KR0150250B1 - Preparation of powder of crystalized sorbitol - Google Patents

Abstract

The present invention relates to a method for producing crystalline sorbitol powder. More specifically, the present invention, by adding a sorbitol concentrate or melt to the extruder and adding the final crystals, and then repeatedly extruded by cooling and kneading, it is possible to mass-produce continuously in a short time and simply to produce a crystalline sorbitol powder The crystalline sorbitol powder of the present invention is to concentrate the aqueous sorbitol solution or to melt the sorbitol powder to produce a sorbitol stock solution: the sorbitol stock solution obtained in the electrical process is provided in an extruder having a plurality of cooling / kneading zones. Process of injecting: adding sorbitol seed in the extruder, and extruding by repeatedly cooling and kneading: and manufacturing by the process of cold aging, cutting and pulverizing the extrudate obtained in the electrical process, Crystalline sorbitol powder can be produced continuously in a short time, and by a simple process It has been confirmed that high quality crystalline sorbitol powder can be produced.

Description

Crystalline Solbi Powder Preparation Method

The present invention relates to a method for producing crystalline sorbitol powder. More specifically, the present invention, by adding a sorbitol concentrate or melt to the extruder, and applying a seed, and then repeatedly extruded by cooling and training, it is possible to mass-produce continuously in a short time and simply to produce a crystalline sorbitol powder It is about a method.

Sorbitol is a kind of polyhydric alcohol which is widely contained in natural fruits and is represented by the following molecular formula. The melting point is a compound having a melting point of 90 to 98 ° C depending on the purity, and generally reduces the glucose obtained by hydrolyzing starch. Are prepared.

Since sorbitol has a strong hygroscopicity and a refreshing sweetness, and is chemically stable and soluble in water, it is not only widely used as a moisturizer, supplement, denature agent and quality stabilizer for foods and beverages, but also as a humectant for cosmetics and pharmaceuticals. And it is used as a stabilizer, it is widely used as a synthetic raw material such as various synthetic resins, surfactants and vitamin C.

Such sorbitol is generally marketed in the form of concentrated sorbitol dissolved in water and concentrated. The concentrated sorbitol can be widely used for industrial use due to its low price, but in the manufacture of pharmaceuticals, cosmetics and foods with limited use of moisture It can not be used, and at low temperatures, the viscosity of the concentrated sorbitol is significantly increased or the sorbitol is frozen and has the disadvantage of poor workability.

Therefore, in order to solve the problems of the concentrated sorbitol, attempts have been made to prepare sorbitol powder powdered with sorbitol, but the heating and concentration of the sorbitol aqueous solution to a water content of 1wt% or less according to the manufacturing method of sorbitol powder generally used When the sorbitol powder is prepared by leaving the molten sorbitol in a solid state and then solidifying, the prepared sorbitol powder does not change into an industrially useful crystalline granule or powder state even when pulverized as an amorphous transparent glassy material. The obtained sorbitol powder had a disadvantage that it was difficult to handle and lost the value of the product as it changed to cake form over time even when stored under dry conditions.

In addition, a method of producing crystalline sorbitol powder of high purity is known by adding a seed crystal and a solvent to the sorbitol concentrate, leaving it to stir, and then separating the sorbitol crystal from the mother liquor. It was impossible to have a problem.

Therefore, a series of attempts have been made to solve the problems of the conventional method for preparing sorbitol powder, and such a conventional technique is disclosed in various documents as follows:

Japanese Patent Application Laid-Open No. 52-13801 discloses a creamy sorbitol solution containing 25 to 30% of crystalline sorbitol by adding a seed to a sorbitol concentrate, cooling and stirring, and then spray drying and aging to prepare sorbitol powder. Although this method is disclosed, it is difficult to adjust the crystallization rate for preparing a creamy sorbitol liquid, and when the crystal growth is insufficient, the solid phase of the glass phase solidified during the spraying process is increased, and thus it is easily applied to the wall of the spray dryer. It had a disadvantage of poor workability and difficulty in continuous production.

Japanese Patent Publication No. 49-36206 discloses a method for producing sorbitol powder by continuously supplying and discharging a sorbitol concentrate with a seed to a specific mixer, and then cooling it to room temperature, but not solidified by the electric method. In order to obtain a powder, a long time cooling process is required, which has a disadvantage in that productivity is reduced.

In addition, Korean Patent Publication No. 93-5255 discloses dispersing by adding a seed crystal while stirring the molten sorbitol to a temperature at which the molten sorbitol is not solidified and the seed is not melted, cooled to about 50 to 80 ℃ to obtain a solid, and then A method of preparing crystalline sorbitol in powdery or granular form by maintaining it at the same temperature and cooling to room temperature is disclosed. The foregoing method improves the powdering process so that sorbitol powder does not solidify, but the manufacturing process is very complicated and each process Not only does it take a long time, but a separate facility for storing solids obtained during the manufacturing process is required and a lot of labor is required, which makes it difficult to automate.

