JPH01109000A - Method for treatment of beet solution - Google Patents

Abstract

PURPOSE: To separate and collect sucrose as well as useful substances such as inositol and raffinose by passing sugar beet molasses through molasses-boiling and desalting step and chromatographic separation step.

CONSTITUTION: Sugar beet molasses is separated into beet sugar and beet molasses by boiling. The resultant boiled beet molasses is passed through H type cation exchange resin and OH type anion exchange resin in molasses-boiling and desalting step to remove betaine and salts. Then, the resultant desalted solution is separated into inositol-rich, sucrose-rich and raffinose-rich fractions, by chromatographic separation step. In the chromatographic separation step, the front and rear ends of a bed packed by using sodium type or potassium type cation exchange resin as an absorbent are connected by fluid passage and fluid is made to communicate from the front end of the packed bed to the direction of the rear end and circulated.

COPYRIGHT: (C)1989,JPO

Description

[Detailed description of the invention] [Industrial application field] The present invention relates to a method for treating sugar beet liquid.

Specifically, the present invention aims to recover sugar and separate useful substances such as inositol and raffinose by separating silica and other useful substances present in sugar beet molasses using chromatography techniques. The present invention relates to a method for processing a sugar beet solution, which comprises collecting the sugar beet solution.

[Conventional technology]

Conventionally, the method for producing beet sugar from sugar beets is as shown in 1+g: extract sugar beet liquid using a leaching bath, clean it by carbonation, decolorize it with an ion exchange resin, and select it. The resulting sugar juice is a-condensed to around B140 to obtain concentrated juice, and the concentrated juice is roasted with sugar (A-flanked sugar) to obtain product sugar. As A molasses, the sugar is again roasted (B roasted sugar) to obtain B sugar and B molasses. For this B sugar, dissolve it, return it to the concentrated juice, and re-add A.
7i [In the sugar process, boil sugar.

On the other hand, B molasses is diluted before and after BxJO, and then mixed with a cation exchange resin such as Diaion PK220 and Diaion 11.
Then betaine and salt are removed using an anion exchange resin such as No. 30 to obtain a desalted solution.

A portion of the desalted solution is compressed and dried to obtain sugar beet sucrose, while the other portion is returned to the cleaning process to recover the sugar.

Beet molasses sugar is used as a flavorful sweetener because it contains various components found in molasses, and as a health food because it contains 7% or more of raffinose.

[Problem that the invention seeks to solve]

However, the problem with this production method is that although it is desirable to have as much raffinose content as possible in the beet sugar, the raffinose content becomes too thick and the recovery of the beet sugar is inhibited. The limit seems to be 5-4%.

On the other hand, the present inventors invented a method for easily and efficiently separating multiple organic compounds into three fractions using a chromatographic separation method, and previously filed a patent application (Japanese Patent Application No. 47-30
7/2J issue).

Therefore, in order to solve the above problems, the present inventors separated the desalted solution into high-purity siliceous sugar fraction and raffinose using the above-mentioned chromatographic separation method. We thought that a method of separating the i1-treated fraction and other fractions would be effective and conducted a test.

As a result, if the chromatographic separation method described above is used, even if a desalted solution with a low raffinose content is used (i.e., in a state where it is easy to boil sugar), sugar beet nectar with any raffinose content within the range of It was discovered that while sugar can be obtained, high-purity inositol powder and liquid sugar with high utility value can be obtained as by-products from other fractions by simply concentrating and crystallizing them. completed.

(See Figure 2) [A rounding means to solve the problem] Generally, when a beet sugar solution is chromatographed using a Na-type or Ni-type strongly acidic cation exchange resin as an adsorbent, the following flow occurs in the following order.

(1) Ash (inorganic salts) (2) Polysaccharides and their derivatives (3) Raffinose and other Jlis (4)
Sucrose and other disaccharides (5) Monosaccharides (liquid sugar) and inositol (6)
When industrially chromatographically separating betaine and amino acids and beet sugars, it is not impossible to separate each of the above six fractions using a single-base method; however, with a single-base method, the separation function is poor, and It is not economically viable due to the low recovery rate. Special Public Showa 4ct-23jt
The method disclosed in Japanese Patent Publication No. Shoj3-λr23 is an example of this, and since the inositol fraction contains a large amount of sucrose,
Inositol cannot be recovered unless Category 1 is removed using a mound or the like.

