JP2003153700A - Method for reducing viscosity of maskit and its use - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for reducing the viscosity of MASKIT obtained by crystallizing a saccharide solution substantially without lowering the crystallization rate of the MASKIT, and to provide a method for producing saccharide crystals or saccharide powder containing the saccharide crystals by using the obtained MASKIT. SOLUTION: This method for easily producing the saccharide crystals or the saccharide powder containing the saccharide crystals comprises raising the temperature of MASKIT obtained by crystallizing a saccharide solution to largely lower the viscosity of the MASKIT substantially without lowering the crystallization rate, sending the MASKIT with a pump, stirring the MASKIT, and subjecting the MASKIT to a centrifugal treatment or a spray- drying treatment.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a method for reducing the viscosity of a musket and its use, and more particularly, to increasing the temperature within a range that does not substantially reduce the crystallization rate of the musket obtained by co-crystallizing a sugar solution. And a method for reducing the viscosity of a musket, and a method of centrifuging the sprayed musket or spray-drying the sugar crystal to easily produce sugar crystals or a sugar powder containing the same. Regarding the method.

[0002]

2. Description of the Related Art Generally, anhydrous crystalline glucose (glucose), sucrose (sugar), etc. have a relatively high crystal formation rate, the crystals are hard, and the shape thereof is columnar, and the viscosity of a musket containing the crystals is also high. Since it is relatively low, a method of concentrating a sugar solution and promoting crystals in the same container using a decoction method has been adopted for the production of these crystalline sugars. Specifically, a vacuum evaporation can (concentrated crystal can) at the end of the decoction operation
Seed crystals are added to a concentrated solution of a sugar solution having a volume of 10 v / v% to 30 v / v% to crystallize, and the solution is concentrated under reduced pressure while continuously supplying the sugar solution. , While keeping the degree of sugar supersaturation (a state in which the solution contains more than the amount of solute corresponding to the solubility at a certain temperature) at a constant value, continue to concentrate until the liquid volume in the evaporator reaches the set value, and at the same time This is a method of crystallizing crystals.

However, for example, in the case of producing anhydrous fructose crystals, the solubility of fructose in water is very high, and it is necessary to support crystals from a sugar solution containing a high concentration of fructose. Therefore, in the case of producing high-purity anhydrous fructose crystals, for example, JP-A-4
As described in JP-A-9-102853, JP-A-49-118843, etc., the purity is 92 w / w% in terms of an anhydride (hereinafter, in this specification, unless otherwise specified, w / w% is simply abbreviated as%.) A sugar solution containing at least the above fructose is concentrated to a concentration of 80% or more, transferred to an auxiliary crystal can, and seed crystals are added at 1% to 4%,
Keep the temperature constant and slowly concentrate under reduced pressure to promote the auxiliary crystal while keeping the fructose concentration constant.After cooling to a certain temperature to crystallize a certain amount of crystals, further slowly concentrate under reduced pressure to keep the fructose concentration constant. By assisting the crystallization while maintaining, or gradually cooling to a set temperature while slowly stirring to aid the crystallization, a mass kit containing anhydrous fructose crystals at a crystallization rate of 40% or more and 75% or less is prepared, The obtained musket is centrifuged to separate crystals and honey (honey), and if necessary, a small amount of warm water is sprayed on the crystals to wash the crystals to further remove honey, and then dried. A method for producing high-purity anhydrous fructose crystals has been proposed.

The mass kit produced by the above method is
In addition to the high concentration of the sugar solution before the eutectic, it becomes a non-Newtonian fluid as the crystallization progresses, the viscosity increases significantly, and at the end of the eutectic, compared to the case of sucrose (sugar),
Viscosity increases several hundred times or more.

