DE2329773A1 - PROCESS FOR INCREASING THE YIELD OF SACCHAROSE IN SUGAR PRODUCTION - Google Patents

Description

DR. MOLLER-BORe DIPL.-PHYS. DR. MANITZ DIPL.-CHEM. DR. DEUFEL DIPL-ING. FINSTERWALD DlPL.-lNG. GRÄMK0W

PATENT LAWYERS? T? Q 7 7

_{A 23O7} »1 June 2, 1973

Agency of Industrial Science & Technology 3-1, Kasumigaseki 1 chome, Ghiyoda-ku, Tokyo, Japan

Hokkaido Sugar Go., Ltd.

Hokkaido Sugar Go., Ltd. No. 1, 2 chome, Jinbocho Kanda, Ghiyoda-ku, Tokyo, Japan

Process for increasing the yield of sucrose in the

Sugar production

409882/0485

Dr. Müller-Bor * Dr. Manitz Dr. Deufel ■ Dipl.-Ing. Finsterwald Dipl.-Ing. Grämkow Braunschweig, Am Bürgerpark 8 8 Munich 22, Robert-Koch-Strasse 1 7 Stuttgart-Bad Cannstatt, Marktstrasse Telephone (0531) 73887 Telephone (0811) 293645, Telex 5-22050 mbpat ^Telephone «" * ")» 7261 Bank: Central Cash Office · Bayer. Volksbanken, Munich. Account no. 9822 Post check: Munich 95495

The invention relates to a method for increasing the yield of sucrose in the production of sugar from sugar beet or sugar beet molasses by cleaning, thickening, boiling and centrifuging the resulting sugar-containing solution with, if necessary, repeated repetition of the boiling and centrifuging treatment.

According to a conventional method for the extraction of sugar beets Extracted sugar solution contained sucrose is known to be purified, then concentrated and the sugar solution crystallizes to form a crystal mass, whereupon the crystal mass is centrifuged in mother liquor and sucrose crystals is separated. The sugar crystals are then isolated. In this case, albeit slightly, the amount of Isolated sucrose usually increases with increasing sucrose unit in the sugar solution. The amount of recovery is for each Boiling and centrifugation treatment in most cases in the area from $ 45 to $ 60. It is not possible to see the entire Sucrose containing sugar solution by just one boiling and centrifuging treatment to isolate.

This explains the fact why sugar beet processing factories The sugar boiling and centrifuging treatments of the sugar solution usually repeat with the aim of removing the sugar solution isolate as much sucrose as possible. However, if the sugar boiling and centrifuging treatments are repeated, so Raffinose and impurities gradually build up in the molasses, making cooking and centrifuging difficult. As well as the sugar boiling and centrifuging treatment therefore needs more and more time. The isolation of sucrose hardly pays off any longer. The molasses, which is an economic one Sugar production is no longer permitted, is withdrawn from the process as waste molasses.

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A possible cause for the limited insulation possibilities of Sucrose is based on the behavior of the impurities and raffinose that are present in the sugar solution · As soon as the Amount of ash, soluble nitrogen compounds and other impurities contained in the sugar solution When a certain level is reached, these impurities make the normal formation of sucrose crystals more difficult. The one in the sugar solution The presence of raffinose not only inhibits the formation of the sucrose crystals, but also leads to the sucrose crystals take the form of needles. They therefore tend to degrade the economy of sucrose isolation. In the cleaning process stage, e.g. B. deionization using ion exchange resins or the saccharate process, most impurities can but very little raffinose is removed. Increasing the yield of sucrose produced by a Improvement in sucrose purity achieved by removing impurities is therefore comparatively small when the purification process step does not remove the raffinose even if other impurities are effectively removed.

The isolation of sucrose inhibiting substances are mainly Ash, soluble nitrogen compounds and other impurities, as well as raffinose. Most contaminants can be in the deionization process stage can be removed with the help of an ion exchange resin or in the saccharate process, but succeeds hardly any removal of raffinose. Even if the impurities are removed by such treatment, the isolation of sucrose is inhibited if the raffinose is not removed with it.

For the purpose of increasing the amount of sucrose crystals to be isolated, it is sufficient to put the sucrose unit in the final Molasses by lowering the saxharose unit in the final

409882 / CK8S

reduce the amount of crystal mass and at the same time lower the amount of final molasses. If, in conventional known processes, an attempt is made to lower the sucrose unit in the final crystal mass, this leads to an increased raffinose content in the crystal mass. The consequence of this is that the sugar boiling treatment takes a longer time and the centrifugation either takes longer or is no longer feasible at all. Thus, it is hardly possible, the sucrose purity in the final molasses to a value of about 60 i "to decrease (in the production of sucrose from molasses after the barium saccharate method is, for the sucrose purity. B. final molasses in the Order of magnitude from 65 to 70 ^). If the known method is carried out without modification, it is difficult to increase the amount of isolated sucrose by further lowering the sucrose unit in the final molasses.

