JP2018203631A - Dentifrice composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a dentifrice composition having an excellent plaque removing effect and a reduced feeling of granules at the time of use. SOLUTION: The following components (A), (B), (C) and (D): (A) abrasive silica powder 40 to 95 mass with an oil absorption amount of 80 to 150 mL / 100 g and an average particle diameter of 3 to 20 μm. %, The arithmetic mean roughness (Ra value) by line analysis of the granules is 0.5 to 5 μm, the average particle size is 100 to 250 μm, and the disintegration strength is 1 to 20 g / piece. Containing 20% by mass, (B) sorbitol 20 to 45% by mass, (C) 10 to 60% by mass of water, (D) 0.01 to 1% by mass of hydroxyalkyl cellulose, component (A) and component (D). A dentin composition having a mass ratio of {(A) / (D)} of 10 to 1000 and a viscosity at 20 ° C. of 1000 to 5000 dPa · s. [Selection diagram] None

Description

  The present invention relates to a dentifrice composition.

Conventionally, for the purpose of removing plaque, granules obtained from an abrasive powder and an inorganic binder are blended in a dentifrice.
For example, Patent Document 1 discloses a dentifrice composition containing an abrasive powder and a water-insoluble inorganic binder, and a granule having a specific shape, particle size distribution, and disintegration strength. It describes that the foam performance and stability of the composition can be ensured while exhibiting the dirt removal performance. Further, Patent Document 2 discloses that a dentifrice containing abrasive powder and a water-insoluble inorganic binder and having a granule having a clear concavo-convex surface has a cleanability between the tooth surface and the gap between teeth. Is maintained from before the disintegration of the granule to after the disintegration, and it is described that it can continue to remove plaque and colored stains from the beginning to the end of brushing.

JP, 2015-117206, A JP 2011-11998 A

  However, with dentifrices containing such granules, some users may feel that the granular feeling in the oral cavity, tooth surface and gingiva is undesirable, reducing the granular feeling while ensuring the ability to remove dirt in the oral cavity. There was a social request.

  The present inventor uses a powder of a base material of a specific granule, a granule having a surface shape and a disintegration strength, and uses sorbitol, water, and hydroxyalkyl cellulose at a specific content, and further uses the granule and hydroxyalkyl cellulose. It has been found that a dentifrice composition can be obtained by using a specific ratio, while having a high plaque removal effect, a reduced granule feel during use, and an excellent agent adhesion.

The present invention includes the following components (A), (B), (C) and (D):
(A) Abrasive silica powder having an oil absorption of 80 to 150 mL / 100 g and an average particle diameter of 3 to 20 μm 40 to 95% by mass
3 to 20 having an arithmetic average roughness (Ra value) of 0.5 to 5 μm, an average particle size of 100 to 250 μm, and a disintegration strength of 1 to 20 g / piece mass%,
(B) Sorbitol 20-45% by mass,
(C) 10-60% by mass of water,
(D) Hydroxyalkyl cellulose 0.01-1% by mass
A dentifrice composition containing 10 to 1000 in mass ratio {(A) / (D)} of component (A) to component (D) and having a viscosity at 20 ° C. of 1000 to 5000 dPa · s About.

  The dentifrice composition of the present invention has a high plaque-removing effect, has a reduced granule feel at the time of use, and is excellent in the adhesion of the agent, and can be suitably brushed. is there.

In the granule of the component (A) used in the present invention, 40% or more of the surface area is formed with an uneven surface, and the average height difference on the uneven surface is preferably 2 to 10 μm, more preferably 2 to 8 μm, and more preferably 2 to 5 μm. Is more preferable. The average height difference is an average value obtained by measuring the distance from the bottom of the concave portion to the apex of the adjacent convex portion with respect to the concave and convex portions on the periphery of the virtual cross section when the granule is cut by a plane including the center. Ask.
The irregularities on the surface of the granule can be obtained as arithmetic average roughness (Ra value) by line analysis. The Ra value by line analysis can be obtained by averaging the heights of the surface irregularities at the periphery when viewed in the virtual cross section, as with the average height difference. Ra value by the line analysis of the granule of this invention is 0.5-5 micrometers, and what is 1-3 micrometers is preferable.
Furthermore, the average height difference on the uneven surface of the granule of the present invention is preferably 1/5 to 1/2 of the average particle diameter of the abrasive powder contained in the component (A), and is preferably 1/4 to 1. What is / 2 is more preferable, and what is 1/3 to 1/2 is more preferable.
In addition, the unevenness | corrugation height of the surface of the granule of a component (A) can be measured with a scanning electron microscope (made by VK-9500 Keyence Corporation).

