JP2018104294A - Granules for dentifrices, and dentifrice composition containing the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide granules for dentifrices that exert a high removing effect to strongly adhering dental plaque and staining and the like (dental plaque and the like) to the tooth surface while effectively inhibiting formation of such dental plaque and the like on the tooth surface, and to provide dentifrice composition containing the same.SOLUTION: Provided is a granule for dentifrices containing the following component (A) and (B): (A) a granulated substance comprising a water-insoluble powder material, and (B) saturated or unsaturated fatty acid, or salts thereof, having 14 or more to 22 or less carbon atoms, the component (B) being carried by the component (A), the average grain diameter being 50 μm or more to 500 μm or less, and the collapse strength being 0.2 gf/piece or more to 30 gf/piece or less in wet conditions.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a dentifrice granule and a dentifrice composition containing the granule.

  If various stains (plaque etc.) such as plaque and colored stains adhere to the tooth surface, it can cause dental caries and periodontal disease. Therefore, such plaque etc. can be removed efficiently or these plaques etc. In order to prevent the formation and adhesion of dentifrices, dentifrice technology using various components has been developed. Under such circumstances, it is possible to effectively improve the ability to remove plaque etc. by blending granules with dentifrice. Many dentifrices using granules with added physical properties have also been developed.

  For example, Patent Document 1 discloses a dentifrice granule that contains a specific component and exhibits a specific disintegration behavior with respect to a load, and reaches a narrow region such as a gap between teeth. Until now, the effect of removing plaque and the like is enhanced, and a smooth feeling and a feeling of removing dirt are also improved.

  On the other hand, attempts have been made to develop techniques for preventing plaque and the like from adhering to the tooth surface. For example, Patent Document 2 discloses a tooth surface coating agent containing a fatty acid salt. The fatty acid salt exerts a tooth surface coating action, protects the tooth surface from acids produced by bacteria, The effect of preventing adhesion of fungi and food waste is enhanced.

JP 2014-94923 A JP 2000-103726 A

  However, even if plaque and the like once adhered to the tooth surface can be effectively removed by using the technique described in Patent Document 1, as the time elapses or after eating and drinking etc. thereafter, the tooth is again formed. There is a possibility that these plaques and the like are not sufficiently formed on the surface. Moreover, even if the technique described in Patent Document 2 is used, in order to maintain the state in which the fatty acid salt is favorably adsorbed on the tooth surface, and to sufficiently maintain the formation suppressing effect such as plaque on the tooth surface, It still needs to be improved.

  Therefore, it is a technology that not only exhibits a high removal effect on plaque that has already firmly adhered to the tooth surface, but also can effectively prevent such plaque from forming on the tooth surface again. Realization is strongly desired.

  Therefore, the present invention exhibits a high removal effect on plaque and colored stains (such as plaque) firmly adhered to the tooth surface, and effectively suppresses the formation of such plaque on the tooth surface. It is related with the dentifrice granule which can be used, and the dentifrice composition containing this.

  Therefore, the present inventor has a specific average particle size and disintegration strength while a specific saturated or unsaturated fatty acid or a salt thereof is supported on a specific granulated product, so that the plaque already adhered to the tooth surface. It was found that granules for dentifrice that can further maintain the effect of suppressing the formation of dental plaque and the like on the tooth surface can be obtained while enhancing the removal effect.

That is, the present invention includes the following components (A) and (B):
(A) A granulated product containing a water-insoluble powder material, and (B) a saturated or unsaturated fatty acid having 14 to 22 carbon atoms or a salt thereof, and the component (B) is carried on the component (A). And a dentifrice granule having an average particle diameter of 50 μm or more and 500 μm or less and a disintegration strength of 0.2 gf / piece or more and 30 gf / piece or less in a wet state.
Moreover, this invention relates to the dentifrice composition which contains the said granule for dentifrice 1 mass% or more and 50 mass% or less.

According to the granule for dentifrice of the present invention, it is possible to effectively enhance the removal effect of plaque and the like firmly adhered to the tooth surface, and sufficiently maintain the state of the tooth surface to which plaque and the like are difficult to adhere. It can exhibit the effect of suppressing the formation of high plaque and the like. Therefore, by using a dentifrice composition containing such dentifrice granules, it becomes possible to prevent reattachment of plaque and the like to the tooth surface, and to maintain a smooth feel on the tooth surface, A good feeling of use can be brought about.
In addition, the touch that is smooth is a touch that allows the tongue to slide smoothly on the surface of the teeth without getting a feeling that plaque or the like is attached when the tooth surface is touched with the tongue. Say.

