JPS6193192A - Manufacturing method of oligosaccharide powder - Google Patents

Abstract

PURPOSE:To obtain powdery oligosaccharide, economically in an industrial scale, by carrying out the chromatographic separation, concentration, drying, and recovery successively in respective specific methods. CONSTITUTION:A pseudo-moving bed is formed in a bed filled with a cation exchange material, by circulating a fluid through a bed in a manner to form an adsorption zone, a refining zone, a desorption zone and a concentration zone from the upstream- side to the downstream side, and shifting the positions of the feeding zone and the extraction zone of the liquid intermittently toward downstream-side. An aqueous solution containing maltose and an oligosaccharide is passed through said pseudo- moving bed under the following conditions. The ratio (phi2) of the volume flow rate to the apparent volume flow rate of the cation exchange material in the refining zone is controlled to 0.3-0.5, and the ratio (phi4) in the concentration zone is controlled to 0.3-0.6. The solution is separated into the adsorbed maltose solution and the non- adsorbed oligosaccharide solution continuously by the above chromatographic process. The aqueous solution of the oligosaccharide is made to contact with hot air in the form of mist in a drying chamber furnished with an atomizer, a hot-air inlet, and an air outlet, and is pulverized. The powder of the oligosaccharide is separated from the exhaust discharged from the drying chamber.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing oligosaccharide powder, and more specifically, to a method for producing oligosaccharides from an aqueous solution containing maltose and oligosaccharides having a molecular weight greater than maltotriose. The present invention relates to an industrially advantageous method for producing sugar (hereinafter abbreviated as oligosaccharide) powder as a main component.

The oligo ring is α-1. It is a mixture mainly consisting of maltotriose, which has three glucose units linked together through a Hirobond, and also contains maltotetraose, which has three glucose units linked together,
It is expected to be used in a variety of applications due to its low sweetness and excellent hygroscopicity and water retention. For example, it is expected to be used for the purpose of imparting water retention and wettability to foods, etc., or as an infusion solution in the medical field.

For these reasons, it is desirable to obtain oligosaccharides in powder form not only from the viewpoint of handling but also from the viewpoint of utilization in various applications.

[Prior Art] Oligo rings are contained in so-called maltose starch syrup obtained by saccharifying starch. Therefore, in order to produce oligosaccharide powder, it is first necessary to separate maltose from maltose starch syrup.

A method for chromatographically separating maltose from maltose starch syrup containing oligosaccharides is disclosed in JP-A No. 7-7-2009.
, It-ko J7 Tade, etc., but all of them are based on batch methods, and it is difficult to perform them efficiently on a large scale.

[Purpose of the invention]

An object of the present invention is to provide an industrially advantageous method for producing oligosaccharide powder.

Therefore, the object of the present invention is to provide a method for producing sugar powder whose main component is oligosaccharide (hereinafter abbreviated as oligosaccharide) from an aqueous solution containing maltose and oligosaccharide having a molecular weight higher than maltotriose. a separation step (A) of continuously chromatographically separating the aqueous solution as a raw material and water as a desorbent into an aqueous maltose solution as a sorbate component and an aqueous oligosaccharide solution as a non-sorbate component; a step (B) of concentrating the aqueous oligosaccharide solution obtained in the separation step; a drying step (C) of contacting the concentrated aqueous solution obtained in the concentration step with hot air in a spray state to powderize the oligosaccharide; A collecting ball 8 (D) separates the oligosaccharide powder from the exhaust air containing the oligosaccharide powder derived from the drying process; In the packed bed, which is connected to the rear end by a fluid passage, there is an adsorption zone from the raw material supply section to the non-sorbent extraction section, a purification zone from the withdrawal section to the desorbent supply section, and a purification zone from the extraction section to the desorbent supply section. Four zones, a desorption zone from the sorbate extraction section to the sorbate extraction section and a concentration zone from the extraction section to the raw material supply section, are formed in the above order upstream while the fluid is circulated. The purification zone is constructed by a pseudo-moving bed in which the position of the purification zone is intermittently moved in the downstream direction, and the volume of circulating fluid in the purification zone is 1 t! The ratio φ of the flow rate to the apparent volumetric flow rate of the cation exchanger is 0. J~O8! The ratio φ of the volumetric flow rate of the circulating fluid in the concentration zone to the apparent volumetric flow rate of the cation exchanger is 0. J~o,
6, the concentration step (B) is constituted by known concentration equipment, but in the concentration step, concentration is performed so that the total sugar concentration in the oligosaccharide aqueous solution is 30 to 70% by weight. The drying step (C) is composed of a drying chamber equipped with an atomizer 1 hot air inlet and an exhaust air outlet, and the hot air introduction temperature is from to to 200°C, absolute humidity is 10
(f water/9 dry air) Below, the exhaust air temperature is po~
/20°C, and the absolute humidity is ≠j (water/cooled air) or less.

