JPH0629173B2 - Granules - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a novel granule, and more particularly to a granule capable of stably retaining its shape even in a multi-aqueous composition.

[Conventional technology and its problems]

BACKGROUND ART Heretofore, granules have been blended in multi-aqueous compositions such as dentifrices and facial cleansers for the purpose of stably blending active ingredients and improving the appearance.

On the other hand, ordinary granules are manufactured with a water-soluble polymer such as methyl cellulose or sodium carboxymethyl cellulose as a binder. However, a granule prepared using such a water-soluble polymer has no problem when used in a dry state such as a drug, but in a multi-aqueous composition as described above in which a large amount of water is present. Then the strength is significantly reduced,
There was a drawback that the shape could not be retained.

In order to improve such drawbacks, a method in which a wax is blended with a pigment to form granules (Japanese Patent Laid-Open Nos. 49-132249 and 50-81)
No. 594), or a method of granulating powder of calcium carbonate or the like with a binder that dissolves in an organic solvent such as ethyl cellulose (JP-A-58-126806).

However, although the granules are usually prepared by a wet extrusion granulation method or a spray granulation method, the method using the above wax has a drawback that it is not suitable for any of the granulation methods, and ethyl cellulose is also used. The method of using as an organic solvent is accompanied by a risk of fire and the like, so that there is a drawback that equipment and strict operation are required to prevent this.

[Means for solving problems]

In such an actual situation, the present inventor has conducted diligent research and as a result, after granulating using a conventional water-soluble polymer as a binder and then crosslinking the water-soluble polymer with a polyvalent metal ion, The present invention was completed by finding that the water-soluble polymer becomes water-insoluble and stable granules can be obtained in a multi-aqueous composition.

That is, the present invention provides a granule obtained by treating a granular material containing a powder substantially insoluble in water and a water-soluble polymer having a functional group that reacts with a polyvalent metal ion, with a polyvalent metal ion. It is provided.

In the present invention, the substantially water-insoluble powder is not limited as long as it is used for cosmetics, dentifrices, pharmaceuticals, etc.
Silicic anhydride, hydrous silicic acid, calcium hydrogen phosphate, calcium phosphate, zirconium silicate, aluminum hydroxide, alumina, calcium carbonate, magnesium carbonate, aluminum silicate, calcium sulfate, talc, zeolite, titanium oxide, red iron oxide, ultramarine blue, fine Examples include plastic beads such as polyethylene.

Further, the water-soluble polymer is not particularly limited as long as it has an anionic functional group such as a carboxy group or a sulfuric acid group and becomes insoluble by reacting with a polyvalent metal ion to form a crosslink, for example, carboxymethyl cellulose. , Alginic acid, poly (meth) acrylic acid, carrageenan or alkali metal salt or ammonium salt of sulphurised cellulose, polymer of monoalkali metal salt of alkyl phosphate ester containing ethylene group, phosphoric acid ester monoalkali metal salt is introduced into the polymer chain And the like, which may be used alone or in combination of two or more. The blending ratio of these water-soluble polymers in the granule composition is appropriately determined according to the required strength of the granule, but is generally preferably 1 to 50% with respect to the entire composition. If it is less than 1%, the strength of the obtained granule becomes insufficient, and if it exceeds 50%, the properties of the granule are largely controlled by the properties of the water-soluble polymer. This is not preferable because it tends to be difficult to obtain the granules.

Polyvalent metal ions are not particularly limited unless they are highly toxic metals such as mercury and cadmium, and calcium ions,
Magnesium ion, zinc ion, aluminum ion, strontium ion, etc. are mentioned. In practice, it is preferably used as a water-soluble compound containing the above element, and its counter ion is preferably pharmaceutically acceptable. Specifically, calcium chloride, aluminum chloride,
Examples thereof include zinc chloride, calcium nitrate, magnesium chloride, stannous chloride and strontium chloride. Also,
The higher the concentration of the treatment liquid containing polyvalent metal ions, the more effective it is. However, considering the washing operation after the treatment, the maximum concentration is preferably about 10%.