Further, for example, in the case of producing β-maltose hydrated crystals, the rate of crystal formation is very slow, and the β-maltose hydrated crystals have a triangular flat plate shape, which is soft and can be rapidly cooled. More fragile crystals in the shape of triangular thin plates are likely to be produced, and the viscosity of the musket containing crystals is higher than that of sucrose (sugar).
Therefore, in the case of producing a high-purity β-maltose hydrous crystal-containing powder, for example, Starch Science Handbook (45
0-461 pages, 1977, Asakura Shoten), Japanese Patent Publication No. 62-
As described in Japanese Patent Publication No. 51120, etc., a sugar solution containing maltose having a purity of 90% or more is concentrated so as to have a concentration of 50% or more as a total solid content in terms of an anhydride, and then it is added to an auxiliary crystal can. Then, 0.1% to 5.0% of seed crystals are added, and the mixture is slowly stirred and gradually cooled to a set temperature to promote the crystallization, and β-maltose hydrous crystals are crystallized at a rate of 30% or more 8
A mass kit containing 0% or less was prepared, pumped to a basket type centrifuge, centrifuged to separate crystals and honey, and if necessary, a small amount of cold water was sprayed on the crystals to form crystals. By washing the honey to remove nectar and drying
A method for producing higher purity β-maltose hydrous crystals has been proposed.

On the other hand, in the case of producing a powder containing β-maltose hydrous crystals in which the whole amount is pulverized by spray drying without changing the purity, for example, Japanese Patent Publication No. 62-5112.
As described in Japanese Patent No. 0, etc., 60% of a sugar solution containing maltose having a purity of 75% or more is calculated as an anhydride.
It is concentrated to 80% or less, transferred to a can of auxiliary crystals, and seed crystals are added to 0.1
% To 20.0% is added, the mixture is slowly stirred and gradually cooled to a set temperature to carry out an auxiliary crystal, and a mass kit containing a crystallization rate of β-maltose of 25% or more and 60% or less is prepared and pumped. A method of producing a stable β-maltose hydrous crystal-containing powder by transferring, spraying into a spray drying tower using a pressure nozzle or a rotating disk, pulverizing, drying and aging is proposed.

The musket containing anhydrous fructose crystals or the musket containing β-maltose hydrated crystals obtained as described above has, in addition to its high viscosity, a fructose anhydrous crystal or β-maltose hydrated crystal. The decrease in fluidity due to crystallization, and the increase in viscosity due to the decrease in temperature of the musket associated with cooling, etc. are interrelated, resulting in extremely high viscosity, the fluidity of the musket is significantly decreased, and the energy required for stirring is large. Become.
Furthermore, when centrifuging or spray drying, pumping the mass kit, increasing the load of agitation, or depleting the honey when performing the syrup treatment,
Various problems occur such as an increase in spray pressure when performing spray processing, uneven spray droplets, and enormous growth.

Therefore, in order to solve these problems,
Shorten the crystallization time at the time of preparing a mass kit containing fructose anhydrous crystals or β-maltose hydrated crystals, or suppress the crystallization rate to a low level by setting the minimum temperature during the crystallization to be higher, or By maintaining a high minimum crystallization temperature for producing a mass kit by promoting crystallization of fructose- or maltose-containing liquid concentrated to a high concentration at a high temperature, the viscosity can be kept low while maintaining a high crystallization rate. Possible countermeasures are. However, in the cases of the former two methods, the yield of anhydrous fructose crystals or β-maltose hydrate crystals obtained by one operation is low, and as a result, there is a drawback that work efficiency is deteriorated. on the other hand,
In the case of the latter method, although the yield of crystals obtained can be expected, the sugar is exposed to a high temperature for a long time, which causes deterioration of the sugar and coloring of the musket. Unable to obtain anhydrous fructose crystals, β-maltose hydrous crystals or β-maltose hydrous crystals-containing powders, and it is necessary to re-refining the fructose anhydrous crystals or β-maltose hydrous crystals by separating the nectar after coloring. As a result, there are drawbacks such as a poor crystal yield.

Various methods have been proposed so far as a method of reducing the viscosity of a mass kit having an increased viscosity.
It is conceivable to apply the method of diluting a musket having an increased viscosity, which is used during the production of sucrose (sugar) by the infusion method, with water to reduce the viscosity. In the case of this method, control of water used, dissolution of fructose anhydrous crystals or β-maltose hydrous crystals in the mass kit by adding water to reduce viscosity, further,
There is a drawback that a large amount of energy is required to uniformly stir and mix the musket in a short time.

