TW201524524A - Dentifrice - Google Patents

Abstract

The present invention relates to a dentifrice that is formed by distributing grains as follows. The grains break down inside the oral cavity when a load is applied, have a good granular feel without feeling foreign, and penetrate to fine recesses having a width of no more than 150 [mu]m such as tooth perikymata, mesiolabial grooves, central ridges, and distolabial surface grooves, so as to exhibit high plaque-removal capability and stain-removal capability. The dentifrice of the present invention is formed by distributing grains containing a water-insoluble powder material (A) and an inorganic binder (B). In the grains that are present in the dentifrice after distribution, the average value for the ratio (SA/SS) between the area (SA) of a projection surface of the grains and the area (SS) of a circumscribed circle having the maximum longest diameter (DL) in the projection surface as the diameter thereof is 0.5-0.9. The collapse strength of the grains after distribution is more than 1 gf/granule and less than 20 gf/granule.

Description

Dentifrice

The present invention relates to a dentifrice.

In recent years, there has been known a dentifrice formulated with particles which are highly effective in removing plaque, which is a cause of insect teeth or periodontal disease, and which can be used to detect the effect. In order not to cause damage to the enamel or gums on the surface of the tooth, the particles are substantially formed into spherical agglomerated particles, and those having a functional material such as a drug, an enzyme, or an abrasive, or a visual effect thereof.

As the binder of the particles, a water-soluble binder such as methyl cellulose or carboxymethyl cellulose or a water-insoluble organic binder such as a wax is known. Further, a dentifrice containing particles obtained by binding a water-insoluble inorganic binder such as colloidal cerium oxide to a water-insoluble powder material such as zeolite is known (see Patent Document 1).

Further, a dentifrice containing cerium oxide particles having a spherical shape and a high deformation ratio which is produced by a specific method using a wet method (gel method) using phthalic anhydride is also known (see Patent Document 2).

[Patent Literature]

[Patent Document 1] Japanese Patent Laid-Open No. 1-299211

[Patent Document 2] Japanese Patent Laid-Open Publication No. 2010-275260

The present invention relates to a dentifrice which is prepared by mixing particles containing a water-insoluble powder material (A) and an inorganic binder (B), and with respect to the formulated particles present in the dentifrice, The average value of the area (S _A ) of the projection surface of the particle and the ratio (S _A /S _S ) of the area (S _S ) of the circle other than the longest diameter (D _L ) of the projection surface is 0.5 or more. It is 0.9 or less, and the disintegration intensity of the particle after preparation is 1 gf / more and 20 gf / or less.

Further, the present invention relates to a dentifrice which is prepared by blending particles containing a water-insoluble powder material (A) and an inorganic binder (B), and the particles which are formulated in the dentifrice The following particles (a) to (d) in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement:

(a) Particles having a particle diameter of 50 μm or more and less than 100 μm

(b) particles having a particle diameter of 100 μm or more and less than 150 μm

(c) particles having a particle diameter of 150 μm or more and less than 200 μm

(d) particles having a particle diameter of 200 μm or more and less than 250 μm

The volume ratio (b/c) of the amount of the particles (b) to the amount of the particles (c) is 0.7 or more and 1.2 or less, and the volume ratio (d/c) of the particles (d) to the particles (c) is 0.2. Above and below 1 , the volume ratio (b/d) of the amount of the particles (b) to the amount of the particles (d) is more than 1 and 5 or less, and the amount of the particles (c) in the prepared particles is 15% by volume or more. And 55 volume% or less, and the disintegration intensity of the particle after preparation is 1 gf / more and 20 gf / or less.

With the changes in dietary life and living habits in recent years, the factors causing the deterioration of the oral environment are increasing. Therefore, there are various kinds of dirt that are easy to adhere and remain in the presence of glazed transverse lines (perikymata) and near middle lip. The condition of the surface of the teeth of various sizes such as the groove, the central ridge, and the distal lip lobe. Although the pellet of the above-mentioned Patent Document 1 has an appropriate particle strength which is easily disintegrated, there is still room for improvement in sufficiently removing the dirt adhering to the surface of the tooth having various irregularities on the surface of the tooth. Further, although the particles of the above Patent Document 2 have a high deformation rate and excellent graininess, they are also attached to various sizes of the tooth surface under a small load in the case of using a soft toothbrush which is considered to reduce the load on the gums. There is room for improvement in terms of sufficient removal of the dirt in the recess. Therefore, it is desirable to use granules for dentifrice which easily enter the concave portion of the surface of such a tooth, In the case of a dentifrice formulated with the granules, it is expected that the tartar or soil removal ability can be improved even under a small load in the case of using a soft toothbrush which reduces the load on the gums.

Therefore, the present inventors conducted various studies and found that if a dentifrice having a special shape or a special particle size distribution and having a specific disintegration strength is prepared, the particles are easily interacted with each other. When entering the fine recess of the tooth, it can exert a high degree of tartar removal or dirt removal ability even under a small load in the case of using a soft toothbrush.

The dentifrice according to the present invention has a special shape or a special particle size distribution and a specific disintegration strength, and if the load is loaded, the specific particles are disintegrated, so that there is a good particle having no foreign body sensation. Sense, and the granules enter into the fine dents of 150 μm or less, such as the glazed transverse stripes of the teeth, the proximal middle lip groove, the central ridge, and the distal middle lip groove, etc., so that the load from the toothbrush can be effectively transmitted to the tartar Or dirt such as stained dirt is sufficiently removed. Therefore, even in the case of using a soft bristle toothbrush, the load can be efficiently transmitted to the fine concave portion to exhibit a high dirt removing ability.

Particle size distribution of particle B' before X‧‧‧ preparation

Particle size distribution of particle B after Y‧‧‧ blending

Figure 1 is a diagram showing the laser preparation of the pre-formed particles B' used to obtain the prepared particles present in the dentifrice of Example 2, and the blended particles B present in the dentifrice of Example 2 by laser A graph of the particle size distribution obtained by the emission/scattering particle size distribution measurement.

Figure 2 is a SEM photograph of the formulated particles B present in the dentifrice of Example 2.

Fig. 3 is a graph showing the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement of the prepared particles F present in the dentifrice of Comparative Example 1.

Hereinafter, the present invention will be described in detail.

The dentifrice of the present invention is formulated to have a special shape or a special particle size distribution and Made of particles with specific disintegration strength. The granules which are present in the dentifrice are granules containing a water-insoluble powder material (A) and an inorganic binder (B), hereinafter also referred to as "prepared granules". On the other hand, the particles to be formulated in the dentifrice for the presence of the formulated granules in the dentifrice are hereinafter referred to as "pre-mixed granules".

The water-insoluble powder material (A) is preferably a user generally used for an abrasive of teeth, and specifically, an inorganic material is preferable. Here, "water insoluble" means that the amount of dissolution (20 ° C) with respect to 100 g of water is 1 g or less. Specific examples thereof include, for example, light calcium carbonate, heavy calcium carbonate, zeolite, cerium oxide, calcium hydrogen phosphate, calcium phosphate, insoluble sodium metaphosphate, aluminum hydroxide, magnesium phosphate, calcium pyrophosphate, and magnesium carbonate. One or two or more of the above. These may be used alone or in combination of two or more.

In the water-insoluble powder material (A), the following special shape or special particle size distribution is imparted to the formulated particles present in the dentifrice, even if the load is low using a soft toothbrush. It is preferably selected from light calcium carbonate and heavy, from the viewpoint of sufficiently removing dirt such as tartar or stained dirt and improving the smooth touch and stain removal of the tooth surface. One or two or more kinds of calcium carbonate, zeolite, and cerium oxide are more preferably one or two selected from the group consisting of light calcium carbonate and heavy calcium carbonate, and more preferably heavy calcium carbonate. Here, the smooth touch is a feeling that the tongue can be smoothly slid on the surface of the tooth when the tongue is touched with the tongue, and the touch is sensible. It means a tactile sensation that the surface of the tooth becomes smooth and the dirt disappears.

The average particle diameter of the water-insoluble powder material (A) is preferably 0.1 μm or more, more preferably 0.5 μm or more, and still more preferably 0.8 μm or more from the viewpoint of removing plaque or dirt after particle disintegration. Further, it is preferably 1 μm or more. Moreover, from the viewpoint of reducing the foreign body sensation, it is preferably 20 μm or less, more preferably 15 μm or less, further preferably 10 μm or less, and further preferably 5 μm or less. Further, the average particle diameter of the water-insoluble powder material (A) is preferably from 0.1 to 20 μm, more preferably from 0.5 to 15 μm, still more preferably from 0.8 to 10. Further, μm, further preferably 1 to 5 μm.

Further, the average particle diameter can be measured by the method described in the examples.

The content of the water-insoluble powder material (A) is preferably 60% by mass or more, more preferably 60% by mass or more in the dry state, from the viewpoint of achieving a behavior of slowly disintegrating and improving the polishing force. It is 70% by mass or more, more preferably 80% by mass or more, and further preferably 82% by mass or more. The content of the water-insoluble powder material (A) is preferably 98% by mass or less, more preferably 96% by mass or less, more preferably 96% by mass or less, more preferably in the dry state, from the viewpoint of suppressing damage to the teeth. It is 90% by mass or less. Further, the content of the water-insoluble powder material (A) is preferably from 60 to 98% by mass, more preferably from 70 to 96% by mass, even more preferably from 80 to 96% by mass, in the dry state in the prepared granules. Further, it is preferably 82 to 90% by mass.

The inorganic binder (B) contained in the formulated granules present in the dentifrice of the present invention can sufficiently remove tartar by having voids in the granules after blending and combining with the water-insoluble powder material (A), and It has the effect of improving the smooth touch and stain removal of the tooth surface. The inorganic binder (B) may be one or more selected from the group consisting of a water-soluble inorganic binder and a water-insoluble inorganic binder. Specific examples of the water-soluble inorganic binder include one or more selected from the group consisting of sodium citrate, polyacrylic acid, modified cellulose, polyvinylpyrrolidone, and polyfluorene. It is sodium citrate. Specific examples of the water-insoluble inorganic binder include one or more selected from the group consisting of colloidal cerium oxide, magnesium metasilicate aluminate, synthetic aluminum silicate, calcium citrate, and alumina sol. Good for colloidal cerium oxide. Among them, from the viewpoint of exhibiting the effects of the present invention satisfactorily, it is preferred to contain a water-soluble inorganic binder, and more preferably sodium citrate. By containing one or two selected from the group consisting of sodium citrate and colloidal cerium oxide as the inorganic binder (B), the foam, the foaming property, and the sensation of the granules can be further improved, thereby improving the tooth surface. Smooth touch and stain removal.

The sodium citrate may be selected from the group consisting of sodium metasilicate (Na ₂ SiO ₃ ), sodium orthosilicate (Na ₄ SiO ₄ ), sodium diguate (Na ₂ Si ₂ O ₅ ), and sodium tetradecanoate ( One or two or more kinds of hydrates of Na ₂ Si ₄ O ₉ ) and the like.

Sodium citrate is usually Na ₂ O. nSiO ₂ . The molecular formula of mH ₂ O. The coefficient n (the molecular ratio of SiO ₂ to Na ₂ O) is called a molar ratio and can be represented by the following formula (I).

Mohr ratio = mass ratio (SiO ₂ mass% / Na ₂ O mass%) × (molecular weight of Na ₂ O / molecular weight of SiO ₂ ) (I)

As sodium citrate, water glass of various molar ratios can be used in addition to sodium citrate No. 1, No. 2, No. 3 described in JIS K1408, and among them, sodium citrate No. 3 is further preferable.

The physical properties of sodium citrate differ depending on the above molar ratio (coefficient n), but the alignment of the pharmaceutical raw material standard is well adapted to the effect of the present invention, and the obtained preparation is obtained. The molar ratio (coefficient n) is preferably 2.0 or more, more preferably 2.4 or more, still more preferably 2.8 or more, and still more preferably 3.0 or more, from the viewpoint that the pH of the particles becomes alkaline. It is preferably 4.0 or less, more preferably 3.5 or less, further preferably 3.4 or less, and further preferably 3.3 or less. Further, the molar ratio (coefficient n) is preferably from 2.0 to 4.0, more preferably from 2.4 to 3.5, still more preferably from 2.8 to 3.4, still more preferably from 3.0 to 3.3.