[Structure of the invention]

The method for producing oligosaccharide powder of the present invention includes a separation step (A),
It consists of a concentration step (B), a drying step (C), and a recovery step (D).

In the present invention, the oligosaccharide powder is a so-called oligosaccharide mixture such as maltotriose and maltotetraose, and the content of glucose and maltose is
It means a powder that is less than heavy gas.

First, the separation step (A) will be explained.

The separation process of the present invention is constituted by a simulated moving bed. According to the invention, any type of simulated moving bed can be used to carry out the separation of maltose. FIG. 1 is a schematic diagram of one example of a pseudo moving bed used in the method of the present invention, and the second
The figure is a schematic diagram of another example.

In Figure 1, a packed bed (1
000) is divided into two unit packed beds of (100/) to (102≠). Each unit packed bed is filled with a salt-type cation exchanger that has a high adsorption power for maltose as well as oligosaccharides. As the cation exchanger, various commercially available cation exchange resins or zeolites can be used. Usually, a strongly acidic cation exchange resin in which a sulfonic acid group is bonded to a crosslinked copolymer of styrene and divinylbenzene is used.

Cation exchange resins are usually used to increase the difference between the adsorption power for maltose and the adsorption power for oligosaccharides.
Used in sodium, potassium, or calcium form.

In addition, maltose water/candy usually has a total sugar concentration of 30
-to heavy'! #, %, oligosaccharide content in total sugars! ~60
An aqueous solution of - is used.

Spaces (102j) to (10≠ri) are provided between each unit packed bed, and each space has a maltose syrup introduction pipe (104!-2) and a water introduction pipe (104!-2) to the packed bed. !
0), a maltose aqueous solution extraction tube (10'/) and an oligosaccharide aqueous solution extraction tube (io) from the packed bed.
s2) is open (most of it is omitted in FIG. 1). Although the provision of this space is not essential, it is preferable to introduce the maltose syrup introduced into the packed bed into this space because it can be quickly diffused into the liquid flowing down the bed.

In FIG. 1, maltose starch syrup is introduced into the space (to4!r), and water is introduced into the space (1036).

Further, an oligosaccharide aqueous solution is extracted from the space (IO col), and a maltose aqueous solution is extracted from the space (101fO). Therefore, the packed bed (1000) is (100/
) or ioo≠) an adsorption zone consisting of an increasing number of unit packed beds, a purification zone consisting of one unit packed bed of (1001) or 1012), (10/J) or 1
oitr), and a concentration zone consisting of t unit packed beds of (lO17) or 1024c). The action of each zone is equivalent to that of a known simulated moving bed with maltose as the sorbing component and oligosaccharides as the non-sorbing component. The temperature inside the bed is usually 4Cj -5F 0℃, preferably 6o-
maintained at to°C. If the temperature inside the bed becomes higher than Po°C, the sugar solution that is extracted may become uncolored. Furthermore, if the temperature is low, the viscosity of the maltose syrup will be high and the pressure loss in the bed will increase.

