JPH0714953B2 - Maltitol crystalline densities and method for producing the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION 2. TECHNICAL FIELD The present invention relates to crystalline maltitol containing densities and a method for producing the same, and more particularly to crystalline maltitol containing densities having improved physical properties and a method for producing the same.

3. BACKGROUND ART Among sugar alcohols, the existence of crystals and molten crystals of sorbitol, mannitol, etc. has long been known, and various methods for producing them are already known.

On the other hand, maltitol is more likely to form a supersaturated state than mannitol or sorbitol, which are known to form crystals, making it extremely difficult to obtain crystals. The method for producing maltitol crystals or molten crystals was only recently invented. Until then, the method was described in Jiro Nikuni's Starch Science Handbook, page 461, lines 14 and 17-18 (July 20, 1977,
As stated in the book "The Crystallographic Study of the Crystal ... Earth," published by Asakura Shoten, it was previously thought to be impossible to produce crystals of the crystal.

Maltitol crystals with a melting point of 146.5-147°C or molasses-containing crystals containing sorbitol, maltotriitol, maltotetriitol, and other molasses components in addition to maltitol were first produced in 1981, and the method for producing them is described in Japanese Patent Publication No. 63-2439.

Maltitol molasses crystals, which contain components other than maltitol as honey components and therefore have a lower melting point than maltitol crystals, occupy a more important position in the market than crystals produced by the molasses separation method due to their excellent properties and economic reasons.

However, since maltitol crystalline syrup was only recently discovered and it is prone to forming a highly supersaturated state,
Many aspects of the physical behavior of the densified crystals during their production remain unclear, and therefore the production methods are limited.

The method for producing crystalline maltitol densities described in the above patent publication involves preparing an aqueous solution of maltitol with a purity of 65% or more (hereinafter, unless otherwise specified, % means % by weight), preferably with a concentration of about 65 to 95%, in the presence of seed crystals to produce a massecuite, which is then subjected to one of the well-known methods of block grinding, fluidized bed drying, or spray drying.

For example, in the case of spray drying, the concentration is usually 70 to 85%.
Masseuse with a crystallization rate of about 25 to 60% is sprayed from a nozzle using a high-pressure pump, and the temperature is kept at a temperature where the crystal powder does not melt, e.g., 60 to 10
The method involves aging the product in hot air at 0°C for approximately 1 to 20 hours.

The block crushing method is a method in which masseuse, which usually has a moisture content of 5 to 15% and a crystallization rate of about 10 to 60%, is left to stand for 0.5 to 5 days until the masseuse crystallizes and solidifies into blocks, which are then crushed by grinding or cutting and dried.

Among these methods, the block crushing method is the main manufacturing method because, although the steps are complicated, each step can be carried out relatively easily and the equipment scale and process costs are smaller than those of the other two methods.

The dense crystalline maltitol obtained by these methods has the following properties:
When powdered to 20-50 mesh, the apparent specific gravity is 0.43-
It is lighter than other sugar alcohols such as sorbitol, with an average molecular weight of about 0.59, and has a high oil absorption rate of 15-22%.
When observed at a magnification of about 00x, it had a relatively sparse and porous crystalline structure.

The dense crystalline maltitol produced by the above-mentioned conventional methods has many problems in terms of its physical properties.

For example, the maltitol crystalline solids produced by the conventional method have the following problems: (a) their apparent specific gravity is light, so that their volume is large, and when packaging materials or containers for other sugar alcohols are used, they do not fit into the containers that are supposed to hold a certain amount of product;
Special packaging materials and containers are required, and large spaces and transporting equipment are also required for storage and transportation.

(b) Because the powder is light, it is prone to scattering as fine powder, limiting its applications.

(c) Because the crystalline structure is sparse, the hardness of the tablets tends to be insufficient when directly compressed into tablets. Furthermore, many problems remain with the manufacturing methods previously introduced, such as the fluidized bed drying method and spray drying method, as well as the conventionally employed block crushing method.

For example, the fluidized bed drying method involves placing maltitol crystals or molten crystals in a fluidized bed, spraying an aqueous maltitol solution onto the bed, and granulating and drying the resulting product. However, the crystallization rate of maltitol is slow, and the fluidized bed drying process takes a relatively long time, which requires large-scale equipment and makes mass production difficult.

When attempting to employ the spray drying method, there remain problems such as the difficulty in adjusting the crystallization rate when preparing maltitol massecuite, the fact that when maltitol massecuite is sprayed into dry air, the crystals do not grow sufficiently and the proportion of glassy solid components increases, and as a result, the resulting powder adheres to the walls of the dryer, making continuous production impossible, and the high equipment costs.