The content of one or two selected from the group consisting of sodium citrate (solid content) and colloidal cerium oxide in the inorganic binder (B) contained in the formulated granules present in the dentifrice of the present invention, The component (B) is preferably 60% by mass or more, more preferably 80% by mass or more, and still more preferably 90% by mass or more, from the viewpoint of granulating the water-insoluble powder material as the inorganic binder. From the viewpoints of spraying with droplets, suppressing coarse particles, and improving the wet disintegration strength of the particles after blending, it is preferably 100% by mass or less. Further, the amount of sodium citrate (solid content component) and colloidal cerium oxide in the inorganic binder (B) is the amount of moisture removed after the prepared granules extracted from the dentifrice are dried at 90 ° C or higher. .

Regarding the presence of the granules in the formulated granules present in the dentifrice of the present invention The content of one or two of the components (B) of sodium (solid content) and colloidal cerium oxide, in terms of the dry state of the particles, the moderate disintegration strength in water, the stability in the dentifrice, or From the viewpoint of the behavior of the slow disintegration, the particles after the preparation are preferably 1% by mass or more, more preferably 2% by mass or more, even more preferably 5% by mass or more, and further more preferably in the dry state. Preferably, it is 10% by mass or more. The content of sodium citrate in the granules after the preparation of the dentifrice of the present invention is preferably 30% by mass or less, more preferably 20% by mass, based on the viewpoint of improving the yield. Hereinafter, it is more preferably 18% by mass or less. Moreover, the content of sodium citrate in the formulated granules present in the dentifrice of the present invention is preferably from 1 to 30% by mass, more preferably from 2 to 20% by mass, still more preferably from 5 to 18% by mass, Further, it is preferably 10 to 18% by mass.

In the blended granules present in the dentifrice of the present invention, the inorganic binder is obtained from the viewpoint of granulating the water-insoluble powder material to have a moderate disintegration strength and achieving a behavior of slowly disintegrating. The mass ratio of the (B) to the water-insoluble powder material (A) (the inorganic binder (B) / water-insoluble powder material (A)) is preferably 0.02 or more, more preferably 0.05 or more, still more preferably 0.08 or more. Moreover, from the viewpoint of reducing the coarse particles and having an appropriate disintegration strength, the mass is preferably 0.5 or less, more preferably 0.3 or less, still more preferably 0.18 or less. Further, the mass is preferably from 0.02 to 0.5, more preferably from 0.05 to 0.3, still more preferably from 0.08 to 0.18. Further, the content of the case where sodium citrate is contained in the component (B) is a solid content conversion value.

The viewpoint of imparting an effect of suppressing the formation of tartar and enhancing the physical property of slowly disintegrating by a network structure formed of a water-soluble citrate or a colloidal cerium oxide, the present invention is present in the dentifrice The granule after blending preferably further contains one or more kinds of binding assistants (C) selected from the group consisting of calcium citrate, magnesium oxide, titanium oxide, and zinc oxide, and more preferably contains at least the component (C). Zinc oxide, and further preferably contains zinc oxide and other binding aids.

Regarding the content of the component (C), the effect of inhibiting the formation of tartar is increased and the disintegration is slowly disintegrated. From the viewpoint of the physical properties, the particles after the blending are preferably 0.2% by mass or more, more preferably 0.5% by mass or more, and still more preferably 0.8% by mass or more in the dry state. In addition, the content of the component (C) is suppressed from the viewpoint of excessively increasing the disintegration strength, the viewpoint of improving the foaming property or the foaming property of the dentifrice prepared with the prepared particles, and the viewpoint of suppressing the metallic taste. In the dry state, the particles are preferably 5% by mass or less, more preferably 3% by mass or less, and still more preferably 2% by mass or less. Further, the content of the component (C) is preferably from 0.2 to 5% by mass, more preferably from 0.5 to 3% by mass, even more preferably from 0.8 to 2% by mass, in the dry state of the particles after blending.

Regarding the mass ratio (C/B) of the component (C) to the component (B) in the granule after the blending, the viewpoint of achieving a moderate disintegration strength, and the foaming property or the foaming property of the dentifrice having the formulated granules are improved. From the viewpoint of the cleaning performance of the concave portions of various sizes on the surface of the tooth, it is preferably 0.02 or more, more preferably 0.05 or more, still more preferably 0.08 or more, and still more preferably 1 or less, still more preferably 0.5 or less. Further, it is preferably 0.3 or less, more preferably 0.2 or less. Further, the mass ratio (C/B) of the component (C) to the component (B) in the granule after blending is preferably 0.02 to 1, more preferably 0.05 to 0.5, still more preferably 0.08 to 0.3, and further, Good is 0.08~0.2.

The blended granules present in the dentifrice of the present invention may contain organic fibers, medicinal ingredients, coloring agents, and the like in addition to the above components, as needed within the scope of the effects of the present invention.

The other components other than the above components may be used alone or in combination of two or more.

The formulated particles present in the dentifrice of the present invention have a special shape, and the area of the projection surface of the particle (S _A ) and the area of the circle which is the diameter of the longest diameter (D _L ) in the projection surface ( average _S S) ratio _{(S a} / S S) of 0.5 or more and 0.9 or less. The area of the projection surface of the prepared particles in the present invention means that the 150 μm sieve of the JIS Z8801-1 standard is used to wash the aqueous solution of the dentifrice diluted with purified water to 10% by mass with purified water, and remains in the sieve. The granules on the net were dried at room temperature (25 ° C) for 1 day, and the obtained granules were used to measure the values obtained. The projected surface of the particle after blending means the surface obtained by photographing with KEENCE VH-5500 (100 times magnification), and the projection surface of the particle is obtained by using the analytical software (WinroOF (Sangu Trading Co., Ltd.) from the digital image obtained by photography. The area (S _A ) and the ratio (S _A /S _S ) of the area (S _S ) of the circle outside the diameter (D _L ) of the projection surface, and further based on the projection surface from other directions, or Using the projection surface obtained from the other prepared particles, the average value of S _A /S _S is obtained. Thus, the area (S _S ) and the projection surface of the circle are defined by the longest diameter (D _L ) in the projection surface. The average value of S _A /S _S obtained from the area (S _A ) is such that the closer the particle is to the spherical shape, the closer the value is to 1, in terms of the formulated particles present in the dentifrice of the present invention, the S _A The average value of /S _S is such that the area (S _S ) of the circle beyond the longest diameter (D _L ) in the projection surface is 0.5 or more and 0.9 or less, and therefore is not a spherical particle but a surface. There are a plurality of shapes of deformation of the concavities and convexities, that is, special shapes, so-called amorphous particles. Moreover, after the preparation of the present invention The granules exhibit a moderate amorphous shape in which the bulges are broken or partially deficient, so that no foreign body sensation is felt in the mouth, and on the other hand, the shape gradually disintegrates by the shape of the amorphous shape. At the end of brushing, it can also provide a large amount of granule disintegration and the feeling of brushing the end of the tooth.

It is considered that the formulated particles present in the dentifrice of the present invention have such a special shape, and even when a load such as a toothbrush is used in the oral cavity, the load is applied to the convex portion in a concentrated manner, so that it is easily disintegrated. Further, the convex portion is gradually disintegrated as a starting point. It is considered that the reason is that one of the particles after the preparation of the dentifrice of the present invention is formed by agglomerating a primary particle and forming an intermediate particle, which is further formed by agglomeration, so that the void is appropriately dispersed in the particle, with The intermediate particles from the protrusion to the surface begin to gradually disintegrate under load. Further, during the final disintegration of the particles, the intermediate particles are initially changed, and the intermediate particles gradually disintegrate gradually while being pulverized finer. Further, the granules after the preparation of the dentifrice of the present invention are preferably granules obtained by stirring the granules before they are formulated in the dentifrice. Thus, in the case of using the dentifrice of the present invention in which the post-dispensing granules obtained after the stirring at the time of manufacture are used, the granules after the blending are not It will disintegrate in one fell swoop due to the load of the toothbrush. During the brushing, the particles gradually disintegrate gradually, and the one side collides with the concave surface of the tooth to enter the fine concave portion of the glazed surface of the tooth to effectively transmit the load from the toothbrush. Thereby, the tartar or dirt removing ability can be sufficiently exerted, and the smooth touch feeling and the stain removing feeling of the tooth surface can be improved.

Regarding the average of the ratio (S _A /S _S ) of the area of the projection surface of the particle after the preparation (S _A ) to the area (S _S ) of the circle (S _S ) which is the diameter of the longest diameter (D _L ) in the projection surface, From the viewpoint of ensuring the behavior of slowly disintegrating, it is 0.5 or more, preferably 0.6 or more, more preferably 0.65 or more, still more preferably 0.7 or more. Regarding the average of the ratio (S _A /S _S ) of the area (S _A ) of the projection surface of the particle after the blending to the area (S _S ) of the circle (S _S ) which is the diameter of the longest diameter (D _L ) in the projection surface, In view of exhibiting moderate disintegration, it is 0.9 or less, preferably 0.85 or less, and more preferably 0.82 or less from the viewpoint of effectively transmitting the load with a toothbrush having a soft bristles. The average of the ratio (S _A /S _S ) of the area of the projection surface of the particle after the preparation (S _A ) to the area of the circle (S _S ) which is the diameter of the longest diameter (D _L ) in the projection surface is 0.5 The above is 0.9 or less, preferably 0.6 to 0.9, more preferably 0.65 to 0.85, and still more preferably 0.75 to 0.82. Further, examples of the soft bristles include tapered bristles in which the cross-sectional area of the bristles is gradually reduced. The tapered bristles are thin at the front end, so they have a soft touch and the hair ends easily enter the gap between the teeth and the teeth.

Regarding the average value of the ratio of the longest diameter (D _L ) to the shortest diameter (D _S ) in the projection surface of the prepared particles (D _L /D _S ), it becomes an amorphous particle and exhibits a slow disintegration behavior. The viewpoint and the weight of the toothbrush having the soft bristles are preferably 1.2 or more, more preferably 1.3 or more, and still more preferably 1.4 or more. Regarding the average value of the ratio of the longest diameter (D _L ) to the shortest diameter (D _S ) in the projection surface of the prepared particles (D _L /D _S ), it exhibits moderate disintegration and effectively transmits the toothbrush. From the viewpoint of the load, it is preferably 1.8 or less, more preferably 1.7 or less, still more preferably 1.65 or less. Moreover, the average of the ratio of the longest diameter (D _L ) to the shortest diameter (D _S ) (D _L /D _S ) in the projection surface of the prepared particles is preferably 1.2 to 1.8, more preferably 1.3 to 1.7, and further It is preferably 1.4 to 1.65.

Further, the formulated particles present in the dentifrice of the present invention have a special particle size distribution, and the following particles (a) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement on the particles (d):

(a) Particles having a particle diameter of 50 μm or more and less than 100 μm

(b) particles having a particle diameter of 100 μm or more and less than 150 μm

(c) particles having a particle diameter of 150 μm or more and less than 200 μm

(d) particles having a particle diameter of 200 μm or more and less than 250 μm

The volume ratio (b/c) of the amount of the particles (b) to the amount of the particles (c) is 0.7 or more and 1.2 or less, and the volume ratio (d/c) of the particles (d) to the particles (c) is 0.2. Above and below 1 , the volume ratio (b/d) of the amount of the particles (b) to the amount of the particles (d) is more than 1 and 5 or less, and the content of the particles after the preparation of the particles (c) is 15% by volume or more. And 55 vol% or less.

That is, by making the volume ratio (b/c) of the amounts between the particles (a) and the particles (b) within the above range, the particles (b) are made to the same extent with respect to the particles (c). Exist in the dentifrice, in contrast, since the above volume ratio (d/c) is within the above range and the particles (b/d) are greater than 1 and 5 or less, the particles (b) are more than the particles (d) The amount exists. Therefore, a large amount of particles (b) having a particle diameter of 100 μm or more and less than 200 μm and having a particle diameter of 200 μm or more are present in a moderate amount, and thus it is easy to transfer a toothbrush having a diameter of about 200 μm. The particles (d) of the stress of the bristles are moderately present, and there are many particles (b) and particles (c) which are easy to enter into the fine recesses of the glazed transverse stripes of the tooth surface which are not easily accessible to the bristles of the toothbrush. It is considered that, as the load of the brushed toothbrush is applied, the particles gradually disintegrate while interacting with each other, and enter the fine recessed portion such as the glazed surface of the tooth while effectively transmitting the surface. The granules of the toothbrush can fully exert the tartar or soil removal performance, and improve the smooth and smooth touch of the tooth surface or the touch of dirt removal.

Further, the blended particles present in the dentifrice of the present invention means those having a particle diameter of 50 μm or more as determined by laser diffraction/scattering particle size distribution measurement. Further, it is considered that the particles after the preparation of the dentifrice of the present invention are amorphous particles as described above, and the particle diameter determined by the laser diffraction/scattering particle size distribution measurement is approximately similar to The value of the average value of the longest diameter (D _L ) and the shortest diameter (D _S ).