Therefore, a method that has been used industrially in recent years is a simulated moving bed chromatographic separation device.

This method only allows separation into two fractions.

For example, when separating between (3) and (4) of the above six components, components (5) and (6) are separated in order, so
Usually, the result is that μ04 is fractionated into the sucrose fraction and the remaining 1.0% is fractionated into the raffinose fraction.

However, if this is chromatographically separated using the method described in Japanese Patent Application No. 47-307123, it can be efficiently separated into three fractions at the same time. It can be separated into three fractions: fraction and fractions (5) and (6).

However, if betaine and amino acids are contained in fractions (6) to 6) separated in this way, betaine will precipitate out first when this fraction is concentrated and crystallized.
High purity inositol cannot be obtained.

However, Bt/Petai/Bt
! It can be removed in a desalting step.

The cation exchange resin used here is:

Examples of the exchange group include styrene-divinylbenzene-based strongly acidic cation crosslinking resins having a sulfonic acid group.

These ion exchange resins 11& may be made of gel-like ion exchange resin or porous ion exchange resin.

For example, Diamondion BK1B%SK//0°PKJ/A, PK220, etc. can be mentioned.

The anion exchange resin used in the desalting process for the above cation exchange resin is DIAIO 72AJOr%'
PAJ/J, PA4'/J, EIA/lm, WA co1%
11AJO and the like.

Diaion is a registered trademark of Mitsubishi Chemical Industries, Ltd.

When using the above ion exchange resin to remove betaine by passing the decocted molasses through a type cation exchange resin column, it is necessary to remove not only betaine but also ions such as sodium, potassium, and calcium. It is also cultivated by removing it,
In the treatment of molasses according to the present invention, leakage of betaine from the cation exchange resin tower makes it necessary to stop the operation of passing the molasses and recondition the cation exchange resin used.

Leakage of betaine can usually be detected using the Reinecke salt method.

The cation exchange resin can be easily regenerated by using an appropriate amount and concentration of mineral acid when regenerating a normal cation exchange resin, but when used in the present invention, It is necessary to first treat a cation exchange resin whose function has decreased with an alkali and then regenerate it into an H-type cation exchange resin using an appropriate amount and concentration of mineral acid. Examples of the alkali agent used in the alkali treatment include sodium hydroxide, potassium hydroxide, ammonium hydroxide, and the like.

The alkaline treatment of the cation exchange resin is usually performed at the same time as the regeneration of the anion exchange resin.

Regeneration of the anion exchange resin can be carried out, for example, by using 10"it% water of sodium hydroxide in an amount of 1ose4 of the exchange capacity of the cation exchange resin, at a capacity rate (v/h) ≠
, j, and the effluent is allowed to pass through the cation exchange resin tower overnight, thereby completing the alkali treatment of the cation exchange resin at the same time. The alkali-treated nine cation exchange resin may be washed with light and then regenerated into H type with mineral acid.

Examples of mineral acids include hydrochloric acid and sulfuric acid.

As the regeneration conditions, for example, when using a 5[07% aqueous solution, 100 equivalents of the exchange capacity of the cation exchange resin are used, and the liquid is passed through the packed column at a volumetric rate [vL]. Good.

In this way, the desalted solution obtained by passing it through the ■ type cation exchange resin (A resin and the OH type anion exchange resin to remove betaine and salt) is then treated in a chromatographic separation step. The mixture is separated into an inositol-enriched fraction, a Si-I-tang enriched fraction, and a raffinose-enriched fraction.

Next, the details of the chromatographic separation process will be explained.The liquid is chromatographically separated.As the adsorbent used for the chromatographic separation, a sodium type or potassium type cation exchange resin is conveniently used.

As the cation exchange resin, a styrene-divinylbenzene-based sulfonic acid type strongly acidic cation exchange resin is preferably used.

