KR930001317B1 - Polydextrose and process therefor - Google Patents

Abstract

(a) mixing 10-90 % polysaccharide syrup (DE= 1-90) with 0.1-10 % acid, e.g. citric acid, malic acid or tataric acid; (b) removing the O2 gas of the mixt. by using vacuum pump; (c) mixing the mixt. with reducing sugar, e.g. maltitol, sorbitol or xylitol, under 5 mmHg or less at 130-200 deg.C and polymerizing; (d) dissolving the polymerized mixt. with hot water to obtain the final product. The obtd. polydextrose is useful for the prodn. of diet food, health food, beverage, drug etc..

Description

Method for producing polydextrose from liquid polysaccharides

The present invention relates to a method for producing polydextrose based on liquid polysaccharides.

Polydextrose is dietary fiber used as diet food, health food, confectionery, bakery, beverage or pharmaceutical ingredient. In the present invention, "plant fiber" means a total of refractory food components that are not hydrolyzed by human intestinal digestive enzymes.

Recently, the development of new physiological fibers with physiological function is active, and among them, there are many proposals regarding a method for producing a polymer material based on various sugars present in nature. For example, US Pat. No. 2,563,014 discloses a method for preparing glucose, a glucose polymer, based on starch decomposition products, and US Pat. No. 3,533,800 for preparing polydextrose and dialdehyde, an oxidation polymerization product of this material. A method is disclosed. U.S. Patent No. 3,766,165 and its counterpart U.S. Patent No. 1,262,842 disclose a process for the preparation of non-nutritive carbohydrate substituents by condensation polymerization of sugars in the presence of a polycarboxylic acid catalyst under reduced pressure. Substances prepared as described above are useful in the composition of diet foods. In addition, Japanese Patent No. 58-36945 describes fatty acid triglycerides and / or carbohydrate-containing foods by substituting a part of fatty acid triglycerides normally contained in foods with polyglucose having a highly water-soluble, highly branched structure in which 1 to 6 bonds are dominant. A method of making a composition is disclosed.

However, the above method has a number of problems, for example, US Patent No. 2,563,014 is an acid catalyst in the production method using a non-volatile weak acid boric acid and phosphoric acid or volatile strong acid hydrochloric acid and acid chloride to release the acid and the like. Because of this, the product thus prepared is not suitable for use in food immediately, there is a problem that a separate purification process is required to use for food. In addition, U. S. Patent No. 3,766, 165 and its corresponding patents, UK Patent No. 1,262, 842 and Japanese Patent No. 58-36945, reacted by starting a reaction by melting the raw material in powder form with high temperature heating in contact with air, and then starting the reaction. There is a problem of discoloration from the beginning.

The present invention is to provide a method for producing a polydextrose to solve the above problems.

The present invention does not require a separate purification process because it uses an edible acid catalyst as a catalyst, as compared to the prior art described above. However, in the above-mentioned US Patent No. 2,563,014, the drying process and the heating process are carried out separately. The production process was shortened and improved so that a separate drying process was not required in the reactor using liquid raw materials. In addition, although US Pat. No. 3,533,800 used an organic solvent, dimethyl sulfone or tetramethyl sulfone, as a reaction solvent, the present invention proceeds the reaction in an aqueous solution so that a separate purification step for the remaining organic solvent is not necessary. Instead of phosphoric acid, an edible acid catalyst was used. On the other hand, the present invention is heated and melted by using a raw material in a liquid state to prevent discoloration of the initial reaction, which is a problem in the United States Patent No. 3,766,165 and the corresponding patents British Patent No. 1,262,842 and Japanese Patent No. 58-36945 The reaction process was improved by removing the process, and the oxygen contained in the powder sample was removed by the degassing process before the start of the reaction.

In addition, the present invention maximizes the action of reducing sugars by adding liquid reducing sugars during the reaction, and shortens the reaction time and increases the degree of polymerization by using a saccharide raw material containing a large amount of polysaccharides. Improved.

In addition, the patent requires a separate separation process due to precipitation of an insoluble material when the reaction is excessively progressed, but the present invention is shortened the process because the insoluble material is not produced when the raw material has the same degree of polymerization as the water-soluble polymer polysaccharide The effect of yield improvement can also be expected.