In the formulated granules present in the dentifrice of the present invention, the behavior of slowly disintegrating is exhibited, and it is effective to enter the fine concave portion, and more preferably, it is effective to enter the concave portion having a width of 150 μm or less. The volume ratio of the amount of the particles (b) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution to the amount of the particles (c) from the viewpoint of improving the smooth touch of the tooth surface after brushing ( b/c) is 0.7 or more, preferably 0.75 or more, more preferably 0.8 or more. In the formulated particles present in the dentifrice of the present invention, the laser (b) collides with the particles (c) while slowly disintegrating and exists in the presence of particles of various shapes. The volume ratio (b/c) of the amount of the particles (b) to the amount of the particles (c) in the particle size distribution obtained by the diffraction/scattering particle size distribution measurement is 1.2 or less, preferably 1.1 or less, more preferably 1.0. Hereinafter, it is more preferably 0.95 or less. Further, in the formulated particles present in the dentifrice of the present invention, the amount of the particles (b) and the amount of the particles (c) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement The volume ratio (b/c) is 0.7 or more and 1.2 or less, preferably 0.75 or more and 1.1 or less, more preferably 0.8 or more and 1.0 or less, still more preferably 0.8 or more and 0.95 or less.

In the formulated particles present in the dentifrice of the present invention, the particles (d) which are easy to transmit the stress load of the bristles of the toothbrush are slowly disintegrated while interacting with the particles (b) and particles (c). The volume ratio of the amount of particles (d) to the amount of particles (c) in the particle size distribution obtained by laser diffraction/scattering particle size distribution from the viewpoint of particles of various shapes (d/c) It is 0.2 or more, preferably 0.25 or more, more preferably 0.3 or more. In the formulated particles present in the dentifrice of the present invention, by the particles (d), the particles (b) and the particles (c) are also effectively introduced into the fine recesses, from the viewpoint of the laser The volume ratio (d/c) of the amount of the particles (d) to the amount of the particles (c) in the particle size distribution obtained by the diffraction/scattering particle size distribution measurement is 1 or less, preferably 0.9 or less, more preferably 0.85. Hereinafter, it is further preferably 0.8 under. Further, in the formulated particles present in the dentifrice of the present invention, the amount of the particles (d) and the amount of the particles (c) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement are The volume ratio (d/c) is 0.2 or more and 1 or less, preferably 0.25 or more and 0.9 or less, more preferably 0.25 or more and 0.85 or less, still more preferably 0.3 or more and 0.8 or less.

In the formulated granules present in the dentifrice of the present invention, the granules of the granules after the blending are centered on the content of the granules (c) and contain more granules than the granules (d) which are easily accessible to the toothbrush. The fine particles (b) of the concave surface of the tooth, the viewpoint of improving the dirt removal performance of the fine concave portion of the tooth surface, and the viewpoint of improving the foaming property or foam quality of the dentifrice having the prepared particles The volume ratio (b/d) of the amount of the particles (b) to the amount of the particles (d) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution is greater than 1, preferably 1.1 or more, more preferably 1.2 or more. With regard to the formulated particles of the present invention, the particles (d) are slowly disintegrated while interacting with the particles (c) and the particles (b) while being subjected to the load of the bristles of the toothbrush, and are present in the form of particles having various shapes. The volume ratio (b/d) of the amount of the particles (b) to the amount of the particles (d) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is 5 or less, preferably 4 or less. More preferably 2.8 or less. Further, in the formulated particles present in the dentifrice of the present invention, the amount of the particles (b) and the amount of the particles (d) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement are The volume ratio (b/d) is more than 1 and is 5 or less, preferably 1.1 to 4, more preferably 1.2 to 2.8.

Furthermore, the particle size distribution of the prepared particles present in the dentifrice of the present invention and the particles before preparation is determined by a laser diffraction/scattering particle size distribution, and is present in the dentifrice. In the case of the granules after the preparation, the aqueous solution is diluted with an ion-exchanged water to a 10% by mass aqueous solution, and is used as an ion for the preparation of the pre-dispersed particles in the dentifrice. The exchanged water was diluted into a 5 mass% aqueous solution for measurement. More specifically, an aqueous solution in which the dentifrice having the formulated particles is diluted to 10% by mass by ion-exchanged water (or an aqueous solution in which the pre-prepared particles are diluted to 5 mass% by ion-exchanged water) is mixed by Machine (ROTARY MIXER NPC-20, NISSIN company Manufactured) The particles were dispersed at 75 rpm in a horizontal direction for 2 hours. Next, the aqueous solution obtained by diluting the dispersed dentifrice in the presence of the formulated particles (or the aqueous solution in which the pre-dispensing particles are dispersed) is stored at room temperature (25 ° C) for 1 day. After the aqueous solution after the storage was dispersed for 10 minutes by the above-mentioned mixer, the aqueous solution was used, and a laser diffraction/scattering particle size distribution measuring apparatus (Partica LA-950V2, manufactured by HORIBA) was used, and the refractive index was 1.58. The measurement was carried out under the conditions of a circulation speed (scale: 5) and a stirring speed (scale: 5).

In the formulated particles present in the dentifrice of the present invention, the amount of the particles (c) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is 15% by volume or more in the prepared particles. And 55 vol% or less. Regarding the amount of the particles (c), the dirt removal performance of the concave portion having a width of 150 μm or less on the surface of the tooth, and the interaction with other particles when brushing with a toothbrush and the width of the tooth surface are not as large as 200 μm. From the viewpoint of the removal performance of the concave portion, it is 15% by volume or more, preferably 20% by volume or more, more preferably 23% by volume or more, and 55% by volume or less, and preferably 50% by volume, in the particles after blending. Hereinafter, it is more preferably 45% by volume or less, still more preferably 40% by volume or less. Further, the amount of the particles (c) is 15% by volume or more and 55% by volume or less, preferably 20 to 50% by volume, more preferably 23 to 45% by volume, still more preferably 23 to 40% by volume in the blended particles. %.

For the formulated particles present in the dentifrice of the present invention, by granulating (c) the particles (a) to (d) to the maximum amount, or the particles (c) and particles (b) A relatively large amount of the same amount exists, and there are many particles in the dentifrice which have a recess which is not easily accessible to the bristles of the toothbrush and whose width is less than 200 μm. The total amount of the particles (b) and the particles (c) is preferably 30% by volume or more in terms of the fine dirt removal performance of the fine concave portion in which the bristles of the toothbrush are not easily obtained. It is more preferably 35 vol% or more, further preferably 40 vol% or more, and still more preferably 50 vol% or more. Regarding the total amount of the particles (b) and the particles (c), the stress generated by the bristles of the toothbrush is also sufficiently transmitted. When the particles (a) to (c) are applied, even in the case of using a toothbrush having a soft bristles, not only the concave portion having a width of less than 200 μm but also a fine concave portion having a width of 100 μm or less can be effectively used. From the viewpoint of exhibiting high dirt removal performance, the particles after blending are preferably 85% by volume or less, more preferably 80% by volume or less, and still more preferably 75% by volume or less. Further, the total amount of the particles (b) and the particles (c) is preferably 30 to 85% by volume, more preferably 35 to 80% by volume, still more preferably 40 to 80% by volume, and further preferably 40 to 80% by volume. It is preferably 50 to 75 vol%.

In the formulated granules present in the dentifrice of the present invention, even with a toothbrush having a soft bristles, the brushing stress generated by the toothbrush is transmitted to the particles of less than 200 μm, and the formulated granules are effectively From the viewpoint of entering the concave portion of the tooth surface having a width of 200 μm or less, and improving the foaming property or foam quality of the dentifrice having the prepared particles, the laser diffraction/scattering particle size distribution measurement is obtained. The volume ratio of the total amount of the particles (a) and the particles (b) to the total amount of the particles (c) and the particles (d) in the particle size distribution ((a+b)/(c+d)) is preferably 0.5). The above is more preferably 0.6 or more, further preferably 0.65 or more, and is preferably 1 or less, more preferably 0.9 or less, still more preferably 0.85 or less. Further, the volume ratio of the total amount of the particles (a) and the particles (b) to the total amount of the particles (c) and the particles (d) ((a+b)/(c+d)) is preferably 0.5 to 1, More preferably, it is 0.6 to 0.9, and further preferably 0.65 to 0.85.

The prepared particles of the present invention may further have particles (e) having a particle diameter of 250 μm or more and less than 350 μm in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement. Regarding the volume ratio of the total amount of particles (a) and particles (b) in the particles after the blending to the amount of the particles (e) ((a+b)/e), the use of the particles (a) to (d) is improved. From the viewpoint of the cleaning performance, it is preferably more than 1, more preferably 1.1 or more, still more preferably 1.2 or more, still more preferably 1.3 or more, and still more preferably 20 or less, still more preferably 18 or less. Further, the volume ratio of the total amount of the particles (a) and the particles (b) to the amount of the particles (e) ((a+b)/e) is preferably more than 1 and 20 or less, more preferably 1.1 to 20, Further preferably, it is 1.2 to 18, and more preferably 1.3 to 18.

In the formulated granules present in the dentifrice of the present invention, by arranging in the granules Laser diffraction/scattering method from the viewpoint that the diameter is larger than the particle (a) to ensure the behavior of slow disintegration, and the fine particles entering the fine concave portion of the tooth surface after the preparation to improve the tartar removal performance The amount of the particles (a) in the particle size distribution obtained by the particle size distribution measurement is preferably 3% by volume or more, more preferably 5% by volume or more, based on the particle size distribution, in terms of improving foam quality and foaming property. Further, it is preferably 7% by volume or more, and is preferably 15% by volume or less, more preferably 12% from the viewpoint of allowing the particles (b) or the particles (c) to interact to promote penetration of the particles into the fine concave portion. % or less, further preferably 10% by volume or less. Further, in the formulated particles present in the dentifrice of the present invention, the amount of the particles (a) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is preferably 3 in the prepared particles. ~15% by volume, more preferably 5 to 12% by volume, still more preferably 7 to 10% by volume.

In the formulated particles present in the dentifrice of the present invention, the amount of the particles (b) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is good with the particles (a). The ground interaction is preferably 12% by volume or more, more preferably 15%, in terms of the behavior of ensuring a slow disintegration between the particles having a particle diameter larger than that of the particles (b). % or more is more preferably 20% by volume or more, and is preferably 50% by volume or less, more preferably 40% by volume or less, still more preferably 35% by volume or less.

In the formulated particles present in the dentifrice of the present invention, the amount of the particles (d) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is performed by brushing the toothbrush by one side. The stress is transmitted to the particles (a) to (c) which are preferably interacting with the particles to ensure a slow disintegration behavior, preferably 5% by volume or more, preferably more preferably, after the blending. It is 10% by volume or more, more preferably 12% by volume or more, and is preferably 25% by volume or less, more preferably 22% by volume or less, still more preferably 20% by volume or less.

Further, in the formulated particles present in the dentifrice of the present invention, the amount of the particles (e) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is improved by using the particles (a) From the viewpoint of the cleaning performance of ~(d), it is preferable to have more particles after the preparation. It is 0% by volume, more preferably 1% by volume or more, still more preferably 2% by volume or more, and is preferably 25% by volume or less, more preferably 20% by volume or less, still more preferably 18% by volume or less.

In the formulated particles present in the dentifrice of the present invention, the amount of particles having a particle size of 350 μm or more in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is preferably in the prepared particles. It is 0% by volume, or more than 0% by volume and is 35% by volume or less, more preferably 15% by volume or less, further preferably 10% by volume or less, and still more preferably 5% by volume or less. In the pre-dispensing particles for obtaining the formulated particles present in the dentifrice of the present invention, the amount of the particles having a particle diameter of 350 μm or more is preferably 10% by volume or more, more preferably 15% by volume in the pre-formulation particles. % or more, further preferably 20% by volume or more, and preferably 35% by volume or less. It is generally believed that the formulated particles present in the dentifrice of the present invention are preferably subjected to a particle size distribution in a mixing step after formulating the particles in the dentifrice by causing a portion of the particles to be insufficient or to break the particles. If the prepared granules are present in the dentifrice after the mixing step, when the dentifrice is used, the touch of the granules can be well contacted while the teeth are being cleaned, and the brush is washed by using a toothbrush. It disintegrates and thus becomes easy to enter into the fine recess of the tooth surface.