Here and in the following, "crystal mass ¹ · denotes the mixture of sucrose crystals and mother liquor that is obtained in the sugar-cocoa process, and" molasses "denotes the sugar solution that remains after the sucrose crystals have been removed from the crystal mass.

The object of the invention is to provide a simple method for increasing indicate the yield of sucrose, which is the numerous known in the production of sucrose from sugar beet Procedure eliminates any disadvantages.

Typical presently known processes for the production of sucrose from sugar beet or sugar beet molasses are z. B. the method in which with the aid of an ion exchange resin a deionization treatment is carried out, furthermore the so-called saccharate processes (e.g. the calcium saccharate and Barium saccharate process), as well as a process that uses neither deionization nor saccharate treatment (in the Rule called "Non-Steffen procedure"). According to these procedures

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the sugar solution purified in the purification process step and concentrated in the evaporation process step is converted into a crystal mass by the sugar boiling treatment. The crystal mass obtained is separated into sucrose and molasses by centrifugation. The molasses obtained is subjected again to the sugar boiling treatment and the crystal mass obtained is again separated into sucrose and molasses by centrifugation. In repeating the Zuckerkoch- and -zentrifugierbehandlung the accumulation of raffinose increases accordingly and make the economic isolation of sucrose increasingly difficult despite the fact that the resulting molasses contains more than 50 f <> sucrose.

According to the invention, an additional isolation of sucrose from the sugar solution, which the specified cleaning and concentration or was subjected to centrifugation treatment, aspired and achieved. This additional sugar production is brought about by the fact that α-galactosidase act on the sugar solution is left with hydrolysis of the raffinose contained therein into sucrose and galactose, and the hydrolyzate obtained is returned to the process stage that follows the process stage in which the sugar solution was removed, whereupon it is subjected to the sugar boiling treatment.

Using in the production of sucrose from sugar beet the deionization treatment with the help of ion exchange resins can lead to the hydrolysis of the raffinose by the oc-galactosidase a wide variety of solutions can be used, e.g. B. the diffusion juice, the sugar solution, which the carbonation and The sugar solution, which the sulphiting and pilgrim treatment (as an optional measure carried out), the sugar solution that has been cooled or is in the stage of cooling for the deionization treatment with the help of ion exchange resins is located and already on a hydrolysis of raffinose by oc-Glactosidase

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suitable temperature is cooled, furthermore the sugar solution, the deionization treatment with the help of ion exchange resins (possibly only with the help of a cation exchange resin) was subjected to the purified sugar solution, which concentrated or was thickened, the sugar solution, which was treated with activated charcoal (carried out as an optional measure), the sugar solution, which undergoes the decolorization treatment with the help of an ion exchange resin (as an optional s-measure carried out), the molasses, which started with any centrifugal treatment of crystal mass in the case of the first molasses up to the molasses intended for the final boiling treatment that were obtained through Redissolving the sugar obtained solution, as well as the sugar solution, which is intended for the sugar boiling treatment.

Using in the production of sucrose from sugar beet of the calcium saccharate process are also very different for the hydrolysis of raffinose by oc-galactosidase Solutions can be used, e.g. B. the diffusion juice, the sugar solution, which has been carbonized and filtered, the sugar solution, which of the sulphiting and filtering treatment (as an optional measure carried out), the sugar solution, which was decalcified with the help of an ion exchange resin (carried out as an optional measure and, if necessary, before the sulphiting treatment), the purified sugar solution, which was concentrated, the sugar solution, which was treated with activated charcoal (carried out as an optional measure), the sugar solution, which has been subjected to the decolorization treatment with the aid of an ion exchange resin (as an option s measure carried out), the molasses that are present in the various Centrifugation treatments of crystal mass arise and can range from the first to the last molasses solution obtained by redissolving sugar as well as the sugar solution intended for the sugar boiling treatment.