The present invention mixes a liquid sugar containing a large amount of polysaccharides with an edible acid catalyst and maintains a high vacuum state to remove oxygen present in the reaction solution, and then polymerizes by dividing and adding a reducing sugar several times under high temperature and high vacuum. The present invention relates to a method for producing polydextrose, wherein water is added to dissolve the reactants.

In the present invention, the polysaccharide saccharide is a liquid starch which can be easily purchased on the market, and a DE value (dextrose equivalent value) of 1 to 90 may be used. For example, low sugar syrup (DE 22 ± 2), general starch syrup (DE 42 ± 2), malt syrup (DE42 ± 2), high sugar syrup (DE 50 to 64) or liquid glucose (DE 90) or mixtures thereof There is this. However, polysaccharide saccharides having a low DE value have an advantage of obtaining a high degree of polymerization in a short reaction time. However, the DE value is preferably 2 to 60 because the reverse reaction proceeds due to high viscosity and strong water holding power.

In the present invention, the concentration of the raw material, i.e., starch syrup, is 10 to 100%, preferably 40 to 80%, depending on the effect of the concentration on the reaction time, economical efficiency, ease of handling and storage, and the like.

In the present invention, the acid catalyst is a conventional edible acid, and polycarboxylic acid having many reactors is used. For example, citric acid, malic acid or tartaric acid. The amount of the catalyst used may vary slightly depending on the influence on the degree of polymerization of the acid catalyst, the reaction time, the color, the amount of the remaining acid catalyst, and the pH of the final product, but is usually 0.1 to 10%, preferably 0.1 to 10, for the polysaccharide saccharide dry matter. 0.3% is used.

In the present invention, the reducing sugar serves to reduce the viscosity of the reactants and improve the color and taste, and can be used as both sorbitol, maltitol or xylitol with reducing action, but can be used in both powder and liquid phases. In view of consideration, a liquid phase is preferable, and a high concentration is more preferable. The amount of reducing sugar added increases the effect, but is 1 to 50%, preferably 5 to 20%, compared to the dry matter of the polysaccharide saccharide used, the addition time of the reducing sugar than the addition of all of the reducing sugar at the beginning of the reaction In order to maximize the effect, it is preferable to add the mixture several times before the reaction, that is, the completion of the reaction, and the number of additions is better, but preferably 2 to 5 times. The addition of the reducing sugar significantly decreases its effect after completion of the reaction or when discoloration proceeds considerably. Therefore, it is preferable before the completion of the reaction to be added and before the discoloration proceeds.

The present invention removes the oxygen present in the reaction raw material in a high vacuum state, for example, 0.01 to 50mmHg after mixing the reaction raw material to prevent discoloration of the reaction product and improve color.

In addition, when the temperature of the reaction raw material used in the present invention is too high, the reaction liquid is boiled, so that the raw material in the reactor leaks into the vacuum pump.

In addition, in the present invention, the reaction temperature is preferably 130 to 200 ℃ in consideration of the reaction time, degree of polymerization and color, etc., which may be slowly heated at a rate of 10 ℃ / min or less using a thermostat set to the temperature. have. The degree of vacuum during the reaction is maintained at 5 mmHg or less by using nitrogen, and nitrogen is added at the time of raw material input before the reaction and at the end of the reactor replacement at the end of the reaction.

In the present invention, the reaction time may vary depending on temperature, degree of polymerization or color, but is preferably 2 to 5 hours.

In the present invention, the polymerized reactant may be ejected in any of the aqueous state by adding molten state or hot water, but when it is ejected in the molten state, the yield is lowered due to the material remaining in the reactor and remains in the next reaction. In order to reduce the color and make the continuous process difficult, it is preferable to add hot water and spray the solution in an aqueous state. At this time, the higher the water is added, the better the temperature is maintained with the heat of the reactor to keep the temperature of the reactor at a high temperature to dissolve the reactants.

As described above, the polydextrose obtained according to the present invention has a simpler manufacturing process than the conventional manufacturing method and has an improved yield, thereby greatly improving the economics of production.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, the present invention is not limited to this.