The average particle diameter r (μm) of the particles after the preparation of the dentifrice of the present invention is preferably 75 μm or more, more preferably 100 μm or more, and further preferably from the viewpoint of having sufficient polishing power. From the viewpoint of suppressing the foreign body sensation in the oral cavity, it is preferably 250 μm or less, more preferably 220 μm or less, further preferably 210 μm or less, and still more preferably 180 μm or less. Further, the average particle diameter r (μm) of the particles after the formulation in the dentifrice of the present invention is preferably 75 to 250 μm, more preferably 100 to 220 μm, still more preferably 125 to 210 μm, and still more preferably 125. ~180μm.

Further, the average particle diameter r of the particles after blending is a volume average particle diameter, and is a median diameter in a particle size distribution of particles having a particle diameter of 50 μm or more obtained by laser diffraction/scattering particle size distribution measurement.

The special shape or special particle size distribution present in the dentifrice of the present invention The disintegration strength of the particles after the above blending is 1 gf / more and 20 gf / or less. By having the above-described disintegration strength, it is possible to gradually and gradually disintegrate by the shape of the amorphous shape when using a load such as a toothbrush, and it is possible to prevent the foreign matter from being felt in the mouth, and the particles can be made to enter the fine concave portion. Dirt such as tartar or stained dirt is sufficiently removed. Regarding the disintegration strength of the particles after the formulation, the viewpoint of the slow disintegration behavior and the improvement of the soil removal performance is exhibited, and even the softness is achieved by the interaction of the particles with the special shape or the special particle size distribution. The bristles of the bristles may be 1 gf or more, preferably 2 gf/piece or more, more preferably 3 gf/piece, from the viewpoint that the particles are gradually disintegrated by the stress of the toothbrush and enter the fine concave portion. the above. The disintegration strength of the particles after the above-mentioned blending is 20 gf/piece from the viewpoint of imparting a moderate disintegration property by a load of a lower load when using a soft toothbrush or the like, and reducing the foreign body sensation. In the following, it is preferably 15 gf/s or less, and more preferably 10 gf/piece or less, and further preferably 8 gf/piece or less, from the viewpoint of improving the foaming property or the foaming property of the dentifrice having the particles after blending. Further, the disintegration strength of the particles is 1 gf/piece or more and 20 gf/piece or less, preferably 2 to 15 gf/piece, more preferably 3 to 10 gf/piece, and still more preferably 3 to 8 gf/piece.

Furthermore, the disintegration strength of the granules after blending used in the present invention refers to the value measured in a wet state, and 10 to 20 formulated granules are extracted from the dentifrice, and a compression tester (Shimadzu) is used. In the production facility, MCTM-500), the load at the time of the particle size (180-200 μm) at a load rate of 1.51 gf/sec was measured for each particle, and the load was measured, and the average value was obtained. Further, the particle after blending used in the present invention has the same disintegration strength in a wet state and a disintegration strength in a dry state.

The formulated particles present in the dentifrice of the present invention may be prepared by using an inorganic binder of the component (B) as an aqueous solution (hereinafter referred to as "inorganic binder aqueous solution") and a water-insoluble powder material of the component (A). For mixing, it is preferred to use particles obtained by adding an aqueous solution of an inorganic binder to the component (A) as a pre-preparation granule, which is formulated in a dentifrice. When these are mixed, the bonding auxiliary of the component (C) may be further added.

In the case where sodium citrate is contained as the component (B), an aqueous solution of sodium citrate can be used as the sodium citrate, and the content of sodium citrate (solid content) in the aqueous sodium citrate solution is disintegrated. From the viewpoint of the properties of the granules, the aqueous solution of sodium citrate is preferably 20% by mass or more, more preferably 30% by mass or more, and still more preferably 35% by mass or more, from the viewpoint of suppressing coarse particles. It is preferably 65 mass% or less, more preferably 60 mass%. Further, sodium citrate (solid content component) in an aqueous solution of sodium citrate can be obtained by the method described in the examples. Further, when sodium citrate is contained as the component (B), the mass ratio of the component (A) to the aqueous inorganic binder solution (A/inorganic binder aqueous solution) is approximately 10 to 1, preferably 8 to 5. When the range is prepared, the inorganic binder solution can be prepared by diluting the inorganic binder of the sodium salt of the component (B) with water of 3 times or less. Further, it may be diluted with water to be mixed with the water-insoluble powder material of the component (A), and it is preferred to add an aqueous solution of the inorganic binder to the component (A) to form a pre-mixed particle. The inorganic binder aqueous solution is preferably added to the water-insoluble powder material of the component (A) at a moderate speed from the viewpoint of efficiently forming a void and agglomerating to form particles.

Specifically, for example, the rate of addition of the aqueous solution of the inorganic binder is preferably 35 parts by mass or less, more preferably 20 parts by mass or less, based on 100 parts by mass of the water-insoluble powder material (A). It is preferably 10 parts by mass or less, and preferably 0.5 parts by mass or more, more preferably 0.8 parts by mass or more, and still more preferably 1 part by mass or more. The above range is preferably in the case of using sodium citrate No. 1, No. 2 or No. 3 described in JIS K1408. In addition, the addition rate of the aqueous solution of the inorganic binder is preferably from 0.5 to 35 parts by mass, more preferably from 0.8 to 20% by mass, even more preferably from 100 to 20% by mass, based on 100 parts by mass of the water-insoluble powder material (A). 1 to 10% by mass.

In addition, the rate of addition of sodium citrate (solid content) is preferably 19 parts by mass or less, more preferably 100 parts by mass or less, based on 100 parts by mass of the water-insoluble powder material (A). Preferably, it is 11 parts by mass or less, and further preferably 5.5 parts by mass/minute. The amount is preferably 0.1 parts by mass or more, more preferably 0.2 parts by mass or more, and still more preferably 0.3 parts by mass or more. In addition, the addition rate of the sodium citrate (solid content component) is preferably 0.1 to 19 parts by mass, more preferably 0.2 to 11% by mass, even more preferably 100 parts by mass, based on 100 parts by mass of the water-insoluble powder material. It is 0.3 to 5.5% by mass.

As described above, when the aqueous solution (inorganic binder aqueous solution) of the component (B) and the component (C) as needed are added to the component (A) to form a pre-dispersed granule for obtaining the granulated particles, it is preferred to borrow Manufactured by rolling granulation. By blending the pre-formulation granules produced by the rolling granulation method into the dentifrice, particles having a special shape used in the present invention can be obtained without being obtained by the spray granulation method which has been conventionally used. The spherical particles, in turn, can obtain a wide range of broadly distributed pre-dispersed particles, whereby particles having a special particle size distribution used in the present invention can be obtained, and more voids can be dispersed in the particles. Thus, the formulated particles having the above characteristics and exhibiting a behavior of slowly disintegrating can be obtained.

Further, in the case of preparing the pre-dispensing particles for the prepared particles by the rolling granulation method as described above, it is preferred to use a container rotary granulator. Examples of the container rotary granulator include a drum type granulator and a pot type granulator. The drum type granulator is not particularly limited as long as it is processed by rotating the drum in a drum shape. In addition to the horizontal or slightly inclined drum type granulator, a cone roller type granulator, a multi-stage cone roller granulator, or the like can be used. These devices can be either batch or continuous.

Further, as described above, when the aqueous solution of the inorganic binder is added to the water-insoluble powder material of the component (A) at a relaxation rate, it is preferred to use a multi-fluid nozzle. In addition, the multi-fluid nozzle refers to a nozzle that allows a liquid and a gas for atomization (air, nitrogen, or the like) to flow through the independent flow path to the vicinity of the tip end portion of the nozzle to be mixed and atomized. Specifically, two nozzles are exemplified. Fluid nozzles, three-fluid nozzles, four-fluid nozzles, and the like.

The temperature of the aqueous solution of the inorganic binder when the aqueous solution of the inorganic binder is supplied by using the multi-fluid nozzle is preferably 5 ° C or more, more preferably from the viewpoint of stability at the time of addition. It is 10 ° C or more, and preferably 50 ° C or less, more preferably 30 ° C or less. Further, the temperature of the aqueous solution of the inorganic binder when the aqueous solution of the inorganic binder is supplied by the multi-fluid nozzle is preferably 5 to 50 ° C, more preferably 10 to 30 ° C.

Further, in the case of using the bonding auxiliary of the component (C), it is preferred to mix the component (C) together with the component (A). Specifically, the step of preparing the pre-dispensing particles in the case of obtaining the compounding component (C) preferably comprises a combination of the water-insoluble powder material of the component (A) and the component (C) using a container rotary granulator. The mixing step, and more preferably, comprises supplying the inorganic binder aqueous solution as the component (B) to the component (A) and the component (C) (preferably a mixture of the component (A) and the component (C)) using a multi-fluid nozzle. step.

From the viewpoint of ensuring the stability of the particles after blending, it is preferred to further dry the particles before the preparation to obtain the prepared particles. Specific examples of the drying include shed drying, fluidized bed drying, reduced pressure drying, and microwave drying. Among them, from the viewpoint of equipment, it is preferred that the shed is dried and the fluid layer is dried.

From the viewpoint of heat load, the drying temperature is preferably 60 ° C or higher, more preferably 70 ° C or higher, and still more preferably 80 ° C or higher. Further, it is preferably 200 ° C or lower, more preferably 150 ° C or lower, further preferably 110 ° C, and further preferably 90 ° C or lower. Further, the drying temperature is preferably from 60 to 200 ° C, more preferably from 70 to 150 ° C, still more preferably from 80 to 110 ° C, still more preferably from 80 to 90 ° C.

The drying time is preferably 10 minutes or longer, more preferably 20 minutes or longer, further preferably 30 minutes or longer, and is preferably 24 hours or shorter, more preferably 20 hours or shorter, further preferably 5 hours or shorter. Further, the drying time is preferably from 10 minutes to 24 hours, more preferably from 20 minutes to 20 hours, and still more preferably from 30 minutes to 5 hours.

Regarding the pre-proformed particles for obtaining the formulated particles present in the dentifrice of the present invention, the following particles (b') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement E-1'):

(b') particles having a particle diameter of 100 μm or more and less than 150 μm

(c') particles having a particle diameter of 150 μm or more and less than 200 μm

(d') particles having a particle diameter of 200 μm or more and less than 250 μm

(e-1') particles having a particle diameter of 250 μm or more and less than 300 μm

Among them, the volume ratio (b'/c') of the amount of the particles (b') to the amount of the particles (c') is preferably 0.6 or more and 1.25 or less, and the amount of the particles (d') and the particles (c') The volume ratio (d'/c') is preferably 0.7 or more and 1.2 or less, and the volume ratio of the amount of the particles (e-1') to the amount of the particles (c') (e-1'/c') It is preferably 0.4 or more and 1.1 or less. That is, the pre-dispensing particles have broad peaks in which the particles having a particle diameter of 100 μm or more and less than 300 μm are present in substantially the same extent, and by blending them, the special shapes or specialities as described above can be obtained. The particles are present in the dentifrice after blending of the particle size distribution.

Further, the so-called pre-dispensing particles means particles prepared before the dentifrice is prepared to obtain the formulated particles present in the dentifrice of the present invention, and is determined by laser diffraction/scattering particle size distribution. The particle diameter obtained was 50 μm or more. Further, it is considered that the particle diameter determined by the laser diffraction/scattering particle size distribution measurement is approximately equal to the average value of the longest diameter (D _L ') and the shortest diameter (D _S ').

In the pre-dispensing granule, the laser diffraction/spray is made from the viewpoint that the volume ratio (b/c) of the amount of the particles (b) in the prepared granules to the amount of the particles (c) becomes a desired value. The volume ratio (b'/c') of the amount of the particles (b') to the amount of the particles (c') in the particle size distribution obtained by the scattering particle size distribution measurement is preferably 0.6 or more, more preferably 0.75 or more, and further It is preferably 0.8 or more. The amount of particles (b') in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement from the viewpoint of effectively imparting a slow disintegration behavior to the particles after blending. The volume ratio (b'/c') to the amount of the particles (c') is preferably 1.25 or less, more preferably 1.15 or less, still more preferably 1.05 or less. Further, in the pre-mixed particles, the volume ratio of the amount of the particles (b') to the amount of the particles (c') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (b'/c' It is preferably 0.6 or more and 1.25 or less, more preferably 0.75 to 1.15, still more preferably 0.8 to 1.05.

