not allowed to exceed 140 ° D.

Preferred drying conditions / nitrogen conditions are as follows: inlet air temperature of about 170 to 250 ° D, preferably 170 to 200 ° C, outlet air temperature of about 130 to 145 ° P, product temperature of about .125 to 135 ° D and a moisture content of the product below about 0.1 /, preferably lower than about 0.07 7.

.Conditioning / reaching the required state /

It has been found that if fructose crystals are stored too warm, lumps will form during the stay. This phenomenon is also observed when receiving dextrose and sucrose. As the exact mechanism has not been studied, it is assumed that moisture migrates from the larger crystals to the smaller ones and causes further crystallization of the boundary surface. This process is the result of either a temperature difference or a difference in humidity, both of which are due to the fact that the crystals are not in equilibrium. Tests show that drying the product to a lower value (about 0.05) and cooling it to room temperature results in a free-flowing product without lumps. To be in balance, fructose crystals with a humidity of 0.05 / air at 70 ° must have a relative humidity below 50 / -.

For these purposes it is appropriate to use. reciprocating cooler with counterflow of air. .Cooling of the crystalline product to temperatures below about 75 ° D, preferably below 72 ° D, is used

Cold dry air. It is recommended that the inlet cooling air be at a temperature below about 70 ° D and a relative humidity below about 40 ° C. The residence time in the cooler must be sufficient to ensure good product conditioning. The moisture content of the final product is preferably lower than about 0.07 /

The final product can be sorted by sieving and / or grinding. Prolonged storage of the product at high temperature causes the product to shrink and stain even if it is placed in non-greasy bags. Storage must be carried out under conditions of controlled humidity.

Mixing The ethereal liquid separated from the crystalline product by centrifugation can be returned to the production cycle to produce enriched fructose syrup (OPS).

In addition to being capable of being mixed with dextrose, the mother liquor that remains after crystals are separated can simply be diluted with water to give a very enriched fruit58 syrup / ...666/.

After separation of crystalline fructose, the mother liquor may be mixed with dextrose or with a solution containing dextrose to obtain as a final product a liquid sweetener containing dextrose and fructose, e.g. 55 /, bchl *. ^ as, shown in Figure 3, part of the containing dextrose streams may be mixed with the mother liquor prior to feeding to the final finishing operations, the selection of individual streams, or only one of them, with N ^and V1Y§b & 1 ^ then the mass balance, aiming to obtain the desired level of fructose content in the liquid sweetener as a final product. Most often, by carrying out the combined method according to the invention, a liquid product with a content of 55 (w / w) fructose is obtained. If a sufficient amount of fructose is present in the mother liquor, it is even possible to mix with it the dextrose flow of saccharification, which usually contains 94-96 (w / w / dextrose).

Alternatively, the mother liquor, which typically contains 90-92 / fructose, can simply be diluted with water to obtain a liquid sweetener. Such dilution is recommended if it is desirable to retain fructose as a liquid, since further crystallization of fructose from the mother liquor is possible, provided that it is not diluted below the saturation point for all possible temperatures at which it is the following diluents are suitable for dilution of the mother liquor: aqueous sugar syrups such as dextrose syrups, high fructose enriched fructose-rich syrup / "" 666 / 'or enriched fructose syrup / bbs / asstreams from the production of such syrups, another way of preventing fructose crystallization from the mother liquor separated involves taking measures to protect the solution from evaporating the water therein, or reducing the amount of evaporating water, and adding additives, to inhibit crystallization.

another way of treating the separated lateral fluid, or j portions of it, was to obtain a non-crystalline or semi-crystalline fructose sweetener. This is accomplished by dispersing the mother liquor on the eatable particles and drying the dispersion to obtain a Fructose-containing sweetener, where the fructose is in amorphous or semi-crystalline form. the preferred particles on which the liquid is dispersed are fructose crystals.