In addition, the average particle size of the granule of component (A) is 100 μm or more from the viewpoint of reducing granule feeling at the time of use while providing a high plaque removal effect and providing a suitable feeling at the time of brushing. The thickness is preferably 130 μm or more, more preferably 170 μm or more, and still more preferably 190 μm or more. Further, the average particle size of the granule of component (A) is 250 μm or less, preferably 230 μm or less, more preferably 220 μm, from the viewpoint of reducing the granule feeling at the time of use and providing a suitable feeling when brushing teeth. It is as follows. And the average particle diameter of the granule of a component (A) is 100 micrometers or more and 250 micrometers or less, Preferably it is 130-230 micrometers, More preferably, it is 170-220 micrometers, More preferably, it is 190-220 micrometers.
Here, the average particle diameter of the granule refers to a value measured by a sieving method (sonic sieve, Tsutsui Rika SW-20-AT).

Furthermore, the disintegration strength of the granule of component (A) is such that the granule in the mouth can be palpated and the effect can be recognized, but there is almost no foreign body feeling and plaque is not damaged. Or from the point which has the removal power of coloring stains, it is 1-20 g / piece, 2-15 g / piece is preferred, and 3-8 g / piece is more preferred.
Here, the disintegration strength is represented by an average value obtained by measuring 10 to 20 granules having a particle size near the average particle size using a micro compression tester (Shimadzu Corporation, MCTM-500).
The granule of component (A) has the same strength even when blended in a dentifrice composition (wet state).

The granule of component (A) contains abrasive silica powder.
The average particle size of the abrasive silica powder was 3 μm or more from the viewpoint of excellent plaque removability on the surface of the tooth before the granule disintegrated and a feeling of granule at the time of use by reducing the granular feeling at the time of use. More preferably, it is 5 μm or more, more preferably 7 μm or more. In addition, the average particle size of the abrasive silica powder is excellent in terms of removing plaque on the surface of the tooth before the dentifrice granules disintegrate, and reducing the feeling of granules during use, thereby providing a favorable feeling during brushing. Therefore, it is 20 μm or less, preferably 15 μm or less, and more preferably 10 μm or less. And the average particle diameter of the abrasive silica powder is the viewpoint that the excellent dental plaque removal on the surface of the tooth before the dentifrice granule disintegrates and the feeling of granule at the time of use is reduced to provide a suitable feeling at the time of brushing. From 3 to 20 μm, preferably from 5 to 15 μm, more preferably from 7 to 10 μm.

The abrasive silica powder usually has higher abrasiveness as the oil absorption is smaller. However, dentifrice granules prepared using an abrasive powder with too little oil absorption have no irregularities on the surface, and as a result, the effect of removing plaque on the tooth surface tends to be low. Therefore, the oil absorption amount of the abrasive silica powder is 80 to 150 mL / 100 g from the point of forming irregularities on the surface of the granule and the plaque removability from the surface of the tooth before the granule collapse, and 90 to 130 mL / 100 g is preferred.
The RDA value (abrasiveness) of the abrasive silica powder is preferably 150 to 90, more preferably 140 to 90 from the viewpoint of prevention of harmfulness and a balance between usability and abrasiveness in the oral cavity.

Here, the oil absorption amount of the abrasive silica powder is specified by the amount of oil to be absorbed in the boiled sesame by a method according to JIS K5101-13-2. Specifically, the oil is dripped into the abrasive powder to be measured and kneaded with a steel spatula, and when the whole can be rolled into a spiral shape with the steel spatula, the end point is reached, and the boiled rice that is absorbed Identify the amount of oil. In addition, the oil specified in JIS K5421 is used for boiled sesame oil.
Further, the RDA value of the abrasive silica powder is measured by ISO 11609 abrasive test method appendix A.