In addition, Japanese Patent Publication No. 52-20444 provides a crystalline sorbitol by adding a crystalline sorbitol or concentrate to a concentrated solution and vigorously stirring at an appropriate temperature to form a lump of fine crystals. The method of the present invention is disclosed, but the electric method takes a long time to stir using a kneader, and when extruded the lumps in which the fine crystals are grown, the workability is inferior due to the open-type molding process. Difficulties in the adoption of continuous processes have led to the problem of unsuitable mass production.

Therefore, in order to solve the above problems of the prior art, the need to develop a method capable of producing a high-quality crystalline sorbitol powder in a short time and can be continuously produced in a short time has been constantly emerging.

After all, it is an object of the present invention to provide a method capable of producing a high-quality crystalline sorbitol powder by a simple process that can be mass-produced in a short time continuously.

The crystalline sorbitol powder of the present invention is injected into an extruder equipped with a plurality of cooling / kneading zones, sorbitol concentrate or melt, and extruded repeatedly by cooling and kneading by applying sorbitol seed, followed by cold aging, cutting and grinding It is manufactured by.

Hereinafter, the manufacturing method of the crystalline sorbitol powder of the present invention will be described in detail for each step.

First step: manufacturing process of sorbitol stock solution

A conventional sorbitol solution is heated to be concentrated so as to have a solid content of 85 to 99 wt%, or a conventional sorbitol powder is heated to melt to prepare a sorbitol stock solution.

2nd process: raw material extruder input process

The temperature of the sorbitol stock solution obtained from the above process was adjusted to 85 to 100 ° C, and then put into an extruder. In this case, when the temperature of the sorbitol solution is 100 ° C or higher, the seed that is injected in the subsequent process is melted, and the crystallization of the sorbitol solution takes a long time, and when the temperature of the solution is 85 ° C or lower, the viscosity of the sorbitol solution is increased to determine Dispersion becomes difficult. On the other hand, the extruder is provided with a plurality of cooling / kneading zone in which the cooling and kneading means is installed in the extruder, it is preferable to use an extruder equipped with an inlet and transfer function of the secondary raw material, more preferably the cooling and kneading means One area: the second area in which the cooling and kneading means and the auxiliary raw material inlet is installed: One or more areas in which the cooling and kneading means are installed and it is preferable to use an extruder having the final area in which the cooling and kneading means is installed. In addition, as the extrusion nozzle of the extruder, it is preferable to use a nozzle provided with a plurality of holes having a diameter of 2 to 6 mm, and it is preferable to lay it perpendicular to the screw axis of the extruder. In addition, the feed rate of the sorbitol stock solution may vary depending on the capacity of the extruder, the residence time of the stock solution in the extruder, the cooling capacity of the cooling means and the stirring ability of the kneading means, but is preferably 20 to 40 kg / hr. In addition, it is preferable to use an extruder equipped with a twin screw as the extruder.

Third Step: Addition and Extrusion of Seeds

In the electric process, the mixture is kneaded while maintaining the temperature of the sorbitol solution fed into the first zone of the extruder at 80 to 95 ° C, and the sorbitol seed is introduced through the secondary raw material inlet attached to the second zone, and then kneaded while cooling to 75 to 90 ° C. Kneading while cooling to 70 to 80 ℃ in to discharge the crystalline sorbitol of the facet through the extrusion nozzle. In this case, the amount of sorbitol seed may vary depending on the temperature and concentration of the sorbitol solution, but preferably 5 to 50% by weight relative to the sorbitol solution, and the sorbitol seed may be continuously or intermittently added, but crystallization of sorbitol In order to shorten time, it is preferable to add continuously. The rotational speed of the screw during the extrusion process depends on the yield of the final product and the residence time of the raw material in the extruder for crystallization, but 40 to 60 rpm is preferred. In case of continuing cooling and kneading by adding sperm to sorbitol stock solution in the second area, the mixed material is changed to flowable magma due to temperature drop of mixed material due to seed pour and heat generation due to crystallization of sorbitol. The residence time of the sorbitol magma in the extruder is suitable for 1 to 2 minutes.

4th process: aging and grinding process

In order to completely crystallize the sorbitol on the facet obtained from the electrical process and not to be solidified even after long-term storage, it is cooled and matured at 10 to 60 DEG C on a cooling belt for 5 to 10 minutes and cut into lengths of 5 to 30 mm using a crusher The crystalline sorbitol powder of the present invention is prepared by grinding into granular or powdery form.

Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention in more detail, it will be apparent to those of ordinary skill in the art that the scope of the present invention is not limited by these examples in accordance with the gist of the present invention. .