US Patent No. 4,517,021 discloses a process for the preparation of a semi-crystalline fructose composition, the methods described therein may be used but the method of the present invention. The separated mother liquor according to the invention can be used as a fructose syrup to carry out the process and the resulting crystalline fructose can be used as an initiator of crystallization. thus, a combined method for the preparation of crystalline fructose, semi-crystalline fructose and one or more fructose-containing liquid sweeteners has been devised.

The above description is directed to the specific embodiments of the invention in accordance with the requirements of the formulations in the United States to clarify and illustrate the method. However, it will be apparent to those skilled in the art that many modifications and modifications to the devices, compositions and methods are possible without departing from the scope and meaning of the invention. it is intended that the following claims will be interpreted to cover all such modifications and modifications.

Claims (10)

Patents IlPhThrMh 1 is a method of producing a liquid sweetener containing fructose and dextrose, characterized in that it involves crystallization of fructose and a fructose aqueous solution and the addition of dextrose and the solution after fructose removal. An ethode according to claim 1, characterized in that the flow of the fructose and dextrose containing aqueous solution is split into two streams, the first of which is fractionated to give a high fructose stream, the fructose crystallizes a stream and at least part of that stream after fructose removal is combined with the second stream. A method according to claim 2, characterized in that the aqueous solution containing fructose is subjected to a process of isomerisation of a portion of dextrose therein, to obtain an aqueous solution containing fructose and dextrose. 4. The method according to claims 1 to 3, characterized in that the crystallization of the fructose is carried out at a pH of 3.7 to 4.3. 5. The process according to claims 1 to 4, characterized in that, before crystallization, the aqueous solution containing Fructose is treated with charcoal, and then a portion of the solvent is evaporated. 6.; an ethode according to claims 1 to 5, characterized in that the aqueous solution containing fructose and dextrose is fractionated to obtain a solution enriched with dextrose, a first fructose solution and a second fructose solution, the second fructose solution having higher fructose content than the first fructose solution and fructose crystallizes from the second fructose solution or i solutions derived therefrom - 61 and the solution after removal of the fructose is added to the first fructose solution a to an aqueous solution containing dextrose which has a higher concentration of dextrose (dry solid) than the first solution. 7. The method according to claim 6, characterized in that the solution containing fructose and dextrose is separated into the first and second stream, the first stream being subjected to the fractionation and crystallization of the fruit, and the second stream is added to the first. solution and to the solution remaining after removal of the fruit, as an aqueous solution containing dextrose. 8. a process for the preparation of crystalline fructose and a liquid sweetener containing fructose, characterized in that it comprises the following steps; crystallization of fructose from an aqueous solution of Fructose to yield a mixture containing crystalline fructose and mother liquor; separation of crystalline fructose from the mother fluid; e inhibition of further crystallization in the mother liquor to obtain a liquid sweetener containing Fructose. 9. A t-process for producing crystalline fructose, characterized in that it comprises fractionation of a dextrose and fructose-containing stream to produce a high-fructose stream having a Fructose content greater than 96 (9). (dry solid) treatment of this high-fructose activated carbon stream to obtain a purified printose stream; evaporation of this purified / ruptose stream to give a more concentrated solution of fructose; and crystallization of fructose from this solution. 16. A process for the preparation of crystalline fructose, characterized in that it consists in crystallizing fructose from a solution of Fructose to form a mixture of crystalline fructose and - 62 mother liquor containing fructose; separation of crystalline Fructose from the mother fluid; mixing at least a portion of the mother liquor with an aqueous solution to obtain a lower solids fructose solution; treatment of this solution with activated carbon; and evaporation of this solution with a lower fructose content as a solid to give a rutous solution with a higher solids content, 11, 1 &apos; for the preparation of crystalline fructose from a Fructose solution, characterized in that the cooling of the solution in the original temperature range is carried out at an initial cooling rate; thereafter, cooling in the intermediate temperature range occurs at an intermediate rate which is less than the original cooling rate; and the cooling of the solution in the final temperature range is carried out at a rate which is greater than the rate at the intermediate cooling stage.