A method of adding a sugar solution instead of the above-mentioned water has been proposed, for example, in JP-A-49-102853 and JP-B-5-79316. In the case of this method, the crystallization rate does not decrease, but in order to control the sugar solution used for dilution and to reduce the viscosity, more sugar solutions than the water are uniformly stirred in the musket, Since it needs to be mixed, more energy is required, and in order to add a large amount of sugar solution for dilution, it is necessary to reduce the amount of the mass kit to be prepared first. There are drawbacks.

On the other hand, in the case of producing fructose anhydrous crystals, in order to reduce the viscosity of the fructose-containing solution and the viscosity of the musket obtained by the co-crystallization, a concentrated sugar solution and an organic solvent such as ethyl alcohol or methyl alcohol are used. There is also proposed a method of producing an anhydrous crystal of fructose by subjecting the obtained musket to centrifugation by using a liquid obtained by mixing and crystallizing. In the case of this method, although it is possible to improve the crystallization rate of anhydrous fructose crystals at the time of auxiliary crystal by containing an organic solvent, it is necessary to completely remove the organic solvent contained in the crystals and mother liquor, Furthermore, in order to recover and reuse the organic solvent, an expensive explosion-proof type organic solvent recovery device is required, which causes a problem of increasing the manufacturing cost of anhydrous fructose crystals.

As shown in the examples of fructose and maltose described above, in the case of a sugar having a high viscosity of the musket, the crystallization rate of the musket is increased during the production of crystals or sugar powder containing the sugar. With the increase, the fluidity of the musket decreases significantly, the energy required for stirring increases, and further, the pumping of the musket during centrifugation and spray drying, and the processing such as stirring, honey and spraying Problems such as breakage of honey, increase in spray pressure, unevenness of spray droplets and enlargement, and low crystal yield occur, and the establishment of a technique for ameliorating these drawbacks is awaited.
Examples of saccharides having a high viscosity of the musket include saccharides derived from starch, and particularly those having high solubility in water and easily forming microcrystals are applicable, for example, fructose, maltose, trehalose, neotrehalose, panose. ,
Maltopentaose, cyclic tetrasaccharide, isomaltitol, maltotriitol, etc.

The cyclic tetrasaccharide means four glucose, α as described in “Carbohydrate Research”, Vol. 329, pp. 655 to 665 (2000) by Gale M. Bradburg et al. -1,3 and α-
It is a non-reducing carbohydrate that is linked in a ring by 1,6 bonds.
This saccharide is an enzymatic saccharification method utilizing α-isomaltosylglucosugar synthase and α-isomaltosyl transferase from starch according to the method described in Japanese Patent Application No. 2000-234937 by the applicant. Can be used for manufacturing.

[0014]

DISCLOSURE OF THE INVENTION According to the present invention, in the case where a musket obtained by supporting a sugar solution with high crystallinity has a high viscosity and is treated to manufacture sugar crystals or sugar powder containing the sugar crystals. However, problems such as pumping, stirring, mashing and spraying of the musket occur, and problems such as low crystal yield occur, so in order to improve this, the crystallization rate of the musket should be adjusted. The first object is to provide a method for reducing the viscosity without lowering the viscosity, and to easily manufacture a sugar crystal or a sugar powder containing the sugar crystal using the obtained viscosity-reduced mass kit. The second problem is to provide a method.

[0015]

DISCLOSURE OF THE INVENTION For the purpose of solving the above-mentioned problems, the present inventors do not reduce the crystallization rate of a musket obtained by promoting crystallization of a sugar solution and reduce the viscosity. With that in mind, I have continued my research. as a result,
Surprisingly, it was newly found that by raising the temperature of the musket after the completion of the auxiliary crystal within a certain temperature range, the viscosity can be greatly reduced without substantially reducing the crystallization rate, and a new viscosity is newly found. The present invention has been completed by establishing a reducing method and a method for easily producing a sugar crystal or a sugar powder containing the same by using a viscosity-reduced mass kit.

That is, the crystallization rate of the musket is substantially lowered and the temperature is raised in the inner range to drastically reduce the viscosity. The musket having the reduced viscosity is pumped, stirred, centrifuged or spray-dried. The present invention has been completed by establishing a method for easily producing a sugar crystal or a sugar powder containing the sugar crystal by performing a treatment such as the above.

