DE2624795A1 - METHOD OF OBTAINING CARBOHYDRATES - Google Patents

Description

SUCRES! ' CORPORATION
Few York, NY, V.St.A.

"Process for the production of carbohydrates"

Priority: June 2, 1975 / V.St.A., No. 582 809 April 27, 1976, V.St.A.,

The invention relates to a method for the production of carbohydrates and other valuable products made from materials containing carbohydrates, in particular from molasses.

There are a number of products containing carbohydrates, some or all of which contain valuable carbohydrates can be won. Examples include fruit juices, sugar juices from sugar cane and sugar beet, starch hydrolysates, hardwood sulphite liquors and whey are valuable starting products for the production of carbohydrates such as sucrose, fructose, glucose, Invertsucker, lactose and xylose. Often the yields are the conventional processes are so low that the costs associated with these processes are not justified.

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are finished. In addition to these economic considerations, there is the fact that it is not possible to do so from these materials to gain additional valuable products without further elaborate cleaning processes and thus the costs for the carbohydrate to compensate for insulation.

The difficulties mentioned above play a role particularly in the field of sugar refining, v / o in considerable quantities by-products such as molasses arise. It is known that molasses contain many valuable products, for example Sucrose, fructose, glucose, invert sugar and inorganic salts. However, attempts to obtain these products fail that they cannot be separated economically.

The production of sugars, for example refined sucrose, generally starts from sugar cane or sugar beet the end. During the individual process stages in the production of pure sucrose varies depending on the starting product molasses are generally obtained as a by-product. Molasses can be found at numerous points throughout the sugar production process are formed and therefore do not have a precisely defined composition. Generally is under Molasses is to be understood as a mother liquor that remains in the production of sugar after sucrose has crystallized. Molasses generally contain sucrose, glucose, fructose, inorganic salts and organic non-sugar compounds. the The composition of molasses depends on the processing

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conditions, the sugar source used and the processing stage, from which the molasses comes from.

In practice, molasses is understood to mean, in particular, sugar solutions from which, due to the depletion of sucrose, Enrichment of non-sugar components and increased viscosity of the mother liquor not sufficiently pure sucrose more can be crystallized. Such molasses are generally referred to as terminal molasses or "black molasses". There are several uses for pure terminal molasses. For example, they can be made into yeast, vinegar and through microbiological processes various organic compounds, such as alcohols, can be processed. However, technical developments made them more economical Synthesis options for these products are available so that the importance of molasses as a chemical raw material has declined. In general, they are terminal molasses not suitable for human consumption. In contrast, molasses from earlier stages of sugar production, for example first and second molasses, for many years as food and as raw materials for the production of bakery and confectionery used. However, molasses are rarely used in foods in such amounts that a corresponding one Market for the large quantities of molasses produced in sugar factories.

End molasses are mainly fed directly to ruminants or used as raw materials for animal feed. Because molasses at

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when fed in too large quantities act as a laxative, they can only be fed to a limited extent.

In some areas, molasses is used as a fertilizer. However, this only proves to be economical if no other use is available for the molasses.

Molasses from sugar beet production has long been a treatment for removing Subjected to sugaring. The most commonly used desugarization process is the so-called Steffen method, in which the diluted Lime can be added to molasses solutions. With this Steffen process, up to 95 percent of the Sugar can be obtained from beet molasses. However, it is not suitable for treating cane molasses because of this process essentially destroys the invert sugar. Furthermore, according to the Steffen method for the treatment of beet molasses, that only provides a single product, namely sugar, other valuable molasses components are not fully utilized. Furthermore, in the Steffen process, raffinose is formed in large quantities, the presence of which leads to errors in the polarization analysis for sucrose and the crystal growth of sucrose adversely affected. For this reason, in systems who work according to the Steffen method, discard the molasses every 24 hours at intervals of 1 or 2 weeks. These garbage molasses are another source of molasses for which there is a need for economical use.

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It is known that working according to the ion exclusion principle Methods for separating sugars from raw materials such as molasses are generally applicable; see TJS-PS 2 937 959 However, difficulties arise in the treatment of certain molasses, such as terminal molasses, because of the efficiency of the exclusion resins progressively decreases over time. In addition, such processes occur on a large scale Scale presents significant problems.

The object of the invention is to provide a method for treating materials containing carbohydrates, that an isolation and removal of the carbohydrate fraction as well as the extraction and utilization of other valuable products permitted. In particular, this method should be suitable for the treatment of molasses, regardless of their origin various valuable products that enable full molasses utilization are to be obtained. By the invention Molasses treatment are to be formed in each case products, which for the sugar production, fertilizer production and feed production are valuable. The quantities of these products are designed to be economical and practical Usability. Finally, according to the invention, it should be possible to produce solutions containing carbohydrates Clarify materials, especially final or black molasses.

This multi-part object is achieved in that a solution of the carbohydrate-containing material via an ionic

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exclusion resin used to separate carbohydrates from inorganic ones Compounds in the starting material is able to exist. Then water is poured over the resin. The received Eluate can be separated into different solutions, which mainly contain salts or carbohydrates as solids.

According to a preferred embodiment of the method according to the invention, the solution supplied to the exclusion resin is grounded Viscosity changes made to significantly reduce channel effects or other flow disturbances in the column. Channel effects, i.e. the formation of certain flow paths within a packed column to which the material fed follows, lead to bypassing a large part of the active centers of the exclusion resin and thus to a decrease in the efficiency and the degree of isolation and separation of carbohydrates.

Furthermore, it was found according to the invention that when the sucrose fraction is obtained from starting materials containing sucrose the exclusion resin must not be used in the hydrogen form, as this is an inversion of the sucrose to invert sugar causes.

As already mentioned, the method according to the invention can be used particularly for the treatment of molasses with the recovery of valuable Apply products. Molasses, especially terminal molasses, have grown due to their viscosity and the large amount they contain Number of non-sugar impurities so far than only a small one

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Proven scope accessible for conventional separation processes. This is due to the particularly difficult handling of molasses traced back. Part of the following is concerned with the applicability of the method according to the invention such molasses. From these statements with reference to molasses and from the parts of the description and examples that deal with other carbohydrate-containing solutions, it will be apparent to those skilled in the art that the inventive Method can be used for an effective treatment of a large number of starting products.

The following explanations relate to techniques for Molasses treatment used in certain other carbohydrates containing materials are not necessary. It can also be used in the processing of certain types of carbohydrates containing Materials additional or modified treatment stages may be required or appropriate.

