JPH0748300A - Method for producing sorbitol powder having high fluidity - Google Patents

Abstract

PURPOSE:To provide a method for producing sorbitol powder having high fluidity, capable of continuously producing and having high economical efficiency. CONSTITUTION:An aqueous solution of sorbitol adjusted to 89.0-99.9wt.% purity, 69-80wt.% concentration and 10-40 deg.C temperature is continuously fed to a sorbitol massecuite tank previously kept in the range of 5-35wt.% crystal amount at a rate corresponding to 0.5-80wt.% of the massecuite weight per hr. At the same time, the massecuite continuously pulled out from the outlet of the massecuite tank at a similar rate as feed rate of the aqueous solution of sorbitol is introduced into spray-drying apparatus controlled to 30-90 deg. air temperature and spray-dried. Thereby, sorbitol powder having high fluidity and free from scattering of fine powder is obtained.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing sorbitol powder, and more particularly to a method for producing sorbitol powder having high fluidity.

[0002]

2. Description of the Related Art Sorbitol is a typical sugar alcohol contained as a sweetening component in fruits and the like, and is widely used as various foods, pharmaceuticals, cosmetics, various industrial raw materials and the like. This sorbitol is industrially produced by catalytically reducing glucose, and its product form is about 70 wt% (hereinafter "wt%" may be simply referred to as "%") of an aqueous solution and powder. Although there are two types, the conventional powders are mainly crystalline powders having low hygroscopicity, that is, the gamma-type sorbitol crystal component in the powders is required to have high quality.

As a conventional method for producing the above-mentioned powder product,
For example, Japanese Patent Publication No. 52-20444 and Japanese Patent Publication No. 49-362.
A method for producing a sorbitol powder product as disclosed in Japanese Patent Publication No. 06, etc. is known. However, the products obtained from these production methods have a crystal content of 96.
It was adopted because it emphasized that it was as high as ~ 99%, and its manufacturing method was a concentrated aqueous solution in which the water content was reduced to about 15% or less by heating and concentrating the sorbitol aqueous solution, or melted by further concentrating the water content to 1% or less. While continuously pouring the sorbitol in the form of high temperature into the kneader, the sorbitol concentrated aqueous solution or the melt has a solid content of about 1 to about 1% by weight.
50% powdered sorbitol was added as a seed, kneaded to promote the growth of fine crystals, shaped into noodles and extruded, and the solidified spaghetti-like sorbitol was cooled and then pulverized.

In addition to the above-mentioned manufacturing method, Japanese Patent Laid-Open Publication No. 51-108005 and Japanese Patent Publication No. 55-36646.
The method disclosed in the publication is also known. That is, the former is based on the fluidized-drying method that emphasizes the fluidity of the powder,
This is a manufacturing method in which a sorbitol liquid is sprayed and adhered to the surface of fine powder sorbitol. The latter is based on a fluidized-drying method that emphasizes the fluidity of the powder. A slurry is prepared by aging for a long time by a batchwise method, and only an amount adjusted by the batchwise method is spray-dried to form sorbitol. The manufacturing method is to obtain powder.

[0005]

However, in the fields of pharmaceuticals and foods, sorbitol powder with high fluidity is demanded, and further higher economic efficiency is required for its production method. Various problems associated with sorbitol powders produced by the method have been emphasized. That is, sorbitol has a phenomenon in which the viscosity of the slurry rapidly increases due to the abrupt formation of crystals in the supersaturated aqueous solution.
When the manufacturing method disclosed in Japanese Patent No. 444 is used, a very strong force is required for kneading, and accordingly, a kneading device having high strength and strong power are required. In addition, this manufacturing method has a problem that it is economically inefficient because it is necessary to use a large amount of seeds, that is, seed crystals of 20 to 30%. Furthermore, this manufacturing method requires a crushing step,
The sorbitol produced by this method has a very low fluidity, that is, the angle of repose when powdered to about 50 mesh is about 45 °, so it is a commonly used means for automation such as flowing with air in piping. However, its use is limited due to the difficulty of handling due to the low fluidity of the powder, and with this manufacturing method, about 20% of fine powder is generated. Since it is unavoidable, when producing sorbitol powder or when using sorbitol powder, fine powder scatters, contaminates the work environment, or uses a classification process for applications requiring a specific range of particle size, etc. In addition, there is a problem that both the powder fraction having a large particle size and the fine powder fraction need to be returned to the dissolving step or the kneading step again. The manufacturing method disclosed in Japanese Examined Patent Publication No. 49-36206 has substantially the same manufacturing and quality problems as the manufacturing method of Japanese Examined Patent Publication No. 52-20444.