[0017]

BEST MODE FOR CARRYING OUT THE INVENTION A musket is a sugar solution that is concentrated to a supersaturated state and then seed crystals are added and cooled slowly with stirring, or a supersaturated state is slowly concentrated to a constant value. It is a mixture of crystals and a sugar solution (mother liquor) having a supersaturated concentration, which is obtained by crystallizing sugar crystals by a method such as keeping. The thus-obtained musket exhibits high viscosity depending on the kind of sugar, and as described above, it is often the case that the musket is difficult to process.

It was tested whether the viscosity could be reduced by heating the highly viscous musket without substantially reducing the crystallization rate of the musket, and it was found that the temperature was raised within a certain temperature range. Thus, it was found that the viscosity can be significantly reduced and the handling operability thereof can be significantly improved without lowering the crystallization rate of the contained sugar.

In the present invention, the crystallization rate of the musket is not substantially reduced, that is, when the temperature of the musket is raised, the sugar crystals contained therein are not dissolved,
It means that the crystal content is not reduced, or even if dissolution occurs, the rate is low and the rate of reduction can be suppressed to a range of less than 10% with respect to the crystallization rate before temperature rise.

The mother liquor of the musket during or after the auxiliary crystallization is in a supersaturated state, and when the viscosity is reduced by raising the temperature of the mother liquor in a relatively narrow temperature range, the mother liquor is in a supersaturated state. However, the inventors found that there was a temperature range in which no crystal dissolution phenomenon was observed and the crystallization rate did not decrease. Further, it was revealed that when the temperature was raised beyond that, the crystallization rate decreased due to the temperature rise temperature and the time of exposure to the high temperature after the temperature rise. From the experimental results, it was found that the temperature range of the temperature rise is preferably 20 ° C. or less, more preferably 15 ° C. or less, although it varies depending on the supersaturated state of the sugar solution of the musket. If the temperature range of temperature rise exceeds 20 ° C., the crystallization rate of the mass kit is greatly reduced, and thus the yield of crystals obtained by centrifugation is reduced, or the crystal-containing powder obtained by spray drying. In order to prevent the deterioration of the crystallization rate (crystal content rate) and deterioration of the physical properties, there arises a problem that it is necessary to extend the aging time after spraying.

[0021] The temperature rising time may be appropriately selected depending on the temperature range of temperature rising and the stirring ability of the auxiliary crystal can within a range where the crystallization rate does not decrease. Usually, when raising the temperature, temperature rise is likely to occur if the temperature rises rapidly or stirring is not successful, and there is a concern that the crystallization rate of the mass kit may decrease. To avoid this, it is desirable to raise the temperature as slowly as possible. .
Usually, in consideration of workability, equipment utilization efficiency, etc., it is preferable that the heating time of the mask is within 5 hours, more preferably within 3 hours. The holding time after heating is 0.1 to 3 hours,
More preferably, 0.5 to 1 hour is suitable.

As described above, it became clear that by raising the temperature of the musket within a specific temperature range, a musket having a significantly reduced viscosity can be obtained without substantially lowering the crystallization rate. .

For example, β-maltose hydrous crystals or β
-In the case of producing a powder containing maltose hydrated crystals, 0.1% to 2% of β-maltose hydrated crystals as a seed crystal in a maltose solution containing 75% or more in terms of anhydride.
20% of the mass kit having a crystallization rate of 30% or more and 80% or less of the obtained β-maltose hydrated crystal was obtained by adding 0.0% to promote the crystallization.
By raising the temperature within a temperature range of ℃ or less, a mass kit having a reduced viscosity can be obtained without substantially lowering the crystallization rate.

When the mass kit is subjected to pumping, stirring, centrifugal separation or spray drying to produce crystals or sugar powder containing the crystals, the operation is easy because of low viscosity. Not only β-by centrifugation
When maltose hydrous crystals are produced, maltose purity is increased due to better conglomeration, and β-
When producing maltose hydrous crystal-containing powder, it is possible to obtain a high crystallization rate because the viscosity can be reduced by raising the temperature in a specific temperature range even if the viscosity increases by increasing the crystallization rate of the musket. Thus, the aging time after spraying can be shortened, and a powder having good physical properties such as low hygroscopicity can be produced.

