JPH08117000A - Desalting purification apparatus of sugar liquid - Google Patents

Abstract

PURPOSE: To provide an apparatus for purifying suger solution, capable of efficiently producing high-purity prurified sugar solution. CONSTITUTION: This desalting purification apparatus for sugar solution is constituted by a plural layer beds type anion exchange tower 1 in the former stage composed of a Cl-based strongly basic anion exchange resin layer and an OH- based strongly basic anion exchange resin and a mixed bed tower 2 in the latter stage in which an OH-based strongly basic anion exchange resin is mixed with an H-based weakly acidic cation exchange resin and, in the apparatus, a raw sugar solution is passed through the plural layer beds type anion exchange tower in the former stage in the order of the Cl-based strongly basic anion exchange resin layer, the OH-based strongly basic anion exchange resin layer, and then passed through the mixed bad tower in the latter stage.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for desalting and refining a sugar solution, and more specifically, a double-layer bed type anion exchange of a Cl type strongly basic anion exchange resin and an OH type strongly basic anion exchange resin. The present invention relates to an apparatus for desalting and refining a sugar solution, which is characterized in that the tower is provided in front of the mixed bed tower.

[0002]

2. Description of the Related Art Conventionally, in the case of refining sugar solution, the raw sugar solution is first purified by means such as carbonation, granular activated carbon filtration, bone charcoal filtration, etc., and then ion exchange treatment is carried out to desalt and decolorize the sugar solution. Then, the sugar solution is refined.

As an ion exchange treatment mainly intended for decolorization, there is a method in which a sugar solution is passed through a single bed of a Cl type strongly basic anion exchange resin for decolorization.

On the other hand, as an ion exchange treatment mainly for desalting, the sugar solution is passed through an anion exchange column filled with an OH type strongly basic anion exchange resin to remove color and anionic impurities. After the removal, a so-called reverse type two-bed tower type purifying device for removing cationic impurities by passing through a cation exchange column filled with an H-type weakly acidic cation exchange resin is known, and is industrially known. Widely used.

Further, as a purifying apparatus mainly for desalting, a mixture of a OH type strong basic anion exchange resin and an H type weakly acidic cation exchange resin is used to pass a sugar solution through a mixing bed column. Floor type refining devices are known.

Further, as an improved type of the mixed bed type purification apparatus, the mixed bed of the OH type strongly basic anion exchange resin and the H type weakly acidic cation exchange resin is mixed and packed in the front stage,
A sucrose desalting and refining apparatus equipped with an anion exchange column filled with an OH-type strongly basic anion exchange resin is known (Japanese Patent Laid-Open No. 2-295499).

[0007]

However, although the conventional reverse type purification apparatus has the advantage that it is excellent in removing anionic impurities and has a large treatment amount, the treatment liquid pH of the weakly acidic cation exchange resin is the same as that of the passing liquid. Since the amount of treatment increases from a low start state as the amount of treatment increases, it is difficult to keep the pH of the treatment liquid constant and the purity of the treatment liquid is poor. In addition, the mixed bed type refiner has a drawback in that although the purity of the treatment liquid is excellent, the treatment amount is small.

An improved type of mixed bed type refining apparatus
The purification device described in Japanese Patent No. 295499 is superior in desalting performance as compared with the case of using a mixed bed type purification device alone, but it is decolorizing when treating a reduced sugar solution containing a large amount of coloring components. There is a drawback that it is a little dissatisfied with respect to.

Further, since the above-mentioned conventional production apparatus is not originally considered so as to cope with the fluctuation of the quality of the raw sugar solution such as the salt concentration and the pigment component concentration, when treating the raw sugar solutions having significantly different qualities, However, there is a drawback in that it is not possible to carry out a process corresponding to the fluctuation of the quality of the raw sugar solution.

The problem to be solved by the present invention is to solve the drawbacks of the conventional sugar solution refining apparatus, to efficiently obtain a purified sugar solution with high purity, and to deal with the fluctuation of the quality of the raw sugar solution. An object of the present invention is to provide an apparatus for purifying a sugar solution that can be used.

[0011]

As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that C
It was found that the sugar solution can be efficiently purified by using a multi-layer bed type anion exchange column of the l-type strongly basic anion exchange resin and the OH type strongly basic anion exchange resin, and the present invention is completed. I arrived.