On the other hand, although the block crushing method is a method currently in use, it has many problems, such as: (a) the process is complicated and each step takes a long time; (b) therefore, containers and space are required to store large amounts of work-in-progress during crystallization; (c) when storing the product during the process, hygiene considerations, equipment, buildings, etc. are required; and (d) each step is labor-intensive, making automation and labor-saving difficult.

Therefore, there has been a demand for the development of a densified maltitol crystal having improved physical properties and a method for producing the same, which solves these various problems.

4. Disclosure of the Invention The inventors have intensively studied the physical properties of maltitol crystalline syrup and methods for producing maltitol crystalline syrup, and as a result have succeeded in producing maltitol crystalline syrup with improved physical properties in an extremely short time, using small equipment, in a labor-saving, hassle-free manner, by using an extruder having a long, narrow cooling and kneading zone consisting of multiple consecutive zones to generate plastic maltitol magma from an aqueous maltitol solution, and have thus completed the present invention.

That is, the present invention provides, firstly, a) a powder obtained after pulverization and classification,
It can be seen at 1000x magnification using a scanning electron microscope.
b) crushed and classified,
The apparent specific gravity of the crystalline powder of 50 mesh or more and 20 mesh or less is 0.650 to 0.750, and c) the oil absorption of the crystalline powder of 50 mesh or more and 20 mesh or less after crushing and classification is 7.0% to 17.
% and d) dense crystalline maltitol, which has a lower melting point than crystalline maltitol.

Second, the maltitol crystalline solids according to the first aspect of the present invention contain 80 to 98% by weight of maltitol in the solid matter, and the remaining components are 0.5 to 15% by weight of sorbitol and 1.5 to 10% by weight of maltotriitol or higher in degree of polymerization (DP).
Maltitol crystalline molten sugars consisting of ≧3 sugar alcohols.

Third, the aqueous maltitol solution is continuously fed into an extruder having an elongated cooling and kneading zone, and cooled and kneaded in the presence of seed crystals to generate maltitol magma,
A dense crystalline maltitol according to any one of the first and second aspects above, produced by continuous extrusion from an extrusion nozzle.

Fourth, an aqueous maltitol solution having a concentration of 80 to 98% by weight and a maltitol content of 80 to 99% by weight in the solid content is continuously fed into a first zone of an extruder having an elongated cooling and kneading zone consisting of a plurality of continuous zones, and the maltitol is kneaded at a temperature of 50 to 90°C.
Cool and knead until the maltitol solution inside is 50-80℃
In the second zone, when the temperature reaches 100°C, 3 to 80% by weight of seed crystals based on the extrusion amount are added continuously or intermittently and kneaded, and the mixture is further cooled and kneaded in the third zone, and then kneaded in the final zone until the temperature reaches 25 to 50°C.
The maltitol crystalline mixture according to claim 1, which is produced by cooling and kneading the maltitol magma formed to 60°C and then continuously extruding the maltitol magma from an extrusion nozzle.

Fifth, a) a concentration of 80 to 98% by weight and a solid content of sorbitol
An aqueous maltitol solution having a composition of 0.5 to 15% by weight, 80 to 98% by weight of maltitol, and 1.5 to 10% by weight of maltotriitol and sugar alcohols having a molecular weight of maltotriitol or higher (DP≧3) is continuously fed to a first zone of an extruder having a long and narrow cooling and kneading zone consisting of a plurality of continuous zones, and cooled and kneaded to 50 to 90°C. In the second zone where the aqueous maltitol solution therein has reached 50 to 80°C, 300g of the aqueous maltitol solution is added to the extrusion amount.
a first step in which up to 80% by weight of seed crystals are added continuously or intermittently and kneaded, followed by further cooling and kneading in a third continuous zone, and then cooling and kneading to 25-60°C in a final zone, after which the formed maltitol magma is extruded through an extrusion nozzle;
b) The extruded maltitol magma is heated at 15-80°C for 5-30 minutes.
The maltitol molten crystals described in 1 above are produced by sequentially passing through the following steps: a) a second step of maturing the maltitol magma for 60 minutes; b) a third step of coarsely crushing the matured maltitol magma, drying it at 80 to 115°C for 60 minutes or more, and crushing and classifying it.

Sixth, a method for producing crystalline maltitol containing molten crystalline maltitol, characterized in that when producing crystalline maltitol containing molten crystalline maltitol, an aqueous maltitol solution is continuously supplied to an extruder having a long cooling and kneading zone, and cooled and kneaded in the presence of seed crystals to generate maltitol magma, which is then continuously extruded from an extrusion nozzle.