A maltose and oligosaccharide concentration distribution is formed in the liquid in the packed bed, and this concentration distribution moves downstream while maintaining its shape. To follow this movement, the pipes for introducing maltose starch syrup and water into the packed bed and the pipes for extracting the aqueous maltose solution and aqueous oligosaccharide solution from the packed bed are sequentially switched to the downstream pipes. The switching may be performed simultaneously for all types of pipes, or may be performed at different times for each pipe. The time for continuous introduction or extraction from the same pipe varies depending on the size of the unit packed bed, the type of cation exchanger, the flow rate of the liquid flowing down the bed, etc., but is usually a few minutes to several minutes. .

By this switching, the three zones described above sequentially move their positions in the packed bed. However, the length of each band is always substantially constant. That is, each zone circulates through the packed bed while maintaining its size and relative position.

The degree of separation of maltose and oligosaccharides in a simulated moving bed using a cation exchanger as a separation agent is influenced by various factors, but the most important factors are the rate of flow of the liquid in the bed and the rate at which the liquid is removed from the same tube. It is time to continue the introduction or extraction. This means that switching the liquid inlet and outlet tubes to the downstream tubes is equivalent to moving the cation exchanger upstream while keeping the positions of the inlet and outlet tubes constant. In addition, it is also inferred that the concentration distribution of the lily in the liquid in the bed is formed by the interaction between the cation exchanger moving in the upstream direction and the liquid moving in the downstream direction. As is well known, the flow rate of the liquid flowing down the bed differs from zone to zone. Of the flow rates in each of these zones, the flow rate in the purification zone within the packed bed (non-sorbent The ratio φ of the volumetric flow rate of the circulating fluid to the apparent volumetric flow rate of the cation exchanger in the zone from the extraction section to the desorbent supply section), and the concentration zone (zone from the sorbate extraction section to the raw material supply section) is the ratio of the volumetric flow rate of the circulating fluid to the apparent volumetric flow rate of the cation exchanger, φ, and the maltose and glucose content!
In order to obtain an oligosaccharide of Q weight or less, the above φ and φ.

It is necessary to operate the simulated moving bed by adjusting the values to 0.3 to 0.3 and 0.3 to 0.1, respectively.

In order to obtain more favorable results, the ratio of the volumetric flow rate of the circulating fluid in the adsorption zone (the zone from the raw material supply section to the non-sorbate extraction section) to the apparent volumetric flow rate of the cation exchange body, φ, and φ, (φ1/φ,) is 10.2 to 1.
It is desirable that it be within the range of 7. φ! Alternatively, if the value of the φ number is not within the above range, the oligosaccharide will be distributed throughout the packed bed, and a large amount of the oligosaccharide will be mixed into the maltose aqueous solution that is extracted. However, if the above-mentioned conditions are satisfied, oligosaccharides will be distributed in the packed bed downstream of the adsorption zone, purification zone and enrichment zone, and will be almost absent from the desorption zone, so that glucose and It is possible to obtain an oligosaccharide aqueous solution containing less than 1 oz.

In this specification, the apparent volumetric flow rate of the cation exchanger is defined as the apparent volume of the cation exchanger in the packed bed divided by the time required for the purification zone to go around the packed bed. . However, if there are unfilled areas in the packed bed as shown in Figure 1, the refining zone is filled with the quotient obtained by dividing the total volume of liquid in these unfilled areas by the liquid volume velocity in the refining zone. The volume of cation exchanger in the packed bed shall be divided by the difference subtracted from the time required to go around the bed. This unfilled part is installed for the purpose of dispersing maltose starch syrup as a raw material, but from the viewpoint of separation phenomenon, this part merely causes a time delay.

Since it is the cation exchanger itself that has an effective effect, the validity of this correction calculation can be easily understood.

Therefore, the total sugar concentration of the oligosaccharide aqueous solution obtained by separating maltose etc. in the above-mentioned separation step varies depending on the composition of the raw material aqueous solution supplied to the simulated moving bed, the amount of water supplied, etc., but in general, The oligosaccharide aqueous solution is extracted from the aqueous oligosaccharide solution extraction tube (ioz) in the separation step shown in FIG. 1 and is supplied to the next concentration step.