Example 1

333.8 g of 80% high sugar syrup (DE62), 40 g of 75% maltitol, and 3 g of citric acid were added to a 500 ml separate glass reactor, and the air was present in the reaction raw material using a vacuum pump while stirring well with a deceleration stirrer having an anchor stirring bar. Remove it. Subsequently, the reactor was placed in a constant temperature oil bath at 160 ° C. and reacted with stirring at a speed of 60 rpm.

At this time, while reducing the pressure to 100mmHg with a vacuum pump equipped with a condenser using dry ice and methanol, the viscosity is inferred by an ampere meter attached to the stirrer. After the reaction proceeds for 3 hours, the vacuum is released and 200 ml of boiling water is added to the reaction to completely dissolve the reaction. This yields 500 g of a dark yellow reactant that is completely dissolved. The color of the reactants was measured using a colorimeter (Hunter's colorimeter), and the composition of the reactants was measured using GPC (GPC column, TSK G3000PWXL + TSK OLIGO, Tosho, Japan) and the pH was measured. Table 1 shows.

TABLE 1

* L: Lightness

** a: Redness

*** b: Yellowness

Example 2

5 kg of 80% high sugar syrup (DE62), 533 g of 75% sorbitol, and 40 g of citric acid were added to a 10 L vacuum reactor, and degassed. The temperature of the reactor was maintained at 150 ° C. while stirring at 60 rpm.

At this time, the vacuum degree is 1.0mmHg and the condenser using dry ice and methanol and the condenser using cooling water collect the raw materials and the water generated during the reaction. After the reaction was continued for 5 hours, the temperature of the reactor was raised to 180 ° C. to eject 3 kg of a dark yellow molten reactant. The composition and pH of the reactants obtained using GPC were similar to those of Example 1.

Example 3

338 g of 70% high sugar syrup (DE 70) and 3 g of citric acid were added to a 500 ml separate glass reactor, and 80 g of 75% maltitol was divided into three times until the viscosity increased at ampere meter while reacting in the same manner as in Example 1. The aqueous solution of the ejected reactant was 500 g, and the composition of the material was measured using GPC and the pH was measured. Similar to Example 1, the color was markedly improved as shown in Table 2.

TABLE 2

Example 4

52.7 kg of 70% high-sugar starch syrup (DE 70) and 400 g of citric acid are added to a 150-l high-temperature vacuum machine, and the temperature of the reactor is maintained at 160 ° C. while gradually converting to vacuum. After the reaction proceeds for 4 hours while adding 5.7 kg of 75% sorbitol until no more water is produced, the reaction is ejected in a molten state while raising the temperature of the reactor to 180 ° C. At this time, the weight of the jet was 32.5 kg and dark yellow. The composition and pH of the reaction jet were measured using GPC, and the results are shown in Table 3.

TABLE 3

Claims (11)

After mixing the liquid sugar containing a large amount of polysaccharides and the edible acid catalyst and maintaining a high vacuum state to remove the oxygen present in the reaction solution, and by adding the reducing sugars several times under high temperature and high vacuum to polymerize, A method for producing a polydextrose, characterized in that the reaction to dissolve. The method for preparing polydextrose according to claim 1, wherein the liquid sugar is one selected from the group consisting of low sugar starch syrup, general starch syrup, malt syrup, high sugar syrup syrup or liquid glucose, or a mixture thereof. The method of claim 2, wherein the liquid sugar has a concentration of 10 to 90%. The process for producing polydextrose according to claim 1 or 2, wherein the liquid sugar has a DE value of 1 to 90. The method of claim 1, wherein the acid catalyst is one selected from the group consisting of citric acid, malic acid or tartaric acid. The method for producing polydextrose according to claim 1 or 5, wherein the amount of the acid catalyst used is 0.1 to 10% in the carbohydrate. The method of claim 1, wherein the high vacuum for removing oxygen has a vacuum degree of 0.01 to 50 mmHg. The method of claim 1, wherein the high temperature and high vacuum are 130 ° C to 200 ° C and 5 mmHg or less. The method of claim 1, wherein the reducing sugar is one selected from the group consisting of sorbitol, maltitol or xylitol. The method for producing polydextrose according to claim 1 or 9, wherein the reducing sugar is liquid. The method of claim 1, wherein the number of times is 2 to 5 times.