JP7214426B2 - Sugar solution refiner and refinement method - Google Patents

Description

TECHNICAL FIELD The present invention relates to a sugar liquid purification apparatus and purification method.

BACKGROUND ART A method using an ion-exchange resin is widely used in purification such as decolorization and desalting of a sugar solution such as a sucrose solution (see, for example, Patent Document 1). As a desalting treatment system for a sugar solution, a reverse system in which a sucrose solution is passed through an OH-type strongly basic anion exchange resin tower and an H-type weakly acidic cation exchange resin tower in order, and an OH-type strongly basic anion exchange resin. and H-type weakly acidic cation exchange resin mixed bed system, OH-type strongly basic anion exchange resin tower and mixed bed of OH-type strongly basic anion exchange resin and H-type weakly acidic cation exchange resin Systems such as those in which the liquid is passed through the columns in sequence are known.

The mixed-bed system, in which liquid is passed through a mixed-bed tower of OH-type strongly basic anion-exchange resin and H-type weakly-acidic cation-exchange resin, has excellent desalination performance, and since only one resin tower is required, the equipment was started up. The advantage is that the amount of dilute sugar solution (hereinafter sometimes referred to as “sweet water”) that is difficult to produce as a product, which is generated in the process of replacing the water in the resin tower with sugar solution, is reduced. There is However, the H-type weakly acidic cation exchange resin does not fully exhibit the ion exchange action of the functional groups unless it is in an alkaline atmosphere, and the sucrose solution at the entrance of the resin tower is neutral. The exchange capacity of the H-form weakly acidic cation exchange resin present in the upper part of the is not fully used up, leading to a decrease in throughput.

Japanese Patent Application Laid-Open No. 2002-238600

SUMMARY OF THE INVENTION An object of the present invention is to provide a sugar liquid purification apparatus and a purification method capable of improving throughput while maintaining the desalinization performance and amount of sweet water of a mixed bed system.

The present invention is a sugar liquid purification apparatus for purifying a sugar liquid, wherein a single bed layer of an anion exchange resin is placed above a mixed bed layer formed by mixing a cation exchange resin and an anion exchange resin. a packed resin tower ; after purification of the sugar solution, a cation exchange resin layer containing the mixed bed layer of the cation exchange resin, and the single bed layer of the anion exchange resin and the mixed bed layer in the resin tower; Separating means for separating and forming an anion exchange resin layer containing an anion exchange resin; Regenerating means for regenerating the cation exchange resin of the cation exchange resin layer and the anion exchange resin of the anion exchange resin layer; From the state in which the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin are separated, the regenerated cation exchange resin and the regenerated anion exchange resin are mixed to obtain a restructuring means for reconstituting a state in which the regenerated single bed layer of the regenerated anion exchange resin is filled above the formed regenerated mixed bed layer , wherein the reconstitution means reconfigures the regenerated regenerated Formed by mixing the regenerated cation exchange resin and the regenerated anion exchange resin in a state in which the regenerated cation exchange resin layer containing the cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin are separated. mixing means for forming a regenerated mixed bed layer; and agitating the regenerated cation exchange resin and the regenerated anion exchange resin in a portion of the upper portion of the regenerated mixed bed layer and placing the regenerated anion exchange resin above the regenerated mixed bed layer. a second separation means for separating into a state in which the regenerated single bed layer containing

Further, the present invention relates to a method for purifying a sugar solution, wherein a single bed of an anion exchange resin is placed above a mixed bed layer formed by mixing a cation exchange resin and an anion exchange resin. After purifying the sugar solution, in the resin tower, a cation exchange resin layer containing the cation exchange resin of the mixed bed and an anion exchange resin of the single bed and the mixed bed are used. a separation step of separating and forming the anion exchange resin layer containing the anion exchange resin of the bed layer; a regeneration step of regenerating the cation exchange resin of the cation exchange resin layer and the anion exchange resin of the anion exchange resin layer; From the state in which the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin are separated, the regenerated cation exchange resin and the regenerated anion exchange resin are separated. a reconstitution step of reconstituting in a state in which the reconstituted single bed layer of the reconstituted anion exchange resin is filled above and in contact with the reconstituted mixed bed layer formed by mixing; The regenerated cation exchange resin and the regenerated anion exchange resin are separated from the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin. a mixing step of forming a regenerated mixed bed layer formed by mixing the regenerated mixed bed layer; and a second separation step of separating into a state in which the regenerated single bed layer containing the regenerated anion exchange resin is packed .

INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide an apparatus and a method for purifying a sugar liquid, which can improve the throughput while maintaining the desalting performance and the amount of sweet water of a mixed bed system.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic configuration diagram showing an example of a sugar liquid purification apparatus according to an embodiment of the present invention, and a schematic diagram showing an example of an operation method of the sugar liquid purification apparatus. 1 is a schematic diagram showing an example of a method of operating a sugar liquid purification apparatus according to an embodiment of the present invention. FIG. 1 is a schematic diagram showing an example of a method of operating a sugar liquid purification apparatus according to an embodiment of the present invention. FIG. 1 is a schematic diagram showing an example of a method of operating a sugar liquid purification apparatus according to an embodiment of the present invention. FIG. 1 is a schematic diagram showing an example of a method of operating a sugar liquid purification apparatus according to an embodiment of the present invention. FIG. 4 is a graph showing electrical conductivity (μS/cm) versus anion-exchange resin-equivalent liquid flow rate (L/L-AER) in Example 1 and Comparative Example 1. FIG.

An embodiment of the present invention will be described below. This embodiment is an example of implementing the present invention, and the present invention is not limited to this embodiment.

FIG. 1 shows an outline of an example of a sugar liquid purification apparatus according to an embodiment of the present invention, and the configuration thereof will be described.

The sugar liquid purification apparatus 1 is an apparatus for purifying a sugar liquid, and is in contact with the upper part of a mixed bed layer 14 formed by mixing a cation exchange resin and an anion exchange resin. A resin tower 10 packed with a single bed layer 12 is provided.

In the refiner 1 of FIG. 1, a pipe 16 is connected to the liquid inlet of the resin tower 10, and a pipe 18 is connected to the liquid outlet. A collector 20 is installed at a predetermined position inside the resin tower 10 as a discharge means for discharging the liquid in the resin layer to the outside, and a pipe 22 is connected to the collector 20 . A distributor 24 is installed at a predetermined position inside the resin tower 10 as a stirring water supply means for supplying stirring water in an upward flow into the resin layer, and a pipe 26 is connected to the distributor 24 .

The method for purifying a sugar solution and the operation of the purifier 1 according to this embodiment will be described.

In the purification apparatus 1 of FIG. 1, the sugar solution to be purified is supplied from the upper part of the resin tower 10 through the pipe 16, and the single bed layer 12 of the anion exchange resin and the mixed bed layer 14 of the cation exchange resin and the anion exchange resin are provided. , and recovered as a refined sugar solution from the lower part of the resin tower 10 through the pipe 18, and subjected to purification such as desalination and decolorization (purification step).

In the sugar liquid purification method and purification apparatus 1 according to the present embodiment, the anion exchange resin tower is filled with the single bed layer 12 of the anion exchange resin above the mixed bed layer 14 of the cation exchange resin and the anion exchange resin. and a system in which liquids are passed through a mixed-bed tower of anion-exchange resin and cation-exchange resin in order. It is possible to improve the processing amount while maintaining the

When preparing a sugar solution purification apparatus filled with a single bed layer 12 of anion exchange resin in contact with the mixed bed layer 14 of such a cation exchange resin and anion exchange resin, after the ion exchange resin regeneration step, It has been difficult with conventional techniques to fill the single bed layer 12 of the anion exchange resin so as to be in contact with the mixed bed layer 14 of the cation exchange resin and the anion exchange resin. On the other hand, in the sugar solution purification method and purification apparatus 1 according to the present embodiment, as described below, the cation exchange resin and the anion exchange resin after the purification treatment are separated and regenerated, and the regenerated cation exchange resin and the regenerated anion are regenerated. By constructing a regenerated single bed layer of regenerated anion exchange resin above a regenerated mixed bed layer formed by mixing with exchange resin, the ion exchange resin can be reused.

After the purification step is completed, washing water is supplied from the upper part of the resin tower 10 through the pipe 16 and discharged from the lower part of the resin tower 10 through the pipe 18 to replace the sugar liquid in the resin tower 10 with water. Next, as shown in FIG. 2, the cation exchange resin layer 34 containing the cation exchange resin of the mixed bed layer 14 of FIG. 1 and the anion exchange resin and mixed bed of the single bed layer 12 of FIG. The layer 14 is formed separately from the anion exchange resin layer 32 containing the anion exchange resin (separation step). For example, washing water (backwash water) is supplied from the lower part of the resin tower 10 through the pipe 18 so that the cation exchange resin and the anion exchange resin flow, and is discharged through the pipe 16, so that the cation exchange resin and the anion exchange resin are separated. The anion exchange resin layer 32 containing the anion exchange resin having a low specific gravity is formed in a form of being agitated and in contact with the cation exchange resin layer 34 containing the cation exchange resin having a high specific gravity. By washing with this washing water (backwashing water), the sugar solution remaining inside the resin tower 10, the sugar solution adhering to the cation exchange resin and the anion exchange resin, etc. are removed. Here, the collector 20 is installed in the resin tower 10 so as to be below the separation plane between the anion exchange resin layer 32 and the cation exchange resin layer 34 .