The concentration step (B) (not shown) of the present invention is constituted by conventionally known concentration equipment. For example, multiple effect evaporators,
A thin film falling type concentrator or the like is preferably used. In the concentration step, the oligosaccharide aqueous solution has a total sugar concentration of 30 to 70% by weight,
Preferably, it is concentrated to a range of jO to toss% and supplied to the next drying step. If the sugar concentration in the oligosaccharide aqueous solution is higher than the above range, the oligosaccharide becomes flocculent upon contact with hot air in the next drying process, and good powdering cannot be achieved.If the total sugar concentration is lower than the above range, However, it is necessary to significantly increase the temperature or amount of hot air used in the drying process, which is not only economically disadvantageous but also poses a risk of melting the oligosaccharide powder.

Next, the drying step (C) will be explained.

The drying process according to the invention basically consists of a drying chamber which is known per se and is equipped with a spray device, hot air inlet and outlet. Examples of the spray device include a nozzle-type or rotating disk-type atomizer, but a rotating disk-type atomizer is preferable from the viewpoint of supplying the concentrated liquid.

The drying chamber is equipped with the above-mentioned elements and is shown in a schematic diagram.

In Fig. 3, the drying chamber (1) consists of a cylindrical container whose lower part is shaped like an inverted truncated cone, and the upper part of which is a drying chamber (1).
An atomizer (2) is provided with an opening at the top of the atomizer (2), and a hot air inlet (3) is provided at the upper side wall and the truncated lower part of the atomizer (2).
) and exhaust air outlet 0) are provided.

Total sugar concentration concentrated in the concentration step (B) 30 to 70 weight f
The oligosaccharide aqueous solution is supplied to the conduit (atomizer-Q through two pipes) and introduced into the drying chamber (1) in the form of a spray. On the other hand, hot air is generated by the blower (j) and the heater (6), and the conduits (3) and the hot air inlet (3)
is introduced into the drying chamber (1) through. The hot air introduced into the drying chamber is dispersed and ejected by a ring-shaped distribution pipe (■) placed around the atomizer (2), and the flow is further directed by the guide plate <r> to the tip of the atomizer (Q). It is designed to surround the area.

In the drying chamber (1), a sprayed oligosaccharide aqueous solution (A
) is brought into contact with hot air, dried and powdered, but at this time,
The temperature at which the hot air is introduced is 20 to 200°C, preferably 100°C.
-160°C, absolute humidity must be below 10 (f water/dry air), preferably below r (7 kg water/dry air).

If the temperature of the hot air is higher than the above range, there is a risk of melting of the oligosaccharide powder as described above.On the other hand, if the temperature of the hot air is lower than the above range or the absolute humidity exceeds the above range, sufficient drying and powdering may occur. is not performed.

Use of hot air necessary for drying and powdering oligosaccharide aqueous solutions
tFi, hot air temperature, amount of oligosaccharide aqueous solution and sugar concentration (
Although it cannot be determined unambiguously because it depends on the amount of water (moisture content), in order to obtain good results, these conditions should be adjusted appropriately to ensure that the temperature of the exhaust air drawn from the drying chamber (1) is 41CO-7
20℃, preferably in the range of 60 to 100℃, and the absolute humidity is ≠! (f water/cod drying air) or less.

The oligosaccharide powdered in the drying chamber (1) is discharged together with the exhaust air from the exhaust air outlet ←) and is supplied to the next recovery step through the conduit (see).

Next, the recovery step (D) of the present invention will be explained.

The recovery process is a process of separating and recovering the oligosaccharide powder from the exhaust air containing the oligosaccharide powder derived from the above-mentioned drying process,
In the method of the present invention, various conventionally known gas-solid separation devices can be employed, but usually a cyclone device (y') shown in FIG.
A tick tube device consisting of an exhaust fan (/) is preferably used.

In the recovery process consisting of the cyclone device shown in Figure 3, the exhaust air containing oligosaccharide powder is introduced into the cyclone body (ri) through the conduit (μ') and the cyclone inlet (//), and is separated from the exhaust air. The chewed oligosaccharide powder is collected from the lower part of the cyclone body through the conduit (12), and
The exhaust air passes through a conduit (13) and an exhaust fan (l), and is exhausted from the conduit (l).