In order to produce the granules of the present invention, first, an aqueous solution in which the water-soluble polymer is dissolved is mixed with a powder insoluble in water, and the mixture is extruded and granulated by a usual method such as a spray granulation method. Granulation is carried out by the method to obtain granules bound with the water-soluble polymer. Then, the particulate matter is immersed in an aqueous solution containing polyvalent metal ions and left for a while, or is gently stirred or shaken to bring the particulate matter into contact with the polyvalent metal ions to carry out a crosslinking reaction. Here, it is preferable that the concentration of the polyvalent metal ion is not less than the amount at which the ion reacts stoichiometrically with the water-soluble polymer.

[Action]

Next, an experimental example showing that the granules of the present invention do not easily disintegrate even in water will be given.

First, granules having the composition shown in Table 1 were produced by an extrusion granulation method using water as a solvent. The granules were dried with an electric dryer at 60 degrees Celsius for 2 hours. Then, 300 mg of the granules were mixed at room temperature with 10 m of the solution as shown in Table 1.
The sample is treated with polyvalent metal ions for a minute and the granules are separated and collected with a filter paper.
After washing with deionized water, it was dried under the same conditions. Further, 100 mg of these granules were taken, immersed in 10 m of deionized water at room temperature for 24 hours, and then shaken vigorously up and down for 10 seconds to evaluate the strength of the granules. At this time, the granules in which the granules were completely disintegrated and dispersed were marked with X, the granules in which some of the granules were disintegrated and dispersed were marked with Δ, and those which were not disintegrated at all were marked with ◯.

The results are shown in Table 2. The untreated granules completely disintegrated and dispersed, but most of the granules treated with polyvalent metal ions such as calcium, aluminum and zinc did not disintegrate at all, and none of the granules completely disintegrated and dispersed. That is, it can be seen that the granules of the present invention easily retain their shape even in a system containing a large amount of water.

[Examples] Next, the present invention will be described in more detail with reference to Examples.
The invention is not limited to these examples.

Example 1 (Composition) Zeolite 30 (parts by weight) Titanium oxide 5 Carboxymethylcellulose sodium 3 The above components were kneaded with water to form a clay-like mixture, extruded through pores and dried at 70 ° C. to give granules. . This was immersed in a 1% aqueous solution of aluminum chloride for 10 minutes, washed with water separated by filtration, and then similarly dried. The granules did not easily disintegrate even when placed in water and stirred vigorously.

Example 2 (Composition) Calcium hydrogen phosphate 40 (parts by weight) Carrageenan 5 The above components were kneaded with water to give a clay-like composition, extruded through pores and dried at 70 ° C. to give granules. This was immersed in a 1% aqueous solution of aluminum chloride for 10 minutes, separated by filtration, washed with water, and similarly dried. The granules did not easily disintegrate even when placed in water and stirred vigorously.

Example 3 (Composition) Silicic anhydride 35 (parts by weight) Ultramarine blue 5 Sodium polyacrylate 5 The above components were kneaded with water to give a clay-like composition, extruded through pores and dried at 70 ° C. to give granules. This was immersed in a 2% aqueous solution of calcium chloride for 10 minutes, separated by filtration, washed with water, and similarly dried. The granules did not easily disintegrate even when placed in water and stirred vigorously.

Example 4 (Composition) Zeolite 40 (parts by weight) Titanium oxide 3 Magnesium metasilicate 15 Carboxymethyl cellulose ammonium 2 The above components were kneaded with water to form a slurry and granulated by spray granulation. This was immersed in a 0.5% zinc chloride aqueous solution for 10 minutes, separated by filtration, washed with water, and then dried at 70 degrees Celsius. The granules did not easily disintegrate even when placed in water and stirred vigorously.

〔The invention's effect〕

The granules of the present invention can be produced by a granulation method using water as a solvent,
Moreover, it is unlikely to disintegrate even in a system having a large amount of water, and is suitable for blending into a multi-aqueous composition such as cream, lotion and toothpaste.

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁵ Identification number Office reference number FI technical display location A61K 9/50 R 7329-4C V 7329-4C

Claims (1)

[Claims] 1. A polyvalent metal ion is added to a granular material prepared by granulating a mixture containing a powder substantially insoluble in water and a water-soluble polymer having a functional group capable of reacting with the polyvalent metal ion. A granule obtained by contacting and cross-linking the water-soluble polymer with a polyvalent metal ion.