Seventh, when producing crystalline maltitol,
80-98% by weight of maltitol in solids
The maltitol aqueous solution containing maltitol of 100% by weight is continuously fed to the first zone of an extruder having a long and narrow cooling and kneading zone consisting of a plurality of continuous zones, and cooled and kneaded to 50 to 90°C. The maltitol aqueous solution is then cooled and kneaded to 50 to 80°C in the second zone.
In the third zone, seed crystals are added continuously or intermittently in an amount of 3 to 80% by weight based on the extrusion amount, and the mixture is then cooled and mixed in the third zone, and cooled to 25 to 60°C in the final zone.
A method for producing dense crystalline maltitol, characterized in that after kneading, the formed maltitol magma is continuously extruded from an extrusion nozzle.

Eighth, in producing crystalline maltitol, a)
Concentration of 80-98% by weight, maltitol content in solids of 80-
The maltitol aqueous solution having a weight of 99% is continuously fed to the first zone of an extruder having a long and narrow cooling and kneading zone consisting of a plurality of continuous zones, and cooled and kneaded to 50 to 90°C. The maltitol aqueous solution is then kneaded to 50 to 80°C in the second zone.
In the third zone, seed crystals are added continuously or intermittently in an amount of 3 to 80% by weight based on the extrusion amount, and the mixture is then cooled and mixed in the third zone, and cooled to 25 to 60°C in the final zone.
a) a first step of extruding the resulting maltitol magma from an extrusion nozzle after kneading; b) a second step of maturing the extruded maltitol magma at 15 to 80°C for 5 to 30 minutes;
c) The matured maltitol magma is then coarsely crushed;
A method for producing crystalline maltitol, characterized by sequentially carrying out the steps of drying at 80 to 115°C for 60 minutes or more, and a third step of grinding and classifying the crystalline maltitol.

Ninth, the maltitol aqueous solution is prepared by dissolving 0.5 to 15% of sorbitol in water.
% by weight, maltitol 80-98% by weight, and maltotriitol and sugar alcohols of higher molecular weight (DP ≥ 3) 1.
9. A method for producing crystalline maltitol densities described in any one of items 6 to 8, characterized in that the crystalline maltitol densities are 5 to 10% by weight.

The present invention will be described in detail below.

The extruder that can be used in the present invention has a long, narrow cooling and kneading zone consisting of multiple consecutive zones, and must be configured so that raw materials can be continuously introduced, seed crystals can be continuously or intermittently introduced to form plastic maltitol magma, and the magma produced can be continuously discharged from the final cooling zone.However, as long as the structure satisfies these conditions, the shape and the methods of kneading, cooling, transport, and discharge are not important.

Here, the continuous multiple zones consist of a first zone where the raw material is introduced and cooled/kneaded, a second zone where the seed crystals are introduced and cooled/kneaded, a third zone and subsequent zones where the seed crystals are introduced and then cooled/kneaded, and a final zone. However, if the third zone and subsequent zones are a single zone, the third zone itself becomes the final zone.

For example, structures having the functions of kneading, cooling, and transporting include a single-screw extruder structure, a twin-screw extruder structure, a rotary gear pump structure, a structure in which a transport device such as a piston is inserted into a cylindrical structure with fixed blades, and other structures, and any of these can be employed in the present invention.

Among these various types of equipment, commercially available extruders can be advantageously used to achieve the objects of the present invention, and examples thereof include the Alpha Riser manufactured by Suehiro Iron Works, Ltd., the KRC Kneader manufactured by Kurimoto Iron Works, Ltd., the Twin Screw Extruder manufactured by Kowa Kogyo Co., Ltd., and various food extruders manufactured and sold by The Japan Steel Works, Ltd.

The maltitol aqueous solution that can be used in the present invention needs only to be of such quality that it can form plastic maltitol magma when cooled in the presence of seed crystals, and the origin of the raw materials and manufacturing method are not important.However, those with a maltitol content of 80 to 99% in the solids and a solid concentration of 80 to 98% are preferred, as they are more likely to form maltitol magma.

Also, in particular, sorbitol 0.5-15%, maltitol 80
1.5-10% of maltotriitol and sugar alcohols of higher molecular weight (DP≧3),
A concentration of 80 to 98% is more preferred in achieving the objectives of the present invention, as it is more likely to form maltitol magma continuously, and among sugars with a similar sugar composition, a concentration of 85 to 97% is even more preferred.

Among the components of maltitol aqueous solution, if the sugar alcohols with DP≧3 increase by more than 10%, it becomes difficult to form maltitol magma with sufficient hardness, so it is preferable to avoid increasing the amount of maltotriitol and sugar alcohol components with a molecular weight higher than that.

Furthermore, the aqueous maltitol solution used in the present invention does not necessarily have to be a clear liquid, and may have crystals precipitated and suspended before being fed to the extruder.