In the above explanation, the recovery step (D) is exemplified using equipment independent of the drying step (C), but in the method of the present invention, it is not necessary for both steps to be independent equipment, and for example, the drying step As the equipment for step (C), it is also possible to use equipment that also has the function of a recovery process. As equipment for such a drying process, for example, a rotating disk type vertical downward mixing type spray drying apparatus can be mentioned.

The oligosaccharide powder recovered as described above is normally transferred to a storage tank (not shown) and stocked in the storage tank which also functions as a supply tank during packaging.

Therefore, maltotriose, which is a component of oligosaccharide powder, has extremely high hygroscopicity, and most of the maltose contained in the oligosaccharide powder of the present invention becomes amorphous due to the spray drying process. It has relatively high hygroscopicity due to its

Therefore, it is preferable that the oligosaccharide powder obtained by the method of the present invention be stored in a storage tank maintained at positive pressure with dry air to cut off contact with the outside air. As dry air,
It is best to use air with an absolute humidity of 10 (f water/&Il dry air) or less, preferably A-t (r water/&Il dry air).

In addition, the pressure inside the tank is in the range of λ to 10rnynH20.
Enclosure is sufficient.

Further, the transfer from the recovery process to the storage tank is preferably carried out by pneumatic transport using dry air using a pneumatic conveyor. As dry air, the absolute relative humidity is IO (
(7 kg of water/dry air) or less, preferably a-r (water/dry air), especially 3.
It is more preferable to use dry air heated to aO 0 C, since the effect of flash drying can be achieved during the transfer of the oligosaccharide powder.

The method of the present invention is configured as described above, and the oligosaccharide powder obtained from the recovery step (C) is usually
It is a powder with a particle size of 5O-200 μm and a water content of 3 to j weight fi:%.

〔Example〕

Next, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to the following Examples unless the gist thereof is exceeded.

In the following examples, "%" means "weight [1].

Example 1 Glucose 7.3%, maltose - 67.6%, ilutriose l≠, 1%,! An oligosaccharide powder was produced using maltose starch syrup with a sugar concentration of 60 T and 77.0 T of lutotetraose as a raw material using the apparatus shown in FIGS. 2 and 3.

In FIG. 2, the unit packed bed 10/~101 has an inner diameter j≠
Cabinet, height 00. It is a cylinder, and inside the cylinder is a Na-type strongly acidic cation exchange resin (Diaion FRK-Jl,
(manufactured by Mitsubishi Chemical Corporation) is 10. r4tt filled. Each unit packed bed is connected in an endless manner through a circulation pump /J/~isr, and a maltose aqueous solution extraction pipe 110 is connected to the fluid passage connecting each unit packed bed via a pulp ///-//lr. ．． Oligosaccharide aqueous solution extraction tube via pulp/2/-/21/20. A water introduction pipe /30 is installed through pulp /J/~/31, and a maltose starch syrup introduction pipe iao is installed through pulp l≠l~/≠l.

The temperature in the bed of the apparatus shown in Fig. λ is maintained at 7s'CK,
The supply amount of maltose starch syrup and water was 0.27 t/ each.
hr and hekoz z z/hr, and the amount of maltose aqueous solution and oligosaccharide aqueous solution to be extracted is 08λ4'jt, respectively.
/hr and 1. , 2 r t/hr, and the flow rates of the adsorption zone, purification zone, and concentration zone are set to j and J 7 t/hr, respectively, by the flow rate control valve IO2. Adjustments were made to ivy t/hr and J, 001/hr.

In this case, for example, when maltose starch syrup is being supplied through Pulp/4', water is supplied through Pulp/Jl, and the maltose aqueous solution and oligosaccharide aqueous solution are extracted through Pulp/Saw and Pulp/24, respectively, and are filled. Desorption zone in beds 10/ and 102, enrichment zone in packed beds 103 and 70≠, packed bed 103
and adsorption zones in iot, packed beds 107 and 1
A purification zone is formed at 0r. Each pulp is 7
Every 5 minutes, the pulp that is one downstream is switched all at once, and 2
Each band goes around the floor in time.