  The content of the abrasive silica powder in the granule is 40 to 95% by mass and 50 to 95% by mass in terms of the abrasiveness, disintegration, and abrasiveness after the granule collapse before the granule collapse. Is preferable, 60-90 mass% is more preferable, and 80-90 mass% is further more preferable.

  The water-insoluble inorganic binder contained in the granule is preferably one or more selected from colloidal silica, magnesium aluminate metasilicate and synthetic aluminum silicate, and in particular, the operability in the spray granulation method, etc. Therefore, colloidal silica is more preferable.

  The content of the water-insoluble inorganic binder in the granule is preferably 10 to 45 mass%, more preferably 10 to 40 mass%, more preferably 15 to 35 mass%, from the viewpoint of the balance between the strength and disintegration of the granule. Is more preferable.

Moreover, it is preferable from the point of disintegration and plaque removal property to make the granule of a component (A) contain a water-insoluble fiber.
As the water-insoluble fiber, water-insoluble dietary fiber is preferable, and examples thereof include cellulose, water-insoluble hemicellulose, lignin, chitin, chitosan, etc. Of these, from the viewpoint of disintegration of granules, removal of plaque, and removal of colored stains. Cellulose is preferred. Cellulose may be microcrystalline powder cellulose or the like whose crystal structure is recognized by processing, in addition to cellulose purified as a powdery dry product using pulp or the like as a raw material. In addition to the above-mentioned cellulose, beet fiber, corn fiber, apple fiber and the like purified from plants can be mentioned. These are made of cellulose, water-insoluble hemicellulose, lignin, etc., and some contain water-soluble fibers, but water-insoluble dietary fibers can be used.

  The content of the water-insoluble fiber in the granule is preferably 1 to 40% by mass, more preferably 2 to 30% by mass, from the viewpoint of the disintegration property of the granule, the plaque removal property and the color stain removal property. -25% by mass is more preferable, and 2-20% by mass is more preferable.

Moreover, the granule of a component (A) can contain components other than the above in the range which does not inhibit formation, intensity | strength, and disintegration of a granule. For example, a colorant such as titanium oxide or ultramarine can be contained in the granule, and an aesthetic effect by the colored granule can be added to the dentifrice.
0.01-10 mass% is preferable and, as for content of the coloring agent in a granule, 0.1-5 mass% is more preferable.

The granule of a component (A) can be manufactured by a well-known granulation method. For example, since it is preferable that the shape of the granule is spherical, there is a spray granulation method in which the shape of the granulated product can be made almost spherical, which is easy to handle and suitable as a method for producing the granule. It is.
Further, in the case of a granulated product having an irregular shape such as an extrusion granulation method or the like, the tip region of the angular portion protruding in the range of approximately 1/6 to 1/2 of the particle width (particle diameter) For example, spherical particles can be obtained by performing a spheroidizing operation with a Malmerizer or the like.

The granule of component (A) is preferably obtained by spray granulation of a water slurry which is a mixture containing abrasive silica powder, a water-insoluble inorganic binder and water. The viscosity at 25 ° C. before spraying the water slurry is preferably from 100 to 600 mPa · s, more preferably from 200 to 500 mPa · s, from the viewpoint of producing granules having irregularities on the surface.
The viscosity of the water slurry can be adjusted by the oil absorption of the abrasive powder or the content of the abrasive powder. Here, the concentration of solids such as abrasive powder in the water slurry is preferably 40 to 60% by mass.

  The content of the component (A) is 3% by mass or more, preferably 5% by mass or more, more preferably 7.2% by mass or more in the dentifrice composition from the viewpoint of providing a high plaque removal effect. . In addition, the content of the component (A) is 20 mass in the dentifrice composition from the viewpoint of reducing granule feeling during use and providing a suitable feeling during brushing while having a high plaque removing effect. % Or less, preferably 17% by mass or less, and more preferably 12% by mass or less. And content of a component (A) is 3-20 mass% in a dentifrice composition, 5-17 mass% is preferable and 6-12 mass% is more preferable.

