Process for demineralizing a sugar solution

Sugar – starch – and carbohydrates – Processes – Carbohydrate manufacture and refining

Reexamination Certificate

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Reexamination Certificate

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06224683

ABSTRACT:

The present invention relates to a process for demineralizing a beet sugar solution before sugar “boiling” (hereinafter referred to as “boiling”). Herein, the term “beet sugar solution before boiling” is intended to mean not only a beet sugar solution before first boiling but also a beet sugar solution (molasses or the like) before boiling in the case where a residue after boiling (i.e., molasses) is to be subjected again to boiling, and to encompass those in cases where an ion exchange step and/or a concentration step, if necessary, is taken after the demineralization step according to the present invention and before the boiling step, and should not necessarily be construed as being limited to those in cases where the boiling step is taken later.
BACKGROUND ART
There are various conventional methods of refining sucrose (beet sugar) abstracted from sugar beet, representative examples of which include the following methods having respective merits and demerits.
A method (1) is one comprising sugar beet cutting, extraction, carbonation (coagulation and sedimentation for removal of impurities through adsorption thereof on a precipitate of calcium carbonate during formation of the precipitate by adding lime milk to raw juice obtained by extraction and blowing carbon dioxide therein), filtration, softening (removal of hardness components such as Ca and Mg with cation exchange resin in Na form), concentration, and boiling (boiling sucrose crystals out of the concentrate through crystallization). This method is simple because no demineralization is done although softening is done, but involves demerits of poor sucrose crystallization during the boiling step and hence formation of a large amount of molasses because of an insufficient sucrose purity of the sucrose-containing concentrate as the object of boiling.
A method (2) is one comprising the same sugar beet cutting, extraction, carbonation and filtration as in the method (1), and further comprising subsequent softening and demineralization by ion exchange treatment (removal not only of hardness components such as Ca and Mg but also of other salt components), concentration, and boiling. Use of the following four kinds of ion exchange resins: a strongly acidic cation exchange resin, a weakly basic anion exchange resin, a strongly basic anion exchange resin and a weakly acidic cation exchange resin in this order is best for the ion exchange treatment in this method. This method does not involve the demerits of the method (1), but involves demerits of frequent regeneration of the ion exchange resins, use of large amounts of regenerants, and various troublesome treatments of regeneration waste because much salts are contained in sucrose-containing filtrate as the object of ion exchange treatment to decrease the throughput per unit quantity of the ion exchange resins. In view of much salts as mentioned above, decomposition of sucrose by the cation exchange resin in the hydrogen ion form (H form) in the first stage of ion exchange treatment must be avoided by cooling the above-mentioned sucrose-containing filtrate once to at most 10° C. for the treatment thereof with the cation exchange resin in the H form (so-called cold process demineralization), and the resultant treated solution must be heated up to a temperature of 50 to 55° C. for the second stage of ion exchange treatment thereof (polishing for demineralization, decoloration, deodorization, etc.), thus giving rise to demerits of complexity of operations and large energy costs.
A method (3) is a recently proposed one comprising filtration, softening, concentration, demineralization by ion exclusion chromatographic separation, concentration, and boiling without carbonation after the same extraction as in the foregoing 2 methods (PCT International Publication No. WO 95/16794). This method, which does not involve the demerits of the method (2) but indispensably requires filtration in order to avoid clogging of a chromatographic separator and an increase in the pressure loss therethrough (no details of filtration are described in the above-mentioned patent literature), involves demerits such as an incapability of removal of sticky substances derived from the plant (beet) and called “gum” as well as colloidal substances, a difficulty in filtration, a great cost involved in the filtration step, so grave a pressure loss in chromatographic separation due to colloidal substances unremovable by filtration as to result in a failure in liquid passage through the chromatographic separator in an extreme case, an unavoidable decrease in the feed rate of a starting solution (starting chromatographic solution) as an object of chromatographic separation for decreasing the pressure loss in the chromatographic separation operation, and a failure in obtaining such high-quality sucrose crystals as in the method (2) due to insufficient demineralization. The cause of all such demerits is that the coagulation and sedimentation step such as the carbonation step is not taken.
Demineralization of a beet sugar solution before boiling according to such ion exchange treatment or chromatographic separation is aimed at improving the quality of sucrose crystals precipitated by later boiling. Further, sucrose is recovered as much as possible by repeating demineralization (by ion exchange or chromatographic separation), concentration, and boiling of molasses obtained after boiling.
Ion exchange resins used in demineralization by such conventional ion exchange as in the method (2) must be subjected to the regeneration step at a certain point of time. Regenerant chemicals for use in this step and washing water for use in the subsequent washing step pose a problem of raising the cost of demineralization. Further, various treatments of regeneration waste discharged in the regeneration and washing steps are so troublesome as to raise the product cost. On the other hand, when demineralization is done by chromatographic separation like in the method (3), the throughput is limited if a high separability of components is to be attained, with the result that the separator must inevitably be scaled up to pose a problem of a high construction cost thereof. In chromatographic separation, sucrose as the desired component is diluted with eluent water to pose another problem of raising the running cost of the later concentration step. Still another problem is a loss of the desired component (sucrose) involved in separation.
An object of the present invention, which has been made in view of the foregoing problems of the prior art technologies, is to provide a process for efficiently demineralizing a beet sugar solution before boiling.
DISCLOSURE OF THE INVENTION
As a result of extensive investigations on demineralization of a beet sugar solution before boiling according to simulated moving bed chromatographic separation with a view to solving the foregoing problems, the inventors of the present invention have found operating conditions under which a sucrose fraction having as high a sucrose concentration as possible can be obtained with a throughput increased substantially at least two times as much as the general one in conventional simulated moving bed chromatographic separation while maintaining a high separation performance and diminishing the loss of sucrose as the desired component and the amount of used eluent water as much as possible.
More specifically, the inventors of the present invention have found out that the loss of sucrose as the desired component can be decreased to at most 0.7%, the throughput (throughput per hour, based on whole chromatographic packing) can be increased to at least 7 vol. %, and the dilution ratio of the desired component (value calculated by dividing the sucrose concentration of a chromatographically separated sucrose fraction by the sucrose concentration of a beet sugar solution subjected to chromatographic separation) can be lowered to less than 2 by feeding a starting solution and eluent water at a starting solution/eluent water volume ratio of 1/2.5 to 1/3.5, withdrawing fractions at a stro

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