It has been found according to the invention that the effectiveness of Ion exclusion resins for the separation of valuable components from molasses is greatly increased if one is made from the molasses before the passage through the exclusion resin removes a considerable proportion of organic non-sugar materials. With the conventional The process of separating these materials was largely left to the resin itself, since these materials are in the generally have a higher molecular weight than sugar and are therefore excluded from the resin particles. It

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however, previous effective removal was found to be of these materials plays an important role in achieving a high degree of separation in the resin bed.

According to one embodiment of the method according to the invention aluminum or iron (III) ions, preferably in the form of iron (III) chloride, iron (III) sulfate or aluminum sulfate, added to the starting molasses, which leads to a highly effective removal of materials in the form of a precipitate otherwise would hinder the ion exclusion process.

Furthermore, the invention has been found that for effective Separation of sugars and salts, certain synthetic resins and physical properties of the synthetic resin bed are important Role-play. For example, it has been found that certain resins are based on sulfonated styrene-divinylbenzene copolymers in the form of the sodium salt with a crosslinking or. a divinylbenzene content that is well above the corresponding proportion of resins used hitherto, and for example at least about 4 percent, is particularly good for separating molasses, especially terminal molasses. Apparently, the added strength of the Betts is an important separation factor for these materials. In general, copolymers with higher degrees of crosslinking can be used with success, for example up to one Content of about 8 percent divinylbenzene. However, as the degree of crosslinking increases, the flow rate through the resin decreases.

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_ 9 -

It was also found that the ratio of the height of the exclusion column to its diameter, the size of the resin particles and the temperatures of the molasses solution and the subsequently used water influence the effectiveness of the separation.

It was found that from particularly low-grade molasses, such as terminal molasses, using conventional precipitation, Clarifying and flocculating agents and using separation processes commonly used to clarify sugar solutions, Surprisingly, not a high proportion of non-sugar components can be removed beforehand. According to the invention, however, it was found that by centrifuging molasses or the solutions of which allow an unexpectedly high proportion of non-sugar components, including ash, to be removed. This distance leads to a significant improvement in effectiveness the subsequent chemical separation of non-sugar components and the exclusion separation method.

The eluate leaves the exclusion resin in different fractions, in which at least one valuable material is predominantly present. In at least one of these factions this is im Carbohydrate contained in the starting material, i.e. sucrose

contain,
the treatment of molasses / The eluate fractions can therefore be used for various purposes, whereby an almost complete utilization and marketing of the starting molasses is achieved.

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According to a further embodiment of the invention, membrane filtration, generally referred to as ultrafiltration, is used to remove a considerable proportion of organic
To remove non-carbohydrate constituents, generally coloring bodies or their precursors, from the carbohydrate-containing material. This purification can be carried out either before the exclusion separation process or as a means of further clarifying that obtained from the ion exclusion treatment
Carbohydrate rich fraction are applied.

The term molasses used here is to be understood as meaning all types of liquids from which sucrose has been crystallized or can still be crystallized. This expression therefore also includes full juice molasses, so-called "first molasses", ie mother liquors which remain after the first sucrose crystallization and still contain crystallizable sucrose, as well as all liquids which have been obtained after crystallization processes. This term also applies to terminal molasses or mother liquors because of their viscosity
and their high content of impurities, such as ash, non-sucrose sugar, and organic non-sucrose components, are no longer capable of forming sucrose during crystallization for practical and economic reasons. Furthermore
the term molasses should also be independent of the raw material source, ie it should refer to products made from sugar cane and sugar beet regardless of the process stage. Sojiiit includes the term the first, subsequent and terminal molasses,

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that are created during sucrose crystallization when processing raw cane sugar, molasses that are created during refining obtained from sucrose crystals with a thin molasses film during the refining process, "refined molasses" , which arise during the sucrose crystallization during the refining of cane sugar, beet molasses from the Sucrose crystallization from beet sugar solutions as well as waste molasses arising from the Steffen process. Except for molasses the process according to the invention can also be successfully applied to other products containing carbohydrates, such as Whey, starch hydrolysates, fruit juices, products containing sugar, e.g. sugar cane and sugar beet juices, as well as concentrates from these products.

According to the method according to the invention, the various starting materials containing carbohydrates are prepared according to the principle of ion exclusion treated, reducing the carbohydrate fraction isolated and removed while preserving other valuable products.

The ion exclusion method is known per se and has become general proposed for use in the sugar industry. The exclusion resins tend to cause physical adsorption of one or more ingredients to the exclusion of the other ingredients as an ion exchange. For example a cation exchange resin has a more pronounced affinity for a weakly ionizable material such as sugar and

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thus enables the material to be adsorbed by the resin, while more ionizable materials such as inorganic salts remain in the liquid in the interstices. If water is poured over the resin bed, a solution of the highly ionizable material appears first, which finally appears the physically adsorbed weakly ionizable material follows. Such resins are hereinafter referred to as ion exclusion resins designated.

When applying the ion exclusion method to carbohydrates containing materials, in particular molasses, often occur channel effects, which lead to a very poor separation effect to lead. These problems are common in processes in which a liquid flows through a packed column. These Difficulties arise with exclusion procedures due to the special physical nature of the resin bed and the fact that for effective exclusion at least two liquid streams, namely the starting material and then a liquid, such as water, must be passed through the column. According to the invention, these difficulties are largely eliminated. It also increases the effectiveness of the exclusion one or more procedures which can be used in particular for exclusion procedures. In one embodiment the channel effect or "leap-frogging", as described below, is significantly reduced by introduces the starting material containing carbohydrates into the exclusion column in an increasing manner, so that the vis-

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viscosity of the liquid can be changed. For example a typical molasses introduced into the exclusion column has a density in the range from about 45 to 55 ° Brix. It was found that the. Subsequent to elution of the various fractions of water introduced, the viscosity of which is considerably lower than that of the molasses introduced is, migrates through the exclusion column at a rate above the flow rate of the molasses. Since that Water mixes with the molasses and eventually bypasses them ("leap frog"), the resin's ability to adsorb of carbohydrates and the ability of water to extract and elute adsorbed and unadsorbed Material considerably reduced.

The aforementioned circumvention processes are particularly pronounced in the case of exclusion columns with low ratios of height to Diameter, i.e. where the vertical distances between the different fractions are small. When performing in large-scale, where the highest possible throughput is important, the use of columns with low Height to diameter ratios on the order of about 0.8 to about 5.0 are preferred. Thus, this flow problem occurs particularly strong on an industrial scale.