On the other hand, when carrying out the present invention, the aqueous maltitol solution is continuously supplied to the extruder, and it is preferable that the temperature of the aqueous maltitol solution at this time be 50 to 150°C in order to prevent phenomena such as decomposition of the components of the aqueous maltitol solution or discoloration due to burning, etc. Furthermore, this is also preferable because it reduces the viscosity of the aqueous maltitol solution, increases its fluidity, making it easier to handle, and is a temperature that is easy to adjust when cooling to a temperature at which maltitol magma is easily formed after introduction into the extruder.

The supply rate of the maltitol aqueous solution depends greatly on the internal capacity, residence time, cooling capacity, stirring capacity, etc. of the extruder used. For example, when using a commercially available food extruder, TEX38FSS-20AW-V type manufactured by The Japan Steel Works, Ltd., a supply rate of approximately 10 to 30 kg per hour is preferred because it ensures sufficient cooling and kneading and the discharged maltitol magma has sufficient hardness.

The aqueous maltitol solution is introduced into the first zone of the extruder, cooled and kneaded, and then transported to the second zone connected to the first zone. The preferred temperature range in the first zone is 50
~90℃.

If the temperature of the aqueous maltitol solution in the first zone is below 50°C or above 90°C, good production of maltitol magma cannot be expected, and this is not preferred.

Next, seed crystals are added in the second zone of the extruder, but the seed crystals do not necessarily have to be maltitol crystalline molten crystalline maltitol; maltitol crystalline molten crystalline maltitol obtained by a molten crystalline molten crystalline maltitol fractionation method can also be used.

The quality of the maltitol seed crystals is preferably the same as that of the aqueous maltitol solution supplied, in order to facilitate quality control of the finished product, but it does not necessarily have to be the same.

The timing for adding and kneading the seed crystals is preferably when the temperature of the aqueous maltitol solution supplied to the extruder reaches 50 to 80°C. If the seed crystals are added at a temperature lower than 50°C, the viscosity of the aqueous maltitol solution will be high, and it will take time to knead the seed crystals.
This is undesirable because it has the disadvantages of slow crystal growth rate after the maltitol magma is generated, and the proportion of glassy solid in the generated maltitol magma becomes high, which has an adverse effect on the shelf life of the product.

Moreover, if the temperature exceeds 80°C, it is not preferable because the seed crystals may dissolve.

Furthermore, the addition rate of the seed crystals is influenced by and varies depending on the concentration, introduction rate, quality, addition temperature, etc. of the maltitol aqueous solution. However, it is preferable to add the seed crystals at a rate of approximately 3 to 80% of the weight of maltitol magma extruded per unit time (extrusion rate), as this contributes to the production of maltitol magma with an appropriate hardness. For example, when the extrusion rate of maltitol magma is 30 kg/Hr, the addition rate should be 0.9 kg/Hr to 2.0 kg/Hr.
This is about 4kg/Hr.

The addition method may be either continuous or intermittent.

However, continuous addition is preferred, since uniform dispersion of seed crystals in the aqueous maltitol solution is advantageous for forming maltitol magma in a short period of time.

Next, the aqueous maltitol solution and seed crystals supplied as described above are cooled and kneaded in the third zone or later of the extruder, but the third zone or later does not necessarily have to be a single zone and may be composed of multiple zones.

If there is only one zone after the third zone, the third zone becomes the final zone; if there are two zones after the third zone, the fourth zone becomes the final zone; and if there are three zones after the third zone, the fifth zone becomes the final zone.

The cooling and kneading conditions are as follows in the case of the extruder:
The temperature in the final cooling and kneading zone is kept in the range of 25 to 60°C, the screw rotation speed is set to about 60 rpm, and 1
It is preferable to hold the mixture for about 2 minutes to obtain maltitol magma of appropriate hardness.

Furthermore, when discharged from the extruder, the shape of the maltitol molten crystals with improved magma-like properties is linear,
The shape can be freely selected from rods, plates, etc., but for example, when forming thin rods, it is preferable to discharge them at a diameter of about 2 to 6 mm, as this facilitates subsequent steps such as aging, coarse crushing, and drying, which may be carried out as needed.

The maltitol crystalline solids obtained in this manner have improved physical properties and are significantly more moisture-absorbent than maltitol crystalline solids produced by spray drying or fluidized bed drying. Furthermore, the growth direction of the maltitol crystalline solids is more uniform than that of maltitol crystalline solids produced by block crushing, so that they have excellent compression properties, allowing tablets of high hardness to be obtained even when directly compressed.

Furthermore, the powder has a high apparent specific gravity, so there is little scattering of fine powder, and the powder can be stored and transported using small containers and transport equipment.
It has excellent features such as the ability to reuse containers for other sugar alcohols.

The discharged magma-like maltitol crystalline solids with improved physical properties can be used as a product as is, but may be subjected to processes such as aging, coarse grinding, drying, grinding, and classification depending on the storage properties and ease of handling of the product.