It is a graph showing the in vitro biofilm formation inhibitory effect of the HAp board | substrate processed with the 13 mass% glycerol solution of the granule of Examples 1-11 and Comparative Examples 1-3. The vertical axis represents the biofilm formation inhibition rate (%). It is a graph showing the in vitro biofilm formation inhibitory effect of the HAp board | substrate processed with the dentifrice of Example 12 and Comparative Examples 4-5. The vertical axis represents the biofilm formation inhibition rate (%). It is a graph showing the result of a human test performed using the dentifrice of Example 12 and Comparative Example 4. The vertical axis shows the plaque formation inhibition rate (%).

Hereinafter, the present invention will be described in detail.
The granule for dentifrice of the present invention contains a granulated product containing a water-insoluble powder material as the component (A). The granulated product of component (A) may be an aggregate or agglomerate of particles or powder having a granular shape.
The water-insoluble powder material contained in the component (A) is preferably a material usually used as a tooth abrasive, and specifically an inorganic material. Here, “water-insoluble” means that the amount dissolved in 100 g of water (20 ° C.) is 1 g or less. More specifically, for example, from light calcium carbonate, heavy calcium carbonate, zeolite, silica, dicalcium phosphate, tricalcium phosphate, insoluble sodium metaphosphate, aluminum hydroxide, magnesium phosphate, calcium pyrophosphate, magnesium carbonate, etc. 1 type or 2 types or more selected are mentioned.

  The average particle diameter of the water-insoluble powder material is preferably 0.1 μm or more, more preferably 0.5 μm or more, from the viewpoint of enhancing the effect of removing plaque and the like after granule disintegration and the effect of suppressing formation. The average particle diameter of the water-insoluble powder material is preferably 20 μm or less, more preferably 15 μm or less, and further preferably 10 μm or less, from the viewpoint of reducing the feeling of foreign matter. And the average particle diameter of water-insoluble powder material (A) becomes like this. Preferably it is 0.1-20 micrometers, More preferably, it is 0.5-15 micrometers, More preferably, it is 0.5-10 micrometers. The average particle diameter can be measured by a laser diffraction / scattering particle size distribution measuring apparatus.

The content of the water-insoluble powder material is determined in the component (A) from the viewpoint of improving the effect of removing plaque and the like and suppressing the formation by imparting a stepwise disintegration behavior or increasing the polishing power. In a dry state, it is preferably 50% by mass or more, more preferably 60% by mass or more, further preferably 70% by mass or more, still more preferably 80% by mass or more, preferably 100% by mass. % Or less, or when the component (A) contains an inorganic binder described later, it is preferably 95% by mass or less, more preferably 90% by mass or less, and still more preferably 85% by mass or less. The content of the water-insoluble powder material is such that when the component (A) contains an inorganic binder described later, it is possible to remove plaque and the like by providing stepwise disintegration behavior or increasing the polishing power. From the viewpoint of improving the effect and the effect of suppressing formation, the component (A) is preferably 50 to 95% by mass, more preferably 60 to 90% by mass, and further preferably 70 to 85% by mass. More preferably, it is 80-85 mass%.
When the content of the water-insoluble powder material in the dry state in the component (A) is 100% by mass, the component (A) is a water-insoluble powder material without any inorganic binder described later. It corresponds to an aggregate (aggregate (a1) of water-insoluble powder material) having a granular shape formed by particles or powder.

  Component (A) may further contain an inorganic binder. The component (A) containing such an inorganic binder is formed by combining the water-insoluble powder material and the inorganic binder and interposing the inorganic binder with voids in the component (A). It corresponds to a granulated product (granulated product containing a water-insoluble powder material and an inorganic binder (a2)) that is processed or granulated by the above particles or powder.

  Examples of the inorganic binder include one or more selected from 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 sodium silicate, polyacrylic acid, processed cellulose such as powdered cellulose, polyvinyl pyrrolidone, and silicone. Sodium silicate Powdered cellulose is preferred. Specific examples of the water-insoluble inorganic binder include one or more selected from colloidal silica, magnesium aluminate metasilicate, synthetic aluminum silicate, calcium silicate, alumina sol, and the like, and colloidal silica is preferable.