It has been found that this bypass problems can be greatly reduced or eliminated when, to a certain sequence of supply to. Adheres to the exclusion column, whereby the

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fed material in at least two fractions of different Viscosity is present. The first fraction consists of the normal feed to the column, i.e. in the case of molasses from a feed at about 45 to 60 ° Brix. The second, subsequent fraction has a lower viscosity (i.e. a lower

Brix degree) as the first fraction. Then a dilute aqueous medium, such as water, or a dilute molasses solution, added to remove the various solutions from the To elute exclusion column. The difference in viscosity between the elution medium and the second fraction supplied, the is less than when feeding material with constant viscosity would occur serves to prevent the supplied material from being bypassed by the elution medium.

According to a preferred embodiment, three or more different fractions applied one after the other. The first fraction of the molasses introduced into the column consists of one Low density molasses solution, for example from about 15 to about 25 ° Brix. Molasses with a higher density is then placed on top, typically about 45 to about 55 ° Brix. In the end a third fraction follows with a density in the range from about 15 to about 25 ° Brix. Thus the molasses actually supplied is i.e. the 45 to 55 Brix molasses, buffered or padded with a low density molasses. The following water or another dilute aqueous solution is then applied to the column in order to add the various product fractions elute. This rinse can be done using water and / or

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a dilute solution with a density of about 5 Brix or less. It was found that the buffering zones around the high density molasses supplied serve to reduce the tendency of the washing fraction to mix with the molasses or to bypass them, reduce them or eliminate them entirely. In this way there are corresponding dwell times for a suitable adsorption through the exclusion column and subsequent elution of the various product streams possible.

The quantities of the various components of the supplied material, which are necessary to create an appropriate buffer zone around the supplied To ensure high density molasses can ever depending on the type of column, the density of the buffer layers and the material supplied, and on the basis of similar considerations "considerable vary. In general, the respective amounts of buffer (measured as bed volumes) should be approximately as large as the amount of high density molasses fed. For example, the amount of the buffer is about 0.8 to 2.5 times the amount of the high density fraction.

For the person skilled in the art it is self-evident that the relative Densities, viscosities or concentrations are directly related and thus as another way of describing them of viscosity and flow differences between the in- ■ fractions can be used. The Brix degree expresses a density measurement, but it is clear that for example higher Brix values on solutions of higher viscosity

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(and focus) let it close.

Another procedure, alone or, preferably, together with the aforementioned viscosity change is applied, is that for washing out the various materials from the column used water or another dilute solution to pass through the bed at a temperature below the temperature of the fed material. This temperature difference is preferably of the order of magnitude at least about 11 C. According to a particularly preferred embodiment, the aforementioned changes in density are used in the fed material and maintains the temperature of the fed "Low density buffer material below the temperature of the fed High density fraction. In this embodiment there is both a mixing of the interfaces of the supplied materials and the tendency of the washing liquid to bypass of the fed material is reduced.

The effectiveness of ion exclusion separation depends on some starting materials containing carbohydrates, such as molasses, depends heavily on effective pretreatment with removal of non-carbohydrate organic components. The need or the desirability of such a pretreatment and the extent of this pretreatment depend on the starting material used away. As in this regard with molasses due to their large proportion of organic non-sugars, colored compounds or whose forerunners encounter the greatest difficulties

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the following explanations of preferred embodiments for molasses are particularly valid. As already mentioned at the beginning, Pretreatment of the molasses is not absolutely necessary, but it is preferable to do so.

According to one embodiment of the method according to the invention the molasses is first used to remove organic non-sugar components treated in the form of a precipitate. The precipitate is removed by an appropriate device, leaving behind a clarified molasses solution, largely from a coloration caused by these organic constituents is exempt.

Preferably, an iron compound, especially FeCl ^ or 1 ^ 2 (SO,) ^ added to the molasses solution. These ferric salts or corresponding other materials form complexes with the impurities in the molasses solution with the result that a flocculation is formed which settles on the bottom of the vessel and a large proportion of the organic non-sugar impurities carried away.

The degree of flocculation and removal of non-sugar / color organic matter mainly depends on the pH of the solution and its solids content. When using Iron compounds and a cane sugar molasses (black molasses) as added material result in flocculation or precipitation within a wide pH range on the order of about

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2.0 to about 9 * 0. The precipitation and removal of constituents from the molasses solution is achieved to varying degrees within this range. The most effective precipitation and discoloration or desirable coloration of the supernatant molasses can be reached in a preferred pH range of about 2.0 to _3} 0 and especially from about 2.1 to more than 2.5 "Since most molasses an initial pH -Value of about 5.5 to about 9jO, an adjustment of the pH is necessary in most cases before the addition of the flocculant. Corresponding acids, such as hydrochloric acid, are used for this purpose.

When using iron compounds as a precipitation additive, it was found that the molasses3 solution was relatively low in concentration should be to promote flake formation. Preferably the solids content of the molasses solution is below about 30 percent by weight and especially at about 5 to 25 percent by weight. Excellent discoloration can be achieved by using solutions with a solids content of 10 percent by weight below Use of iron (III) chloride or iron (III) sulfate.

The temperature of the molasses during clarification with iron (III) -

is ions is not critical. The temperature / however in terms of the viscosity of the molasses and a subsequent slight precipitation of organic spruce sugar components must be taken into account. A temperature range of about 15 to 82 ° C. and in particular (especially in the case of basic solutions) of

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about 71-82 ⁰ C. Mr acidic solutions is a preferred temperature range from about 15 to 49 ° C. The amount of additive used for the precipitation can vary widely and depends heavily on the utilization of the additive, the solids concentration of the molasses to be treated and the amount of organic impurities contained therein. In general, iron (III) compounds are used in an amount of 1 to 25 percent by weight, based on the solids content. At least 3 percent by weight and in particular 6 to 15 percent by weight for FeCl and about 22 percent by weight for Pe ₂ (SO,), are preferred. In general, the color of the supernatant molasses solution appears to improve with increasing amounts of the additive.