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Sugar - in / production from sugar beet without using deionization treatment with the help of ion exchange resins or saccharate treatment the same sugar solutions can be used for the hydrolysis of raffinose by ot-galactosidase, as in the production of sucrose from sugar beet by the calcium saccharate process, namely the diffusion juice, the Sugar solution which has been carbonized and filtered, the sugar solution which has been subjected to the sulfiting and filtering treatment was carried out (as an eventual measure), the Sugar solution, which has been decalcified with the help of an ion exchange resin (as an optional measure and, if necessary, carried out before the sulphiting treatment), the purified sugar solution, which has been thickened, the sugar solution which has been treated with activated charcoal (carried out as an optional measure), the sugar solution, which has been decolorized with the help of an ion exchange resin (carried out as an optional measure), the molasses used in the various centrifugation treatments occur from crystal masses and range from the first to the molasses intended for the last boiling treatment, the solution obtained by redissolving sugar, as well as the sugar solution ready for the sugar boiling treatment.

In the production of sucrose from sugar beet molasses by the barium saccharate process, raffinose can be hydrolyzed a wide variety of solutions can also be used by ot-galactosidase, e.g. B. that used as the starting material Sugar beet molasses, the sugar solution that has been carbonized and filtered, the sugar solution that has been treated with sodium sulfate and filtered, the sugar solution which was treated with bone charcoal (or the sugar solution which was treated with a Ion exchange resin has been decolorized or treated with activated carbon), the purified sugar solution, which has been thickened, the Molasses obtained from the various centrifugation treatments of crystal mass, starting from the first Melaae up to the ready-to-use for the last cooking treatment

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let the solution obtained by redissolving sugar, and the sugar solution intended for the sugar boiling treatment.

The specified processes for the production of sugar from sugar beet using the deionization treatment with the aid of ion exchangers include, for. B. the Imacti process, the modified Imacti process and the Nitten-Organo process, in which the deionization treatment with the aid of ion exchange resins is carried out before the sugar boiling treatment, and methods in which the deionizing treatment is carried out after the sugar boiling treatment, e.g. B. the BMA procedure. Known deionization methods using ion exchange resins include a method in which a strongly acidic cation exchange resin of the Η type is used in combination with a moderately basic anion exchange resin of the OH type or a weakly basic anion exchange resin of the OH type, and a method , in which a weakly basic cation exchange resin of the Η type is used in combination with a strongly basic anion exchange resin of the OH type or a moderately basic anion exchange resin of the OH type or a weakly basic anion exchange resin of the OH type. To carry out the process of the invention, it is possible to use sugar-containing solutions which are obtained in the known processes for producing beet sugar which are carried out using all of these deionization methods.

The molasses on which oc-galactosidase is allowed to act is first diluted with water to a suitable concentration (20 to 60 ° Brix). Then the oc-galactosidase is the added to diluted molasses. The sugar beet juice, (the sugar solution, which is in a process stage ranging from the cleaning process to the process preceding the sugar boiling treatment) ^ usually has a concentration in the range of 10 to 60 ° Brix. Or-galactosidase can therefore be added to the sugar beet

409882/0486

Juice can be added directly without diluting or concentrating the liquid proving to be necessary. Is the Concentrated sugar beet juice, it is diluted as required before adding the oc -galactosidase.

The oc-galactosidase to be added to the specified molasses or the sugar beet juice can be any conventional known method. It proves to be particularly advantageous if there is only a low level of invertase activity is present. If the α-galactosidase belongs to a type with high invertase activity, its invertase activity should if possible deactivated before they are used.

Typical K-galactosidases suitable for carrying out the method of the invention are e.g. B. those obtained from plant seeds are extractable, e.g. B. from coffee beans, Vicia sativa and Vicia faba, as well as <* - galactosidases, which are produced by microorganisms be e.g. B. Brewer's yeast, Aspergillus oryzae, Aspergillus niger, Penicillium paxilli, Calvatia cyathiformis, Mortierella vinacea var. raffinose-utilizer, Streptomyces olivaceus var. raffinoseutilizer, Streptomyces fradiae, Streptomyces roseospinus, E. co-Ii, Aerobacter aerogenes, Streptococcus bovis, Bacillus Delbrückii, Bacillus circulans and Pseudomonas eisenbergii. Of the specified enzymes, a ° t-galactosidase proves to be the most suitable, obtained by cultivating Mortierella vinacea var. raffinose-utilizer (ATCC 20034).

The hydrolysis of raffinose by 06-galactosidase changes with the concentration of the sugar solution, the type of sugar solution, the activity of the enzyme to be used and with various other factors, e.g. The time, pH and temperature chosen for the enzyme to act. In the As a rule, this hydrolysis of raffinose increases in inverse proportion to the concentration of the sugar solution and in direct proportion Relationship to the activity of the enzyme and that for the enzyme action

409882/0485

applied time and temperature. At temperatures above 65 ^° C., the enzyme is often inactivated and cannot withstand continued use over long periods of time. If the concentration of the sugar solution is above 65 ° Brix, the degree of hydrolysis is reduced to such an extent that the process measure is no longer useful.