The pipe 18 and the like for supplying backwash water function as separation means for separating and forming the cation exchange resin layer 34 and the anion exchange resin layer 32 in the resin tower 10 after purification of the sugar solution.

After the separation step is completed, the cation exchange resin of the cation exchange resin layer 34 and the anion exchange resin of the anion exchange resin layer 32 are regenerated (regeneration step). In FIG. 2, for example, the anion exchange resin regenerant is supplied through line 16 from the top of resin tower 10 through anion exchange resin bed 32 and discharged from collector 20 through line 22 . At this time, water is supplied from the lower part of the resin tower 10 through the pipe 18 so that the anion exchange resin regenerant does not come into contact with the cation exchange resin layer 34 as much as possible, and is discharged from the collector 20 through the pipe 22 together with the anion exchange resin regenerant. After that, washing water is supplied from the upper part of the resin tower 10 through the pipe 16 while water is being supplied from the lower part of the resin tower 10 through the pipe 18 , and discharged from the collector 20 through the pipe 22 , thereby remaining in the anion exchange resin layer 32 . Remove the anion exchange resin regenerant. Cation exchange resin regenerant is then fed through line 18 from the bottom of resin column 10 through cation exchange resin bed 34 and discharged from collector 20 through line 22 . At this time, water is supplied from the upper part of the resin tower 10 through the pipe 16 so that the cation exchange resin regenerant does not come into contact with the anion exchange resin layer 32 as much as possible, and is discharged from the collector 20 through the pipe 22 together with the cation exchange resin regenerant. Next, washing water and backwash water are passed from the top of the resin tower 10 through the pipe 16 and from the bottom through the pipe 18, respectively, and discharged from the collector 20 through the pipe 22 to wash with water.

The pipe 16 for supplying the anion-exchange resin regenerating agent, the pipe 18 for supplying the cation-exchange resin regenerating agent, and the like are regenerating means for regenerating the cation-exchange resin of the cation-exchange resin layer 34 and the anion-exchange resin of the anion-exchange resin layer 32. will function as

In this way, as shown in FIG. 3, a regenerated anion exchange resin layer 36 containing regenerated anion exchange resin is formed above and in contact with regenerated cation exchange resin layer 38 containing regenerated cation exchange resin. formed state.

After the regeneration process is completed, from the state in which the regenerated cation exchange resin layer 38 and the regenerated anion exchange resin layer 36 are separated, above the regenerated mixed bed layer formed by mixing the regenerated cation exchange resin and the regenerated anion exchange resin, , reconstituted into a state filled with a regenerated single bed layer of regenerated anion exchange resin (reconstitution step). In FIG. 3, for example, agitated water, gas such as air, etc., flows from the lower part of the resin tower 10 through the pipe 18. The regenerated cation exchange resin and regenerated anion exchange resin are agitated by supplying and discharging through pipe 16, and as shown in FIG. is formed (mixing step). Stirring of the regenerated cation exchange resin and regenerated anion exchange resin may be performed by vibration, stirring using a stirring device, or the like.

After the mixing step is completed, as shown in FIG. 4, for example, agitated water is supplied from the distributor 24 installed at a predetermined position in the regenerated mixed bed layer 40 through the pipe 26 to the regenerated cation exchange resin and the regenerated anion exchange resin above the distributor 24. is supplied in an upward flow so as to flow, and discharged through the pipe 16, the regenerated cation exchange resin and the regenerated anion exchange resin are agitated in a part of the upper part of the regenerated mixed bed layer 40, and as shown in FIG. , the regenerated single bed layer 42 containing a regenerated anion exchange resin with a low specific gravity is packed above the regenerated mixed bed layer 40 (second separation step) and reconfigured, and the purification shown in FIG. The same state as the apparatus 1 is assumed.