The precipitate obtained in the above-described step can be removed in any way. The procedure used depends to a certain extent on the used additive and on the type of precipitate formed. Filtration has proven beneficial. According to the preferred embodiment in which iron compounds are used as precipitating agents, after removing the aforementioned precipitate, the pH value for the precipitation of iron ions raised above 7jO. For example, is used for this purpose Calcium oxide or calcium hydroxide is used. It was found that a further precipitate forms and an additional one Discoloration occurs. An optimal pH range is about 7.5 to 8.6, and preferably about 8.1. In the -Solution remaining iron can by adding appropriate

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Materials such as inorganic phosphates, preferably sodium or calcium phosphates. Monocalcumin phosphate is preferred used. The amount of these materials necessary to remove a substantial amount of the iron can vary widely and can be easily determined by a person skilled in the art. For example, quantities from 2 to 6 result Weight percent monocalcium phosphate based on weight

in
of the solids in the solution, / a slightly basic medium a

almost complete removal of iron.

As it is desirable to use molasses solutions of relatively less To use solids concentration in this precipitation stage, a concentration can then be achieved, for example by evaporation, be made to a higher. To achieve solids content. Evaporation to around 60 Brix can create another Form a precipitate that can be removed in the usual way. If necessary, a further concentration can then be carried out be made.

In general, it is desirable to remove at least 90 percent of the color of the molasses solution. The aforementioned materials and conditions can be varied to achieve even greater discoloration, e.g., up to about 93 percent.

According to a further embodiment of the invention, which in particular for terminal molasses, preferably blackstrap, the molasses is centrifuged

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and then filtered. This results in an unexpectedly effective removal of non-sugar materials, such as ash and color bodies, even in the absence of chemical agents for precipitation, clarification or flocculation. However, the last-mentioned clarification processes are preferably used at the same time. Furthermore, black molasses with a density of more than 70 Brix can be successfully treated by the method according to the invention. When using molasses such a high density as Ausgangsmelassen it is generally necessary to heat the molasses before centrifugation at elevated temperatures, for example about 60 to about 82 ⁰ C to ·. In general, molasses with a density of less than about 45 ° Brix do not need to be heated as high.

Centrifugation also provides better separation than Usual precipitation processes using additives such as lime, lime and carbon dioxide, lime and sulfur dioxide or phosphoric acid, achieved with subsequent filtration. Such processes have also proven useful for low density black molasses proved largely unsuccessful.

In certain cases it was found that the addition of a Polyelectrolytes this previous separation by centrifugation is reinforced. Such materials are known and are commercially available, for example under the name "Separan".

The centrifugal force required for effective separation is easy to determine and is, for example, in the range of

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about 6,000 to about 15,000 grams, preferably about 8,000 to about 11,000 g.

The molasses solution clarified in this way is then applied to the ion exclusion resin put on, using the principle of ion exclusion is used to separate the molasses solution into the desired end products. The procedures described at the beginning to operate the exclusion column, to create a channel effect or others Avoiding flow disturbances can be applied to the individual systems as required. Generally such Techniques required when high density or viscosity sunt he differentiated between the applied material and the Elution medium 'exist.

According to the invention, the molasses pre-cleaned in the above manner is passed over an ion exclusion resin. The gate cleaning is important, since it has been found that in the presence of considerable amounts of materials, precipitate formation occurs are able to coat the ion exclusion resin with the precipitate, causing the resin in its Effectiveness in terms of preferential physical adsorption is significantly impaired. Thus, precaution should be taken v / ground that such impurities are essentially absent. If these impurities are not removed in the clarification stage, a subsequent suitable one should be used Removal action can be taken. Resins of the cation or anion type can be used as ion exclusion resin if-

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cation resins are equally preferred.

According to the invention it was found that the composition of the resin as well as the physical properties of the bed and the process conditions are important factors that influence the effectiveness of the molasses separation of around 8 percent for the separation of molasses, especially terminal or black molasses _? preferred. This degree of crosslinking, which is higher than the prior art generally suggests, gives the resin the desired strength. Such resins are commercially available, for example Dowex 50 Wx8. Another suitable exclusion resin is sold under the trade name Amberlite IR-120. Resins with a percent crosslinking of 4 to 8 percent can also be used successfully to treat molasses and other carbohydrate containing products. In general, a crosslinking of more than about 8 percent leads to a reduction in the flow rate which is too great for a large-scale industrial application.

by

As mentioned earlier, / becomes the ratio of height to diameter in the case of vertical, cylindrical columns in which the contact with the synthetic resin is made, the quality and effectiveness affected by the exclusion process.

For resin particle diameters of 20 to 50 mesh (U.S. Sieve; clear mesh size 0.841 to 0.297 mm) should be the ratio of

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Height to diameter are at least 1 and preferably 3 to 50. For particle sizes from 50 to 80 mesh (0.297 to 0.177 mm) the corresponding ratio is in the range from about 1 to about 20.

The flow rate at which the molasses runs through the bed of the exclusion resin should be adjusted so that an optimal separation results. Since this separation is the result of physical adsorption, the flow rate should not exceed the rate of adsorption of the sugar on the synthetic resin. For the aforementioned cation exclusion resins, the flow rate is preferably less than about 0.0024 liters / cm ² / min (0.60 gal / ft ² / min).

Subsequent to the molasses, water is added via the exclusion resin given. The relative ratio of this subsequent water to molasses can be varied within a wide range. The optimum conditions can be easily determined from the degree of removal of the component adsorbed by the synthetic resin and the Determine the concentration of the eluate. Preferably the volume of the subsequent water is at least about two times of the molasses volume and especially two to three times the molasses volume.

If the molasses is converted into monovalent directly on a cation exclusion resin Given form, it is found that the separation the added molasses may decrease over time,

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which is presumably due to the exchange of monovalent ions in the ion exclusion resin by calcium or other polyvalent ions. As soon as calcium or similar ions appear on the exchange tunnel, the composition of the synthetic resin changes and it loses its preferred adsorption capacity. Accordingly, molasses can first be "softened" by passing through an ion exchange column, calcium and other polyvalent ions being replaced by monovalent ions, for example sodium ions. When using cation exclusion resins, a preferred upstream exchange bed consists of Amberlite IR-120 when using a molasses of 82 C and 60 Brix or less. The exchange observed may be similar to that described in US Pat. No. 2,937,959. Higher flow rates than the ion exclusion stage can be used to perform the ion exchange process. For example, velocities from 0.004 to 0.008 liters / cm / min (1 to 2 gal / ft / min) or higher can be used. When using cation exclusion resins, the sugars in the molasses solution, such as sucrose, fructose and glucose, are adsorbed by the synthetic resin, while the highly ionizable salts are excluded and remain in the intermediate areas. Furthermore, some very large (high molecular weight) color bodies (organic and therefore not ionizable) are too large for adsorption on the resin and therefore remain in the surrounding liquid.