  The component (B), sorbitol, is used to reduce the granular feeling during use, to ensure excellent adhesiveness of the agent, and to allow the agent to act suitably on the tooth surface during tooth brushing.

  The content of the component (B) reduces the granular feeling at the time of use, ensures the adhesion of the excellent agent, and from the viewpoint of causing the agent to act suitably on the tooth surface during tooth brushing, in the dentifrice composition, It is 20% by mass or more, preferably 22% by mass or more, and more preferably 24% by mass or more. In addition, the content of the component (B) is 45% by mass or less in the dentifrice composition from the viewpoint of ensuring excellent shape retention of the agent and allowing the agent to act appropriately on the tooth surface during tooth brushing. 40 mass% or less is preferable and 35 mass% or less is more preferable. And content of a component (B) is 20-45 mass% in a dentifrice composition, 22-40 mass% is preferable, and 24-35 mass% is more preferable.

  In the present invention, the mass ratio ((A) / (B)) of the content of the component (A) and the content of the component (B) is preferably 0.1 or more from the viewpoint of providing a high plaque removal effect. More preferably, it is 0.2 or more, more preferably 0.24 or more, and still more preferably 0.27 or more. Moreover, the mass ratio ((A) / (B)) of the content of the component (A) and the content of the component (B) reduces granule feeling at the time of use and provides excellent shape retention of the agent. From the viewpoint of ensuring, it is preferably 1 or less, more preferably 0.8 or less, still more preferably 0.6 or less, and even more preferably 0.5 or less. The mass ratio ((A) / (B)) between the content of component (A) and the content of component (B) is preferably 0.1 or more and 1 or less, more preferably 0.2. It is -0.8, More preferably, it is 0.24-0.6, More preferably, it is 0.27-0.5.

  The dentifrice composition of the present invention contains (C) water. The water of component (C) in the present invention includes not only purified water blended in a dentifrice composition, but also contained in each blended component such as a 70% sorbitol solution (aqueous solution) used for formulation. It means the total moisture contained in the dentifrice composition, including moisture. By containing the water of the component (C), each component is dispersed or dissolved well and diffused well in the oral cavity while maintaining a good shape retaining property, thereby providing a suitable feeling when brushing teeth. Can do.

  The content of the component (C) is 10% by mass or more, preferably 20% by mass or more from the viewpoint of dispersing or dissolving each component in the dentifrice composition and diffusing it well in the oral cavity. More preferably, it is 30% by mass or more. Further, the content of the component (C) is 60% by mass or less, preferably 55% by mass or less, more preferably 50% by mass or less, from the viewpoint of maintaining good shape retention of the agent. And 10-60 mass% is preferable in dentifrice composition, as for content of a component (C), 20-55 mass% is more preferable, and 30-50 mass% is further more preferable.

  In the present invention, the mass ratio ((B) / (C)) of the content of the component (B) and the content of the component (C) reduces granule feeling and further ensures excellent agent adhesion. From this point of view, it is preferably 0.35 or more, more preferably 0.45 or more, and further preferably 0.5 or more. In addition, the mass ratio ((B) / (C)) of the content of the component (B) and the content of the component (C) is reduced from the viewpoint of reducing granule feeling and ensuring excellent agent adhesion. , Preferably 4 or less, more preferably 3 or less, and even more preferably 2 or less. The mass ratio ((B) / (C)) between the content of the component (B) and the content of the component (C) is preferably 0.35 or more and 4 or less, more preferably 0.45. It is -3, More preferably, it is 0.5-2.

The component (D) hydroxyalkyl cellulose is a component obtained by introducing a hydroxyalkyl group into cellulose. By using this, it is possible to realize a dentifrice composition that has a high plaque removing effect, reduces granule feeling, and is excellent in the adhesion of the agent.
Preferably carbon number of a hydroxyalkyl group is 1-5, More preferably, it is 2-4. Examples of the component (D) include hydroxyethyl cellulose, hydroxypropyl cellulose, and the like, and hydroxyethyl cellulose is more preferable from the viewpoint of realizing a dentifrice composition that reduces granule feeling and is excellent in the adhesion of the agent.