From the above, by carrying out the present invention, whether the musket having a low crystallization rate, which has been used so far, is used or the musket is diluted with water or a sugar solution,
Since it is not necessary to process a highly viscous musket with a large amount of energy or a long time, the working efficiency can be improved, and the physical properties of the finished product are excellent. Is very useful in.

Further, when the fluidity is increased by reducing the viscosity of the musket, the smashing during centrifugation is improved, so that the obtained crystals are easily washed, and the viscosity is not reduced by raising the temperature. Compared to the case, by reducing the remaining honey, it is possible to increase the purity, but further, it becomes easier to remove impurities other than molasses, and contains pyrogen, which is a causative substance that causes fever when entering the body. It is also advantageous when making products that do not fit. In order to make a product that does not contain pyrogen, the sugar solution for making crystals is highly purified and is not contaminated with pyrogen, the water and equipment used is not contaminated with pyrogen, and sugar solution or The fact that the air that contacts the crystals is clean is also an important factor. By producing in this way, it is possible to produce a crystalline powder that can be used as a raw material for foods and also as a raw material for intravenous sugar.

The method of heating the musket of the present invention to a temperature that does not substantially reduce the crystallization rate to reduce the viscosity of the musket will be described in detail below by using experimental examples of β-maltose hydrous crystals. explain.

[0028]

[Experimental Example 1-1] <Effect of temperature rising on viscosity and crystallization rate of musket> In order to study the effect of temperature rising on viscosity and crystallization rate of musket, β-maltose hydrous crystals of the sample were analyzed. The containing mask was prepared as follows. Maltose is a commercial product and has a purity of 9 in terms of anhydride.
A 5% reagent maltose (trade name “Maltose HH” manufactured by Hayashibara Biochemical Laboratory Co., Ltd.) was used. Add 60 kg of "maltose HH" to 70 kg of ion-exchanged water
After heating to 0 ° C. to completely dissolve it, it was concentrated under reduced pressure to a sugar concentration of 75% using a vacuum concentrator. This solution was transferred to an auxiliary crystal can equipped with a stirrer and a jacket, and commercially available as a seed, a reagent with a purity of 99% in terms of anhydride, maltose (manufactured by Hayashibara Biochemical Laboratory Co., Ltd., trade name "Maltose HHH") was used. Add 500g, while stirring slowly, 6
The mixture was cooled to 20 ° C. over 4 hours to carry out auxiliary crystallization to crystallize β-maltose hydrated crystals to prepare a mass kit. The crystallization rate of β-maltose at this time was 66%, and the β-maltose thus obtained was slowly crystallized by cooling over a long period of time.
Maltose hydrous crystals are large crystals and the degree of supersaturation of the musket is relatively low, and the viscosity of the musket at this time is 4
It was 5,000 cp.

The effect of the elevated temperature on the viscosity and crystallization rate of the musket was measured by taking a part of the musket obtained by the above method in a container with a jacket and slowly stirring at a rate of 1 ° C./10 minutes. However, the temperature was raised to each temperature, the temperature was maintained for 1 hour at each temperature, and then the viscosity and the crystallization rate of the mass kit were measured to investigate.

For the viscosity (cp) of the mass kit, a BH type rotational viscometer was used, 4 rp with 7 rotor
The value was measured when rotated by m. The crystallization rate was determined by the following equation after separating the musket into crystals and honey. Crystallization rate (%) = {(sugar mass in the mass kit-sugar mass in the mother liquor) / sugar mass in the mass kit} x 100 The sugar mass is measured using "Abbe refractometer" manufactured by Atago Co., Ltd. It was calculated from the sugar concentration. The sugar composition or purity of the sugar solution, crystals, etc. can be determined by "MCI GEL C" manufactured by Mitsubishi Chemical Corporation.
HPLC manufactured by Tosoh Corporation equipped with "K08EC" column
It was measured using the device "CCPD". Table 1 shows the experimental results
It was shown to.