When water flows through the exclusion bed, a number of eluates occur which, according to their composition -

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and their elution time can be divided. In general The first eluate fraction appears to be a solution with less than about 1 percent by weight of sugar, the solids of which are to a large extent Partly or largely made up of ash (inorganic salts). Furthermore, color bodies appear in this fraction, the rom resin excluded due to their size. This fraction is suitable as a regeneration agent for the plasticizer resin. she can also be evaporated to a concentrated salt mixture and used as a fertilizer. Furthermore, from this Solution potassium salts are crystallized. The second eluate fraction is generally a dilute solution of the feed Molasses. This fraction can be recycled for further separation. Since this group is in its composition the Is similar to molasses, it can be evaporated and then fed to ruminants. Since the molasses only in relative If small amounts are obtained, the restrictions mentioned at the beginning do not play an excessive role in molasses feeding.

The third eluate fraction is a solution with a high sugar content and very low in ash and non-sugar organics. This faction can under Formation of a valuable sugar solution to be evaporated. If necessary, the removal of residual dyes can be used this group will be required.

The fourth fraction is a highly diluted sugar solution, which is particularly suitable for diluting starting molasses,

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where the prior precipitation or the ion exclusion process requires it. The final fraction consists essentially of colored Water and has little practical value ".

According to a further embodiment of the method according to the invention can not softened molasses solutions to carry out the separation via an exclusion resin, which is in divalent form present, be given. In this embodiment, the molasses are first mixed with a polar organic solvent, like ethanol, mixed. After removing the resulting precipitate, the supernatant molasses solution is directly on given an exclusion resin in the calcium form. In general a first eluate fraction is obtained, which contains large amounts of mineral salts and trace amounts of sugar, and a second fraction Eluate fraction; which contains large amounts of sugar and color bodies and is low in ash, and a third one Fraction consisting essentially of dilute alcohol.

According to a further embodiment of the method according to the invention The ion exclusion stage can be preceded by a membrane filtration of the molasses solution to remove the aforementioned high molecular weight Remove body of dye. In this way one obtains eluate from the ion exclusion column, which are relatively free of such dye bodies and can thus be directly supplied to their intended use. For this purpose, membranes can be used made of cellulose acetate can be used. For such ultrafiltrations, relatively dilute solutions are required, which

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for example less than about 4-0 Brix, preferably less than that than about 15 Brix. Conventional reverse osmosis equipment can be used on condition that the membrane is chosen so that there is sufficient permeability for the passage of at least one of the pesticide materials is available. Water can be used to flush such systems.

The ultrafiltration, which is preferably used before the ion exclusion treatment, can additionally also be used to clarify the carbohydrate fraction obtained from the exclusion column is used will.

According to the method described above, an eluate is obtained With a high content of mineral salts, especially potassium. This eluate is particularly suitable as a fertilizer. Furthermore, an eluate obtained that contains essentially pure sugar and when using terminal or black molasses as the starting material, in the Vv 'es borrowed the valuable properties of invert sugars having. Mixtures of salts and sugars, which are thus very similar to normal molasses, can be used directly as Feed are used. The initial molasses are expediently separated into products which, as far as possible, ever find use according to the respective needs, the amount of waste products is practically negligible.

The examples illustrate the invention.

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example 1

End molasses, which is obtained from cane sugar in the production of sugar, is used ("blackstrap molasses"). The final molasses is diluted to 10 ° Brix and, at a pH value of 2.5, 12 percent by weight (based on the solids) are added. The mixture is ^{heated to 71 °} C. and filtered. The pH of the supernatant is brought to 8.6 with 4 percent calcium oxide. It is then ^{heated to 71 °} C. and filtered. The solution is then adjusted to pH 4.7 with H-PO and filtered. Then 5 percent by weight of acid disodium pyrophosphate is added. The mixture is then left to stand for 5 minutes at 71 ^{° C. and then filtered.} The supernatant is treated with 5 percent KB carbon at 71 ^° C. for 5 minutes and filtered. This process results in a 97.3 percent discoloration of the molasses used.

Example 2

End molasses is diluted to 10 ° Brix and mixed with 18 percent by weight FeCl-z (based on the solids content). The solution is ^{heated to 71 °} C., filtered off, adjusted to pH 8.1 with calcium oxide and filtered again. 90 percent discoloration is achieved.

Example3

2032 g of blackstrap molasses with 10.5 ° Brix is heated at 71 ⁰ C with 11 weight percent (based on the solids content, 23.43 g)

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) .2 offset. Then 1 g (0.47 percent) calcium oxide and then 11 percent Fep (SO ~) are added. The solution is then adjusted to pH 2.5 with calcium oxide. The supernatant obtained after centrifuging the solution is ^{heated to 60 °} C. and brought to pH 8.1 with calcium oxide. Then it is centrifuged. 2 percent monocalcium phosphate is added to the solution obtained. The pH value is adjusted to 8.0 and the resulting mixture is centrifuged. About 90 percent discoloration is achieved.

Example 4

250 ml of final molasses are diluted to about 45 ° Brix and heated to 82 ° C. The molasses is centrifuged. The received Liquid is filtered through a paper filter in a Buchner funnel. The filtration is quick and very effective.

When the same molasses solution is filtered without centrifugation only 5 ml of filtrate is obtained before the filtration comes to a standstill. Similarly, if used, one obtains of lime in amounts that lead to pH values of 6.0, 6.5? 7.0 and 8.0 lead, no filtrate. Similarly, it receives unsatisfactory results when using phosphoric acid. When centrifugation is carried out, the supernatant obtained can in each case filter quickly.

Example 5

200 ml of terminal molasses (79.5 ° Brix) are heated to 82 ° C and at centrifuged about 11,000 g. A liquid is obtained from

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improved clarity and reduced viscosity. The ash content is about 30 percent lower by weight than in the original final molasses.