In the pre-dispensing granule, the laser diffraction/spray is made from the viewpoint that the volume ratio (d/c) of the amount of the particles (d) in the prepared granules to the amount of the particles (c) becomes a desired value. The volume ratio (d'/c') of the amount of the particles (d') to the amount of the particles (c') in the particle size distribution obtained by the scattering particle size distribution measurement is preferably 0.7 or more, more preferably 0.8 or more, and further It is preferably 0.85 or more. The amount of particles (d') in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement from the viewpoint of effectively imparting a slow disintegration behavior to the particles after blending. The volume ratio (d'/c') to the amount of the particles (c') is preferably 1.2 or less, more preferably 1.15 or less, still more preferably 1.05 or less. Further, in the pre-mixed particles, the volume ratio of the amount of the particles (d') to the amount of the particles (c') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (d'/c' It is preferably 0.7 or more and 1.2 or less, more preferably 0.8 to 1.15, still more preferably 0.85 to 1.05.

Particles (e-1') in a particle size distribution obtained by laser diffraction/scattering particle size distribution from the viewpoint of easily obtaining the particles after slow disintegration in the pre-dispensing particles The volume ratio (e-1'/c') of the amount to the amount of the particles (c') is preferably 0.4 or more, more preferably 0.5 or more, still more preferably 0.6 or more, still more preferably 0.7 or more. In the particle before the blending, the particle (e-1') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution is determined from the viewpoint of effectively imparting a slow disintegration behavior to the particle after blending. The volume ratio (e-1'/c') of the amount to the amount of the particles (c') is preferably 1.1 or less, more preferably 1 or less. Further, in the pre-mixed particles, the volume ratio of the amount of the particles (e-1') to the amount of the particles (c') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (e-1) '/c') is preferably 0.4 or more and 1.1 or less, more preferably 0.5 to 1.1, still more preferably 0.6 to 1, and further preferably 0.7 to 1.

Further, (a') in the particle size distribution obtained by laser diffraction/scattering particle size distribution, from the viewpoint of easily obtaining the prepared particles having a tendency to slowly disintegrate in the pre-dispensing particles The volume ratio (a'/c') of the amount of the particles (particles (a')) having a diameter of 50 μm or more and less than 100 μm to the amount of the particles (c') is preferably 0.2 or more, more preferably 0.3 or more. In the pre-dispersion granules, the behavior of slowly disintegrating is obtained and can also be effectively entered into the fine concave From the viewpoint of the particle after the blending, the particle size distribution (a') obtained by the laser diffraction/scattering particle size distribution has a particle size of 50 μm or more and less than 100 μm (particle (a')). The volume ratio (a'/c') of the amount to the amount of the particles (c') is preferably 1.2 or less, more preferably 1 or less. Further, in the particle before the blending, the amount of the particles (particles (a')) having a (a') particle diameter of 50 μm or more and less than 150 μm in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement. The volume ratio (a'/b') to the amount of the particles (b') is preferably from 0.2 to 1.2, more preferably from 0.3 to 1.

In the pre-mixed particles, the particle size distribution is determined by the laser diffraction/scattering particle size distribution from the viewpoint that the particles (a) or particles (b) in the prepared particles interact well to ensure the slow disintegration behavior. The amount of the particles (a') in the obtained particle size distribution is preferably from 3 to 20% by volume, more preferably from 5 to 18% by volume, even more preferably from 7 to 15% by volume, based on the particles before preparation.

In the pre-dispense granules, the particles (c) are present in the desired amount in the formulated granules, and the particles (a) or granules (b) are well interacted to ensure slow disintegration. In view of the above, the amount of the particles (c') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is preferably 5 to 30% by volume, more preferably 8 to 25% by volume in the pre-proformed particles. %, further preferably 10 to 20% by volume.

Further, in the particle before blending, it is easy to obtain the particle after the blending of the particle size distribution obtained by the laser diffraction/scattering particle size distribution from the viewpoint of easily obtaining the particle after the slow disintegration behavior (e-2' The volume ratio (e-2'/b') of the particles having a particle diameter of 300 μm or more and less than 550 μm (particles (e-2')) to the amount of the particles (b) is preferably 0.3 or more, more preferably It is 0.4 or more. The particle size distribution obtained by laser diffraction/scattering particle size distribution is obtained from the viewpoint of obtaining a post-dispersion particle having a slow disintegration behavior and being able to effectively enter the fine concave portion in the pre-dispensing particles. The volume ratio (e-2'/b') of the amount of the particles (e-2') to the amount of the particles (b') is preferably 1 or less, more preferably 0.95 or less. Further, in the pre-mixed particles, the volume ratio of the amount of the particles (e-2') to the amount of the particles (b') in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (e-2) '/b') is preferably from 0.3 to 1, more preferably from 0.4 to 0.95.

In the pre-mixed granules, the particles (a) or granules (b) in the prepared granules are well phased. From the viewpoint of interaction to ensure the behavior of slow disintegration, the amount of particles (e-2') in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement is preferably in the pre-proformed particles. 2 to 15% by volume, more preferably 5 to 12% by volume, still more preferably 7 to 12% by volume.

Further, in the pre-dispensing particles, the amount of the particles having a particle diameter of 350 μm or more in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement is preferably 5 to 50% by volume in the particles before preparation. More preferably, it is 10 to 45 vol%, and further preferably 15 to 42 vol%.

The average particle diameter r' (μm) of the particles before blending is preferably 50 μm or more, more preferably 75 μm or more, and still more preferably 100 μm or more, from the viewpoint of having sufficient polishing force, thereby suppressing foreign matter in the oral cavity. From the viewpoint of sensation, it is preferably 500 μm or less, more preferably 450 μm or less, and still more preferably 400 μm or less. Further, the average particle diameter r' (μm) of the particles before preparation is preferably from 50 to 500 μm, more preferably from 75 to 450 μm, still more preferably from 100 to 400 μm.

Further, the average particle diameter r' of the particles before preparation is a volume average particle diameter, and is a median diameter in a particle size distribution of particles having a particle diameter of 50 μm or more obtained by laser diffraction/scattering particle size distribution measurement. .

Regarding the disintegration strength of the granules before the preparation, in the formulated granules present in the dentifrice of the present invention, from the viewpoint of ensuring the slow disintegration behavior and the high soil removal performance, it is preferably 1 gf/ More preferably, it is 2 gf / or more, More preferably, it is 3 gf / or more. Regarding the disintegration strength of the particles before the above-mentioned blending, even if a load of a lower load when using a soft toothbrush or the like is applied, the disintegration property of the formulated particles present in the dentifrice of the present invention is imparted, The viewpoint of reducing the foreign body sensation is preferably 20 gf/s or less, more preferably 15 gf/s or less, further preferably 10 gf/s or less, and further preferably 8 gf/s or less. Further, the disintegration strength of the particles is preferably 1 gf/piece or more and 20 gf/piece or less, preferably 2 to 15 gf/piece, more preferably 3 to 10 gf/piece, still more preferably 3 to 8 gf/piece.

Furthermore, the disintegration strength of the pre-dispensing particles used in the present invention means wet The value measured in the state can be determined by the same method as the disintegration strength of the particles after the blending. Further, regarding the particles before blending, the disintegration strength in the wet state is the same as the disintegration strength in the dry state.

The ratio of the area of the projection surface of the particle before the preparation (S _A ') to the area of the circle (S _S ' with the longest diameter (D _L ') in the projection surface (S _A '/S _S ' The average value of the particles is preferably 0.5 or more, more preferably 0.6 or more, and still more preferably 0.65 or more from the viewpoint of imparting a slow disintegration behavior to the particles obtained after the preparation of the particles. The ratio of the area of the projection surface of the particle before the preparation (S _A ') to the area of the circle (S _S ' with the longest diameter (D _L ') in the projection surface (S _A '/S _S ' The average value is preferably 0.9 or less, more preferably 0.85 or less, from the viewpoint of exhibiting a moderate disintegration property of the prepared particles obtained by the pre-mixing particles and effectively transferring the load from the toothbrush. Furthermore, the area (S _A ') of the projection surface of the particle before preparation, the longest diameter (D _L '), the area of the circle (S _S '), and the ratio (S _A '/S _S ' The average value is the value obtained by the same method as the above-described blended particles.

Regarding the average value of the ratio of the longest diameter (D _L ') to the shortest diameter (D _S ') (D _L '/D _S ') in the projection plane of the particles before blending, the particles before the blending are obtained into an amorphous shape and displayed. From the viewpoint of the particles after blending which are slowly disintegrated, it is preferably 1.2 or more, more preferably 1.3 or more, still more preferably 1.5 or more. Regarding the average value of the ratio of the longest diameter (D _L ') to the shortest diameter (D _S ') (D _L '/D _S ') in the projection plane of the particles before blending, the particle performance after blending obtained from the pre-mixed particles From the viewpoint of appropriately disintegrating and efficiently transferring the load from the toothbrush, it is preferably 2 or less, more preferably 1.8 or less, still more preferably 1.75 or less. Further, the average of the ratio of the longest diameter (D _L ') to the shortest diameter (D _S ') (D _L '/D _S ') in the projection surface of the particles before preparation is preferably 1.2 to 2, more preferably 1.3. ~1.8, and further preferably 1.5 to 1.75.

Regarding the amount of the particles after the preparation of the dentifrice of the present invention obtained by using the above-mentioned pre-formulation particles, the disintegration behavior of the particles is sufficiently exerted to improve the tartar or soil removal effect and to improve the feeling of use. In view of the above, the dentifrice of the present invention is preferably 1% by mass or more, more preferably 3% by mass or more, and still more preferably 5% by mass or more. on The amount of the granules after the preparation of the dentifrice of the present invention is a dentifrice of the present invention from the viewpoint of not exhibiting a foreign body sensation and exerting a tartar or soil removing effect without damaging the enamel of the teeth. The amount is preferably 50% by mass or less, more preferably 30% by mass or less, further preferably 25% by mass or less, and still more preferably 20% by mass or less. Moreover, the amount of the granules after the preparation of the dentifrice of the present invention is preferably from 1 to 50% by mass, more preferably from 3 to 30% by mass, even more preferably from 5 to 25, in the dentifrice of the present invention. The mass%, and more preferably 5-20% by mass.

In order to obtain the formulated granules having a special shape or a special particle size distribution as described above in the dentifrice of the present invention, it is preferred to prepare the granules after blending the following binders in the dentifrice. Formulated in a dentifrice. Further, in the step of preparing the binder in the dentifrice, after the pre-mixing particles are added to the dentifrice, the stirring speed of the dentifrice is also dependent on the stirring device or the stirring time, but Preferably, the stirring is carried out at 10 rpm or higher, more preferably at a stirring speed of 20 rpm or higher, and the stirring is preferably carried out at a stirring speed of 250 rpm or less. Further, stirring is preferably carried out at a stirring speed of 10 rpm or more and 250 rpm or less, more preferably Stirring was carried out at a stirring speed of 20 rpm or more and 250 pm or less. When the dentifrice is stirred at the above-mentioned stirring speed, for example, a universal mixing mixer (5XDMV-10-r, manufactured by Dalton Co., Ltd.), a paddle mixer (TK Paddle Mixer 2SL-10, Special Machine Co., Ltd.), or the like can be used. The stirring machine is stirred. When the above-mentioned universal mixing mixer is used, it is preferable to set the stirring speed of the rotation to 40 to 230 rpm, more preferably 90 to 200 rpm, and it is preferable to set the stirring speed of the revolution to 20~. 110 pm, and further preferably set to 35 to 75 rpm. In the case of using the paddle mixer described above, the agitation speed of the paddle is preferably 10 to 70 rpm, and the agitation speed of the turbine is preferably 20 to 90 rpm. Further, as for the stirring of the dentifrice, the particles in the dentifrice may be dispersed. When the stirring speed is low, the stirring time may be long, and the stirring speed is high. In the case, the stirring time can be set to a short time. From the above point of view, the stirring time is preferably from 5 minutes to 90 minutes, more preferably 10 minutes. Clock ~ 60 minutes.

In the method for producing a dentifrice of the present invention, it is preferred to include a step of stirring the dentifrice after adding the pre-dispensing particles. By having this step, the prepared particles having the following particle size distribution can be obtained: the particles having a large particle size distribution before the blending contain particles having a larger particle diameter of 100 to 200 μm and containing more particles smaller than the peak of the particle size distribution. path.

The dentifrice of the present invention is prepared by mixing particles containing the above component (A) and component (B), optionally component (C) or component (D), and is formulated in a dentifrice. The post-particles have a special shape or a special particle size distribution and exhibit a behavior of slow disintegration, so that it is preferable to adjust the interfacial activity from the viewpoint of ensuring a high cleaning effect by the synergistic effect of the lathering property. Agent. Thereby, good foaming property can be obtained, and the foaming property can be continued, and the tartar or dirt removal effect can be sufficiently exerted to a narrow area such as a gap between the teeth and the teeth, and the cleaning teeth of the present invention can be used. The oral cavity after the agent imparts a smooth touch to the tooth surface and also improves the feeling of use.