  The mass average molecular weight (Mw) of the component (D) is preferably 300,000 or more, more preferably 50 from the viewpoint of reducing granule feeling in combination with the component (A) and realizing excellent adhesion of the agent. It is 10,000 or more, more preferably 800,000 or more. The mass average molecular weight (Mw) of the component (D) is preferably 2.5 million or less, more preferably 2 million or less, and further preferably 1.8 million, from the viewpoint of the shape retention of the agent in combination with the component (A). It is as follows. Moreover, the mass average molecular weight (Mw) of a component (D) becomes like this. Preferably it is 300,000-2,500,000, More preferably, it is 500,000-2 million, More preferably, it is 800,000-1,800,000. The mass average molecular weight (Mw) can be determined by the GPC method (gel filtration chromatography method). As a commercial product of hydroxyalkyl cellulose having such a mass average molecular weight (Mw), hydroxypropylcellulose includes HPC-M (Mw = 620,000) manufactured by Nippon Soda Co., Ltd., and hydroxyethylcellulose manufactured by Daicel Corporation. HEC Daicel SE550 (Mw = 500,000), HEC Daicel SE600 (Mw = 1.20,000), and HEC Daicel SE850 (Mw = 1.48 million).

As the component (D), the hydroxyalkyl cellulose may be used alone or in combination of two or more.
The content of the component (D) is 0.01% by mass or more and 0.03% by mass in the dentifrice composition from the viewpoint of reducing granule feeling while having a high plaque removing effect. The above is preferable, and 0.06% by mass or more is more preferable. In addition, the content of the component (D) is 1% by mass or less in the dentifrice composition and 0.7% by mass from the viewpoint of reducing granule feeling and further realizing excellent agent adhesion. % Or less is preferable, and 0.5% by mass or less is more preferable. And content of a component (D) is 0.01-1 mass% in a dentifrice composition, Comprising: 0.03-0.7 mass% is preferable, 0.06-0.5 mass% Is more preferable.

  In the present invention, the mass ratio ((A) / (D)) of the content of the component (A) and the content of the component (D) is 10 or more from the viewpoint of providing a high plaque removal effect, Preferably it is 30 or more, More preferably, it is 65 or more, More preferably, it is 75 or more. Moreover, the mass ratio ((A) / (D)) of the content of the component (A) and the content of the component (D) reduces the granular feeling at the time of use, and guarantees excellent agent adhesion. Therefore, it is 1000 or less, preferably 800 or less, more preferably 600 or less, and further preferably 300 or less. And mass ratio ((A) / (D)) of content of a component (A) and content of a component (D) is 10 or more and 1000 or less, Preferably it is 30-800, More preferably Is 65 to 600, more preferably 75 to 300.

  Furthermore, the dentifrice composition of the present invention reduces the feeling of granules, and further, from the viewpoint of realizing a dentifrice composition excellent in the adhesiveness of the agent, carboxymethylcellulose or a salt thereof (E) as a binder. It is preferable to contain.

  As such carboxymethyl cellulose or a salt thereof, carboxymethyl cellulose having a degree of etherification of 0.95 to 1.5 or a salt thereof is preferable. The degree of etherification of such carboxymethyl cellulose or a salt thereof is preferably 0.95 or more, more preferably 1.0 or more, from the viewpoint of imparting an appropriate viscosity and retaining and diffusing the composition in the vicinity of the tooth surface. Preferably, it is 1.5 or less, More preferably, it is 1.15 or less. Further, the degree of etherification of such carboxymethyl cellulose or a salt thereof is preferably 0.95 to 1.5, more preferably from the viewpoint of imparting an appropriate viscosity and retaining and diffusing the composition in the vicinity of the tooth surface. Is 1.0 to 1.15.