The preferred conditions for aging the molten maltitol crystals with improved magma-like properties obtained by carrying out the present invention are 15 to 80°C for 5 to 120 minutes, but it is also possible to ripen them at 55 to 70°C for 15 minutes.
It is more preferable to set the time to about 30 minutes in order to prevent the powder product obtained thereafter from clumping together.

There are no particular restrictions on the method for carrying out the aging, but for example, a method of exposing the material to hot air while moving it on a metal mesh belt, or a method of aging it in an incubator, etc. can be used.

The method and conditions for coarse grinding do not need to be particularly limited. When the maltitol molten crystals having improved magma-like properties as described above are discharged in the form of thin rods, the rods can be crushed for 5 to 10 minutes.
It is sufficient to cut it to a length of about 15 mm.

When performing coarse grinding, for example, a commercially available Feather Mill FM
-1 type (manufactured by Hosokawa Micron Corporation) can be advantageously used.

There are no particular restrictions on the drying of the maltitol crystalline solids with improved physical properties obtained by the present invention. However, if it is desired to keep the moisture content of the product below 1%, the drying temperature should be 80 to 115°C.
By drying at about this temperature, the object can be achieved in a relatively short time.

The drying can be carried out in two or more stages under different drying conditions, and the pressure can range from normal pressure to reduced pressure.

The drying method that can be advantageously adopted is as follows:
For example, there are vibration conveyor type drying methods, disk type drying methods, hopper dryer type drying methods, drum rotation type drying methods, and the like.

5. Brief Description of the Drawings Figure 1 is a scanning electron micrograph of the powdered maltitol crystalline densities after drying, grinding and classification according to the present invention;
(a) is a photograph at a magnification of 200 times, and (b) is a photograph at a magnification of 1000 times.

FIG. 2 shows scanning electron micrographs of conventional powdered maltitol crystalline densities, where (a) is a photograph at 200x magnification and (b) is a photograph at 1000x magnification.

6. BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be explained in more detail below with reference to examples and comparative examples, but the present invention is not limited to these examples. In the following examples, % represents % by weight unless otherwise specified.

Example 1 (1) A maltitol aqueous solution as a raw material was adjusted to a concentration of 93.5%, and the raw material was introduced at a rate of 22 kg/Hr. The first zone was where the raw material was cooled and kneaded, and the second zone was where seed crystals were introduced and cooled and kneaded.
The mixture was fed into the first zone of a food-grade twin-screw extruder (TEX38FSS-20AW-V, manufactured by The Japan Steel Works, Ltd.) having a long, narrow cooling and kneading zone consisting of a first zone, a third zone (final zone) for cooling and kneading continuously from the second zone, and a third zone (final zone) for cooling and kneading the mixture. The mixture was then kneaded and transported at 60 revolutions per minute.

The sugar composition of the maltitol solution is 1.2% sorbitol,
The aqueous maltitol solution used was 94.0% maltitol and 4.8% sugar alcohol with a DP of 3 or more. The temperature of the aqueous maltitol solution before feeding was 98°C, and the temperature of the aqueous maltitol solution in the first zone was adjusted to 80°C.

(2) The temperature of the aqueous maltitol solution in the second zone of the extruder was adjusted to 60°C, and maltitol molten crystals (moisture content: 0.3%) having the same composition as the aqueous maltitol solution as seed crystals were fed into the second zone at a rate of 8 kg/hr (approximately 26.7% of the extrusion rate) to form maltitol magma.

(3) The maltitol magma in the third zone, which is the final zone of the extruder in this example, is cooled to 40°C, and approximately 30 kJ is extruded from a nozzle with 12 4 mm extrusion holes.
When extruded at a rate of 1000g/hr, the temperature of the extruded maltitol magma was 69°C and its moisture content was 3.9%.

The maltitol magma obtained by the first step consisting of (1) to (3) above was easy to handle, with no sticky surface and no plasticity, so that it could be easily broken by bending it by hand.

The average residence time of the contents from the first zone to the final zone was about 1.5 minutes.

(4) The extruded maltitol magma was placed on a stainless steel tray and aged for 20 minutes at 60°C in a circulating air dryer (TR-ED type, manufactured by Trio Science Co., Ltd.), completing the second step.

(5) Next, the matured maltitol magma was removed from the dryer, cooled to room temperature, and coarsely pulverized in a pulverizer (FM-1 Feather Mill, manufactured by Hosokawa Micron Corporation).

(6) After coarse grinding, the product is dried by air at 95°C for 130 minutes to remove moisture.
0.5% of crystalline maltitol with improved physical properties was obtained.

The time required to reach this stage was approximately 2 hours and 40 minutes, which is approximately 1 hour and 15 minutes longer than when a product of similar quality is produced using the block crushing method.
Compared with the time required for the production of maltitol, it was possible to produce dense crystalline maltitol in a significantly shorter time than the time required for the production of maltitol.