As the surfactant, an anionic surfactant, a nonionic surfactant, or a zwitterionic surfactant can be used. Examples of the anionic surfactant include alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate; N-sodium lauric acid-sodium sarcosinate, and N-myristyl-sodium sarcosinate. - mercaptocreatine; N-mercapto glutamate such as N-palmityl glutamate, sodium N-methyl-N-mercapto taurate, N-methyl-N-fluorenyl Sodium alaninate, sodium α-olefin sulfonate, sodium dioctyl sulfosuccinate, and the like. The anionic surfactant is preferably an anionic surfactant, and more preferably an alkyl sulfate such as sodium lauryl sulfate, from the viewpoint of imparting good foaming properties or feeling of use.

The amount of the surfactant to be added is preferably 0.2% by mass or more, more preferably 0.2% by mass or more, from the viewpoint of improving the foaming property and improving the cleaning effect or the feeling of use and bringing about a good flavor. It is preferably 0.3% by mass or more, and more preferably 0.5% by mass or more. Moreover, regarding the amount of the surfactant to be added, in terms of suppressing the damage of the flavor, The dentifrice of the present invention is preferably 2.0% by mass or less, more preferably 1.7% by mass or less, still more preferably 1.5% by mass or less. Further, the blending amount of the surfactant is preferably 0.2 to 2.0% by mass, more preferably 0.3 to 1.7% by mass, still more preferably 0.5 to 1.5% by mass, based on the dentifrice of the present invention. The mass ratio of the above-mentioned formulated particles and the surfactant in the dentifrice of the present invention (particle/surfactant after blending) is preferably from 0.5 to 250, more preferably from 2 to 100, and still more preferably 4 ~40.

The amount of the anionic surfactant is preferably 0.2% by mass or more in the dentifrice of the present invention from the viewpoint of improving the degree of foaming, the cleaning effect, the feeling of use, or the feeling of use. More preferably, it is 0.3 mass% or more, More preferably, it is 0.5 mass% or more. In addition, the amount of the anionic surfactant is preferably 2.5% by mass or less, more preferably 2.0% by mass or less, even more preferably 1.7, in terms of the dentifrice of the present invention. quality%. Further, the blending amount of the anionic surfactant is preferably 0.2 to 2.5% by mass, more preferably 0.3 to 2.0% by mass, still more preferably 0.5 to 1.7% by mass, based on the dentifrice of the present invention. The amount of the alkyl sulfate to be added is preferably 0.2% by mass or more in the dentifrice of the present invention from the viewpoint of improving the degree of foaming, the cleaning effect, the feeling of use, and the feeling of use. More preferably, it is 0.3 mass% or more, More preferably, it is 0.5 mass% or more. Further, the amount of the alkyl sulfate to be added is preferably 2.5% by mass or less, more preferably 2.0% by mass or less, even more preferably 1.7, in terms of the dentifrice of the present invention. Below mass%. Further, the amount of the alkyl sulfate to be added to the dentifrice of the present invention is preferably 0.2 to 2.5% by mass, more preferably 0.3 to 2.0% by mass, still more preferably 0.5 to 1.7% by mass.

The dentifrice of the present invention is preferably further formulated with a binder. Examples of the binder include sodium carboxymethylcellulose, sodium polyacrylate, hydroxyethylcellulose, montmorillonite, sanxian gum, carrageenan, sodium alginate, guar gum, pectin, and the like. One or more selected from the group consisting of a dentifrice, preferably a toothpaste, and further preferably one or two selected from the group consisting of sodium carboxymethylcellulose, triterpene, and carrageenan. More than one species. About the dentifrice of the invention The amount of the binder is such that the above components are dissolved and dispersed while being effectively dispersed in the oral cavity, thereby effectively exerting the tartar or soil removal effect of the particles after the slow disintegration, thereby improving the smoothness of the tooth surface. The touch and the stain removal, the good foaming property is maintained by the synergistic effect with the surfactant, and the good foaming property during the brushing process is maintained by the synergistic effect of the particles and the surfactant. In view of the above, the dentifrice of the present invention is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, further preferably 0.7% by mass or more, and preferably 3% by mass or less, more preferably 2% by weight. The mass% or less is further preferably 1.8% by mass or less. Further, the amount of the binder in the dentifrice of the present invention is preferably from 0.1 to 3% by mass, more preferably from 0.5 to 2% by mass, even more preferably from 0.7 to 1.8% by mass, based on the dentifrice of the present invention. . In the dentifrice of the present invention, the mass ratio of the granules and the binder after the preparation (the granules/adhesives after blending) is such that the above components are dissolved and dispersed while being effectively dispersed in the oral cavity, and the utilization is effectively utilized. The tartar or dirt removal effect of the particles after the disintegration of the ground can improve the smooth touch and the stain removal feeling of the tooth surface, and the good foaming property is preferably 0.2 to 500, and further Preferably, it is from 1 to 60, and further preferably from 2.5 to 30.

The dentifrice of the present invention is preferably formulated with a tackifying cerium oxide in addition to the above-mentioned binder in terms of improving storage stability or a touch in the oral cavity. The so-called viscosity-increasing cerium oxide refers to cerium oxide having an oil absorption of 200 to 400 mL/100 g, which is different from the abrasive cerium oxide having an oil absorption of 50 to 150 mL/100 g. Here, the amount of oil absorption refers to the amount of oil that can carry cerium oxide, and the measurement method is the amount of cooked linseed oil absorbed by the method based on JIS K5101-13-2 (2004). Specific. The amount of the viscous cerium oxide in the dentifrice of the present invention is preferably 1% by mass or more, more preferably 2% by mass or more, still more preferably 3% by mass or more, and more preferably 3% by mass or more. It is preferably 15% by mass or less, and more preferably 10% by mass or less. Further, the amount of the tackifying cerium oxide in the dentifrice of the present invention is preferably from 1 to 15% by mass, more preferably from 2 to 10% by mass, still more preferably from 3 to 10% by mass.

The dentifrice of the present invention can be further formulated with a humectant. Examples of the humectant include sorbitol, glycerin, propylene glycol, 1,3-butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xylitol, maltitol, lactitol, and erythritol. One or two or more of the above. The amount of the wetting agent in the dentifrice of the present invention is such that the above-mentioned components are effectively dispersed in the oral cavity while being dissolved and dispersed, and the tartar or soil removing effect of the particles after the disintegration by the slow disintegration is effectively exhibited. It is preferably 5% by mass or more, more preferably 10% by mass or more, and still more preferably 15% by mass in the dentifrice of the present invention, in combination with a surfactant to give a good foaming property. % or more, and preferably 60% by mass or less, more preferably 50% by mass or less, still more preferably 40% by mass or less. Further, the amount of the wetting agent in the dentifrice of the present invention is preferably from 5 to 60% by mass, more preferably from 10 to 50% by mass, even more preferably from 15 to 40% by mass, based on the dentifrice of the present invention. .

The dentifrice of the present invention can be further formulated with water. The amount of water in the dentifrice of the present invention is such that the above-mentioned components are effectively dispersed in the oral cavity while being dissolved and dispersed, and the tartar or soil removing effect of the particles which are slowly disintegrated is effectively exhibited, even by The load of a lower load such as a soft toothbrush can also exert a high dirt removal ability, and in combination with a surfactant to bring about good foaming property, in the dentifrice of the present invention It is preferably 3% by mass or more, more preferably 5% by mass or more, further preferably 7% by mass or more, and more preferably 50% by mass or less, more preferably 45% by mass or less, still more preferably 40% by mass or less. . Further, the water content in the dentifrice of the present invention is preferably from 3 to 50 in the dentifrice of the present invention from the viewpoint of good solubility or dispersibility and tartar or soil removal ability. The mass % is more preferably 5 to 45% by mass, still more preferably 7 to 40% by mass. In addition, the amount of water refers to an amount obtained by adding all of the water content to be blended and the other components of the blended components, and these may be calculated by calculation of each blending amount, but for example, Kelvin water may be utilized. The agent was measured. As the Kappa water agent, for example, a trace moisture measuring device (Pinguma Industry Co., Ltd.) can be used. For the device, 5 g of a dentifrice can be taken, suspended in 25 g of anhydrous methanol, and 0.02 g of the suspension is taken for measurement. The amount of water measured is set to the amount of water. Regarding the ratio of the above-mentioned blended granules and moisture in the dentifrice of the present invention (particle/water content after blending), from the viewpoint of good solubility or dispersibility, and tartar or soil removing ability, Preferably, it is 0.02 to 15, more preferably 0.1 to 6, and further preferably 0.2 to 3.

The dentifrice of the present invention is preferably formulated with a pH adjusting agent. The pH adjusting agent is a phosphoric acid and a salt thereof (sodium phosphate such as disodium hydrogen phosphate or sodium dihydrogen phosphate), citric acid and a salt thereof, from the viewpoint of improving the taste of the present invention and preventing damage. , malic acid and its salts, gluconic acid and its salts, maleic acid and its salts, aspartic acid and its salts, gluconic acid and its salts, succinic acid and its salts, glucuronic acid and its salts, Fumaric acid and its salt, glutamic acid and its salt, adipic acid and its salt, hydrochloric acid, sodium hydroxide, potassium hydroxide, etc., may be selected from one of these or may be preferably used. 2 or more types. The dentifrice of the present invention preferably comprises phosphoric acid selected from the group consisting of disodium hydrogen phosphate and sodium dihydrogen phosphate and a salt thereof as a pH adjuster. The amount of the pH adjusting agent is not particularly limited as long as it is a desired pH value, and is preferably 0.01 to 5% by mass, more preferably 0.1 to 3% by mass, based on the dentifrice of the present invention. Further, the pH of the dentifrice of the present invention is preferably more than 7, more preferably 7.5 or more, still more preferably 7.8 or more, and still more preferably 11 or less, still more preferably 10 or less, still more preferably 9.5 or less. . Here, the pH value of the dentifrice of the present invention means a value measured at 25 ° C when the pH electrode is diluted with water to 10% by mass.

The dentifrice of the present invention may be formulated with other ingredients than the above, such as abrasives, excipients, sweeteners, preservatives, perfumes, medicinal ingredients, coloring agents, and other commonly used ingredients.

The other components mentioned above may be used alone or in combination of two or more.

Regarding the above-described embodiments of the present invention, the following granules and dentifrice for dentifrice are further disclosed.

[1] A dentifrice comprising a granule comprising a water-insoluble powder material (A) and an inorganic binder (B), and the granules after being formulated in the dentifrice The average of the ratio (S _A /S _S ) of the area (S _A ) of the projection surface to the area (S _S ) of the circle outside the diameter (D _L ) of the projection surface is 0.5 or more and 0.9. Hereinafter, the disintegration strength of the particles after the blending is 1 gf/piece or more and 20 gf/piece or less.

[2] The dentifrice according to the above [1], wherein the ratio of the longest diameter (D _L ) to the shortest diameter (D _S ) in the projection surface of the particle with respect to the formulated particles present in the dentifrice ( The average value of D _L /D _S ) is preferably 1.8 or less, more preferably 1.7 or less, still more preferably 1.65 or less, and is preferably 1.2 or more, more preferably 1.3 or more, still more preferably 1.4 or more.

[3] The dentifrice according to [1] or [2] above, wherein the area (S _A ) of the projection surface of the prepared particles and the longest diameter (D _L ) of the projection surface are outside the diameter The average value of the ratio (S _A /S _S ) of the area (S _S ) is preferably 0.6 or more, more preferably 0.65 or more, still more preferably 0.7 or more, and is preferably 0.85 or less, more preferably 0.82 or less.

[4] A dentifrice comprising a granule containing a water-insoluble powder material (A) and an inorganic binder (B), and the granules after being formulated in the dentifrice, The following particles (a) to (d) in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement:

(a) Particles having a particle diameter of 50 μm or more and less than 100 μm

(b) particles having a particle diameter of 100 μm or more and less than 150 μm

(c) particles having a particle diameter of 150 μm or more and less than 200 μm

(d) particles having a particle diameter of 200 μm or more and less than 250 μm

The volume ratio (b/c) of the amount of the particles (b) to the amount of the particles (c) is 0.7 or more and 1.2 or less, and the volume ratio (d/c) of the particles (d) to the particles (c) is 0.2. Above and below 1 , the volume ratio (b/d) of the amount of the particles (b) to the amount of the particles (d) is more than 1 and 5 or less, and the amount of the particles (c) in the prepared particles is 15% by volume or more. And 55 volume% or less, and the disintegration intensity of the particle after preparation is 1 gf / more and 20 gf / or less.