When using molasses change z. B. the suitable conditions for carrying out the hydrolysis with the concentration of the molasses and the activity of the enzyme to be used. So z. B. 50 to 90? £ of the raffinose contained in the molasses can be hydrolyzed if α-galactosidase is allowed to act on the molasses for two to three hours using such amounts that 2,500,000 to 5,500,000 enzyme units are accounted for per 1 g of raffinose keeping the temperature in the range of 45 to 55 C, the concentration in the range of 15 to 60 ° Brix and the pH in the range of 4.8 to 5.2 (the unit of activity of <*> - galactosidase is defined as the amount that forms 1 / Ug of free glucose when the enzyme acts on melibiose for two hours at a final concentration
pH value of 5.2).

at a final concentration of 0.015 mol at 40 ⁰ C and at one

In the case of juice, the amount of enzyme to be used depends on the type and amount of impurities present in the juice. To z. B. to achieve a degree of hydrolysis of 70 to 90 ^ t in the diffusion juice, it is necessary to allow the enzyme to act on the juice for about 15 minutes in such an amount that 150,000,000 to 200,000,000 enzyme units are used per 1 g of raffinose, keeping the concentration in the range of 13-15 ° Brix and the pH at 5.0. This degree of hydrolysis does not appear to be advantageous with regard to the amount of enzyme to be used. But it is considered that the juice does not require dilution as it proves in the case of molasses as necessary, it can be seen that the hydrolysis in terms of savings in thermal energy is advantageous. In the

409882/0485

Hydrolysis of raffinose results in 342 g of sucrose and 180 g of galactose formed per 504 g of raffinose.

The hydrolysis of raffinose can be carried out in any of the various ways indicated Sugar solutions are made.

Although any of the various sugar solutions indicated to hydrolyze the raffinose he can be rangeζοgen is It is important to consider that various factors must be taken into account in choosing the most suitable sugar solution, e.g. B. the type and concentration of the sugar solution, the degree of raffinose accumulation, the ease with which the raffinose becomes is hydrolyzable by oc-galactosidase as well as the equilibrium the operating conditions and the economic efficiency of the heat balance of the various process stages involved in a sugar factory employing the method of the invention.

So z. B. in a sugar processing plant, which uses the deionization treatment with the help of ion exchange resins before the sugar boiling treatment, the not yet deionized sugar solution is ^{cooled to 50 0} G and adjusted to a pH of 5.0 to 5.2 and then subjected to the raffinose hydrolysis treatment . Furthermore, the molasses can also be diluted with water to 30 to 50 Brix and adjusted to a pH value of 5.0 to 5.2 and then subjected to the refining treatment.

The operational and other requirements are different for every sugar factory. It therefore proves necessary that the Hydrolysis of the raffinose should be started at that point in the overall process implementation which is the most effective and advantageous Elimination of all disadvantages which experience has shown and which can be attributed to the presence of raffinose in the sugar boiling and centrifugation treatment.

409882/0485

This raffinose hydrolysis process can be set up in two or more process stages. So he can z. B. to one Take place at the point in time, which is preceded by the thickening treatment and at another point in time, which is followed by the fourth sugar boiling treatment precedes. In this case, that in the thickening juice obtained by the previous thickening treatment is concentrated raffinose present was hydrolyzed and the hydrolyzate obtained is subjected to the subsequent sugar boiling treatment and the sugar solution separated by centrifugation after the fourth sugar boiling treatment becomes one Subjected to raffinose hydrolysis treatment, followed by the fifth sugar boiling treatment.

The sugar solution in which the majority of the raffinose present is present Was hydrolyzed, is returned to the process stage that follows the process stage from which the Sugar solution had previously been removed. Thereafter, the returned sugar solution is used in the subsequent process steps allowed to run through in the specified order in order to effect the isolation of the sucrose present in it. the Raffine hydrolysis according to the method of the invention can thus be applied to a sugar solution which is in one of several Process stages is obtained.