Furthermore, after this material was crushed and classified, and the third step was completed to obtain a powder of maltitol crystalline molten salts, the powder remained in good condition with no caking or clumping even after being stored in a kraft paper bag for one month.

Example 2 (1) The concentration of the maltitol aqueous solution was 92.5%, and the supply rate was
16 kg/Hr, sugar composition of maltitol aqueous solution: sorbitol 1.0%, maltitol 90.3%, sugar alcohol of DP ≥ 3
8.7%, the temperature of the maltitol aqueous solution before feeding was 95°C,
The temperature of the aqueous maltitol solution in the zone was adjusted to 65°C, and the other operations were the same as in Example 1 (1).

(2) The aqueous maltitol solution in the second zone of the extruder was adjusted to 55°C, and maltitol crystalline syrup (moisture content 0.2%) was fed at a rate of 12 kg/hr (approximately 42.9% of the extrusion rate), and maltitol magma was formed in the same manner as in (2) of Example 1.

(3) In this embodiment, the cooling and kneading zones following the second zone consist of two zones, the third zone and the fourth zone, and the fourth zone is the final zone. The maltitol magma in the third and fourth zones of the extruder is cooled stepwise to 45°C and 38°C, respectively.
The first extrusion step was completed at a rate of approximately 28 kg/hr from a nozzle with 18 3 mm extrusion holes, in the same manner as in Example 1 (3). The temperature of the extruded maltitol magma was 67°C, and its moisture content was 4.1%.

(4) The second step was completed by aging in the same manner as in (4) of Example 1, except that the aging conditions were changed to 70°C and 15 minutes.

(5) Then, the mixture was coarsely crushed in the same manner as in Example 1.

(6) The coarsely ground product was dried in a blower at 90°C for 160 minutes in the same manner as in Example 1(6), to obtain maltitol crystalline molten salts with improved physical properties and a moisture content of 0.6%.

Example 3 (1) The concentration of the maltitol aqueous solution was 93.0%, and the supply rate was
12 kg/Hr, sugar composition of maltitol aqueous solution: sorbitol 4.0%, maltitol 87.8%, sugar alcohol of DP ≧3
8.2%, the temperature of the maltitol aqueous solution before supplying was 85°C,
The temperature of the aqueous maltitol solution in the zone was adjusted to 60°C, and the other operations were the same as in Example 1 (1).

(2) The same procedure as in Example 1 was repeated except that the temperature of the aqueous maltitol solution in the second zone of the extruder was adjusted to 55°C and the rate of crystalline maltitol was 12 kg/Hr (50% of the extrusion rate).
Maltitol magma was formed in the same manner as in 2(2).

(3) In this embodiment, the cooling and kneading zones following the second zone consist of two zones, the third zone and the fourth zone, and the fourth zone is the final zone. The maltitol magma in the third and fourth zones of the extruder is cooled stepwise to 38°C and 35°C, respectively.
The first extrusion step was completed in the same manner as in Example 1 (3) above, except that the extrusion was carried out at a rate of approximately 24 kg/hr from a nozzle with 18 3 mm extrusion holes. The temperature of the extruded maltitol magma was 62°C and its moisture content was 4.9%. The resulting maltitol magma had a slightly sticky surface and was plastic, but was easy to handle, as it could be easily bent by hand a few minutes after extrusion.

(4) The second step was completed by aging in the same manner as in (4) of Example 1, except that the aging conditions were changed to 60°C and 30 minutes.

(5) Then, the mixture was coarsely crushed in the same manner as in (5) of Example 1.

(6) After coarse grinding, the product is first heated at 85°C for 200 minutes.
Thereafter, the mixture was further heated at 105°C for 100 minutes to obtain Example 1(6).
The mixture was dried with a blower in the same manner as in the above to obtain molten crystalline maltitol with improved properties and a moisture content of 0.6%.

Example 4 (1) The concentration of the maltitol aqueous solution was 89.0%, and the supply rate was
The same procedure as in Example 1 (1) was carried out, except that the rate was 11.4 kg/Hr and the sugar composition of the maltitol aqueous solution was 1.0% sorbitol, 95.2% maltitol, and 3.8% sugar alcohol with a DP of 3 or more.

(2) Maltitol crystalline syrup (moisture 0.5%) of the same composition as the maltitol aqueous solution was extruded at a rate of 13.7 kg/Hr (approximately 54.6 times the extrusion rate).
%), the same procedure as in (2) of Example 1 was carried out to form maltitol magma.

(3) After carrying out the same procedure as in (3) of Example 1, maltitol magma was obtained which was at 65°C at the time of extrusion and had a moisture content of 3.1%.

(4) Maltitol magma was aged under the same conditions as in (4) of Example 1.