That is, the present invention is a multi-layer bed type anion exchange column having a Cl type strongly basic anion exchange resin layer and an OH type strongly basic anion exchange resin layer in the former stage, and an OH type strongly basic anion in the latter stage. An apparatus for desalting and refining a sugar solution comprising a mixed bed tower in which an exchange resin and an H-type weakly acidic cation exchange resin are mixed, wherein a raw sugar solution is a Cl-type strong base for a preceding multi-layer anion exchange tower. The present invention relates to an apparatus for desalting and refining a sugar solution, which comprises passing an anionic exchange resin layer through an OH-type strongly basic anion exchange resin layer in this order, and then passing through a latter-stage mixed bed column.

Further, the present invention is characterized in that, in the multi-bed anion exchange column of the desalting and refining apparatus for sugar solution, at least one regenerant feeding / discharging means is provided in the middle of the anion exchange resin layer. The present invention relates to an apparatus for desalting and refining sugar solution.

FIG. 1 shows a schematic view of a sugar liquid desalting and refining apparatus of the present invention. The desalination purification apparatus of the present invention is provided with a multi-layer bed type anion exchange column 1 having a Cl type strong basic anion exchange resin layer in the upper part and an OH type strong basic anion exchange resin layer in the lower part in the preceding stage, and A mixed bed tower 2 of a basic anion exchange resin and an H-type weakly acidic cation exchange resin is provided in the subsequent stage.
In order to treat a sugar liquid using the sugar liquid desalting and refining apparatus of the present invention, a raw sugar liquid that has been pretreated in advance is transferred to the preceding multi-layer bed type anion exchange column 1 with a Cl-type strongly basic anion exchange. The resin layer may be passed through in a descending flow so as to come into contact with the OH-type strongly basic anion exchange resin layer in that order, and the treatment liquid may be passed through the mixed bed column 2 in the subsequent stage.

When the sugar liquid as a raw material is passed through the anion exchange tower 1 of the double-bed type in the preceding stage, first, the coloring component is mainly adsorbed in the upper Cl-type anion exchange resin layer, and then the lower OH.
Mainly anionic impurities (Cl ^-, SO ^2- _4, etc.) in the form anion exchange resin layer is adsorbed, OH ^- are exchanged with ions flows become alkaline. When the sugar solution becomes alkaline, the exchange reaction of the H-form weakly acidic cation exchange resin in the mixed bed column is likely to occur, and the desalination treatment amount in the mixed bed column is dramatically improved.

In the anion exchange resin tower of the multi-layer bed type in the preceding stage, in order to make the anion exchange resin a multi-layer bed of the Cl type strongly basic anion exchange resin layer and the OH type strongly basic anion exchange resin layer, the regenerant feed is used. By performing a regeneration treatment using an exchange column having at least one discharge means provided in the middle of the anion exchange resin layer, a multi-layer bed can be easily formed.

That is, an aqueous NaCl solution is supplied from a distributor provided above the anion exchange resin layer,
The whole anion exchange resin layer is discharged from the lower part of the exchange tower to once become a Cl type strongly basic anion exchange resin layer, and then a regenerant supply / discharge means provided in the middle of the anion exchange resin layer is used to supply N
By supplying the aOH aqueous solution and discharging it from the lower part of the exchange tower, the anion exchange resin layer below the regenerant supply / discharge means is O
An H-type strongly basic anion exchange resin layer can be used.

Further, an aqueous NaCl solution is supplied from a distributor provided above the anion exchange resin layer, and at the same time, an aqueous NaOH solution is supplied from a lower portion of the exchange tower, and a regenerant feeding / discharging means provided in the middle of the anion exchange resin layer supplies Na.
By discharging Cl aqueous solution and NaOH aqueous solution,
The anion exchange resin layer above the regenerant feeding / discharging means may be a Cl type strongly basic anion exchange resin layer, and the lower anion exchange resin layer may be an OH type strongly basic anion exchange resin layer.

Further, by providing two or more regenerant supply / discharge means and changing the supply / discharge position of the regenerant, the layer heights of the Cl type strongly basic anion exchange resin and the OH type anion exchange resin can be changed. it can.

By changing the layer height of the Cl type strongly basic anion exchange resin and the OH type anion exchange resin, a high-quality and stable purified sugar solution can be obtained even if the purity and color value of the raw sugar solution change. be able to. That is, when the salt concentration of the raw sugar solution is higher than the dye component concentration, the OH-type strongly basic anion exchange resin is regenerated so as to increase the layer height, and the sugar having a higher dye component concentration than the salt concentration is used. When processing the liquid,
The Cl type strong basic anion exchange resin may be regenerated so as to increase the layer height. Furthermore, when the dye component concentration of the raw sugar solution is relatively low and the salt concentration is high, the ion exchange resin of the multi-bed anion exchange column is entirely regenerated into the OH type strongly basic anion exchange resin, and conversely the raw sugar is regenerated. When the salt concentration of the liquid is low and the dye component concentration is high, all of the anion exchange resin is C
It is also possible to regenerate the l-form strongly basic anion exchange resin for treatment.