Among these, from the viewpoint of satisfactorily exerting the effects of the present invention, it is preferable to include a water-soluble inorganic binder, and while interspersing voids of various sizes in the granules, the pH of water in the voids is made alkaline. It is more preferable that sodium silicate is included from the viewpoint of enhancing the effect of removing plaque and the like and suppressing the formation and improving the feeling of use such as a smooth feeling on the tooth surface. Such sodium silicates include sodium metasilicate (Na ₂ SiO ₃ ), sodium orthosilicate (Na ₄ SiO ₄ ), sodium disilicate (Na ₂ Si ₂ O ₅ ), sodium tetrasilicate (Na ₂ Si ₄ O ₉ ), and These hydrates are mentioned.

Sodium silicate is generally represented by the molecular formula Na ₂ O.nSiO ₂ .mH ₂ O. The coefficient n (molecular ratio of SiO _{2 to} Na ₂ O) is called molar ratio and can be expressed by the following formula (I).
Molar ratio = mass ratio (SiO ₂ mass% / Na ₂ O mass%) × (Molecular weight of Na ₂ O / Molecular weight of SiO ₂ ) (I)
As sodium silicate, water silicates of various molar ratios can be used in addition to sodium silicate Nos. 1, 2 and 3 described in JIS K1408. Among them, sodium silicate 3 is more preferable.

  Although the physical properties of sodium silicate vary depending on the molar ratio (coefficient n), the viewpoint of adapting to the quasi-drug raw material standard, the viewpoint of satisfactorily exerting the effect of the present invention, and the pH of the resulting dentifrice granules are made alkaline. Therefore, the molar ratio (coefficient n) is preferably 2.0 or more, more preferably 2.4 or more, further preferably 2.8 or more, and further preferably 3.0 or more. It is preferably 4.0 or less, more preferably 3.5 or less, still more preferably 3.4 or less, and even more preferably 3.3 or less. And said molar ratio (coefficient n) becomes like this. Preferably it is 2.0-4.0, More preferably, it is 2.4-3.5, More preferably, it is 2.8-3.4, More preferably, it is 3.0-3.3.

  When the component (A) contains an inorganic binder, the content of the inorganic binder is from the viewpoint of effectively suppressing coarse particles, and from the viewpoint of effectively increasing the disintegration strength of the dentifrice granules of the present invention. In a component (A), Preferably it is 30 mass% or less, More preferably, it is 25 mass% or less, More preferably, it is 20 mass% or less. Further, the content of the inorganic binder is preferably 1% by mass or more, more preferably 2% by mass or more in the component (A) from the viewpoint of facilitating the production of the component (A). Preferably it is 4 mass% or more. And content of an inorganic binder becomes like this. Preferably it is 1-30 mass% in a component (A), More preferably, it is 2-25 mass%, More preferably, it is 4-20 mass%.

  Moreover, when using sodium silicate as an inorganic binder, the content of the sodium silicate (solid content) is a viewpoint that effectively suppresses coarse particles and a viewpoint that effectively increases the disintegration strength of the dentifrice granules of the present invention. Therefore, in the component (A), it is preferably 25% by mass or less, more preferably 20% by mass or less, and further preferably 18% by mass or less. The content of sodium silicate (solid content) is preferably 1% by mass or more, more preferably 2% by mass or more in the component (A) from the viewpoint of facilitating the production of the component (A). Yes, and more preferably 4% by mass or more. The content of sodium silicate (solid content) in the component (A) is preferably 1 to 25% by mass, more preferably 2 to 20% by mass, and further preferably 4 to 18% by mass. is there.

  The dentifrice granule of the present invention contains a saturated or unsaturated fatty acid having 14 to 22 carbon atoms or a salt thereof as the component (B), and the component (B) is supported on the component (A). . That is, whether the component (A) is an aggregate (a1) of a water-insoluble powder material or a granulated product (a2) containing a water-insoluble powder material and an inorganic binder, the component (A) Since there is a gap between the particles to be formed, the dentifrice granule of the present invention is formed by being carried on the component (A) so that the component (B) is interposed in the gap. Therefore, it is possible to disperse the component (B) uniformly in the dentifrice granule without uneven distribution, and when the dentifrice granule disintegrates due to a load such as brushing during use, it melts well in the oral cavity. Thus, it can be efficiently and uniformly adsorbed onto the tooth surface, and the state of the tooth surface where plaque or the like is difficult to form or adhere can be sufficiently maintained. Furthermore, it is possible to alleviate the foaming and flavor deterioration that are easily induced by these fatty acids or salts thereof, and to improve the feeling of use.