(5) Then, the mixture was coarsely crushed in the same manner as in Example 1.

(6) The product after coarse grinding was dried in the same manner as in (6) of Example 1 to obtain crystalline maltitol containing 0.5% water and having improved physical properties.

The powder-like maltitol crystalline syrup with improved physical properties obtained after drying, grinding and classification in the third step of Comparative Example 1 was used as the product of the present invention. To compare with the product of the present invention, maltitol crystalline syrup was prepared by the conventional method described below and used as a control product.

An aqueous maltitol solution having the same sugar composition as in Example 1 was adjusted to a concentration of 88%, placed in a crystallizer, heated to 50°C, and anhydrous crystalline maltitol seed crystals were added in an amount of 2% by weight based on the solid content of the aqueous maltitol solution. The mixture was stirred slowly for 2 minutes.
After being kept for 1 hour, the mixture was transferred to a tray and left to stand for 4 days to crystallize and solidify. The crystallized solid was then removed from the tray, crushed in a cutting-type crusher, and dried to obtain 20 kg of powdered maltitol molten crystals containing anhydrous crystalline maltitol (control product).

The inventive product and the control product were then photographed at magnifications of 200x and 1000x, respectively, using a typical scanning electron microscope.

FIG. 1 is an electron microscope photograph of the product of the present invention, (a) is the magnification.
(a) is a 200x magnification photograph, and (b) is a 1000x magnification photograph.

Figure 2 shows an electron microscope photograph of the control product, (a) at a magnification of 20
(a) is a photograph taken at 0x magnification, and (b) is a photograph taken at 1000x magnification.

Comparing Fig. 1 with Fig. 2, it can be seen that the product of the present invention has a relatively denser crystal structure than the conventional product.

In addition, for the product of the present invention and the control product, 20 meshes of 50 mesh or more were used.
Samples in the particle size range of less than 100 mesh were taken out and prepared, and the apparent specific gravity and oil absorption rate were measured for each.

The oil absorption rate was measured as follows.

Add castor oil to 15 g of powder sample and mix. After 5 minutes, transfer to a centrifuge tube (with holes in the bottom) lined with a filter cloth and centrifuge at 1300 G for 1
The mixture was centrifuged for 10 minutes, the weight of the cake remaining on the filter cloth was measured, and the weight was calculated using the following formula.

Oil absorption rate (%) = {[(cake weight) - 15]/15} x 100 The measurement results are shown in Table 1.

From Table 1, it can be seen that the apparent specific gravity of the product of the present invention is heavier than that of the control product.
It can be seen that the oil absorption rate is low.

As described above, the maltitol crystalline solids with improved physical properties according to the present invention have a crushed, relatively dense crystalline structure that can be seen at 1000x magnification compared to the maltitol crystalline solids obtained by conventional methods, have a high apparent specific gravity, comparable to that of other sugar alcohols such as sorbitol, and have low oil absorption properties.

Therefore, (a) the volume is not increased, no dedicated packaging materials or containers are required, and packaging materials and containers for other sugar alcohols can be used, and no large space or transport equipment is required for storage or transportation.

(b) Because the powder is heavy, scattering of fine powder is unlikely to occur, and the powder can be used for various purposes.

(c) The crystalline structure is dense, so the tablets have excellent hardness when directly compressed.

Furthermore, the method for producing dense maltitol crystals according to the present invention makes it possible to produce dense maltitol crystals with improved physical properties in an extremely short time and through a simple process that does not require much manpower, thereby significantly reducing the storage space and storage containers required for work-in-progress and making it easier to automate the process.

Claims (9)