[5] The dentifrice according to [4] above, wherein in the granule after the blending, the laser is diffracted/dispersed The volume ratio (b/c) of the amount of the particles (b) to the amount of the particles (c) in the particle size distribution obtained by the measurement of the particle size distribution is preferably 0.75 or more, more preferably 0.8 or more, and preferably 1.1. Hereinafter, it is more preferably 1.0 or less, further preferably 0.95 or less.

[6] The dentifrice according to [4] or [5] above, wherein the amount of the particles (d) in the particle size distribution obtained by the laser diffraction/scattering particle size distribution is determined in the blended particles. The volume ratio (d/c) of the amount of the particles (c) is preferably 0.25 or more, more preferably 0.3 or more, and is preferably 0.9 or less, more preferably 0.85 or less, still more preferably 0.8 or less.

[7] The dentifrice according to any one of the above [4] to [6] wherein, in the prepared particles, the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (b) The volume ratio (b/d) of the amount to the amount of the particles (d) is preferably 1.1 or more, more preferably 1.2 or more, and is preferably 4 or less, more preferably 2.8 or less.

[8] The dentifrice according to any one of the above [4] to [7] wherein, in the prepared particles, the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (c) The amount is preferably 20% by volume or more, more preferably 23% by volume or more, and is preferably 50% by volume or less, more preferably 45% by volume or less, still more preferably 40% by volume or less.

[9] The dentifrice according to any one of the above [4], wherein, in the granule after the formulation, the total amount of the granule (b) and the granule (c) is preferably 30% by volume or more. It is preferably 35 vol% or more, more preferably 40 vol% or more, still more preferably 50 vol% or more, and is preferably 85% by volume or less, more preferably 80% by volume or less, still more preferably 75% by volume or less. .

[10] The dentifrice according to any one of the above [4] to [9] wherein, in the prepared particles, the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (a) And the volume ratio of the total amount of the particles (b) to the total amount of the particles (c) and (d) ((a + b) / (c + d)) is preferably 0.5 or more, more preferably 0.6 or more, Further, it is preferably 0.65 or more, and is preferably 1 or less, more preferably 0.9 or less, still more preferably 0.85 or less.

[11] The dentifrice according to any one of the above [4] to [10] wherein, in the prepared particles, the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (a) )and The volume ratio of the total amount of the particles (b) to the amount of the particles (e) ((a+b)/e) is preferably more than 1, more preferably 1.1 or more, still more preferably 1.2 or more, and still more preferably 1.3. The above is preferably 20 or less, more preferably 18 or less.

[12] The dentifrice according to any one of the above [4] to [11] wherein, in the prepared particles, the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (a) The amount is preferably 3% by volume or more, more preferably 5% by volume or more, still more preferably 7% by volume or more, and is preferably 15% by volume or less, more preferably 12% by volume or less, still more preferably 10% by volume or less. Below volume%.

[13] The dentifrice according to any one of the above [4] to [12] wherein, in the prepared particles, the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution measurement (b) The amount is preferably 12% by volume or more, more preferably 15% by volume or more, still more preferably 20% by volume or more, and more preferably 50% by volume or less, still more preferably 40% by volume or less, and still more preferably 35% by volume. Below volume%.

[14] The dentifrice according to any one of the above [4] to [13] wherein the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution are determined in the blended particles (d) The amount is preferably 5% by volume or more, more preferably 10% by volume or more, still more preferably 12% by volume or more, and is preferably 25% by volume or less, more preferably 22% by volume or less, still more preferably 20% by volume or more. Below volume%.

[15] The dentifrice according to any one of the above [4] to [14] wherein the particle after the blending contains a particle size of 250 μm in the particle size distribution obtained by laser diffraction/scattering particle size distribution measurement. The particles (e) above and not up to 350 μm, and the amount of the particles (e) is preferably more than 0% by volume, more preferably 1% by volume or more, still more preferably 2% by volume or more, and preferably 25% by volume. % or less is more preferably 20% by volume or less, still more preferably 18% by volume or less.

[16] The dentifrice of any one of the above [1] to [15], wherein the disintegration strength of the granule after the preparation is preferably 2 gf / more, more preferably 3 gf / more, and preferably 15 gf / or less, more preferably 10 gf / or less, further preferably 8 gf / or less.

The dentifrice of any one of the above-mentioned [1] to [16], wherein the content of the water-insoluble powder material (A) in the granule after blending is preferably 60% by mass or more in a dry state, more preferably It is preferably 70% by mass or more, more preferably 80% by mass or more, further preferably 82% by mass or more, and more preferably 98% by mass or less, still more preferably 96% by mass or less, and still more preferably 90% by mass. %the following.

[18] The dentifrice according to any one of the above [1] to [17] wherein the water-insoluble powder material (A) is preferably selected from the group consisting of heavy calcium carbonate, light calcium carbonate, zeolite, and cerium oxide. One type or two or more types are more preferably heavy calcium carbonate.

[19] The dentifrice according to any one of [1] to [18] wherein the inorganic binder (B) comprises one or two selected from the group consisting of sodium citrate and colloidal cerium oxide, and is formulated. The content of one or both selected from the group consisting of sodium citrate (solid content) and colloidal cerium oxide in the inorganic binder (B) contained in the granule is preferably 60% by mass or more, more preferably 80% by mass. The above is more preferably 90% by mass or more, and is preferably 100% by mass or less.

[20] The dentifrice according to any one of the above [1] to [19], wherein the component (B) is one or two selected from the group consisting of sodium citrate (solid content component) and colloidal cerium oxide. The content of the particles in the dry state is preferably 1% by mass or more, more preferably 2% by mass or more, further preferably 5% by mass or more, further preferably 10% by mass or more, and more preferably in the dry state. 30% by mass or less, more preferably 20% by mass or less, further preferably 18% by mass or less.

[2] The dentifrice according to any one of the above [1] to [20] wherein the granule after the preparation preferably contains one or two selected from the group consisting of calcium citrate, magnesium oxide, titanium oxide and zinc oxide. The content of the above-mentioned bonding auxiliary (C) and the component (C) is preferably 0.2% by mass or more, more preferably 0.5% by mass or more, still more preferably 0.8% by mass or more, and more preferably in the dry state. 5 mass% or less, more preferably 3% by mass or less, further preferably 2 mass% or less, and still more preferably 1.2 mass% or less.

[2] The dentifrice according to any one of the above [1] to [21] wherein the amount of the particles after the blending is preferably 1% by mass or more, more preferably 3% by mass or more, and still more preferably 5 mass%. More than %, and It is preferably 50% by mass or less, more preferably 30% by mass or less, and still more preferably 20% by mass or less.

[23] The dentifrice according to any one of the above [1] to [22] wherein the granule after the preparation is preferably obtained by a rolling granulation method, and preferably, the granule before the preparation is added The agitating agent was stirred at a stirring speed of 10 rpm or more and 250 rpm or less.

[24] The dentifrice according to any one of [1] to [23], which preferably contains a binder, more preferably contains sodium carboxymethylcellulose, triterpene, and carrageenan. One or more types of binders.

[25] The dentifrice according to any one of the above [1] to [24] wherein the particles before preparation for obtaining the formulated particles are obtained by laser diffraction/scattering particle size distribution measurement. The following particles (b')~(e-1') in the particle size distribution:

(b') particles having a particle diameter of 100 μm or more and less than 150 μm

(c') particles having a particle diameter of 150 μm or more and less than 200 μm

(d') particles having a particle diameter of 200 μm or more and less than 250 μm

(e-1') particles having a particle diameter of 250 μm or more and less than 300 μm

Among them, the volume ratio (b'/c') of the amount of the particles (b') to the amount of the particles (c') is preferably 0.6 or more and 1.25 or less, and the amount of the particles (d') and the particles (c') The volume ratio (d'/c') is preferably 0.7 or more and 1.2 or less, and the volume ratio of the amount of the particles (e-1') to the amount of the particles (c') (e-1'/c') It is preferably 0.4 or more and 1.1 or less.

[26] The dentifrice according to the above [25], wherein the disintegration strength of the particles before the preparation is preferably 1 gf/piece or more, more preferably 2 gf/piece or more, still more preferably 3 gf/piece or more, and further preferably It is 20 gf / or less, more preferably 15 gf / or less, further preferably 10 gf / or less.

[27] A method for producing a dentifrice, which is a method for producing a dentifrice according to any one of the above [1] to [26], and after the preparation of the binder, comprising the step of adding particles, and stirring The step of adding a granular dentifrice at a speed of 10 rpm or more and 250 rpm or less.

[Examples]

Hereinafter, the present invention will be specifically described based on examples. In addition, unless otherwise indicated in the table, the compounding amount of each component shows the total amount (mass%) of each component present in the dentifrice. Further, the measurement of each physical property value was carried out by the following method.

<<1: Method for determining average particle diameter of water-insoluble powder>>

The average particle diameter of the water-insoluble powder is a laser diffraction/scattering particle size distribution measuring apparatus (LA-920, manufactured by HORIBA), in solvent: ion-exchanged water, refractive index: 1.2, cycle speed (scale: 4), The measurement was carried out under the conditions of stirring speed (scale: 3).

"2: Solid content of sodium citrate"

It is calculated by using a dropper to drop 2.5 g of a sample into a diameter of 5 to 10 mm in a droplet (to make the droplets do not overlap each other as much as possible) and to spread the diameter to aluminum. In a 11.5 cm container, an infrared moisture meter (manufactured by KETT Scientific Research Institute Co., Ltd., FD240) was used, and the moisture measurement method was used at a temperature of 105 ° C and Auto (the amount of change in the measured value was 30). The measurement was carried out under the condition that the measurement was regarded as the final measurement value within 0.05% in the second, and the measured free radical moisture was removed.

"3: Method for determination of particle size distribution and average particle size of particles before preparation"

The measurement was carried out by using an aqueous solution in which the particles before preparation were diluted to 5 mass% by ion-exchanged water. An aqueous solution in which the particles before the preparation were diluted to 5 mass% by ion-exchanged water was passed through a mixer (ROTARY MIXER NPC-20, manufactured by NISSIN Co., Ltd.) at 75 rpm in the horizontal direction for 2 hours. The particles are dispersed. Next, the aqueous solution in which the particles were dispersed was stored at room temperature (25 ° C) for 1 day. After the aqueous solution after the storage was dispersed for 10 minutes by the above-mentioned mixer, the aqueous solution was used, and a laser diffraction/scattering particle size distribution measuring apparatus (Partica LA-950V2, manufactured by HORIBA) was used, and the refractive index was 1.58. The measurement was carried out under the conditions of a circulation speed (scale: 5) and a stirring speed (scale: 5). Further, ion-exchanged water was used as a solvent.

"4: Area (S _A ) of the projection surface of the particle after blending, the longest diameter (D _L ), the area (S _S ) and the shortest diameter (D _S ) of the circle outside the diameter of D _L "

(i) The area of the projection surface of the granules after the preparation is washed with an aqueous solution of a dentifrice diluted with purified water by a purified water using a 150 μm sieve of JIS Z8801-1 standard, and left on the sieve. The granules were dried at room temperature (25 ° C) for 1 day and measured using the obtained granules.

(ii) The area of the projection surface (S _A ), the longest diameter (D _L ), and the shortest diameter (D _S ) are measured using KEENCE VH-5500 (100 times magnification), using analytical software (WinROOF (Sangu Trading Co., Ltd.) Ltd.) Obtaining the area (S _A ), the longest diameter (D _L ) and the shortest diameter (D _S ) of the projection surface of each of the particles from the digital image obtained by photography. 5 to 10 particles obtained by measurement The average data is set as the area (S _A ), the longest diameter (D _L ), and the shortest diameter (D _S ) of one of the projection surfaces of each particle. Based on the data, the area of one of the projection surfaces of the particles is determined (S _A ) Ratio of the area (S _A / S _S ), the longest diameter (D _L ) and the shortest diameter (Ds) of the area (S _S ) outside the circle with the longest diameter (D _L ) as the diameter (D _L /Ds ).

"5: Method for determination of particle size distribution, average particle size and amount of particles present in formulated dentifrice"

(i) Dispersion treatment of particles in an aqueous solution for measurement: an aqueous solution for diluting a dentifrice into 10% by mass by ion-exchanged water, by a mixer (ROTARY MIXER NPC-20, manufactured by NISSIN) at 75 rpm The particles were dispersed in a minute or two rotation condition for 2 hours. Next, the aqueous solution obtained by diluting the dispersed dentifrice was stored at room temperature (25 ° C) for 1 day. The preserved aqueous solution was again dispersed by the above mixer for 10 minutes, and then treated by a laser diffraction/scattering type particle size distribution device.