For example, Diaion IFRK/J/111FRKl≠
1% TJBK! Examples include JOK, UBKjJOG, and the like.

The adsorbent is packed into a packed column to form a packed bed.

This packed column is a packed bed whose front end and rear end are connected by a fluid passage to form a chromatographic system in which fluid can be circulated from the front end to the rear end.

The present invention utilizes such a romatoseparation system to divide the desalted solution into inositol-enriched nine fractions, silyl sugar-enriched fractions, and raffinose-enriched fractions through the following steps. The fraction is separated into

That is, the first step is to extract the sucrose-enriched nine fractions from the rear end of the packed bed while supplying the desalted solution from the front end of the packed bed, (ii) while supplying water from the middle of the packed bed. a second step of withdrawing the citrus-enriched fraction from the rear end of the packed bed, OiD circulating the fluid in the bed without supplying fluid to the packed bed and withdrawing fluid from the packed bed; The third step consists of a packed bed filled with a zone in which inositol and sucrose that remain without being extracted in the first step are mixed, and is moved to the front end of the bed, (1v) while supplying water from the front end of the packed bed. 4th step of extracting the inositol-enriched fraction from the rear end of the packed bed; (V) extracting the raffinose-enriched fraction from the rear end of the packed bed while supplying water from the front end of the packed bed! Step, (vD) Circulating the adult body in the bed without supplying fluid to the packed bed or withdrawing fluid from the packed bed, and raffinose and silucrose remaining without being extracted in the j-th step are mixed. This is accomplished by repeating the first to sixth steps, including the sixth step of moving the zone consisting of a packed bed to its front end.

[Effect]

In particular, the present invention uses a novel romatoseparation method to extract a desalted solution from which betatai and salts have been removed, to obtain a fraction enriched in citric acid, a fraction enriched in inositol, and a fraction enriched in raffinose. The purpose of this method is to provide a method for fractionating the desalted solution into the above-mentioned novel chromatography solution. By combining this method with a separation method, it became possible for the first time to separate and fractionate into a fraction enriched with sea monosaccharide, a fraction enriched with inositol, and a fraction enriched with raffinose. it is conceivable that.

〔Example〕

Next, the present invention will be further explained with reference to examples, but the present invention is not limited to these examples.

Example I Table 1 shows the composition of a chlorine feed solution obtained by concentrating the desalting solution shown in FIG. 1 to Bx40.

FIG. 3 is a schematic diagram of an apparatus for carrying out the chroma separation step in the present invention.

In the figure, 1 and 2 are packed beds filled with sodium or potassium type cation crosslinking resin as an adsorbent, 3 is a storage tank for chromatography supply liquid, and ≠ is a storage tank for water (desorbent). , j~ri indicates the extraction line of the valley fraction, and i
o to 12 indicate pulp, and 20 indicates a circulation pump, respectively.

In the apparatus shown in FIG. 3 above, the inner diameter is 33,! ■, 1ri in two columns connected in series with packed bed part tacho 0■
o- adsorbent (Na-type strongly acidic cation exchange resin, Diamond σBKjJOK) was used, and the capacity rate was /,00
At 01111/h, the separation operation was repeated according to the time schedule shown in Table 2 below.

Table 1 (weight tubes other than Bx are shown) (Note) (1) Recovery rate of inositol in fraction A (2) Recovery rate of sucrose in fraction B (3) Recovery rate of raffinose in fraction C Table 2 Since a steady state was reached at the 12th cycle, samples of each fraction were taken and analyzed, and the results were as shown in Table 7.

When this A fraction 11 was vacuum concentrated using a rotary evaporator, the liquid became cloudy around 0 Bz and inositol began to precipitate.

Further, it was gradually concentrated, and when it reached Bx40, the contents were taken out, cooled to 2J℃, centrifuged, and the purity was ! White inositol powder / /, / 1
A liquid sugar having the composition shown in Table 3 below was obtained.

1 J Table (weight i%) Example λ Using the same raw materials and the same chromatographic separation apparatus as in Example 1, the separation operation was repeated according to the time schedule shown in the table below.