In the second separation step, the regenerated cation exchange resin and the regenerated anion exchange resin are agitated in a part of the upper portion of the regenerated mixed bed layer 40, and the regenerated cation exchange resin having a heavy specific gravity is contained in the upper portion of the regenerated mixed bed layer 40 and in contact therewith. A recycled cation-exchange resin single bed layer is formed, and a recycled single-bed layer (recycled anion-exchange resin single-bed layer) 42 containing a recycled anion-exchange resin with a low specific gravity is formed in contact with the upper portion of the recycled cation-exchange resin single-bed layer. It may be reconfigured separately. In this case, the apparatus for purifying the sugar liquid is filled with the regenerated cation exchange resin single bed layer in contact with above the regenerated mixed bed layer formed by mixing the regenerated cation exchange resin and the regenerated anion exchange resin, and the regenerated cation Above and in contact with the single bed of exchange resin is a resin tower filled with the single bed of regenerated anion exchange resin.

The pipe 18 for supplying agitated water and gas, the pipe 26 for supplying agitated water, the distributor 24, and the like are arranged to separate the regenerated cation exchange resin layer and the regenerated anion exchange resin layer from the state in which the regenerated cation exchange resin layer and the regenerated anion exchange resin layer are separated. It functions as a reconstituting means for reconstituting a state in which the regenerated single bed layer of the regenerated anion exchange resin is filled above the regenerated mixed bed layer formed by mixing with the exchange resin. Then, the piping 18 for supplying stirring water and gas is formed by mixing the regenerated cation exchange resin and the regenerated anion exchange resin from the state where the regenerated cation exchange resin layer 38 and the regenerated anion exchange resin layer 36 are separated. The pipe 26 for supplying stirring water, the distributor 24, etc. function as mixing means for forming the regenerated mixed bed layer 40, and agitate the regenerated cation exchange resin and the regenerated anion exchange resin in a part of the upper portion of the regenerated mixed bed layer 40. Then, it functions as the second separating means for separating the regenerated single bed layer 42 containing the regenerated anion exchange resin above the regenerated mixed bed layer 40 .

The anion exchange resin used in the mixed bed layer and the single bed layer includes a strongly basic anion exchange resin or a weakly basic anion exchange resin. It is preferable to use a strongly basic anion exchange resin because the decomposition into is accelerated. When the sugar solution is a sugar solution other than sucrose solution, a strongly basic anion exchange resin or a weakly basic anion An exchange resin may be used.

Examples of strongly basic anion exchange resins include Amberlite (registered trademark, hereinafter the same) IRA900, IRA400, IRA402BL, IRA404J, IRA458RF, Diaion (registered trademark) SA10A, SA11A, PA306, PA308 and the like. An anion exchange resin and the like can be mentioned. Examples of weakly basic anion exchange resins include Amberlite XE583 and Diaion WA-30.

Cation exchange resins used in the mixed bed layer include strongly acidic cation exchange resins and weakly acidic cation exchange resins. Exchange resins are preferred.

Examples of strongly acidic cation exchange resins include Amberlite FPC20. Examples of weakly acidic cation exchange resins include Amberlite FPC3500, IRC76, FPC76J, Diaion WK10, WK11, Dowex MAC-3 and the like.

As an anion exchange resin regenerating agent, a sodium hydroxide aqueous solution or the like is used.

Acids such as hydrochloric acid and sulfuric acid are used as the cation exchange resin regenerating agent.

The collector 20 is not particularly limited as long as it can discharge the liquid in the resin layer to the outside. The installation position of the collector 20 may be installed so as to be below the separation plane between the anion exchange resin layer 32 and the cation exchange resin layer 34 after the separation step.

The distributor 24 is not particularly limited as long as it has a structure capable of supplying stirring water in an upward flow into the resin layer. In the second separation step, the distributor 24 is installed so that agitated water can be supplied in an upward flow so that the regenerated cation exchange resin and the regenerated anion exchange resin are agitated in a portion of the upper portion of the regenerated mixed bed layer 40. It should be installed in a position where it is possible.

The sugar solution (raw sugar) to be refined includes sucrose solution, starch sugar, and the like. The method and apparatus for purifying a sugar solution according to this embodiment can be suitably applied to the purification of a sucrose solution.

EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples and comparative examples, but the present invention is not limited to the following examples.

<Example 1>
Using the sugar liquid purification apparatus 1 of the flow shown in FIGS. 1 to 5, after the completion of the regeneration operation, stirring water is passed from the distributor 24 in an upward flow to separate only the upper part of the regeneration mixed bed layer 40. By performing, from the top of the resin tower, a regenerated single bed layer of strongly basic anion exchange resin, a regenerated single bed layer of weakly acidic cation exchange resin, and a regenerated mixed bed of strongly basic anion exchange resin and weakly acidic cation exchange resin The treated liquid quality and treated amount were compared between the case of forming a layer (Example 1) and the case of not performing the separation operation by passing stirring water after the regeneration operation (Comparative Example 1). The ion exchange resin column was filled with 20 mL of regenerated H-form weakly acidic cation exchange resin (Amberlite IRC76) and 40 mL of regenerated strongly basic anion exchange resin (Amberlite FPA60).