[Claims] Claim 1: a) After pulverization and classification, the crushed material can be viewed under a scanning electron microscope at 1000x magnification.
Maltitol crystalline densities are: a) dense crystalline structure; b) apparent specific gravity of the densified crystalline powder after crushing and classification of 50 mesh or more and 20 mesh or less is 0.650 to 0.750; c) oil absorption of the densified crystalline powder after crushing and classification of 50 mesh or more and 20 mesh or less is 7.0% to 17%; and d) melting point is lower than that of maltitol crystals. 2. The maltitol crystalline solids according to claim 1, wherein the maltitol content in the solid is 80 to 98% by weight, the remainder being 0.5 to 15% by weight of sorbitol and 1.5 to 10% by weight of maltotriitol and higher degrees of polymerization (DP)
Maltitol crystalline molten sugars consisting of ≧3 sugar alcohols. [Claim 3] A maltitol molten crystal described in any one of claims 1 or 2, produced by continuously supplying an aqueous maltitol solution to an extruder having an elongated cooling and kneading zone, cooling and kneading the solution in the presence of seed crystals to form maltitol magma, and then continuously extruding the maltitol magma from an extrusion nozzle. 4. A maltitol aqueous solution having a concentration of 80 to 98% by weight and a maltitol content of 80 to 99% by weight in the solid content,
The mixture is continuously fed into a first zone of an extruder having an elongated cooling and kneading zone consisting of a plurality of successive zones, and the mixture is cooled to a temperature of 50 to 1000°C.
Cool to 90°C and knead, and the maltitol solution inside will be 50-
In the second zone, where the temperature has reached 80°C, 3 to 80% by weight of seed crystals based on the extrusion amount are added continuously or intermittently and kneaded. The mixture is then cooled and kneaded in the third zone, which continues to the second zone.
2. The maltitol crystalline mixture according to claim 1, which is produced by continuously extruding the maltitol magma formed after cooling and kneading to 25 to 60°C through an extrusion nozzle. a) A maltitol aqueous solution having a concentration of 80-98% by weight and a solid content of 0.5-15% by weight of sorbitol, 80-98% by weight of maltitol, and 1.5-10% by weight of maltotriitol or a sugar alcohol having a molecular weight of 3 or more (DP≧3) is cooled and cooled in a long, narrow cooling and refrigerating machine comprising a plurality of continuous zones.
a) continuously feeding the maltitol magma into a first zone of an extruder having kneading zones, cooling and kneading it to 50-90°C, and then adding 3-80% by weight of seed crystals based on the extrusion amount continuously or intermittently to a second zone in which the maltitol aqueous solution therein has reached 50-80°C, and kneading the mixture, and then further cooling and kneading the mixture in a third zone, and finally cooling and kneading the mixture in a final zone to 25-60°C, after which the resulting maltitol magma is extruded from an extrusion nozzle; b) the extruded maltitol magma is kneaded at 15-80°C for 5-30 minutes.
a second step of aging for 10 minutes; c) then coarsely grinding the aged maltitol magma;
2. The crystalline maltitol according to claim 1, which is produced by successively passing through the steps of: (a) drying the crystalline maltitol at 80 to 115°C for 60 minutes or more; and (b) grinding and classifying the crystalline maltitol. [Claim 6] A method for producing crystalline maltitol containing molten crystals, characterized in that an aqueous maltitol solution is continuously supplied to an extruder having a long cooling and kneading zone, and cooled and kneaded in the presence of seed crystals to generate maltitol magma, which is then continuously extruded from an extrusion nozzle. [Claim 7] When producing crystalline maltitol, the concentration is 80 to 98% by weight and the maltitol content in the solid content is 80
An aqueous maltitol solution of up to 99% by weight is continuously fed to the first zone of an extruder having a long and narrow cooling and kneading zone consisting of a plurality of continuous zones, and cooled to 50 to 90°C.
A method for producing molten crystalline maltitol, characterized in that 3 to 80% by weight of seed crystals relative to the extrusion amount are added and kneaded continuously or intermittently in a second zone where the maltitol aqueous solution reaches 50 to 80°C, and then the mixture is cooled and kneaded in a continuous third zone, and cooled and kneaded to 25 to 60°C in the final zone, after which the formed maltitol magma is continuously extruded from an extrusion nozzle. [Claim 8] In producing crystalline maltitol, a) a maltitol content in the solid content is 80 to 98% by weight
An aqueous maltitol solution having a weight of 80 to 99% is continuously fed to the first zone of an extruder having a long and narrow cooling and kneading zone consisting of a plurality of continuous zones, and cooled to 50 to 90°C.
a) mixing the maltitol magma in the second zone, in which the aqueous maltitol solution reaches 50 to 80°C, by adding and mixing 3 to 80% by weight of seed crystals continuously or intermittently based on the extrusion amount, and then cooling and mixing in the third zone, and finally cooling and mixing to 25 to 60°C in the final zone, after which the resulting maltitol magma is extruded from an extrusion nozzle; b) mixing the extruded maltitol magma in the second zone, in which the aqueous maltitol solution reaches 50 to 80°C, by adding and mixing 3 to 80% by weight of seed crystals continuously or intermittently based on the extrusion amount, and then cooling and mixing in the third zone, and finally cooling and mixing to 25 to 60°C in the final zone, after which the resulting maltitol magma is extruded from an extrusion nozzle;
a second step of aging for 10 minutes; c) then coarsely grinding the aged maltitol magma;
a third step of drying the crystalline maltitol at 80 to 115°C for 60 minutes or more, and then pulverizing and classifying the crystalline maltitol. 9. The aqueous maltitol solution containing 0.5% sorbitol
9. A method for producing crystalline maltitol with a dense structure according to claim 6, characterized in that the composition of the crystalline maltitol is 80-98% by weight, 1.5-10% by weight of maltotriitol and sugar alcohols with a molecular weight of 3 or higher (DP≧3).