  The number of carbon atoms of the component (B) is 22 or less, preferably 18 or less, from the viewpoint of maintaining good solubility when the dentifrice granules disintegrate due to a load such as brushing during use. More preferably, it is 16 or less, and it is 14 or more from a viewpoint of the flavor at the time of use, Preferably it is 16 or more.

  In addition, examples of the hydrocarbon group that the component (B) has include a saturated hydrocarbon group, a linear hydrocarbon group, and a branched hydrocarbon group, a saturated hydrocarbon group is preferred, and a linear saturated hydrocarbon group is preferred. More preferred. Examples of such hydrocarbon groups include myristic acid, pentadecylic acid, palmitic acid, palmitoleic acid, stearic acid, oleic acid, linoleic acid, linolenic acid, etc., and myristic acid, pentadecylic acid, palmitic acid, stearic acid are preferred. . Among these, myristic acid and palmitic acid are preferable from the viewpoint of ensuring solubility in water, and palmitic acid is preferable from the viewpoint of improving the flavor.

  In addition, as a component (B), the said saturated or unsaturated fatty acid or these salts may be used individually by 1 type, or 2 or more types of saturated or unsaturated fatty acids or these salts may be mixed and used. .

  The content of component (B) ensures that component (B) is supported well on component (A) and is uniformly dispersed in the dentifrice granules, and meltability when the dentifrice granules disintegrate is ensured From the viewpoint of enhancing the adsorptivity to the tooth surface, it is preferably 0.1 parts by mass or more, more preferably 4 parts by mass or more, and further preferably 7 parts by mass with respect to 100 parts by mass of the component (A). It is above, More preferably, it is 11 mass parts or more. In addition, the content of the component (B) is excessively increased as the loading amount of the component (B) on the component (A) increases, and the disintegration property of the dentifrice granule decreases more than necessary. From the viewpoint of avoiding this, it is preferably 40 parts by mass or less, more preferably 35 parts by mass or less, still more preferably 30 parts by mass or less, and still more preferably with respect to 100 parts by mass of the component (A). Is 25 parts by mass or less. And content of a component (B) becomes like this. Preferably it is 0.1-40 mass parts with respect to 100 mass parts of components (A), More preferably, it is 4-35 mass parts, More preferably, it is 7-30. It is a mass part, and is 11-25 mass parts.

  The content of the component (B) is such that the component (B) is favorably supported on the component (A) and dispersed uniformly in the dentifrice granules, and the melting properties when the dentifrice granules disintegrate. In the dentifrice granule of the present invention, it is preferably 1% by mass or more, more preferably 4% by mass or more, and still more preferably 8% by mass or more from the viewpoint of ensuring the adsorbability on the tooth surface. And more preferably 10% by mass or more. In addition, the content of the component (B) is excessively increased as the loading amount of the component (B) on the component (A) increases, and the disintegration property of the dentifrice granule decreases more than necessary. From the viewpoint of avoiding this, it is preferably 25% by mass or less, more preferably 20% by mass or less, and further preferably 17% by mass or less in the dentifrice granule of the present invention. And the content of the component (B) is preferably 1 to 25% by mass, more preferably 4 to 20% by mass, and further preferably 8 to 17% by mass in the dentifrice granule of the present invention. More preferably, it is 10 to 17% by mass.

  From the viewpoint of imparting a plaque formation inhibitory effect, and the dentifrice granule of the present invention, and strengthening the network structure formed by the water-soluble silicate or colloidal silica to ensure the expression of physical properties that gradually collapse, Furthermore, it is preferable to contain one or more binding aids selected from calcium silicate, magnesium oxide, titanium oxide and zinc oxide, and it is more preferred to contain zinc oxide and other binding aids.