The ion exchange resin packed in the multi-layer bed type anion exchange column is not particularly limited as long as it is a strongly basic anion exchange resin. For example, Amberlite (registered trademark,
The same applies hereinafter) IRA-402BL. IRA-411S, X
T-5007, Diaion (registered trademark, the same applies below) P
A312 can be illustrated.

The mixed bed column used in the latter stage of the apparatus for desalting and purifying sugar solution of the present invention is a mixture of an OH-type strongly basic anion exchange resin and an H-type weakly acidic cation exchange resin, and packed in the ion exchange column. Examples of the H-form weakly acidic cation exchange resin include Amberlite IRC-76 and IR.
C-50, Levatit (registered trademark) CNP-80, Diaion KW11, etc. can be used. Also, O
As the H-type strongly basic anion exchange resin, the same anion exchange resin as used for the above-mentioned multi-layer bed type anion exchange or the like can be used.

In the sugar liquid desalting and refining apparatus of the present invention, an OH type strongly basic anion exchange resin and H which are packed in a mixed bed tower are used.
The mixing ratio with the weakly acidic cation exchange resin is preferably 2: 1 by volume ratio, but depending on the ratio of addition to the ion exchange resin, it is 0.3 to 2 with respect to the OH strong basic anion exchange resin 1. You may fill H type weakly acidic cation exchange resin in the range.

[0024]

【Example】

Example 1 FIG. 2 shows one embodiment of the apparatus for desalting and refining sugar solution of the present invention.

The sugar solution desalting and refining device of the present invention is a desalting and refining device having a multi-bed anion exchange column 1 in the front stage and a mixed bed column 2 in the rear stage. In the multi-bed anion exchange tower 1,
The lower part is filled with an OH type strong basic anion exchange resin, and the upper part is filled with a Cl type strong basic anion exchange resin. Cl type strongly basic anion exchange resin and OH
The regenerant feeding / discharging means 8 is provided at the interface with the strongly basic anion exchange resin. A distributor 4 for supplying the raw sugar solution is provided at the top of the tower, and a distributor 6 for supplying a regenerant is provided near the upper portion of the anion exchange resin layer 9. In the mixed bed tower 2 in the latter stage, OH
Form B of strongly basic anion exchange resin and Form H of weakly acidic cation exchange resin are mixed and filled.

The raw sugar solution is passed through the raw material supply pipe 3 to the strongly basic anion exchange resin layer 9 by the distributor 4. The raw sugar solution first passes through the Cl type strong basic anion exchange resin layer to be decolorized, and then passes through the OH type strong basic anion exchange resin layer to remove anionic impurities. The treatment liquid passes through the outflow pipe 10 and the mixed bed tower 2
Is passed through the mixed bed layer in which the OH-type strongly basic anion exchange resin and the H-type weakly acidic cation exchange resin are mixed by the distributor 12 in the upper part of the above, and further decolorization and desalting are performed. The desalted refined sugar solution is discharged from the processing solution outflow pipe 14.

In order to regenerate the strongly basic anion exchange resin of the double bed anion exchange column shown in FIG. 2, the following method can be adopted.

The NaCl aqueous solution supply pipe 5
To the inside of the anion exchange tower 1 through the distributor 6, and after passing through the anion exchange resin layer 9, the regeneration waste liquid is discharged from the regeneration waste liquid discharge pipe 11. By this operation, all the strongly basic anion exchange resins in the anion exchange tower 1 become Cl type.

Next, from the NaOH aqueous solution supply pipe 7, NaO
The H aqueous solution is supplied and passed through the Cl type strongly basic anion exchange resin layer below the regenerant feeding / discharging means (distributor) 8 to be regenerated into the OH type. The recycled waste liquid is discharged from the recycled waste liquid discharge pipe 11.

By this regeneration treatment, the strongly basic anion exchange resin above the regenerant feeding / discharging means 8 becomes the Cl type, and the strongly basic anion exchange resin below the feeding / discharging means 8 becomes the OH type, and the multi-layer bed It can be an anion exchange column.