The degree of etherification of carboxymethylcellulose or a salt thereof refers to the degree of substitution of carboxymethyl groups per glucose unit. The degree of etherification can be obtained, for example, according to the CMC industry association analysis method (ashing method). Specifically, 1 g of carboxymethylcellulose or a salt thereof is precisely weighed, put into a magnetic crucible, incinerated at 600 ° C., sodium oxide formed by ashing is titrated with N / 10 sulfuric acid with phenolphthalein as an indicator, and carboxy The titration amount YmL per 1 g of methylcellulose or a salt thereof is calculated by entering into the following formula, and the degree of etherification can be obtained.
Degree of etherification = (162 × Y) / (10,000-80 × Y)

  Examples of the salt of carboxymethyl cellulose include alkali metal salts such as sodium and potassium, ammonium salts, etc. Among them, sodium carboxymethyl cellulose is preferable.

  The content of component (E) carboxymethylcellulose or a salt thereof is preferably 0.1 mass in the dentifrice composition from the viewpoint of retaining and diffusing the composition in the vicinity of the tooth surface while having an appropriate viscosity. % Or more, more preferably 0.3% by weight or more, further preferably 0.5% by weight or more, preferably 1.4% by weight or less, more preferably 1.2% by weight or less. More preferably 0.9% by mass or less. In addition, the content of the component (E) carboxymethyl cellulose or a salt thereof is preferably 0.1 to 1.4% by mass, more preferably 0.3 to 1.2% by mass in the dentifrice composition. More preferably, it is 0.5 to 0.9% by mass.

  In the present invention, the mass ratio ((A) / (D + E)) of the content of the component (A) and the total content (D + E) of the component (D) and the component (E) has a high plaque removal effect. From the viewpoint of bringing about, it is preferably 1 or more, more preferably 2 or more, still more preferably 6 or more, still more preferably 7.5 or more, and still more preferably 8.5 or more. Moreover, the mass ratio ((A) / (D + E)) of the content of the component (A) and the total content (D + E) of the component (D) and the component (E) reduces the granular feeling during use. And from a viewpoint of ensuring the adhesiveness of the outstanding agent, Preferably it is 100 or less, More preferably, it is 80 or less, More preferably, it is 70 or less, More preferably, it is 60 or less. The mass ratio ((A) / (D + E)) between the content of component (A) and the total content (D + E) of component (D) and component (E) is preferably 1 or more and 100 or less. More preferably, it is 2-100, More preferably, it is 6-80, More preferably, it is 7.5-70, More preferably, it is 8.5-60.

  In the present invention, the mass ratio ((D) / (E)) between the content of the component (D) and the content of the component (E) reduces the granular feeling at the time of use and adheres an excellent agent. From the viewpoint of ensuring the property, it is preferably 0.01 or more, more preferably 0.05 or more, and further preferably 0.1 or more. Further, the mass ratio ((D) / (E)) of the content of the component (D) and the content of the component (E) is preferably 10 or less from the viewpoint of reducing the granular feeling during use. More preferably, it is 3 or less, More preferably, it is 1 or less, More preferably, it is 0.5 or less. And mass ratio ((D) / (E)) of content of a component (D) and content of a component (E) becomes like this. Preferably it is 0.01-10, More preferably, it is 0.01 It is -3, More preferably, it is 0.05-1 and More preferably, it is 0.1-0.5.

The dentifrice composition of the present invention can further contain (F) a fluorine compound, strengthen the tooth quality, and prevent dental caries.
Examples of the fluorine compound include sodium fluoride, sodium monofluorophosphate, stannous fluoride, and amine fluoride. Sodium fluoride and sodium monofluorophosphate are preferred.

  The content of the component (F) is preferably 100 to 2000 ppm and more preferably 500 to 1500 ppm as the fluorine concentration in the dentifrice composition from the viewpoint of favorably adsorbing fluorine to the teeth.

  In addition to the above components, the dentifrice composition of the present invention includes components used in ordinary dentifrice compositions, such as binders, wetting agents, sweeteners, preservatives, pH adjusters, surfactants, fragrances, Medicinal ingredients can be used.