Further, in the fluidized-drying method disclosed in the above-mentioned Japanese Patent Laid-Open No. 51-108005, it is necessary to retain a large amount of fine powdery sorbitol in the apparatus, which is economically inefficient. Since the crystallization rate of sprayed sorbitol is low, the crystallization rate of the surface of the obtained powder is low, and therefore the fluidity immediately after production is high to some extent, but eventually the powder becomes highly hygroscopic. However, it has various quality defects such as deterioration of fluidity during storage and solidification in a lump form, and has not been put to practical use.

Further, in the spray drying method disclosed in Japanese Patent Publication No. 55-36646, there is a method of using 20% or more of seed crystals when preparing a slurry, which is extremely economically disadvantageous. In addition, when the inventors of the present invention additionally tested this manufacturing method, it was impossible to perform continuous spray drying because powder with high hygroscopicity was often deposited and accumulated on the wall of the spray drying device. There was a problem.

[0008] As described above, the conventional manufacturing methods are all focused on obtaining a crystalline powder having a low hygroscopic property, and the fluidity of the powder has been sacrificed. Therefore, continuous sorbitol is used. There has been no method for producing highly flowable powdered sorbitol by an economically advantageous continuous process from preparation of a musket to continuous spray drying.

In order to solve various problems of the above-mentioned conventional manufacturing method and the sorbitol powder obtained as a result of carrying out the method, the inventors of the present invention conducted diligent research and found that the sorbitol mass kit tank in which the amount of crystals was adjusted in advance was used. Sorbitol mass kit was continuously prepared by supplying sorbitol aqueous solution under strict condition settings, and by spray-drying it continuously, it succeeded in solving various problems of conventional methods. Furthermore, the present invention has been completed by succeeding in obtaining a sorbitol powder having high fluidity and free from scattering of fine powder. Therefore, an object of the present invention is to solve the problems of the conventional manufacturing method and to provide a method for continuously and economically manufacturing sorbitol powder having high fluidity.

[0010]

In order to achieve the above object, the method for producing a sorbitol powder having high fluidity according to the present invention has a purity of 89.0-99.9% by weight and a concentration of 69-8.
The sorbitol aqueous solution adjusted to 0 wt% and the temperature of 10 to 40 ° C. was placed in a sorbitol muskit tank in which the crystallization amount was preliminarily kept in the range of 5 to 35 wt%, and the sorbitol weight was adjusted to 0.5 to 80 wt% of the maskit per hour. A spray-drying device in which the mass kit is continuously supplied at a corresponding speed, and at the same time, the mass kit continuously extracted from the outlet of the mass kit tank at the same speed as the supply speed of the sorbitol aqueous solution is adjusted to an air temperature of 30 to 90 ° C. The purpose of this method is to introduce and spray-dry. Further, it is desirable that the supply rate of the sorbitol aqueous solution to the sorbitol mass kit tank is adjusted to a range of 5 to 40% by weight per hour with respect to the weight of the sorbitol mass kit in the sorbitol mass kit tank.

[0011]

According to the method for producing powdered sorbitol having high fluidity according to the present invention, the sorbitol aqueous solution is supplied to a sorbitol mass kit tank in which the amount of crystals is adjusted in advance under predetermined conditions, and the sorbitol mass is continuously supplied. A sorbitol powder can be obtained by preparing a kit and further continuously spray-drying the kit. In addition, the obtained sorbitol powder has a repose angle of about 30 to 35 ° when it is made into a powder of about 20 to 50 mesh, which is extremely high in fluidity as compared with about 40 to 48 ° of conventional products, and it is a fine powder. It is possible to obtain a sorbitol powder which does not scatter.