FIG. 3 is a view for explaining another regeneration treatment method, in which a regeneration waste liquid collector 1 is used as a regenerant supply / discharge means.
6 is provided. At the same time as supplying the NaCl aqueous solution from the NaCl aqueous solution supply pipe 5 through the distributor 6, the NaOH aqueous solution is made to flow from the lower part of the anion exchange column 1 through the NaOH aqueous solution supply pipe 15 in an ascending flow, and the regeneration waste liquid is collected in the collector 16 and the regeneration waste liquid is collected. It is discharged from the discharge pipe 17. By this regeneration treatment, the anion exchange resin above the collector 16 can be regenerated to the Cl type and the lower anion exchange resin to the OH type.

Example 2 FIG. 4 is a diagram showing an example of a double-layer bed type anion exchange column in which the bed height of the Cl type strong basic anion exchange resin and the OH type strong basic anion exchange resin can be changed. .

FIG. 4A shows a distributor 8 as a regenerant supply / discharge means in the middle of the anion exchange resin layer 9.
A and 8B are provided, and FIG. 4 (B) is provided with collectors 16A and 16B as regenerant supply / discharge means. Others are the same as those in FIG. 2 and FIG. 3, and thus description thereof will be omitted.

In the regeneration operation of the anion exchange column of this example, first, an NaCl aqueous solution is introduced into the anion exchange column 1 from the NaCl aqueous solution supply pipe 5 through the distributor 6 in the same manner as in Example 1, and the anion exchange resin layer 9 is supplied. After passing through, the regenerated waste liquid is discharged from the regenerated waste liquid discharge pipe 11. By this operation, all the strongly basic anion exchange resins in the anion exchange tower 1 become Cl type.

In the case of changing the layer height of the strongly basic anion exchange resin of OH type and Cl type by using the apparatus of FIG. 4 (A),
When it is desired to increase the layer height of the OH type strongly basic anion exchange resin, after the operation of regenerating to the Cl type is completed, the upper 8A
NaOH solution is supplied from the distributor of
When it is desired to increase the layer height of the l-type strongly basic anion exchange resin, an NaOH aqueous solution may be supplied from the lower distributor 8B.

In the case of changing the layer height of the strongly basic anion exchange resin of OH type and Cl type by using the apparatus of FIG. 4 (B),
When it is desired to increase the layer height of the OH type strongly basic anion exchange resin, the NaCl aqueous solution is supplied from the NaCl aqueous solution supply pipe 5 through the distributor 6, and at the same time, NaO is added.
The H aqueous solution is made to flow from the lower part of the anion exchange tower 1 through the NaOH aqueous solution supply pipe 15 in an ascending flow, the regeneration waste liquid is collected in the upper collector 16A and discharged from the regeneration waste liquid discharge pipe 17, and the Cl type strong basic anion exchange resin is discharged. When it is desired to increase the bed height, the recycled waste liquid may be discharged from the lower collector 16B.

In the multi-layer bed type anion exchange column shown in FIGS. 2 to 4, the strong basic anion exchange in the column is performed in order to process the raw sugar solution having a high pigment component concentration but a relatively low salt concentration. When it is desired to pass all the resin in the Cl form to pass the liquid, the following may be performed. That is, in the anion exchange tower of FIGS. 2 and 4 (A), a NaCl aqueous solution is made to flow into the tower from the distributor 6 and passed through the anion exchange resin layer 9, and then the recycled waste liquid is discharged from the recycled waste liquid discharge pipe 11. Therefore, the anion exchange resin in the column may be entirely converted to the Cl form and then directly supplied to the treatment of the sugar solution. Further, in the anion exchange column of FIGS. 3 and 4 (B), As in the case of the anion exchange column of (A), an exhaust pipe (not shown) for the regeneration waste liquid is provided in the lower part of the column, and the NaCl flowed through the distributor 6
By discharging the aqueous solution from this discharge pipe, all of the anion exchange resin in the column can be converted to the Cl type.

Contrary to the above, when it is desired to pass all the strongly basic anion exchange resin in the column in the OH form in order to process the raw sugar solution having a high salt concentration but a relatively low dye component concentration, Can flow all the anion exchange resin in the tower into the OH type by flowing the NaOH aqueous solution from the distributor 6 instead of the NaCl aqueous solution.