[0031]

[Table 1]

As is clear from the results shown in Table 1, the viscosity was 45,000 when the temperature rise range was within 10 ° C.
It was greatly reduced from 0 cp to 20,000 cp. However, the crystallization rate gradually disappeared according to the temperature range in which the supersaturated state of the musket was raised, and the crystals did not dissolve, and no decrease was observed. When the temperature is further raised, the viscosity becomes 10,000 at 15 ° C.
cp, 5,000 cp at 20 ° C., 3,000 cp at 25 ° C., and crystallization rate of about 2 at 15 ° C.
%, About 6% when the temperature was raised to 20 ° C., and about 10% when the temperature was raised to 25 ° C. At this time, the rate of decrease when the temperature was raised by 20 ° C. was about 9% with respect to the crystallization rate of the mass kit before the temperature was raised.
When the temperature was raised by 0 ° C., the decrease rate was about 15%.

From the above experimental results, it is possible to apply the present invention to raise the temperature of the musket obtained by co-crystallizing the sugar solution within a specific temperature range without substantially lowering the crystallization rate. Viscosity can be significantly reduced, and sugar crystals or sugar powder containing the crystals can be easily produced by subjecting the mass kit to pumping, stirring, centrifugation, spray drying, or the like. Therefore, it can be said to be very valuable in industrial production.

Hereinafter, the present invention will be described in more detail with reference to specific examples, but the present invention is not limited to these examples.

[0035]

Example 1-a <Preparation of a fructose-containing solution for preparing a musket> A fructose-containing solution was a commercially available fructose having a purity of 95% in terms of an anhydride (trade name: Fujifructo L-95 (Japanese Food Processing Sales)
According to a conventional method, the product was decolorized with activated carbon and desalted with an ion exchange resin to be purified, and a fructose-containing solution containing no pyrogen was obtained. It was confirmed using Single Test Wako Limulus HSJ (Wako Pure Chemical Industries, Ltd.) that no pyrogen was contained.

[0036]

[Example 1-b] <Preparation of a fructose anhydrous crystal-containing mass kit and its use> The water used for the subsequent treatment was the one from which pyrogen was removed, and the equipment used was confirmed to be not contaminated with pyrogen. Then, it was conducted in a room blown with clean air. The fructose-containing solution obtained in Example 1-a was concentrated under reduced pressure to a concentration of 85% using a vacuum concentrator, transferred to an auxiliary crystal can, and ground as a seed crystal, a special grade reagent fructose (manufactured by Wako Pure Chemical Industries, Ltd.) Was added to fructose at a rate of 1%, and the temperature of the musket was gradually decreased to 25 ° C. over 72 hours with slow stirring to crystallize anhydrous fructose crystals. At this time, the crystallization rate of fructose was 32%. At this time, the viscosity of the mass kit was 55,000 cp. When this was heated to 30 ° C. over 5 hours and kept for 1 hour, the viscosity was 3
It could be reduced to 1,000 cp, and the reduction ratio was about 1% with respect to the crystallization rate before the temperature was raised.

This mass kit was fed into a basket-type centrifuge using a pump and centrifuged to separate crystals and honey. Then, the crystals are sprayed with warm ion-exchanged water to remove the adhering and remaining honey, and the crystals are recovered and dried under reduced pressure to give anhydrous fructose crystals having a purity of 99.5% in terms of anhydride. Got

The product can be advantageously used not only in foods, cosmetics and pharmaceuticals, but also as a pharmaceutical sugar which contains no pyrogen and can be administered intravenously.

[0039]

Example 2-a <Preparation of a high maltose-containing solution for preparing a musket> A commercially available bacterial liquefying α-amylase (Spitase HS Nagase & Co., Ltd.) was added to a suspension of 3 parts by weight of corn starch and 7 parts by weight of water. ) Was added, the temperature was raised to 90 ° C., the mixture was heated to gelatinize and immediately heated to 130 ° C. to stop the enzymatic reaction, and a liquefied liquid of DE 3.3 was obtained. 55 of this starch liquefaction liquid
The starch debranching enzyme (isoamylase prepared by culturing Pseudomonas bacterium) was rapidly cooled to ℃ 50 per 1 g of starch.
20 units of β-amylase derived from soybean (trade name # 1500 manufactured by Nagase & Co., Ltd.) were added and saccharified at pH 5.0 for 40 hours to give a saccharified solution having a maltose content of 87.3% based on solids. Obtained. According to a conventional method, this was decolorized by treatment with activated carbon and desalted by treatment with an ion exchange resin for purification, and concentrated under reduced pressure to give a solution having a concentration of 45%, which was used as a fractionation raw material.