The dentifrice composition of this invention can be manufactured in accordance with a normal method. Examples of the dentifrice composition include toothpastes, coating agents, gargles, and liquid dentifrices.
The resulting dentifrice composition retains and diffuses the component (A) granules and abrasives in the vicinity of the tooth surface while having an appropriate viscosity or viscosity, and has excellent plaque removal while reducing granule feel. From the viewpoint of realizing the effect and the shape retention of the agent, the viscosity at 25 ° C. is 1000 to 5000 dPa · s, and preferably 1500 to 4000 dPa · s.
The viscosity was measured using a helipath viscometer (VISCOMETER TVB-10, manufactured by Toki Sangyo Co., Ltd.) at a measurement temperature of 25 ° C., rotor TC, rotation speed 2.5 r / min, 1 minute. It can be measured according to measurement conditions.

Production Example 1 (Production of Granule 1)
Granules 1 having the composition shown in Table 1 were produced.
That is, silicic acid anhydride (trade name: Sorbosil AC77, manufactured by INEOS Silicones Indonesia, volume average particle size 9.5 μm, oil absorption 129 mL / 100 g, RDA value 125) as abrasive silica powder, colloidal silica (Snowtex SK, Nissan Chemical Co., Ltd.), cellulose (KC Flock W-400G, Nippon Paper Chemicals Co., Ltd.) and purified water were mixed to form a water slurry. The water slurry at this time was 50% solid content. Furthermore, the water slurry was sprayed and granulated with a spray granulator at an air blowing temperature of about 200 ° C. and an exhaust air temperature of 80 to 90 ° C. The obtained granules were classified with a sieve of 1 to 90 μm / 500 μm (particle diameter 90 to 500 μm) to produce granules 1. Table 1 shows the composition of the granules after spray drying.
In addition, the disintegration strength was obtained by measuring 10 to 20 granules having a particle size (180 to 200 μm) using a micro compression tester (Shimadzu Corporation, MCTM-500) and calculating an average value.

Production Example 2 (Production of Granule 2)
In the same manner as in Production Example 1, granules 2 having the composition shown in Table 1 were produced.
For the disintegration strength, 10 to 20 granules having a particle size (130 to 150 μm) were measured using a micro compression tester (Shimadzu Corporation, MCTM-500), and an average value was calculated.

Production Example 3 (Production of Granule 3)
Granules 3 having the composition shown in Table 1 were produced.
That is, a mixture of heavy calcium carbonate (product of Calfine, trade name: ACE-25, average particle diameter of about 3 μm) and zinc oxide is put into a 75 L drum granulator (φ40 cm × L60 cm) having a baffle plate. Drum rotation speed 30r. p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, sodium silicate (manufactured by Fuji Chemical Industry Co., Ltd., trade name: No. 3 sodium silicate: Na ₂ .3SiO ₂ solution, solid content 38.5% The mixture was diluted with 3 times or less of water (25 ° C.) and granulated by spray addition using one external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.). The addition rate of the aqueous sodium silicate solution was 3.3 mL / min.
After spraying sodium silicate aqueous solution, after continuing mixing for 1 minute, discharged from the drum granulator,
After drying for 90 minutes at 80 ° C. using an electric shelf dryer, granules 3 were obtained.

The surface state, arithmetic average roughness (Ra value), disintegration strength (g / piece) and average particle diameter (μm) of the granules obtained in the production examples were determined and shown in Table 1.
The surface state of the granule is a result of visual evaluation of the uneven surface of the surface using a scanning electron microscope (VK-9500, manufactured by Keyence Corporation). The arithmetic average roughness (Ra value) is a value obtained by measuring the irregularity state of the granule surface with a scanning electron microscope (manufactured by VK-9500 Keyence Corporation) and by a method defined in JIS B 0601-2001. The disintegration strength (g / piece) is when 10-20 granules before blending are compressed and disintegrated using a compression tester (Shimadzu Corporation, MCTM-500) at a load rate of 1.51 gf / sec. The average value obtained by measuring the load for each granule. The average particle size is 2000, 1400, 1000, 710, 500, 355, 250, 180, 125, 90, 63 of JISZ8801-1 (established on May 20, 2000, final revised on November 20, 2006), This is a value obtained by calculating a 50% average diameter for the under-sieving mass distribution by a sieving method after vibrating for 45 minutes using a 45 μm sieve.