Example 6

A centrifuged and filtered molasses solution with a content of (in each case based on the dry components) 49 »7 percent by weight sucrose, 24» 0 percent by weight invert sugar, 10.0 percent by weight ash, 16.3 percent by weight organic non-sugar components, which have a pH of 5.1 has, is given in several experiments on an ion exclusion resin. The results are shown in Table I. In all experiments the molasses and water flow rates are 0.0016 liters / cm ² / min (0.40 gal / ft ² / m ±: a). The parliamentary group

1 is a colored liquid with a high ash content, which contains less than 1% by weight of sugar. The parliamentary group

2 consists of a dilute solution that has almost the same composition of dry components as the added one Having material. Fraction 3 contains a large amount of sugar and a small amount of ash and organic sugar components. Fraction 4 is a dilute sugar solution. Fraction 5 consists of wastewater. The realtives Ratios of added material and eluate fractions are given as bed volumes (B.V.). In all cases will the molasses with a temperature of 82 C and the water afterwards placed at a temperature of 71 C.

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Table I.

attempt Synthetic resin H / D Density of Inlet (B. .V.) 1 Eluate 4th 5 Parliamentary group 3 Br. attached
Materials material water 2 3 Ash ⁰ BrIx

* 2 * Amberlite
IR-120 50 3 ti 12th 098609 Dowex 50 WX8
(50-80 mesh) 14th

-O

Brix

Brix

-O

Brix

0.20

0.35 0.28

0.60 0.04 0.70 0.08 0.10 0.20 1.5 # 8.0

0.80 0.08 0.65 0.04 0.25 0.08 3.3 $ 6.0 0.64 0.08 0.53 0.08 0.03 0.37 0.6 ^ 7.0

The molasses on top has only been centrifuged.

** The volume of the eluates can be the total volume of the added liquid

because water that is already present in the resin is initially displaced.

cn

NJ • Ρ "»

CO

- 53 -

Example 7

Terminal molasses is diluted to 45 Brix, heated to 82 ° C, centrifuged and filtered. Then it is also at 82 ⁰ G and 45 ° Brix by passing a Katioiienaustausclierharz with Amberlite IR-I20 charged in the sodium form column at a flow rate of approximately 20 to 25 ml / min softened. The column diameter is 5.1 cm and the amount of resin is about 800 ml. The eluate is then placed on a 2.5 x 215 cm column charged with the ion exclusion resin of the trade name Dowex 50 Wx8. The flow rate is about 20 to 25 ml / min. This is followed by water with a similar flow rate. The volume ratio of added water to molasses is about 2.7: 1. The individual eluates are obtained in the following percentages:

First. Fraction (mainly salts) = 6 percent Second fraction (mixture of salts = 45 percent and sugars)

Third fraction (mainly sugar) = 49 percent

The third fraction is then passed through a granulated carbon (Pittsburgh-Activated-Type Cane-Cal). The eluate obtained in this way is passed through a column charged with Amberlite IRA 401 S to decolorize. The eluate is filtered and evaporated to about 67 to 68 ° Brix. Relative to the original In addition, the decolorization in the third fraction is 90 percent. In addition, 80 percent of the ashes have been removed.

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Example 8
The clarified molasses in Example 3 is passed through a reverse osmosis device to bring the Brix level to about 17

she
raise. Then you give / over a bed of granulated

Carbon. The solution is then evaporated to about 50 ° Brix and centrifuged. The remaining solution is then treated according to Example 7.

Example 9

About 500 ml of final molasses are diluted to 50 ° Brix and filtered. The filtrate is mixed with the same volume of ethanol (polar organic Solvent) mixed and left to stand for a short time. About 50 ml of a dark, viscous sludge settles, which is separated from the supernatant liquid.

The supernatant is passed through a column with a diameter of 5j1 cm and a resin content of 1160 ml, charged with Dowex 50 YfxS in the calcium form. The flow rate of the molasses is 20 to 22 ml per minute at a temperature of 82 ^° C.

After the resin is saturated with about 450 ml of molasses, will it elutes with water. The material initially eluted from the column has a high mineral content and traces of sugar. This is followed by a second fraction with a high sugar and a low mineral content. This faction is strongly colored. The third fraction has essentially the same composition

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like the molasses on top, but it is heavily diluted.

Example 10

68 kg of final molasses v / earth diluted to 50 ° Brix with 34 kg of water. The pH value is increased by adding 13 percent (percent by weight based on the solids) of a 50 percent iron (III) sulfate solution lowered to about 2.5. This mixture is then diluted to 16 ° Brix and left to stand overnight. The one with it The resulting clear supernatant is decanted off from the precipitate. Sodami, the supernatant is heated to about 71 C and over a 3 meter column with a diameter of 30 cm, the 77 kg of activated granulated carbon (about 70 percent of the column volume) contains, given. The flow rate is 95 liters per hour.

The product treated in this way is then based on 4 percent ( to the weight of the solids) disodium prophosphate added, warmed to 65 ° C and left to stand overnight. A precipitate forms, which makes up about 17 percent of the volume. The supernatant is removed. It contains 29 staining units per ml at £ 5000. The original final molasses contains comparatively 250 color units / ml.

Example H.

Apple juice with a temperature of 82 ⁰ C, a pH value of 3 _} 9,

one
a density of 11.5 Brix and / resistance of 450 ohms

diameter
through a column of 5.1 cm / containing 1160 ml of Amberlite

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XE-200 resin percolated in the sodium form. The flow rate is adjusted to 20 to 22 ml / min.

Applied volume:

Apple juice 0.39 bed volumes

Wash water 0.60 bed volumes

Volumes of the eluate fractions:

First fraction: waste product 0.15 bed volumes Second fraction: (back in the 0.31 bed volumes Cycle)

Third fraction: product 0.22 bed volumes

Fourth fraction: diluted 0.31 bed volumes of product

The third fraction with a Brix refractometer reading of 7 and a resistance of more than 1500 ohms is about a at 82 C. Given a bed of granulated carbon. The eluate obtained in this way is cooled to 43 ° C. and passed through a deionization column given the three parts of a strong anion resin (Amberlite IRA-401) in the hydroxide form and two parts of a strong one Cation resin (Amberlite IR-120) in the hydrogenprm contains.

The eluate is evaporated to 75 ° Brix. The preserved coal

hydrate solution is colorless. Their content of / organic salts is less than 0.01 percent.

The first fraction containing inorganic salts and colored components is discarded. The second faction will fed to the subsequent ion exclusion cycle. She knows the

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- 57 -

the same composition as the material supplied but slightly more water. The fourth fraction consists of a highly diluted product. It is evaporated to 15 ° Brix and returned to the cycle.