(1) Purification step of sugar solution A sucrose solution raw material (Brix value 55.00%, electrical conductivity 146.3 µS/cm, color value 57) is passed through an ion-exchange resin tower at a liquid temperature of 45°C and a flow rate of 40 mL/h. 1000 mL was passed under the conditions to obtain a purified sucrose solution. As shown in FIG. 6, the conductivity (μS/cm) with respect to the amount of liquid passed (L/L-AER) in terms of the amount of anion exchange resin, when resin separation was performed by supplying stirring water after the regeneration operation (Example 1 ) was able to pass 22.5 times the amount of the anion exchange resin until the conductivity of the treatment liquid reached 2 μS/cm. On the other hand, when resin separation was performed by supplying agitated water after the regeneration operation (Comparative Example 1), the amount of liquid passing until the conductivity of the treatment liquid reached 2 μS/cm was converted to the amount of anion exchange resin. was 20.6 times the amount.

As described above, it was found that the purification apparatus configured as in Example 1 can improve the throughput while maintaining the desalination performance and the amount of sweet water of the mixed bed system.

1 refiner, 10 resin tower, 12 single bed layer, 14 mixed bed layer, 16, 18, 22, 26 piping, 20 collector, 24 distributor, 32 anion exchange resin layer, 34 cation exchange resin layer, 36 regenerated anion exchange resin layer, 38 regenerated cation exchange resin layer, 40 regenerated mixed bed layer, 42 regenerated single bed layer.

Claims (2)

A sugar solution refining device for refining a sugar solution,
a resin tower in which a single bed layer of an anion exchange resin is packed above a mixed bed layer formed by mixing a cation exchange resin and an anion exchange resin ;
After purification of the sugar liquid, a cation exchange resin layer containing the cation exchange resin of the mixed bed layer, an anion exchange resin containing the anion exchange resin of the single bed layer and an anion exchange resin of the mixed bed layer are placed in the resin tower. a separating means for separating and forming a layer;
regenerating means for regenerating the cation exchange resin of the cation exchange resin layer and the anion exchange resin of the anion exchange resin layer;
The regenerated cation exchange resin and the regenerated anion exchange resin are separated from the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin. a reconstituting means for reconstituting a state in which the regenerated single bed layer of the regenerated anion exchange resin is filled above the regenerated mixed bed layer formed by mixing the
with
The reconstruction means is
The regenerated cation exchange resin and the regenerated anion exchange resin are separated from the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin. a mixing means for forming a regenerated mixed bed layer formed by mixing
The regenerated cation exchange resin and the regenerated anion exchange resin are stirred in a part of the upper part of the regenerated mixed bed layer, and the regenerated single bed layer containing the regenerated anion exchange resin is filled above the regenerated mixed bed layer. a second separating means for separating;
A sugar solution refining device comprising : A sugar solution refining method for refining a sugar solution,
Using a resin tower filled with a single bed layer of an anion exchange resin above a mixed bed layer formed by mixing a cation exchange resin and an anion exchange resin ,
After purification of the sugar liquid, a cation exchange resin layer containing the cation exchange resin of the mixed bed layer, an anion exchange resin containing the anion exchange resin of the single bed layer and an anion exchange resin of the mixed bed layer are placed in the resin tower. A separation step of separating and forming a layer;
a regeneration step of regenerating the cation exchange resin of the cation exchange resin layer and the anion exchange resin of the anion exchange resin layer;
The regenerated cation exchange resin and the regenerated anion exchange resin are separated from the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin. a reconstitution step of reconstituting a state in which the regenerated single bed layer of the regenerated anion exchange resin is filled above the regenerated mixed bed layer formed by mixing the
including
The reconstruction step includes
The regenerated cation exchange resin and the regenerated anion exchange resin are separated from the regenerated cation exchange resin layer containing the regenerated cation exchange resin and the regenerated anion exchange resin layer containing the regenerated anion exchange resin. a mixing step of forming a regenerated mixed bed layer formed by mixing
The regenerated cation exchange resin and the regenerated anion exchange resin are stirred in a part of the upper part of the regenerated mixed bed layer, and the regenerated single bed layer containing the regenerated anion exchange resin is filled above the regenerated mixed bed layer. a second separation step of separating;
A method for refining a sugar solution , comprising :

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