[0012]

EXAMPLES Preferred examples of the method for producing a highly fluid sorbitol powder according to the present invention will be described below. The sorbitol used in the present invention is required to have a quality capable of producing a sorbitol mass kit under the conditions of the present invention, and a preferable sorbitol purity is 89.0-9.
9.9% by weight is mentioned, and there are no special restrictions on other manufacturing methods. When the sorbitol purity is less than 89%, the proportion of maltitol, maltotriitol, maltotetriitol, sugar alcohols having a higher degree of polymerization than the remaining components, such as sugar alcohol, is increased, and when applied to the present invention. Although it forms a powder form, it tends to be difficult to handle as a powder product due to its high hygroscopicity, and it adheres to the vessel wall during the spraying process and makes continuous operation difficult. Not desirable for reasons. On the other hand, if the purity exceeds 99.9%, it is difficult to increase the purity in producing the sorbitol aqueous solution, and as a result, a large amount of cost is required, which is one of the features of the present invention. It is not preferable because it impairs economy. The concentration of sorbitol used in the present invention is required to be adjusted to 69 to 80%, but if it is less than 69%, the amount of crystals in the sorbitol mass kit tank is often reduced, and it is obtained after spray drying. The hygroscopicity of the resulting powder is often high, and continuous production, which is one of the major features of the present invention, is often difficult, which is not preferable. Further, when the present invention is carried out under the condition where the concentration exceeds 80%, the amount of crystals in the sorbitol mass kit tank is often too large, and therefore, the viscosity of the mass kit rapidly increases and continuous It is not preferable because it is difficult to manufacture.

The temperature of the sorbitol aqueous solution and the temperature of the sorbitol mask kit used in the present invention are 10 to 40 ° C.
Must be kept in the range of 10 ℃
If less than, the viscosity of the sorbitol mass kit becomes too high and the amount of crystals in the sorbitol mass kit tank becomes too large, and further, the entire mass kit tank may be solidified, which is not preferable. , 40 ° C
It is not preferable to carry out the reaction at a temperature exceeding the above range because the amount of crystals in the mass kit tank tends to be insufficient.

In carrying out the present invention, the rate of supplying the sorbitol solution to the above-mentioned mask kit tank is preferably within the range of 0.5 to 80%, more preferably 5 to 40%, of the weight of the mask kit per hour. By setting the amount of crystals in the mask to a certain range, that is, 5 crystals in the mask.
Can be kept at ~ 35%. If the supply rate of the sorbitol aqueous solution is less than 0.5%, it is possible to manufacture a mass kit, but it is economically disadvantageous because large equipment is required despite the small amount of production, so that condition should be adopted. Should be avoided. On the other hand, when the feed rate is more than 80%, the amount of crystals in the mass kit decreases, and finally spray drying cannot be performed, that is, less than 5%. Recruitment should also be avoided.

Further, the amount of crystals in the sorbitol mass kit for carrying out the present invention can be adjusted to a viscosity range that is easy for the mass kit to handle, and a powder having low hygroscopicity can be obtained when spray-dried. It is preferably 5 to 35% of the weight of the mass kit, but the crystal amount is 5
If it is less than%, the powder crystal content obtained after spray drying is low and the hygroscopicity becomes high, which is not preferable,
If it exceeds 35%, the crystal content of the obtained powder will be high, but the viscosity of the mass kit will be high, and the mass kit may be solidified, which is not preferable.