Because the sugar solution, in which the majority of the raffinose present has been hydrolyzed, through the subsequent process steps is passed in the normal order, it becomes the existing one in the sugar boiling and centrifuging treatments Sucrose isolated. The impurities and the unhydrolyzed Raffinose accumulates more and more as the number of sugar boiling treatments increases. The amount of on this However, wise accumulated raffinose is less than when the raffinose hydrolysis treatment is not turned on. the Accumulation decreases in direct proportion as the amount of hydrolyzed raffinose increases. As a result, the

409882/0485

Centrifugation treatment of the accumulating crystalline mass is easier and takes less time even if the sucrose unit of the final crystal mass further lowers becomes as if the raffinose hydrolysis treatment is not performed

According to the method of the invention, the OC-galactosidase allowed to act on the sugar solution regardless of the cleaning method to which the sugar solution was subjected, to hydrolyze the raffinose it contains and the raffinose content of the sugar solution for the subsequent process stages to humiliate. This can affect the effectiveness and efficiency of the sugar boiling treatment and that of the centrifugal treatment of the final crystal mass is improved, thereby enabling is to lower the sugar purity of the final crystal mass below that value according to conventionally known Method is achievable, as well as lowering the sugar concentration of the final molasses and the amount of final To reduce molasses and, if necessary, to increase the amount of sucrose to be isolated.

So is z. B. in the barium saccharate process, which is used to isolate sucrose from the molasses obtained in beet sugar factories, the following should be noted. If the sucrose in the form of Bariumsaccharat from the molasses, the raffinose and impurities in such high concentrations that isolation of the sucrose by other methods in beneficial way is not possible, isolated so to be about $ 60> the raffinose contained therein removed. The influence of the raffinose is therefore reduced and the economy of the sucrose recovery is improved in direct proportion to the amount of the raffinose removed. In the sugar solution obtained by this process, the sucrose unit reaches values of about 95 ° or more. The sucrose unit of the sugar solution is further increased by the subsequent

A09882 / 0A85

JfI-

following cleaning treatments (ζ. B. by treatment with bone carbon, deionization with ion exchange resins and Treatment with activated charcoal). When isolating sucrose in the sugar boiling treatment from sugar solutions with such a high However, sucrose unit is gradually accumulated in the raffinose and carrying out the sugar boiling treatment itself becomes more and more difficult as the number of sugar boiling treatments increases. The inevitable consequence of this is the molasses with such a high sucrose unit can be discarded as waste molasses. The amount of sucrose isolated is therefore comparatively low with regard to the high sucrose unit of the sugar solution after the cleaning treatment (or the Sugar solution before the sugar boiling treatment)

In this case too, the accumulation of the raffinose can be reduced by using the method of the invention.

When the method according to the invention is carried out, the accumulation decreases in raffinose and therefore lowers the sucrose unit of the waste molasses. As a result, the yield is increased in sucrose.

The invention is further illustrated by the following examples, in which preferred embodiments of the invention in obtaining of sucrose can be illustrated using various methods.

example 1

As a source of oc-galactosidase, lumpy pellet-shaped cells with a content of 06-galactosidase (hereinafter referred to as "enzyme-containing cells") were used, which had only a very low invertase activity and were obtained by using a culture medium with a content of 1 fo Lactose, $ 1

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Glucose, 1 i * corn steep water, 1 _t O ^ ammonium sulfate, 0.1 $ urea, 0.2 ia sodium chloride, 0.3 # primary potassium phosphate, 0.2 ia magnesium sulfate and 1 # calcium carbonate with Mortierella vinacea var. Raffinose-u tilizer inoculated and the microorganism contained therein was cultivated aerobically at 30 C for 3 days.

The molasses intended for hydrolysis was the fourth molasses in a sugar beet processing plant incurred, in which five sugar boiling treatments were carried out and deionization using ion exchange resins was applied. The composition of the molasses used is shown in Table 1 below.

Table 1

Brix concentration sucrose concentration Raffinose concentration

Sucrose purity

76.0 ° Brix 53.5 1 "

1.05fo (9.28 % based on Brix)

70.4 1o

The molasses of the specified composition was diluted with water to 30 ° Brix and the pH was adjusted to 5.0. The enzyme-containing cells were added to the molasses obtained in such an amount that there were no 4,500,000 OC-galactosidase units per g of raffinose. The resulting mixture was ^{stirred at 50 0} O for 2.5 hours in order to allow the enzyme to act on the raffinose present in the molasses. It was found that at the end of the stirring time the degree of hydrolysis of the raffinose had reached 69.5 ^ δ. The mixture was filtered to remove the enzyme-containing cells therefrom, and the obtained molasses had the composition shown in Table 2 below.

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Table 2

Brix concentration sucrose concentration Raffinose concentration

Sucrose purity

30.0 ° 22.2 0.85

74.0

Brix

(2.83 # based on Brix)

Sugar solutions of the composition given in Tables 1 and 2 were separately subjected to the sugar boiling and centrifuging treatment in an amount corresponding to 20 kg of raw molasses, sugar and waste molasses having the composition shown in Table 3 below were obtained.