The resin used for the fractionation was an alkali metal type strongly acidic cation exchange resin (manufactured by Tokyo Organic Chemical Industry Co., Ltd. under the trade name of Amberlite XT-1007Na + type, crosslinking degree of 6).
%) Was used to fill a jacketed stainless steel column with an inner diameter of 5.4 cm with an aqueous suspension, and the two columns were connected so that the sugar solution could flow in series to give a resin layer total length of 10 m.

While maintaining the temperature in the column at 55 ° C., 5 v / v% of the raw sugar solution was added to the resin,
Fractionated by running warm water at ℃ at SV0.3, and separating and removing maltotriose-rich fractions, high maltose-rich maltose-rich fractions and oligo-rich fractions Minutes were collected. Then, according to a conventional method, decolorization by activated carbon treatment and desalting by ion exchange resin treatment were carried out for purification to obtain a maltose-rich sugar solution containing no pyrogen. It was confirmed by using Single Test Wako Limulus HSJ (Wako Pure Chemical Industries, Ltd.) that no pyrogen was contained. The sugar composition of this high-maltose sugar solution was 3.0% glucose, 9% maltose.
4.7%, maltotriose 1.2%, and maltotetraose and above were 1.1%.

[0042]

[Example 2-b] <Preparation of β-maltose hydrous crystal-containing mass kit and its application> It was confirmed that the water used in the subsequent treatment was pyrogen-free and the equipment was not contaminated with pyrogen. Was used in a room blown with clean air. The maltose-rich solution obtained in Example 2-a was concentrated under reduced pressure to a 70% concentration using a vacuum concentrating can, and then transferred to an auxiliary crystal can, where β-as a seed crystal.
1% maltose hydrous crystal powder was added, and the temperature of the musket was gradually lowered to 20 ° C. over 72 hours with slow stirring to crystallize β-maltose hydrous crystals. The β-maltose crystallization rate at this time was 61%, and the β-maltose hydrous crystal obtained was a large crystal because it was slowly cooled and crystallized, and the degree of supersaturation of the musket was also low. , The viscosity of the mass kit at this time is 4
It was 10,000 cp. When this was heated to 25 ° C over 5 hours and kept for 2 hours, the viscosity was 28,000c.
It can be reduced to p, and the rate of decrease with respect to the crystallization rate before heating at this time was about 5%.

This mass kit was fed into a basket-type centrifuge using a pump and centrifuged to separate crystals and honey. Then spray the crystals with ion-exchanged water,
After removing the adhered and remaining honey, the crystals were collected and dried under reduced pressure to obtain β-maltose hydrous crystals having a purity of 99.0% in terms of anhydride.

The product can be advantageously used not only in foods, cosmetics and pharmaceuticals, but also as a pharmaceutical sugar which does not contain pyrogen and can be administered intravenously.

[0045]

[Example 3-a] <Preparation of a maltose-containing solution for preparing a musket> A commercially available bacterial liquefied α-amylase (Spitase HS) was added to a suspension of 1 part by weight of potato starch and 4 parts by weight of water.
Nagase & Co., Ltd.) was added and the temperature was raised to 90 ° C to heat and gelatinize, then immediately heated to 130 ° C to stop the enzymatic reaction, and D
A liquefied liquid of E2.1 was obtained. The starch liquefaction solution was rapidly cooled to 55 ° C., and 100 units of starch debranching enzyme (isoamylase prepared by culturing Pseudomonas bacteria) per 1 g of starch and β-amylase derived from soybean (trade name # 1500 manufactured by Nagase & Co., Ltd.) 50 units per 1 g of starch, and maltogenase (manufactured by Novo Nordisk Co., Ltd.)
It was saccharified for 40 hours while adding 10 units per g and maintaining the pH at 5.0. According to a conventional method, this was decolorized by treatment with activated carbon and desalted by treatment with an ion exchange resin to be purified to obtain a maltose-containing solution. The sugar composition of the maltose-containing solution was glucose 4.3%, maltose 92.9%, maltotriose 1.2%, maltotetraose or more 1.6.
%Met.