In this example, φ8, φ3, φ, and φ1/φ.

The value of is as follows.

φ,=0.603 φ,=0.31.7 φ,=o,zz4L φ,/φ,=1. A≠ The oligosaccharide aqueous solution (sugar concentration 7.1%) extracted in a steady state is concentrated in a multi-effect evaporator and then supplied to the conduit (λ') of the apparatus shown in FIG.

In Figure 3, the height of the drying chamber (1) is Jm, and the diameter of the cylindrical part is 1. , g m.

The conditions for the drying step in this example are as follows.

Sugar concentration of the above aqueous solution: 50% by weight Hot air introduction temperature: 13 degrees Celsius Absolute humidity of hot air', 7. A (Water/Misaki dry air) Exhaust air temperature: tsj℃ Absolute humidity of exhaust air: 36 (F water/Ni 9 dry air) Oligosaccharides recovered from the conduit (12) at the bottom of the cyclone body The composition of the powder is shown in Table-/.

Table: Comparative Example 1 Glucose 1. /%, maltose 72.6%, maltriose 1.2j%, non-maltotetraose 13.7%
The sugar concentration consists of 60. Using flathead maltose starch syrup as a raw material, oligosaccharide powder was produced in the same manner as in Example under the following conditions. The sugar concentration of the aqueous oligosaccharide solution at the outlet of the separation process was 7.7%, and it was concentrated in the same manner as in Example 1 and supplied to the drying process.

[Separation process conditions]

Maltose starch syrup supply amount 0.3 t Ot/hr Water supply amount 0.672 1 Maltose aqueous solution extraction amount 0. JrOt oligosaccharide aqueous solution withdrawal amount 0.67J z adsorption zone flow rate da, 7
4! ? Flow rate in the purification zone t Hiro, 0 Tako I Flow rate in the concentration zone ≠, 31! # Valve switching time A/A seconds φ, = 0.603. φ,=o,zi'yφ,=0. ! r
! ! , φI/φ, =1. /1 [Conditions of drying process] Sugar concentration of the above aqueous solution: 50% by weight Hot air introduction temperature: /4!2℃ Absolute humidity of hot air: r (Water/Jc9 dry air) Exhaust air outlet temperature near 0℃ Exhaust Absolute humidity of wind: '1-JC97kj' to 9 dry air) The composition of the recovered oligosaccharide powder in the steady state is shown in Table-2.

Table 2 Examples Cogelcose 0.7%, 1 luteose 75.5%, orthotriose 16.3%, maltotetraose 7. jt%
Oligosaccharide powder was produced in the same manner as in Example 1 under the following conditions using maltose starch syrup with a sugar concentration of 5% as a raw material. The sugar concentration of the oligosaccharide aqueous solution at the exit of the separation process was 1%; it was concentrated in the same manner as in Example 1 and supplied to the drying process.

[Separation process conditions]

Maltose starch syrup supply amount 0.2 A J' l/
hr Water supply amount o, r t L/
hr Maltose aqueous solution extraction amount 0.332 I
Amount of oligosaccharide aqueous solution extracted 030! #Adsorption zone flow rate -201# Purification zone flow rate 3. 〇〇l Concentration zone flow rate 3.237 1 Pulp switching time try seconds φ, =O1S 3. φ,=0. ≠10 φ4=o, ssz, φ1/φ, = 1.23! [Conditions of drying process] Sugar concentration of the above aqueous solution: 10% by weight Hot air introduction temperature: /sO°C Absolute humidity of hot air near. s (t~1 dry air) Exhaust air outlet temperature Hro℃ Absolute humidity of exhaust air: J'y (t*/w dry air) Table 3 shows the composition of the recovered oligosaccharide powder in a steady state.
Shown below.

Table 3 In addition, the oligosaccharide powder bed obtained in the above recovery process was collected using a 221-machine conveyor, and the absolute humidity r (water/dry air) and the temperature jo°C were heated to dry hot air. ”
(inner diameter: 4 tm, height: 6.6 λm) and stored in a storage tank.