Table 3

Raffinose molasses the end Molasses without raffinose the end kg hydrolysis prey hydrolysis prey kg Saccha- 8.03 kg Saccha- 6.15 Brix rose 9.19 kg Brix rose 11.73 Concentrated pure Concentrated pure tration he it tration is called sugar 95.8 ° Brix 94.2% 95.9 ° Brix 95.3% Waste-
molasses 85.2 ° Brix 51.2% 79.2 ° Brix 54.6%

The molasses not subjected to any raffinose hydrolysis treatment had inferior performance in centrifugation treatment. So the sucrose unit des Sugar can be increased by using about 1 1 hot v / ater.

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The results shown in Table 3 show that 5-62 kg of sucrose were isolated by the procedure of this example in the experimental batch without raffinose hydrolysis, and 7.24 kg of sucrose were isolated in the one comprising raffinose hydrolysis Experimental batch, each using 20 kg of molasses. This means that the yield of sucrose according to the invention increased by 1.62 kg. It can be seen that this increase in sucrose yield is far greater than that Amount of 0.67 kg of sucrose formed as a result of the hydrolysis of raffinose by oc-galactosidase.

Example 2

The sugar solution of the composition given in Table 4, which was ready for use for the ion exchange resin deionization treatment in a process in which deionization takes place prior to the sugar boiling treatment, the pH was adjusted to set from 5.0.

Table 4

Brix conc entrants in sucrose concentration Raffinose concentration

Sucrose purity

13.7 Brix 12.7 fo

0.13 i » (0.95 Ί ° based on Brix)

92.7 fo

The same enzyme-containing cells as were used to carry out the process described in Example 1 were added to this sugar solution in such an amount that 50,000,000 oC-galactosidase units per g of raffinose were omitted. The mixture obtained was ^{stirred at 50 °} C. for 15 minutes in order to allow the enzyme to act on the raffinose. The hydrolysis

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• a

The level of raffinose reached $ 61.1. The by filtration of the The solution obtained from an enzymatically hydrolyzed sugar solution had the composition shown in Table 5.

Table 5

Brix concentration 13.7 ° Brix

Sucrose concentration $ 12.8

Raffinose concentration $ 0.05> (0.37 i ° based on Brix)

Sucrose purity 93 »4 $>

The piltrate obtained was then passed in a customary known manner through a column which contained the ion exchanger (K-type) known under the name "Amberlite IR-120B" and then through a column which contained the ion exchanger known under the name "Amberlite IRA- 68 ¹ * known ion exchanger (OH type). The juice obtained in this way had the composition shown in Table 6.

Table 6

Brix concentration 12.3 Brix

Sucrose concentration 11.9 %

Raffinose concentration 0.04 <? » (0.33 i ° based on Brix)

Sucrose purity 96.7 ^

In further experiments, the sugar solution with the composition given in Table 4 was directly subjected to the deionization treatment using ion exchange resins without applying the raffinose hydrolyzing treatment. That one-

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The sugar solution obtained had the composition shown in Table 7.

Table 7

Brix concentration 12.3

Sucrose concentration 11.8

Raffinose concentration 0.12

Sucrose purity 95.9

Brix

(0.98 i » based on Brix)

The sugar solutions of the composition given in Tables 6 and 7 were concentrated and then subjected to five sugar boiling treatments. The sugar and garbage molasses that at the end of the fifth sugar boiling treatment had the compositions shown in Tables 8 and 9 below on.

Table 8

fifth molasses

Waste molasses

Brix concentration 96.0 "Brix 85.3 " Brix Sucrose purity 95.3 * 51.2 Table 9 fifth molasses Waste-! flelas Brix concentration 95.9 ° Brix 80.1 ° Brix Sucrose purity 95.4 % 54.6 ok

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The amount of sucrose obtained from 120 kg of those listed in Table 6 Sugar solution and obtained from 120 kg of the sugar solution listed in Table 7 was calculated using the formula for the sucrose production, as indicated on page 31 of the "Handbook for Manufacture of Sugar", the values for the Sucrose unit of the sugar solution listed in Table 6 and the waste molasses listed in Table 8 were used in the experimental approach, in which hydrolysis of the raffinose was effected with ion exchange resins before the deionization, and where the values of the sucrose unit of the sugar solution listed in Table 7 and of the waste molasses listed in Table 9 were used in the experimental approach in which the raffinose hydrolysis treatment has been omitted. The results of this calculation are shown in Table 10 below.