Example 12

Prune juice at a temperature of 82 ⁰ C, a pH of 3.8, a density of 18.2 ° Brix and a resistance of 185
Ohm is passed through a column 5 _} 1 cm in diameter that is 1160 ml
Amberlite XE-200 in the sodium form, percolates. the
Flow rate is set to 20 to 22 ml / min.

Applied volume:

Plum juice 0.39 bed volumes

Wash water 0.60 bed volumes

Volume of the eluate fractions:

First fraction: waste product 0.10 bed volumes Second fraction: (back to the '0.58 bed volumes Cycle)

Third fraction: product '0.22 bed volumes

Fourth fraction: diluted 0.09 bed volumes of product

The third fraction has a Brix refractometer reading of 7 »7 on. It is slightly yellow-brown in color and has a resistance of HOO ohms.

The first, second and third fractions are made in a similar fashion

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treated as in Example 11.

example

A whey solution having a Brix refractometer of 17.2, a resistance of 38 ohms and a pH of 5.1 is deproteinized by adjusting the pH with hydrochloric acid to 2.4 and heating to 82 ⁰ C. The material is centrifuged for 5 minutes at 2000 rpm and then filtered.

The deproteinized solution is passed through a 5j1 cm column at 82 ° C containing 1160 ml of Amberlite XE-200 in the matrium form percolated. The flow rate is set to 20 to 22 ml / min.

Applied volume:

Deproteinized liquid washing water

Volumes of the eluate fractions:

First fraction: waste product

Second fraction: (back in the cycle)

Third fraction: product Fourth fraction: diluted product

0.39 bed volumes 0.60 bed volumes

0.09 bed volumes 0.35 bed volumes

0.35 bed volumes 0.20 bed volumes

The third fraction has a Brix refractometer value of 5.6, a resistance of 150 ohms and a lactose content of 5 percent on.'

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The first, second and third fractions are treated in a manner similar to Example 11 ".

Example 14

Clarified molasses (clarified with ferric sulphate) of 8.4 ° Brix and a resistance of 99 ohms is passed through a column 5.1 cm in diameter containing 1160 ml of Amberlite XE-200 given in the sodium form. The temperature is 82 C. The flow rate is set to 20 to 22 ml / min.

Applied volume:

molasses

Wash water

Volumes of the eluate fraction:

First! Traction: waste product Second fraction: (back to the Cycle)

Third faction: product

Fourth fraction: diluted product

1.29 bed volumes 0.60 bed volumes

0.13 bed volumes 1.16 bed volumes

0.25 bed volumes, 0.35 bed volumes

The third fraction shows, based on the added material, a discoloration of 96 percent and a reduction in the ash content from 88 percent up.

Example 15

A hardwood sulphite liquor of 14.9 ° Brix and a resistance of 34 ohms is passed over a column measuring 5 _} 1 cm. Diameter with

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containing 1160 ml of Amberlite XE-200 in the sodium form
given. The temperature is 82 ^° C. The flow rate
is kept at 20 to 22 ml / min.

Applied volume:

Sulphite liquor x 0.39 bed volumes

Wash water '0.60 bed volumes

Volumes of the eluate fractions:

First fraction: waste product 0.05 bed volumes Second fraction: (back to the 0.50 bed volumes Cycle)

Third fraction: product 0.14 bed volumes

Fourth fraction: diluted 0.30 bed volund.na product

The third fraction has a high xylose content. in the
In comparison to xylose, inorganic components and lignosulfonates are present in low concentrations.

Example 16

Centrifuged and filtered final molasses at 40 ° Brix and 82 C is passed through a column with a diameter of 5.1 cm with
containing 1160 ml of Amberlite IR-118 in the ammonium form. The flow rate is maintained at 20 to 22 ml / min.

Applied volume:

Molasses 0.30 bed volumes

Wash water 0.60 bed volumes

Volumes of the eluate fractions:

First fraction waste product 0.08 bed volumes

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Second fraction: (back to the 0.50 bed volume cycle)

Third fraction: product 0.08 bed volumes

Fourth fraction: diluted 0.24 bed volumes of product

The third fraction has a Brix value of 7 and an ash content of 3.0 percent, based on the dry weight,

Example 17

Centrifuged and filtered blackstrap molasses with 40 ° Brix and 82 ⁰ C is percolated through 'a column of 15 * 2 cm diameter with a content of about 0.042 m Amberlite IR-118th The flow rate is kept at 0.38 liters / min.

Applied volume:

Molasses 0.14 bed volumes

Wash water 0.41 bed volumes

Volumes of the eluate fractions:

First fraction: waste product 0.04 bed volumes

Second fraction: (back into the 0.32 bed volume cycle)

Third fraction: product 0.14 bed volumes

Fourth fraction: diluted 0.05 bed volumes product

The third fraction shows the following values:

Brix refractometer value 9

Total sugar content (based on 89.3 percent on the dry ingredients)

Ash (based on the dry matter) 1.2 percent

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Organic non-sugar components 9.5 percent

(based on dry ingredients)

Color 30,000 mau

Example 18

Centrifuged and filtered terminal molasses at 32 ° Brix and 82 ° C is passed through a column with a diameter of 15 »2 cm containing 0.04-0M Amberlite XE-200 in the sodium form percolated. The flow rate is set to 0.38 liters / min.

Applied volume:

Molasses 0.36 bed volumes

Wash water 0.55 bed volume

Volumes of the eluate fractions:

First fraction: waste product 0.04 bed volumes

Second fraction: (back into the 0.63 Bettvoiumina cycle)

Third fraction: product 0.12 bed volumes

Fourth fraction: diluted 0.12 bed volumes of product

Example 19

68 kg of terminal molasses are treated with 4.4 kg of iron (III) sulfate, The Brix value is 17 and the pH value 3.2. The mixture will Left at 27 ° C for 24 hours. The supernatant obtained is placed on an ion exclusion column. The ash content of the applied solution is 11.8 percent, based on the solids content. But this solution becomes a column with 5 * 1 chi Diameter grading 1160 ml Amberlite XE-200 in

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given the ammonium form. The temperature is 27 ⁰ C. The
Flow rate is set to 20 to 22 ml / min.

Applied volume:

Molasses 0.39 bed volumes

Wash water 0.60 bed volumes

Volumes of the eluate fractions:

First fraction: waste product 0.13 bed volumes Second fraction: (back to the 0.45 bed volumes Cycle)

Third fraction: product 0.22 bed volumes

Fourth fraction: diluted 0.19 bed volumes of product

In relation to the originally applied material, the discoloration in the third fraction is 95 percent and the reduction of the ash content 85 percent.