Example 1

A 95% purity aqueous solution of sorbitol (Lucky Co., Ltd.) was heated and concentrated to prepare a sorbitol solution having a water content of 1 wt%, maintained at 100 ° C., followed by a first zone in which cooling and kneading means were installed, cooling and kneading means and subsidiary materials. The sorbitol solution was added to a twinscrew extruder (Namsan, South Korea) equipped with a second zone in which an inlet was installed and a final zone in which cooling and kneading means were installed. Adjust the rotational speed of the screw to 50rpm and knead while cooling the temperature of the sorbitol solution injected into the first zone of the extruder to 93 ° C, and put the sorbitol seed (Lucky Co., Ltd.) into the sorbitol solution through the secondary raw material inlet installed in the second zone. 20wt% was added, cooled and kneaded at 90 ° C., and then kneaded while cooling at 75 ° C. in the final zone, and through a extrusion nozzle equipped with 50 holes having a diameter of 3 mm, a crystalline sorbitol with a facet perpendicular to the screw axis of the extruder. Was discharged. At this time, the residence time of the sorbitol magma in the extruder was 1.2 minutes. The sorbitol on the carded surface was cooled and aged at 20 ° C. for 7 minutes on a cooling belt, cut into a length of 5 mm using a crusher, and then ground to prepare crystalline sorbitol powder. As a result of analyzing the sorbitol powder prepared in this example, the water content was 0.61 wt%, and the melting point was 95 ° C.

Example 2

Sorbitol powder (Roquette Co, France) having a purity of 97% or more was heated and melted to prepare a sorbitol solution having a water content of 3wt%, maintained at 97 ° C, and 25 kg in the same extruder as the extruder used in Example 1 above. Sorbitol stock was added at a rate of / hr. Adjust the rotation speed of the screw to 40rpm and knead while cooling the temperature of the sorbitol solution injected into the first zone of the extruder to 95 ° C, and add 10wt% of the sorbitol solution to the sorbitol solution through the secondary raw material inlet installed in the second zone. After cooling and kneading to 90 DEG C, and then cooling to 80 DEG C in the final region, through a extrusion nozzle equipped with 50 holes having a diameter of 3 mm, the faceted crystalline sorbitol was discharged perpendicular to the screw side of the extruder. The sorbitol on the surface was cooled and aged at 30 ° C. for 5 minutes on a cooling belt, and then pulverized and ground in the same manner as in Example 1 to prepare crystalline sorbitol powder. As a result of analyzing the sorbitol powder prepared in this example, the water content was 0.5wt%, and the melting point was 97 ° C.

As described in detail above, it was confirmed that the crystalline sorbitol powder can be produced continuously in a short time by the production method of the present invention, and that a high quality crystalline sorbitol powder can be produced by a simple process.

Claims (11)

(a) Concentration of sorbitol solution or melting sorbitol powder to prepare sorbitol stock solution: (b) Process of adding sorbitol stock solution obtained in the electrical process to an extruder equipped with a plurality of cooling / kneading zones: (c A process for producing crystalline sorbitol powder comprising the steps of adding a sorbitol seed in the extruder and repeatedly extruding cooling and kneading; and (d) cooling, extruding, cutting and pulverizing the extrudate obtained in the electrical process. The method of claim 1, wherein the sorbitol undiluted solution has a solid content of 85 to 99wt%. The method of claim 1, wherein the temperature of the sorbitol undiluted solution is 85 to 100 ℃. The extruder according to claim 1, wherein the extruder comprises: a first region in which cooling and kneading means is installed: a second region in which cooling and kneading means and an auxiliary raw material inlet is installed; one or more regions in which cooling and kneading means is installed; And, Method for producing a crystalline sorbitol powder characterized in that the extrusion nozzle is provided. The method for producing crystalline sorbitol powder according to claim 4, wherein the sorbitol powder is kneaded while maintaining the temperature of the sorbitol stock solution added to the first region of the extruder at 80 to 95 캜. The method for producing crystalline sorbitol powder according to claim 4, wherein the sorbitol seed is introduced through the secondary raw material inlet provided in the second region and kneaded while cooling to 75 to 90 ° C. The method for producing crystalline sorbitol powder according to claim 4, wherein in the final region of the extruder, the mixed raw material is kneaded while cooling to 70 to 80 ° C. The method for producing crystalline sorbitol powder according to claim 4, wherein the extruder nozzle of the extruder is disposed directly downward on the screw shaft of the extruder. The method for preparing crystalline sorbitol powder according to claim 1, wherein the dose of sorbitol seed is 5 to 50% by weight based on the sorbitol stock solution. The method for producing crystalline sorbitol powder according to claim 1, wherein the residence time in the extruder of the seeded sorbitol undiluted solution is 1 to 2 minutes. The method for preparing crystalline sorbitol powder according to claim 1, wherein the cooling aging is performed at 10 to 60 ° C for 5 to 10 minutes.