Table 10

Isolated amount of sucrose

Raffinose hydrolyzing treatment 13.77 kg

before the ion exchange resin

Deionization treatment carried out

Process without raffinose hydrolysis treatment - 13 »43 kg development carried out

The results show that the yield of sucrose according to the invention was increased by 0.34 kg by performing the raffinose hydrolysis treatment before the deionization treatment with the help of ion exchange resins. It should be noted that this increase in Sucrose yield the amount of 0.07 kg sucrose formed as a result of the hydrolysis of raffinose by oc-galactosidase, exceeds.

k 0 9 8 8 2/0 4 8 5

Example 3

There were diluted 40 kg sugar beet pulp the composition shown in Table 11 to 78 ° Brix, then heated to 80 ⁰ C and then stirred.

Tabel Brix concentration 11 Brix polarization 82.0 ° Sucrose concentration 53.46 Raffinose concentration 47.35 i ° (based on Brix) Sucrose purity 4.10 57.74

A milk made from barium hydroxide, the concentration of which was 30 % _t, calculated as barium oxide, was added to the molasses with stirring in such an amount that 60 g of barium oxide per 100 g of the sucrose present in the molasses were added. The mixture obtained was kept at 80 ^° C. for 1 hour to effect the reaction. The reaction mixture obtained was filtered and then washed with hot water containing 2% barium oxide. The wash filtrate was mixed with 40 l of water, carbonized at 80 ° C., then filtered and finally washed with cold water. 80.4 kg of sugar solution of the composition given in Table 12 were obtained.

Table 12

Brix concentration 22.8 ° Brix

Sucrose concentration 21.44 %

Raffinose concentration 2.84 i » (based on Brix)

Sucrose purity $ 94.04>

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-χι-

Sodium sulfate was added to this sugar solution in order to precipitate the barium ions still present in the form of barium sulfate. The precipitate formed was filtered off and washed with water. In this way 85.4 kg of piltrate were obtained the composition given in Table 13 obtained.

Table 13

Brix concentration 21.5 ° Brix

Sucrose concentration 20.16 i *

Raffinose concentration 2.82 % (based on Brix)

Sucrose purity $ 93.77>

The sodium sulfate-treated sugar solution of the composition shown in the table was divided into two equal portions. One portion was adjusted to pH 5.2 with sulfuric acid and the same enzyme-containing cells as used in Examples 1 and 2 were added to this sugar solution in an amount such that 4,500,000 Qi -galactosidase- Units per g of raffinose were omitted. The resulting mixture was stirred at 50 ° C. for three hours to allow the enzyme to act on the raffinose. It was found that the degree of hydrolysis of the raffinose had reached $ 68.1. When this sugar solution containing hydrolyzed raffinose was filtered, 42.7 kg of filtrate of the composition shown in Table 14 were obtained.

Table 14

Brix concentration 21.5 ° Brix

Sucrose concentration 20.46 i »

Raffinose concentration 0.90 i » (based on Brix)

Sucrose purity 95 _f 16 $>

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This solution was brought to pH with sodium hydroxide δ, O adjusted, concentrated, and then five times of sugar boiling treatment subjected, whereby 8.06 kg of sucrose were isolated. The fifth molasses, which in a total of 1.31 kg had the composition shown in Table 15.

Table 15

Brix concentration 84.5 ° Brix

Sucrose concentration 50.76 #

Raffinose Concentration $ 7.26 (based on Brix)

Sucrose purity 60.07%

The other portion of the sodium sulfate treated solution was concentrated directly without being subjected to the raffinose hydrolysis treatment using ot-galactosidase and then sugar boiling treatment was carried out five times, whereby 6.92 kg of sucrose was isolated. The one with it The fifth molasses obtained, which was obtained in a total amount of 2.69 kg, had the composition shown in Table 16.

Table 16

Brix concentration 83.5 ° Brix

Sucrose concentration 62.45 i °

Raffinose concentration 10.25 i » (based on Brix)

Sucrose purity 74.79 %

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The results obtained show that when sucrose is isolated by the barium saccharate process from 20 kg of sugar beet molasses the sucrose yield according to the invention could be increased by 1.14 kg if the sodium sulfate treated sugar solution containing raffinose by oc-galactosidase was hydrolyzed. It should be noted that this increase in sucrose yield increases the amount of 0.12 kg of sucrose, which is formed as a result of the hydrolysis of the raffinose, far exceeds. The increase in the yield of sucrose is attributed to the fact that sucrose was formed as a result of the hydrolysis of raffinose and that the sucrose unit the sugar solution was increased accordingly, and that the formation of sucrose crystals was facilitated by strong reduction in the raffinose content, which is responsible for inhibiting the formation of sucrose crystals is.