The inside of the storage tank was maintained at a positive pressure of 2 o by dry air with an absolute humidity of 7 (2 water/9 dry air) (the filling rate of the oligosaccharide powder was about 10%).

After 3 days of light pollution, the oligosaccharide powder in the storage tank was taken out and its properties were investigated. The oligosaccharide powder showed smooth fluidity, and no problems such as caking due to moisture absorption were observed. .

〔Effect of the invention〕

According to the method of the present invention, oligosaccharide powder can be industrially advantageously produced by combining specific separation steps, concentration steps, drying steps, and recovery steps. This will greatly contribute to the manufacturing field.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram of seven examples of a simulated moving bed used in the separation step of the method of the present invention, and FIG. 2 is a schematic diagram of another example. Moreover, FIG. 3 is a schematic diagram of an example of a drying chamber and a cyclone device used in the drying step and recovery step of the method of the present invention. In Figure 3, (1) is the drying room, (j) is the blower, and (6) is the heater 1. (ri) is the cyclone body, and (10) is the exhaust fan. Applicant Sanwa Kosan Co., Ltd. Mitsubishi Chemical Industries Co., Ltd. Agent Patent attorney Hase - (and 7 others) Figure A1

Claims (3)

[Claims] (1) A method for producing sugar powder whose main component is oligosaccharide (hereinafter abbreviated as oligosaccharide) from an aqueous solution containing maltose and an oligosaccharide having a molecular weight greater than or equal to maltotriose, the method comprising: using the aqueous solution as a raw material; , water as a desorption agent,
A separation step (A) of continuously chromatographically separating an adsorbate component maltose aqueous solution and a non-sorbate component oligosaccharide aqueous solution; and a step (B) of concentrating the oligosaccharide aqueous solution obtained in the separation step. and a drying step (C) in which the concentrated aqueous solution obtained in the concentration step is brought into contact with hot air in a spray state to powderize the oligosaccharide, and the powder is extracted from the exhaust air containing the oligosaccharide powder derived from the drying step. The separation step (A) consists of a collection step (D) for separating the raw materials, and the separation step (A) includes a collection step (D) in which the raw material is supplied into a packed bed filled with a cation exchanger and whose front end and rear end are connected by a fluid passage. an adsorption zone from the extraction section to the non-sorbate extraction section, a purification zone from the extraction section to the desorbent supply section, a desorption zone from the supply section to the sorbate extraction section, and a raw material supply from the extraction section. By using a pseudo moving bed, the fluid is circulated while forming four concentrating zones in the above order from upstream, and the positions of the supply section and the withdrawal section are intermittently moved downstream. and the ratio φ_2 of the volumetric flow rate of the circulating fluid in the purification zone to the apparent volumetric flow rate of the cation exchanger is between 0.3 and 0.5; The ratio φ_4 to the apparent volume flow velocity of the body is 0.3 to 0.
6, and the concentration step (B) is constituted by known concentration equipment, but in the concentration step, concentration is carried out so that the total sugar concentration in the oligosaccharide aqueous solution is 30 to 70% by weight. The drying step (C) is comprised of a drying chamber equipped with an atomizer, a hot air inlet, and an exhaust air outlet, and the hot air introduction temperature is 80 to 200°C. , the absolute humidity is 10 (g water/kg dry air) or less, the exhaust air temperature is 40 to 120°C, and the absolute humidity is 45 (g water/kg dry air) or less. A method for producing oligosaccharide powder. (2) The ratio φ_1 and φ_2 of the volumetric flow rate of the circulating fluid in the adsorption zone of the separation step (A) to the apparent volumetric flow rate of the cation exchanger, φ_, /φ_2, is 1.2 to 1.7.
A method for producing an oligosaccharide powder according to claim 1, characterized in that: (3) Claim 1 or 2, characterized in that the total sugar concentration in the raw material aqueous solution is 30 to 80% by weight, and the oligosaccharide content in the total sugar is 5 to 60% by weight. A method for producing oligosaccharide powder as described in .