Table 1 (Note) (1) Recovery rate of inositol to mu fraction (2
) Recovery rate of sucrose in fraction B (3) Recovery rate of raffinose in fraction C Since a steady state was reached at the 12th cycle, samples of each fraction were collected, and as shown in Table 5. Ta.

〔Effect of the invention〕

According to the present invention, a sucrose-enriched fraction, an inositol-enriched fraction, and The raffinose-enriched fraction can be easily fractionated. Furthermore, when carrying out the above chromatographic separation step, if the switching time of each of the above steps is adjusted, the raffinose composition of the raffinose-enriched fraction is changed to j-2! It can be adjusted arbitrarily within the range of -.

In addition, the silasugar composition of the inositol-enriched fraction is
! -This fraction can be used for mono-K11
By carrying out lk condensation and crystallization, it is possible to easily obtain highly pure inositol powder and liquid sugar with high utility value.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing a conventional sugar beet processing process, FIG. 2 is a diagram showing a sugar beet processing process of the present invention, and FIG.
The figure is a schematic diagram of an apparatus for performing chromatographic separation according to the present invention. I and Co・・・・・・・・・・・・・・・・・・
・・・・Packed bed 3・・・・・・・・・・・・・・・・・・
・・・・・・・・・・・・・・・・・・ Chromatography supply liquid ・・・・・・・・・・・・・・・・・・・・・・
・・・・・・・・・・・・Aquarium j～ri・・・・・・・
・・・・・・・・・・・・・・・・・・・・・・・・ Extraction line lO～lri・・・・・・・・・・・・・・・
・・・・・・・・・Pulp 20・・・・・・・・・・・・
・・・・・・・・・・・・・・・・・・・・・ Circulation pump applicant Hokuren Agricultural Cooperative Federation Mitsubishi Kasei Techno Engineers Co., Ltd. Agent Patent attorney Hase - (1 other person) ) No. 12 15 Sweets ↓ ↓ t 熾7 Vegetarian 1ai 昂 2 figs Sugar beets ↓ Exuding water ↓

Claims (3)

[Claims] (1) Separate beet sugar solution into beet sugar and roasted molasses,
Then, the roasted molasses is desalted by passing it through an H-type cation exchange resin and an OH-type anion exchange resin to remove betaine and salt, and the desalted liquid obtained by this process is , a treatment of a beet sugar solution characterized by combining a chromatographic separation step of separating into an inositol-enriched fraction, a sucrose-enriched fraction, and a raffinose-enriched fraction. Method. (2) In the method for processing a sugar beet sugar solution according to claim 1, the chromatographic separation step consists of a packed bed filled with a sodium type or potassium type cation exchange resin as an adsorbent; The desalination treatment liquid is passed through a chromatography separation system that is connected to the rear end by a fluid passage and allows the fluid to circulate from the front end to the rear end of the packed bed, and (i) the packed bed. A first step of extracting the sucrose-enriched fraction from the rear end of the packed bed while supplying the desalination treatment liquid from the front end; (ii) from the rear end of the packed bed while supplying water from the middle of the packed bed; a second step of withdrawing the sucrose-enriched fraction; (iii) circulating the fluid in the bed without supplying the fluid to the packed bed and withdrawing the fluid from the packed bed; a third step in which a zone containing a mixture of inositol and sucrose that remains without being extracted is moved to the front end of the packed bed; (iv) inositol is enriched from the rear end of the packed bed while supplying water from the front end of the packed bed; (v) a fifth step of extracting the raffinose-enriched fraction from the rear end of the packed bed while supplying water from the front end of the packed bed; (vi) supplying the fluid to the packed bed. The fluid in the bed is circulated without supplying or extracting the fluid from the packed bed, and the zone where raffinose and sucrose are mixed and remains without being extracted in the fifth step is moved to the front end of the packed bed. A method characterized by repeatedly performing the first to sixth steps of step 6. (3) The method for treating sugar beet liquid according to claim 1, characterized in that the H-type cation exchange resin is an H-type cation exchange resin regenerated with an alkali and an acid. .