When carrying out the present invention for the first time, it is necessary to prepare a sorbitol mass kit in advance. In that case, a small amount of the above sorbitol aqueous solution is used at 10 ° C to 30 ° C.
A sorbitol mass kit tank is filled with what has been crystallized by cooling it to a degree to form a supersaturated state and vigorously stirring this at a peripheral speed of a stirring blade of about 100 m / min. The sorbitol aqueous solution was added as seed crystals to the aqueous solution of sorbitol, and then the mixture was gently stirred to form a sorbitol musket in the tank, and after the crystal content in the tank exceeded 5%, the sorbitol aqueous solution was supplied to the tank. The method of starting can be advantageously employed. Further, as another modified method, the sorbitol aqueous solution filled in the sorbitol mass kit tank is added with 0.1 to 0.1% by weight of the aqueous solution.
After adding about 3% sorbitol powder and gently stirring to form a sorbitol mass kit in the tank, a continuous method can be started in the same manner as described above.

The amount of crystals of the sorbitol mass kit thus obtained is 5 to 3 in the mass kit as described above.
It is necessary to maintain 5%, and it is most certain to take out a part of the mass kit and actually filter to check the amount of crystals, but the amount of crystals generated from the sorbitol solution used in advance. It is also possible to check the relationship between the viscosity and the viscosity and then control the viscosity. When the amount of crystals in the sorbitol mass kit tends to decrease, the amount of crystals is reduced by decreasing the supply amount of the sorbitol aqueous solution, increasing the concentration of the sorbitol aqueous solution, and further lowering the supply temperature of the sorbitol aqueous solution. Although it can be increased, the most effective and fastest of these methods is to reduce the supply of sorbitol aqueous solution. Further, as a modification of the method for keeping the amount of crystals in the sorbitol mass kit constant, it is also possible to advantageously employ a part of the sorbitol mass kit extracted from the mass kit tank to return to the mass kit tank. The sorbitol mass kit obtained as described above is used at a temperature of 10% in order to maintain the amount of crystals, prevent the crystals from settling, maintain the viscosity, etc.
It is preferable to maintain the temperature at -40 ° C and gently stir, but there is no particular restriction on the stirring method, stirring speed, and shape of the stirring blade.

Next, the sorbitol maskit obtained as described above is continuously extracted from the muskit tank at the same rate as the supply rate of the sorbitol aqueous solution supplied to the maskit tank, and spray dried. The preferable wind temperature at this time is 30 to 90 ° C., and more preferable wind temperature is 4
It is 0 to 70 ° C. When the air temperature is less than 30 ° C,
It is not preferable because the obtained powder may not be dried sufficiently. If it is carried out at a temperature higher than 90 ° C, the surface of the dried powder will be dissolved or the hardness will be insufficient, so that the powder adheres or is sprayed. Adhesion to the wall of the dryer may occur, which is not preferable.

The sorbitol powder thus obtained has a repose angle of about 30 to 35 ° when made into a powder of about 20 to 50 mesh, and 40 to 48 ° of the conventional product.
Since the fluidity is extremely high compared to the degree, it is much easier to handle and it becomes possible to apply automated means such as transportation by air. Further, the hygroscopicity is also significantly improved as compared with the powder produced by the method disclosed in JP-A No. 51-108005, and it is possible to solidify into a lump during storage under ordinary storage conditions of sorbitol. It hardly occurs.

Example 1 Purity 9 concentrated to a concentration of 80%
5 liters of a 4% sorbitol aqueous solution with an inner diameter of 30 cm,
The mixture was placed in a cylindrical stainless steel container having a volume of 20 liters, and the mixture was stirred at a speed of 300 revolutions per minute (peripheral speed = 113 m / min) using a paddle type stirring blade having a length of 12 cm and a width of 2.1 cm, and the temperature was adjusted to 25 It was kept at ℃. Approximately 2 minutes after starting the operation, the sorbitol liquid was clouded white and sorbitol crystals were confirmed to be generated, and 3 minutes after the start, 5 liters of the sorbitol aqueous solution prepared at a temperature of 25 ° C. and a concentration of 66% was added and stirred, The amount of crystals in the sorbitol mass kit formed after 15 minutes reached about 10%. In a stainless steel tank having a volume of 1200 liters, 1000 kg of a 73% concentration and 94% purity sorbitol aqueous solution was added, and 10 liters of the sorbitol mass kit was gently added while gently stirring with the temperature kept at 25 ° C., and gently for 6 hours. The mixture was continuously stirred to obtain a sorbitol mass kit having a crystal amount of 28%.