The particles were extracted in the same manner as (i) of "4".

(ii) Measurement of particle size distribution, average particle diameter and amount: Laser diffraction/scattering particle size distribution measuring apparatus (Partica LA-950V2, manufactured by HORIBA), refractive index: 1.58, cycle speed (scale: 5) The obtained powder and the prepared particles were measured under the conditions of stirring speed (scale: 5). Ion exchange water was used as a solvent.

Further, in the present invention, the particles (a) to (e) ((a') to (e') of the respective particle diameters are calculated based on the particle size distribution measured by the laser diffraction/scattering particle distribution measuring device. The amount (% by volume). Specifically, the particle (a) ~ is calculated by multiplying the content of each particle diameter by the ratio of the particle diameter range by the range of the respective particle diameters measured by the laser diffraction. e) an amount, for example, when a particle having a particle diameter of 45 μm or more and less than 51 μm obtained by laser diffraction is 0.2% by volume, 51 μm or more, and particles of less than 101 μm are 7.5% by volume, the particles (a) The content was 0.2% by volume × 1/(51 - 45) + 7.5% by volume × (100 - 51) / (101 - 51), and the calculation result was 7.4% by volume.

[Manufacturing Example 1: Manufacture of particles A' to E' before preparation]

A mixture of heavy calcium carbonate (manufactured by Calfine Co., Ltd., trade name: ACE-25, average particle diameter of about 3 μm) and various binding aids (C) was put into the mixture in such a manner as to have the contents shown in Table 1 75L drum type granulator for partition ( 40 cm × L 60 cm), one side of the drum is rotated at a number of 30 r. pm / a number of rolls of 0.2 / a roller angle of 12.6 °. One side of the external mixing type two-fluid nozzle (Atomax Co., Ltd.) is sprayed with sodium citrate. (Made in Fuji Chemical Industry Co., Ltd., trade name: sodium citrate No. 3: Na ₂ .3 SiO ₂ solution, 38.5% solid content, diluted with water of 3 times or less, 25 ° C) to carry out granulation. Furthermore, the batch size is 8 kg. The addition rate of the aqueous sodium citrate solution was 3.3 ml/min.

After spraying the sodium citrate aqueous solution, the mixture was further mixed for 1 minute, and then discharged from a roller type granulator, and dried at 80 ° C for 90 minutes using an electric shed dryer to obtain pellets A' to E' before preparation.

The particle size distribution of the particles A' to F' before each preparation is shown in Table 2, and the curve of the particle size distribution of the particles B' before the preparation is shown in Fig. 1.

[Examples 1 to 10, Comparative Example 1]

According to the formulation shown in Table 3, each component was added together with the obtained particles A' to F' before the blending, and a stirring speed of 75 rpm and a rotation speed of the rotation was performed using a universal mixing device (5XDMVV10-r, manufactured by Dalton Co., Ltd.). The mixture was stirred at 200 rpm for 10 minutes to obtain a dentifrice having the prepared particles A to F obtained from the particles A'~F' before preparation.

Next, each of the dentifrice was used, and each evaluation was carried out in accordance with the following method.

The results are shown in Table 3.

Further, the particle size distribution of the prepared particles A to F present in the dentifrice is shown in Table 4, and the graph of the particle size distribution of the prepared particles B present in the dentifrice of Example 1 is shown in the figure. 1. A photograph of the SEM (electron microscope: Hitachi S-4800) of the particle B is shown in Fig. 2. Further, a graph showing the particle size distribution of the prepared particles F present in the dentifrice of Comparative Example 1 is shown in Fig. 3 .

[Test Example 1: Evaluation of tartar removal ability (soil removal rate)]

The following embossing model and the dirt model were used, and the brushing test was performed according to the following method, and the dirt removal rate was calculated. The results are shown in Table 3.

(bump model)

A concave-convex model having a groove having a width of 90 ° C and a width of 100 μm and a depth of 100 μm was prepared in parallel on a stainless steel having a length of 15 mm × a width of 15 mm and a thickness of 3 mm at intervals of 620 μm.

(dirt model)

As a dirt model, a red crayon (CRAYON RED, manufactured by Pentel Co., Ltd.) was used, and the entire groove of the above-mentioned concave-convex model was rubbed and filled, and the surface of the blade was slid along the surface of the concave-convex model to be on the surface of the concave-convex model. A prominent dirt model or a dirt model attached to the surface is removed.

(brushing test)

The above-mentioned concave-convex model is embedded in an aluminum plate (30 mm × 80 mm × 5 mm) Central 15mm × 15mm × 3mm square recess, 2g of each dentifrice, toothbrush (Deep Clean Compact, made by Kao), brushing conditions: load 200g, speed 80rpm, amplitude 30mm, 1 minute, brushing direction: parallel The brushing test was carried out under the condition of the direction of the groove of the concave-convex model. Further, at the corner of the concave portion of the square of the aluminum plate, a concave portion for scraping which allows the concave-convex model to be easily taken out is provided on the outer side of the square.

(Method of calculating the dirt removal rate)

After the brushing, the concave-convex model was taken out from the aluminum plate, and after washing with water, the dentifrice adhering to the surface of the concave-convex model was removed by sliding the surface of the concave-convex model against the paper (PPC paper A4 size, KOKUYO).

The concave-convex model before the brushing and the concave-convex model from which the dentifrice was removed were photographed by a digital camera, and the area of the region colored by the crayon in the concave-convex model before the brushing was set as the area of the colored region (mm ² ). And the colored region is performed by brushing the toothbrush of the area of a region of an evaluation area to area (mm ^2), the evaluation area is removed while the crayon of the exposed area of the bottom of the recess (whitening) of the portion (mm ² ) Set to the dirt removal area. Then, the dirt removal area with respect to the entire area of the evaluation area is calculated as the dirt removal rate (%) by the following formula (1). Further, the area of the colored area is the area where the area colored by the pseudo-fouling substance is detected when photographing with a digital camera, and the area brushed by the toothbrush in this area is used as the evaluation area.

Dirt removal rate (%) = (stain removal area / evaluation area area overall) × 100 (1)

Further, when the crayon rubbed into the concave portion of the test plate is brushed by a toothbrush only on a flat surface, the crayon is removed to expose the face of the test plate as long as a specific load is applied. Further, in the photography using a digital camera, a flash lamp is used, and a polarizer is used in order to eliminate surface reflected light.

[Test Example 2: Evaluation of feeling of use]

1 g of each of the dentifrices obtained in Examples 1 to 10 and Comparative Example 1 was brushed using a toothbrush (Check Standard, manufactured by Kao), and foamed according to the basis shown below. Sex, foam (fineness of the bubble), the persistence of the bubble during brushing, the graininess at the beginning of brushing, the smoothness after brushing, the persistence of the graininess during brushing, the foaming, foaming The graininess at the beginning of the brushing and brushing, and the smoothness after brushing the teeth were evaluated on the scale of 1 to 5. The above evaluation was performed on five panel inspectors, and the average value was obtained based on the obtained results.

Further, in the above evaluation, the number of respondents who answered the five functional inspectors was counted for the persistence of the bubble during the brushing process and the persistence of the feeling during the brushing process. The results are shown in Table 2.

"foaming"

5: very good foaming

4: Good bubbling

3: Foaming

2: not easy to foam

1: no bubble

"Powder (fineness of bubble)"

5: I feel very delicate

4: Feel the bubbles

3: I feel a little delicate

2: I feel a little rough

1: feeling bubble rough

"The feeling of graininess in the beginning of brushing teeth"

5: Feel the presence of moderate particles

4: I feel the presence of particles

3: The presence of particles is small

2: The presence of particles is minimal

1: I don’t feel the presence of particles at all.

"Smooth feeling after brushing your teeth"

The touch of the tooth surface after the tooth is brushed (after washing the dentifrice with water).

5: Very smooth and does not feel the presence of dirt

4: smooth, almost no dirt exists

3: A bit smooth, but slightly felt the presence of dirt

2: A slight confirmation of the unevenness, a slight feeling of the presence of dirt

1: I feel the unevenness caused by dirt on the surface of the tooth.

From the above results, it was found that the dentifrice of Examples 1 to 10 had an excellent feeling of use as compared with the dentifrice of Comparative Example 1.

Claims (11)

A dentifrice prepared by mixing particles containing a water-insoluble powder material (A) and an inorganic binder (B), and a projection surface of the particles after the formulated particles present in the dentifrice The average value (S _A /S _S ) of the area (S _A ) and the area (S _S ) of the outer diameter of the diameter (D _L ) of the projection surface is 0.5 or more and 0.9 or less, and The disintegration strength of the particles after the blending is 1 gf/piece or more and 20 gf/piece or less. The dentifrice of claim 1, wherein the ratio of the longest diameter (D _L ) to the shortest diameter (D _S ) in the projection surface of the particle with respect to the formulated particles present in the dentifrice (D _L /D) The average value of _S ) is 1.2 or more and 1.8 or less. A dentifrice prepared by blending particles containing a water-insoluble powder material (A) and an inorganic binder (B), and the particles after being formulated in the dentifrice are surrounded by a laser The following particles (a) to (d) in the particle size distribution obtained by the measurement of the emission/scattering particle size distribution: (a) particles having a particle diameter of 50 μm or more and less than 100 μm (b) having a particle diameter of 100 μm or more and less than 150 μm Particles (c) Particles having a particle diameter of 150 μm or more and less than 200 μm (d) Among the particles having a particle diameter of 200 μm or more and less than 250 μm, the volume ratio of the amount of the particles (b) to the amount of the particles (c) ( b/c) is 0.7 or more and 1.2 or less, and the volume ratio (d/c) of the particles (d) to the particles (c) is 0.2 or more and 1 or less, and the amount of the particles (b) and the amount of the particles (d) The ratio (b/d) is more than 1 and is 5 or less, and the amount of the particles (c) in the prepared particles is 15% by volume or more and 55% by volume or less, and the disintegration strength of the particles after the blending is 1 gf/piece or more And 20gf / less. The dentifrice of claim 3, wherein the particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution are determined in the prepared particles present in the dentifrice (a) and the total amount of the particles (b) and the following particles (e): (e) a volume ratio of the particles having a particle diameter of 250 μm or more and less than 350 μm ((a+b)/e) is greater than 1 and is 20 or less. The dentifrice of claim 3 or 4, wherein the particles (a) and particles in the particle size distribution obtained by the laser diffraction/scattering particle size distribution are determined in the prepared particles in the dentifrice. The volume ratio ((a+b)/(c+d))) of the total amount of (b) and the total amount of the particles (c) and (d) is 0.5 or more and 1 or less. The dentifrice of claim 1 or 3, wherein the amount of the particles after the formulation in the dentifrice is 1% by mass or more and 50% by mass or less. A dentifrice according to claim 1 or 3, wherein the formulated particles present in the dentifrice are obtained by a rolling granulation method. The dentifrice according to claim 1 or 3, wherein the granules which are present in the dentifrice contain one or more binding auxiliaries selected from the group consisting of calcium citrate, magnesium oxide, titanium oxide and zinc oxide. (C). The dentifrice according to claim 8, wherein the mass ratio (C/B) of the component (C) to the component (B) is 0.02 or more and 1 or less in the particles which are present in the dentifrice. A dentifrice according to claim 1 or 3, wherein the particles before being formulated for use in obtaining the prepared particles present in the dentifrice are added to the particles used in the dentifrice, by laser diffraction/scattering The following particles (b') to (e-1') in the particle size distribution obtained by particle size distribution measurement: (b') particles having a particle diameter of 100 μm or more and less than 150 μm (c') have a particle diameter of 150 μm or more and not Particles (b') having a particle size of 200 μm (d') and a particle size of 200 μm or more and less than 250 μm (e-1') having a particle diameter of 250 μm or more and less than 300 μm, the amount of particles (b') and particles (c) The volume ratio (b'/c') of the amount of ') is 0.6 or more and 1.25 or less, and the volume ratio (d'/c') of the amount of the particles (d') to the amount of the particles (c') is 0.7 or more. And 1.2 or less, the volume ratio (e-1'/c') of the amount of the particle (e-1') to the amount of the particle (c') is 0.4 or more and 1.1 or less, and the disintegration strength of the particle before preparation is 1 gf / more and 20 gf / or less. The dentifrice according to claim 1 or 3, wherein the granules which are present in the dentifrice are obtained by adding the granules before preparation, and stirring the dentifrice at a stirring speed of 10 rpm or more and 250 rpm or less.