Example 20

Corn molasses at 82 ° C. is passed through a column 5 »1 cm in diameter containing 990 ml of Amberlite IR-118 in the
Percolated sodium form. The flow rate is adjusted to 20 to ml / min.

Properties of the corn molasses on top:

Brix refractometer value 39 »2

Resistance 438 ohm
pH 4.7

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Applied volume:

Corn molasses 0.45 bed volumes

Wash water 0.70 bed volumes

Volumes of the eluate fractions:

First fraction: waste product 0.14 bed volumes Second fraction: (back in the 0.51 bed volumes Cycle)

Third fraction: product 0.30 bed volumes

Fourth fraction: diluted 0.20 bed volumes of product

The third fraction has a Brix refractometer reading of 22.4 a resistance of 2500 ohms and a D.E. from 85 to.

Example 21

The following materials are passed through an exclusion column with a diameter of 61 cm in the order given

and a content of 0.23 m Amberlite XE-200, (Flow rate 0.02 l / cmVmin):

Molasses (15 ° Brix) 0.11 bed volumes

Molasses (50 ° Brix) 0.055 bed volumes

Molasses (15 ° Brix) 0.055 bed volumes

V / ater 0.37 bed volumes

The following eluates are obtained:

Waste product 0.20 bed volumes

Recirculated product 0.25 bed volumes

Product 0.09 bed volumes

Diluted product 0.05 bed volumes

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Example 22

Terminal molasses with 10 ° Brix is made through a series of cellulose acetate membranes given to De Danske Sukkerfabrikker. The following results are obtained.

membrane
(Manufacturer
description) Eluate Flow rate
(ml / Sta.) Discoloration 865 3.02 430 95.6 800 6.28 1350 86.4 600 6.83 1890 83.2 500 7.98 2280 48.0

Example 23

189 liter final molasses (55 ° Brix) are heated to 82 ⁰ C and centrifuged at 6000th The color measurement of the liquid obtained shows a discoloration of 30 percent, based on the material used.

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Claims (16)

- 46 claims Process for the production of carbohydrates from materials containing carbohydrates using ion exclusion resins, characterized in that one a) the resin with a first portion of the carbohydrate containing Brings materials into contact, b) then the resin with a second portion of the carbohydrates containing material in contact, wherein the density of the second portion is less than the density of the first Share is c) then the resin is brought into contact with a dilute aqueous medium to elute the adsorbed material, and d) an eluate wins whose solids mainly consist of carbohydrates exist. 2. The method according to claim 1, characterized in that that before carrying out step a) the resin with a portion of the carbohydrate-containing material, the density of which is less than that of the first portion, brings into contact. 3. The method according to claim 1 and 2, characterized in that there is the carbohydrate-containing Material molasses used. 4-. Method according to claim 2, characterized in that that you have a first portion with a density 609850/1086 from about 45 to about 60 ° Brix and one used before stage a) Portion and a second portion with a density of about 10 to about 25 ° Brix is used. 5. The method according to claim 2 to 4, characterized in that that the temperature of the portion used before stage a) and the second portion is lower than that Temperature of the first portion selects. 6. The method according to claim 1 to 5, characterized in that there is a sulfonated resin as the exclusion resin Styrene-divinylbenzene copolymer used in the sodium form. 7. The method according to claim 4, characterized by packing the exclusion resin in a column whose height to diameter ratio is less than about 5: 1. 8. Process for the treatment of molasses with the production of valuable products, characterized in that that he a) Iron (IIl) ions are added to a molasses solution and the resulting Precipitation removed, b) the molasses solution treated in this way over an ion exclusion resin gives "on which the sugar is preferentially adsorbed from the solution", c) then gives V / water over the column and d) the eluate obtained in a first fraction, which is a large -609850/1086 Contains salt, a second fraction that contains a mixture of salts and sugars, and a third fraction that contains a contains a large amount of sugar, separates. 9. The method according to claim 8, characterized in that the molasses solution after the addition of the Iron (III) ions with a temperature of about 15 to about 50 ° C begins. 10. The method according to claim 8 and 9, characterized in that the iron (III) ions are removed from the molasses solution after the removal of the precipitate, wherein a phosphate-containing material is added to the molasses and then the pH of the molasses to above about 7.0 raises. 11. The method according to claim 8 to 10, characterized in that that the molasses after removing the precipitate before passing through the ion exclusion resin treated to remove high molecular weight materials, allowing the molasses to pass through a membrane filter. 12 * Process for the treatment of molasses with the recovery of valuable products, characterized in that he a) organic non-sugar components from a molasses solution removed with the formation of a precipitate, b) the molasses solution treated in this way over an ion exclusion resin, that for the preferential adsorption of sugar from the solution in '609850/1086 is able to go, the resin being made of a sulfonated Styrene-divinylbenzene copolymer with a crosslinking or a divinylbenzene content of at least 4 percent, c) then lets water go over the resin and d) the eluate obtained is separated into a fraction, the solids of which i -'- consist largely of salts, and a fraction, the solids of which are largely composed of sugars. 13. The method according to claim 12, characterized in that the density of the molasses, which one over the resin gives, chooses no greater than 60 ° Brix. 14. A method for treating molasses with the production of valuable products, characterized in that that he a) the molasses mixed with a polyelectrolyte and then subject to centrifugal force sufficient to ensure the separation of solids, b) a solution of the molasses treated in this way via an ion exclusion resin which is capable of preferential adsorption of sugar from the solution, c) then gives water over the resin and d) the eluate in a fraction containing mainly salts as solids contains, and separates into a fraction that mainly contains sugar as solids. 609850/1086 15. Process for clarifying molasses or molasses solutions, d a d Li 3 / c π £ e indicates that one is the molasses mixed with iron (III) ions and the resulting Nieaschlag removed, the molasses solution having a pH of about 2.0 to about 2.5 after the addition of the iron (III) ions, 16. Process for separating molasses into a number of valuable products, characterized that one gives an Ifelasselösu: "g over an ion exclusion resin, which is able to preferentially adsorb sugar from the solution, the Hars being made of sulfonated! Styrene-Diviny-Benzene-CopolyKorisat that contains at least about 4 percent divinylbenzene, then gives water over the resin and that the eluate obtained separates. S09850 / 1086