Examples 1-4, Comparative Example 1
In accordance with the prescription shown in Table 2, purified water is preliminarily heated to 60-80 ° C. and put into a thermostatic bath, and then components (A), (B), (D), (E) and other components are added. Each dentifrice composition was prepared by stirring for 10 minutes using a universal mixing device (5XDMVV10-r, manufactured by Dalton Co.) at an orbital stirring speed of 75 rpm and an autogenous stirring speed of 200 rpm.
Using each dentifrice composition obtained, the removal rate and the granular feeling were evaluated according to the following methods. The results are shown in Table 2.
In addition, the viscosity at 20 degreeC of the dentifrice composition of Examples 1-4 and the comparative example 1 is 2500 dPa * s.

(1) Removal rate:
Red lipstick is applied to the groove of the interdental model (5 pastor pipettes of φ4 are aligned and fixed). Thereafter, the excess lipstick was brushed (until red color disappeared) using a toothbrush (Check, manufactured by Kao) and (dishwashing detergent). A certain amount of each dentifrice composition was taken on the model and brushed until the lipstick did not adhere to the toothbrush. The lipstick remaining in the model was ultrasonically washed with 90 mL of ethanol for 10 minutes, and the absorbance of the extract was measured (Abs) at 540 nm. As a result, the value of the dentifrice composition of Comparative Example 1 was evaluated as 100%.

(2) Granule feeling:
The granular feeling in the oral cavity when brushing with each dentifrice composition was evaluated according to the following criteria. This was done for 22 panelists and evaluated based on the following indicators.
<Evaluation of granule feeling>
1: The majority felt that the granular feeling was weak or somewhat weak.
2: The majority felt an appropriate granular feeling.
3: The majority felt that the granular feeling was strong or somewhat strong.

Test example 1
About the dentifrice composition of Example 1 and Comparative Example 1, the adhesiveness of the agent was evaluated. The results are shown in Table 3.

(3) Agent adhesion:
1.0 g of dentifrice composition diluted 1.1 times on one side of the reference line of the test plate placed horizontally on the upper surface of a 30 mm × 80 mm acrylic plate as a test plate. Was attached. Thereafter, the test plate was placed vertically so that the reference line was below, and the maximum distance (mm) to the point where the dentifrice composition slipped below the reference line when 5 minutes passed after the vertical placement. ) Was measured. It shows that adhesiveness is so high that this distance is small. Table 3 shows the measurement results. Adhesion was measured at room temperature (25 ° C.).

  From the results in Table 3, the dentifrice composition of the present invention is excellent in the adhesiveness of the agent, so that it retains its shape when placed on a toothbrush, removes dirt when used, and prevents dripping from the oral cavity. Excellent.

Claims (6)

The following components (A), (B), (C) and (D):
(A) Abrasive silica powder having an oil absorption of 80 to 150 mL / 100 g and an average particle diameter of 3 to 20 μm 40 to 95% by mass
3 to 20 having an arithmetic average roughness (Ra value) of 0.5 to 5 μm, an average particle size of 100 to 250 μm, and a disintegration strength of 1 to 20 g / piece mass%,
(B) Sorbitol 20-45% by mass,
(C) 10-60% by mass of water,
(D) Hydroxyalkyl cellulose 0.01-1% by mass
A dentifrice composition containing 10 to 1000 in mass ratio {(A) / (D)} of component (A) to component (D) and having a viscosity at 20 ° C. of 1000 to 5000 dPa · s .   Furthermore, the dentifrice composition of Claim 1 which contains 0.1-2 mass% of (E) carboxymethylcellulose or its salt as a binder.   The dentifrice composition according to claim 2, wherein the mass ratio {(D) / (E)} of the content of the component (D) and the content of the component (E) is 0.01 to 10.   The dentifrice composition according to any one of claims 1 to 3, wherein the component (A) has an average particle size of 160 to 230 µm.   The dentifrice composition according to any one of claims 1 to 4, wherein the mass ratio {(A) / (B)} of the content of component (A) to the content of component (B) is 0.1-1. .   The mass ratio {(A) / (D + E)} of the content of the component (A) and the total content (D + E) of the component (D) and the component (E) is 1 to 100. Dentifrice composition.