Example 4

The second molasses was used, which was obtained before the start of the so-called Steffen process in a sugar beet factory, in which the calcium saccharate process (Steffen process) is used. The second molasses corresponds to the molasses obtained in sugar production from sugar beet if neither a saccharate process nor an ion exchange resin deionization is used (usually referred to as "Non-Steffen process ¹¹ ). The composition of the second molasses used is shown in Table 17 below.

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Table 17

Brix concentration 85.2 ° Brix

Sucrose concentration 61.9 "/»

Raffinose concentration. 0.87 $> (1.02 ^c ß> based on Brix)

Sucrose purity 72.65 i »

20 kg of this molasses were diluted with hot water to a Brix value of 30 ° and with sulfuric acid to a pH value set of 5.2. The molasses obtained was with the same enzyme-containing cells as used in Example 1 in such an amount added that 4,500,000 ot-galactosidase units accounted for per g of raffinose. The resulting mixture was stirred and kept at a temperature of 50 ° C. to activate the enzyme to let the raffinose take effect. It was found that the degree of hydrolysis of the raffinose had reached $ 60.8. The the hydrolyzed Molasses containing raffinose was filtered to remove the enzyme-containing cells therefrom. Thereby were 56.8 kg Molasses of the composition given in Table 18 was obtained.

Table 18

Brix concentration 30 ° Brix

Sucrose Concentration $ 21.9

Raffinose concentration 0.12 ° fo (0.4 % based on Brix)

Sucrose purity 73 »0 i <>

The total amount of this molasses was concentrated and then subjected to sugar boiling and centrifugation treatment, whereby 6.49 kg of isolated sucrose and 12.3 kg of waste molasses were obtained. It was found that the waste molasses had a Brix value

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of 85.5 ° and a sucrose purity of 56.5 i ° .

In a further experiment, 20 kg of the indicated second molasses were subjected directly to the sugar boiling and centrifuging treatments without hydrolyzing the raffinose, 6.26 kg of sucrose and 12.5 kg of waste molasses being obtained. It was found that the waste molasses had a Brix value of 85.3 ° and a sucrose purity of 57.3 "A.

The results obtained show that 6.49 kg of sucrose was isolated according to the procedure used in this example when carrying out the raffinose hydrolysis treatment according to the invention, and that only 6.26 kg of sucrose were isolated at Omission of this treatment, in each case starting from the second molasses of the same composition, which in a non-Steffen process approaching sugar factory. This means that the raffinose hydrolyzing treatment of the present invention is a increased the yield of sucrose by 0.23 kg. It is noted that this increase in sucrose yield is the kenge of 0.07 kg of sucrose, which is formed as a result of the hydrolysis of raffinose by α-galactosidase, far exceeds.

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Claims (9)

Patent claims (V) Process for increasing the yield of sucrose in the production of sugar from sugar beet or sugar beet molasses by cleaning, thickening, boiling and centrifuging the resulting sugar-containing solution, possibly several times Repetition of the boiling and centrifuging treatment, characterized in that the sugar-containing solution treated with ot-galactosidase before or after at least one process step which precedes one of the cooking treatments. 2. The method according to claim 1, characterized in that a sugar-containing solution, the Brix value of which is 10 to 65 °, preferably 20 to 60, treated with oc_galactosidase. 3. The method according to claims 1 and 2, characterized in that «- used galactosidase derived from plant seeds extracted or formed by Mierο organisms. 4. The method according to claim 3 »characterized in that the extracted from coffee beans, Vicia sativa or Vicia faba ^ - -Galactosidase used. 5. The method according to claim 3 »characterized in that one of brewing yeast, Aspergillus oryzae, Aspergillus niger, Penicillium paxilli, Galvatia cyathiformis, Mortierella vinacea var. raffinose-utilizer, Streptomyces olivaceus var raffinose-utilizer, Streptomyces fradiae, Streptomyces roseospinus, E. coli, Aerobacter aerogenes, Streptococcus bovis, Bacillus Delbrückii, Bacillus circulans or Pseudömonas eisenbergii formed oC-galactosidase is used. 409882/0485 - 2f- 6. The method according to claim 5, characterized in that the cultivation of Mortierella vinacea var. Raffinoseutilizer, deposited under ATGG no. 20034, formed OC-galactosidase used. 7. The method according to claims 1 to 6, characterized in that one is an oc-galactosidase with low invertase activity used. 8. The method according to claims 1 to 7, characterized in that per gram of raffinose present 2 500 000 to 5,500,000 tt-galactosidase units were used. 9. The method according to claims 1 to 8, characterized in that that the treatment with oc-galactosidase at a temperature of 45 to 55 C in a pH range of 4.8 to 5.2 carries out 409882/0485