Example 2 Purity 9 Concentrated to 78% Concentration
10 liter of 2% sorbitol aqueous solution with an inner diameter of 30c
The mixture was placed in a cylindrical stainless steel container having a volume of 20 m and a volume of 20 liter, and the temperature was set to 45 ° C. while gently stirring at a speed of 30 rotations per minute using a paddle type stirring blade having a length of 8 cm and a width of 2.1 cm. Then gradually cool it to 20 ° C after 1 hour,
20 g of sorbitol fine powder having the same purity as the liquid was added, and the mixture was further gently stirred for 12 hours. As a result, a sorbitol mass kit with a crystal amount of 30% was obtained.

[Embodiment 3] A sorbitol mass kit tank made of stainless steel (volume 1200
1010 liters of sorbitol mass kit was prepared in 1 liter) and kept at a temperature of 25 ° C. with gentle stirring, and then a sorbitol aqueous solution having a concentration of 73%, a purity of 94% and a temperature of 25 ° C. It was supplied at a rate of 200 liters per hour, and at the same time, the sorbitol mass kit was extracted from the lower part of the mass kit tank at the same speed as the supply rate of the sorbitol aqueous solution. The extracted sorbitol mass kit was introduced into an atomizer type spray dryer connected to the tank with a jacketed stainless steel tube, and spray-dried at an air temperature of 55 ° C. to obtain a highly fluid sorbitol powder of the present invention. . The angle of repose of the sorbitol powder of about 50 mesh obtained in this example was 31 ° as a result of measurement with a measuring instrument (PT-D type). Further, as a result of measuring the content rate of the gamma-type crystal by differential scanning calorimetry, the content rate of the gamma-type crystal in sorbitol was 94%.

Example 4 As in Example 2, 10 liters of sorbitol mass kit were prepared in advance in a sorbitol mass kit tank (volume: 20 liters) made of stainless steel and kept at a temperature of 20 ° C. with gentle stirring. Then, a sorbitol aqueous solution having a concentration of 77%, a purity of 92%, and a temperature of 20 ° C. was added from the upper part of the mass kit tank at 7% per hour.
The amount of crystals in the mask is 25
%, And at the same time, the sorbitol maskit was extracted from the lower part of the muskit tank at the same rate as the supply rate of the sorbitol aqueous solution. The extracted sorbitol mass kit was introduced into a nozzle-type spray dryer connected to the tank with a jacketed stainless steel tube, and spray-dried at an air temperature of 60 ° C. to obtain a highly fluid sorbitol powder of the present invention. .
The angle of repose of the sorbitol powder of about 50 mesh obtained in this example was measured in the same manner as in Example 3, and as a result, 3
It was 3 °.

[Example 5] 10 liters of sorbitol mass kit was prepared in advance in the same manner as in Example 2 except that a sorbitol aqueous solution having a concentration of 75%, a purity of 95% and a temperature of 25 ° C was used, and gently stirred. While maintaining the temperature at 25 ° C., the same sorbitol aqueous solution as described above is supplied from the upper part of the mass kit tank at a rate of 4.5 liters per hour so that the amount of crystals in the mass kit is 26%. The sorbitol mass kit was extracted from the lower part of the same at the same rate as the supply rate of the sorbitol aqueous solution. The extracted sorbitol mass kit was obtained in the same manner as in Example 4 except that the air temperature of the spray drier was 55 ° C. to obtain a highly fluid sorbitol powder of the present invention. The angle of repose of the sorbitol powder of about 50 mesh obtained in this example was
The result of measurement in the same manner as in Example 3 was 32 °.