[0046]

[Example 3-b] <Preparation of β-maltose hydrous crystal-containing mass kit and its use> The maltose-containing solution obtained in Example 3-a was concentrated under reduced pressure to a 75% concentration using a vacuum concentrator, and then auxiliary crystals were added. Transfer to a can, add 5% of fine powder obtained by pulverizing β-maltose hydrous crystals as seed crystals, and slowly stir the temperature of the musket over 2 hours while stirring slowly.
The temperature was lowered to 5 ° C. to partially crystallize β-maltose hydrated crystals. At this time, the β-maltose crystallization rate of the mass kit was 51%, and since the β-maltose hydrous crystal obtained was cooled and crystallized in a relatively short time, many fine crystals were obtained. Since the degree of supersaturation is also high,
At this time, the viscosity of the musket was 75,000 cp. This can be heated to 40 ° C over 2 hours to reduce the viscosity of the mass kit to 35,000 cp,
At this time, no decrease in the crystallization rate was observed because the degree of supersaturation of the musket was high.

This mass kit was fed with a high-pressure pump and sprayed into a spray-drying tower with a rotating disk. The hot air temperature in the drying tower was 100 ° C., and the amount of air blown was adjusted so that the water content of the dry powder when taken out from the spray dryer was 8.5%. This powder is 80 ℃, relative humidity is 30%
2 hours at 30 ° C and 75% relative humidity
It was kept for a while, dried and aged to obtain a powder containing β-maltose hydrous crystals having a crystallinity of 65% and a water content of 6.5%. The crystallinity is based on the X-ray disintegrator Geiger Flex RD.
A-IIB (using Cu and Kα rays) (manufactured by Rigaku Denki Co., Ltd.)
Based on the powder X-ray diffraction pattern
Land) method (Acta Crystallographica, Vol. 14, p. 1180, 1961).

This product has a reduced drying temperature because the spray particle size can be reduced by decreasing the viscosity.
Since it has little denaturation, high crystallinity, and excellent storage stability, it can be advantageously used as a raw material for the production of various industrial products including foods, cosmetics, and pharmaceuticals.

[0049]

As is clear from the above description, according to the present invention, the temperature of the mass kit obtained by auxiliary crystallizing the sugar solution is raised within a predetermined temperature range, preferably 20 ° C. or less. Thus, the viscosity can be significantly reduced without substantially lowering the crystallization rate of the mask. By using this mass kit and easily performing a process such as centrifugation or spray drying, it is possible to easily produce a sugar crystal or a sugar powder containing the sugar crystal, and further, to obtain the sugar crystal. Alternatively, the sugar powder containing it has high physical properties such as high purity, high crystallinity, and low hygroscopicity, and thus is very useful in industrial production of these. Is.

Claims (6)

[Claims] 1. A method for reducing the viscosity of a musket, which comprises increasing the temperature of the musket within a range that does not substantially reduce the crystallization rate to reduce the viscosity. 2. The musket is a musket containing crystals of fructose, maltose, trehalose, neotrehalose, panose, maltopentaose, cyclic tetrasaccharide, isomaltitol, or maltotriitol. The method for reducing the viscosity of the mass kit according to claim 1. 3. The method for reducing viscosity of a mass kit according to claim 1, wherein the temperature range of temperature rise is within a range of 20 ° C. or less. 4. A method for producing a sugar crystal or a sugar powder containing the same, comprising the step of raising the temperature of the musket within a predetermined temperature range. 5. The sugar crystal or the sugar powder containing the sugar crystal according to claim 4, further comprising a step of centrifuging or spray-drying the mass kit heated at a predetermined temperature range. Manufacturing method. 6. The method for producing a sugar crystal or a sugar powder containing the sugar crystal according to claim 4, wherein the sugar crystal does not contain a pyrogen.