Example 3 An anion exchange column (A) was used in the first stage and a mixed bed column (MB column) was used in the second stage.
The desalting and purifying apparatus of No. 1 was filled with the ion exchange resin shown in Table 1, and the raw sugar solution (sugar concentration: Bx50.9, salt concentration (electrical conductivity): 160 μS / cm, color value: CI150) was changed to 4
The liquid was passed under the conditions of 0 ° C. and 300 ml / h. As the strongly basic anion exchange resin in Table 1, Amberlite IRA-402BL was used in all cases, and as the weakly acidic cation exchange resin, Amberlite IRC was used.
-76 was used.

[0040]

[Table 1]

When the sugar solution was treated under the above conditions, the color value and salt concentration of the treatment solution were measured by the following methods and the results are shown in FIG.
As shown in FIG.

Salt concentration: Electrical conductivity was measured and used as an index of salt concentration.

Color value: The absorbance (OD) at 420 nm and 720 nm was measured using a 5 cm cell and calculated by the following calculation method.

[0044]

[Equation 1]

As is clear from the results shown in FIGS. 5 and 6, the sugar solution desalting and refining apparatus of the present invention has a flow rate of 200.
Even if it exceeded 0 ml, the color value and the salt concentration were low, and a satisfactory refined sugar solution was obtained. However, the apparatus provided with the single bed column of the Cl type strongly basic anion exchange resin of Comparative Example 1 in the preceding stage was When the volume of the solution passed exceeded 1000 ml, both the color value and the salt concentration increased, and a satisfactory refined sugar solution could not be obtained. Also, O
Comparative Example 2 in which an H-type strongly basic anion exchange resin was provided in the preceding stage
Although the device of No. 1 had a better desalting ability than the purification device of the present invention, the color value was about twice as high as that of the device of the present invention at the initial stage of liquid passing, and the decolorization effect was inferior.

[0046]

INDUSTRIAL APPLICABILITY The apparatus for desalting and refining a sugar solution of the present invention exerts an excellent effect on decolorization and desalting of a sugar solution, and even if the salt concentration and color value of the raw sugar solution are varied, Since the layer height of the OH type strongly basic anion exchange resin and the Cl type strongly basic anion exchange resin of the layer bed type anion exchange tower can be changed, a stable purified sugar solution can be obtained.

[Brief description of drawings]

FIG. 1 is a schematic view of a sugar liquid desalting and refining apparatus of the present invention.

FIG. 2 is an explanatory view showing an embodiment of a sugar solution desalting and refining device of the present invention.

FIG. 3 is an explanatory view of a double-layer bed type anion exchange column in the sugar liquid desalting and refining device of the present invention.

4 (a) and 4 (b) are explanatory views showing another embodiment of the multi-layer bed type anion exchange column.

FIG. 5 is a graph showing the relationship between the color value of the purified sugar solution and the passing amount.

FIG. 6 is a graph showing the relationship between the salt concentration of the purified sugar solution and the passing amount.

[Explanation of symbols]

1 Multi-layer bed type anion exchange tower 2 Mixed bed tower 3 Raw material supply pipe 4 Distributor (for raw sugar solution) 5 NaCl aqueous solution supply pipe 6 Distributor (for NaCl aqueous solution) 7 NaOH aqueous solution supply pipe 8, 8A, 8B Regenerant supply / discharge Means (Distributor) (for NaOH aqueous solution) 9 Anion exchange resin layer 10 Outflow pipe 11 Regeneration waste liquid discharge pipe 12 Distributor 13 Mixed resin 14 Treatment liquid outflow pipe 15 NaOH aqueous solution supply pipe 16, 16A, 16B Regeneration waste liquid collector 17 Regeneration waste liquid discharge tube

Claims (2)

[Claims] 1. A multi-layer bed type anion exchange column comprising a Cl type strongly basic anion exchange resin layer and an OH type strongly basic anion exchange resin layer in the former stage, and an OH type strongly basic anion exchange resin and H in the latter stage. A desalting and refining apparatus for a sugar solution comprising a mixed bed tower mixed with a weak acidic cation exchange resin, wherein the raw sugar solution is a Cl-type strongly basic anion exchange resin for a preceding double-layer bed type anion exchange tower. An apparatus for desalting and refining a sugar solution, characterized in that the layers are passed through an OH type strongly basic anion exchange resin layer in this order, and then through a latter-stage mixed bed column. 2. The desalting and refining apparatus for sugar liquid according to claim 1, wherein in the multi-layer bed type anion exchange tower, at least one regenerant supply / discharge means is provided in the middle of the anion exchange resin layer. .