Example 6 A sorbitol mass kit (10 liters) was prepared in advance in the same manner as in Example 2 except that a sorbitol aqueous solution having a concentration of 72%, a purity of 96% and a temperature of 32 ° C. was used, and gently stirred. While maintaining the temperature at 25 ° C., the same sorbitol aqueous solution as described above was supplied from the upper part of the musket tank at a rate of 2.5 liters per hour to set the crystal amount in the musket to 32, and at the same time, The sorbitol mass kit was extracted from the lower part at the same rate as the supply rate of the sorbitol aqueous solution. The extracted sorbitol mass kit was obtained in the same manner as in Example 4 except that the air temperature of the spray drier was set to 65 ° C. to obtain a highly fluid sorbitol powder of the present invention. The angle of repose of the sorbitol powder of about 20 mesh obtained in this example was
The result of measurement in the same manner as in Example 3 was 29 °.

[Example 7] 10 L of sorbitol mass kit was prepared in advance in the same manner as in Example 2 except that an aqueous sorbitol solution having a concentration of 70%, a purity of 97% and a temperature of 35 ° C was used, and gently stirred. While maintaining the temperature at 16 ° C., the same sorbitol aqueous solution as described above was supplied from the top of the mass kit tank at a rate of 2.0 liters per hour to make the crystal amount in the mass kit 28%, and at the same time, the mass kit The sorbitol mass kit was extracted from the lower part of the same at the same rate as the supply rate of the sorbitol aqueous solution. The extracted sorbitol mass kit was obtained in the same manner as in Example 4 except that the air temperature in the spray dryer was set to 70 ° C. to obtain a highly fluid sorbitol powder of the present invention. The angle of repose of the sorbitol powder of about 20 mesh obtained in this example was
The result of measurement in the same manner as in Example 3 was 30 °.

The method for producing a sorbitol powder having high fluidity according to the present invention is not limited to the above-mentioned embodiments, and can be carried out by appropriately modifying it within the scope of the object of the present invention. It goes without saying that it is a thing.

[0028]

As described above, the method for producing a sorbitol powder having a high fluidity according to the present invention is continuously and economically and hygienically compared with the conventional method for producing a sorbitol powder as compared with a conventional product. In comparison, a sorbitol powder having a high fluidity and a low hygroscopicity can be obtained, which has a repose angle of about 30 to 35% when made into a powder of about 20 to 50 mesh.

Further, such improvement of the sorbitol powder makes handling of the powder extremely easy and makes it possible to apply an automatic means such as transportation by air, which is economically advantageous.

In addition, the hygroscopicity is also described in the above-mentioned JP-A-51-108.
It is a significant improvement over the powder produced by the conventional method disclosed in Japanese Patent Publication No. 005, and has a feature that it hardly solidifies into a lump even under the storage condition of ordinary sorbitol powder. The effect obtained by implementing the present invention is extremely large.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Masahiro Niimi 3-24-6 Minami Ushiku-shi, Ibaraki (72) Inventor Kazuaki Kato 2-8-7 Yaesu Chuo-ku, Tokyo Towa Kasei Kogyo Co., Ltd. Within

Claims (2)

[Claims] 1. A purity of 89.0 to 99.9% by weight and a concentration of 6
The sorbitol aqueous solution adjusted to 9 to 80% by weight and the temperature of 10 to 40 ° C. was placed in a sorbitol muskit tank in which the crystallization amount was kept in the range of 5 to 35% by weight in an amount of 0.5 to 80% by weight of the maskit per hour. %, And continuously sprayed from the outlet of the mask kit tank at the same rate as the supply rate of the sorbitol aqueous solution, and the sprayed mass kit was adjusted to a wind temperature of 30 to 90 ° C. A method for producing sorbitol powder having high fluidity, which comprises introducing the sorbitol powder into a drying device and performing spray drying. 2. The supply rate of the sorbitol aqueous solution to the sorbitol mass kit tank is adjusted to a range of 5 to 40% by weight per hour with respect to the weight of the sorbitol mass kit tank in the sorbitol mass kit tank. The method for producing a sorbitol powder having high fluidity according to claim 1.