  The content of the binding aid is preferably 0.2% by mass or more in the dry state in the dentifrice granules of the present invention, from the viewpoint of improving the plaque formation inhibitory effect and gradually disintegrating physical properties. Preferably it is 0.5 mass% or more, More preferably, it is 0.8 mass% or more. In addition, the content of the binding aid suppresses the excessive increase in disintegration strength, suppresses foaming and foam quality of the dentifrice containing the dentifrice granules of the present invention, and suppresses the metallic taste. From the viewpoint of, it is preferably 5% by mass or less, more preferably 3% by mass or less, and further preferably 2% by mass or less in the dry state in the dentifrice granule of the present invention. In addition, the content of the binding aid is preferably 0.2 to 5% by mass, more preferably 0.5 to 3% by mass in the dry state in the dentifrice granule of the present invention, and further preferably. Is 0.8-2 mass%.

The average particle size (μm) of the granule for dentifrice of the present invention is 50 μm or more from the viewpoint of exerting a sufficient effect of removing plaque and the like and the effect of suppressing formation, and imparting good polishing power. Preferably it is 75 micrometers or more, More preferably, it is 100 micrometers or more. In addition, the average particle size (μm) of the dentifrice granule of the present invention is 500 μm or less, preferably 450 μm or less, more preferably 400 μm or less, from the viewpoint of suppressing the feeling of foreign matter in the oral cavity. . And the average particle diameter (micrometer) of the granule for dentifrice is 50 micrometers or more and 500 micrometers or less, Preferably it is 75-450 micrometers, More preferably, it is 100-400 micrometers.
In addition, the average particle diameter of the granule is 2000, 1400, 1000, 710, 500, 355, 250, 180, 125 of JISZ8801-1 (established on May 20, 2000, final revised on November 20, 2006). , 90, 63, and 45 μm sieves are used for 5 minutes, and 50% average diameter is calculated for the weight distribution under the sieve according to the sieving method.

The disintegration strength of the dentifrice granule of the present invention is 0.2 gf / piece or more in a wet state, preferably 0.5 gf / piece or more, more preferably 1 gf / piece or more, and further preferably 3 gf. / Or more. Further, the disintegration strength of the dentifrice granules of the present invention is such that the dentifrice granules are satisfactorily disintegrated by a load such as brushing during use, and the solubility of the component (B) is ensured to effectively prevent plaque and the like. From the viewpoint of enhancing the formation suppression effect, the wet state is 30 gf / piece or less, preferably 25 gf / piece or less, more preferably 20 gf / piece or less, and further preferably less than 15 gf / piece. The disintegration strength of the dentifrice granules of the present invention is 0.2 gf / piece or more and 30 gf / piece or less in a wet state, preferably 0.5 to 25 gf / piece, more preferably 1 to 20 gf / piece. More preferably 3 gf / piece and less than 15 gf / piece.
The disintegration strength of the granules in a wet state means a value measured in a state where the granules are mixed with the dentifrice composition, then dispersed in an aqueous solution and the granules are collected, and specifically described in the examples. Measured by the method.

The granule for dentifrice of the present invention undergoes the step (I) for producing the component (A) in advance and the step (II) for supporting the component (B) on the component (A) obtained in the step (I). Can be manufactured.
Step (I) is a step of producing a granulated product of component (A), and component (A) contains an aggregate (a1) of a water-insoluble powder material or a water-insoluble powder material and an inorganic binder. Any of granulated material (a2) may be sufficient. Moreover, any of a spray drying method and a tumbling granulation method may be used, and as a device, a spray dryer, a stirring tumbling granulator, a container rotating granulator, or the like can be used.

  Examples of the method for producing the component (A) in the step (I) include JP 2010-70458 A, JP 2013-147431 A, JP 2014-001186 A, JP 2014-024837 A, and the like. The methods described can be employed.

  Step (II) is a step of supporting component (B) on component (A) obtained in step (I). In the step (II), the component (A) is not unevenly distributed in the component (A), and from the viewpoint of sufficiently supporting the component (B) until reaching the inside of the component (A), the component (A) B) is preferably heated and mixed. The temperature in the heat mixing is preferably equal to or higher than the melting point of the component (B). Further, the mixing time in the heat mixing is preferably 5 minutes or more, more preferably 10 minutes or more from the viewpoint of uniformly supporting the component (B) with respect to the entire component (A), and from the viewpoint of productivity. Therefore, it is preferably 60 minutes or less, more preferably 45 minutes or less.

Examples of the apparatus used in the step (II) include a Henschel mixer (manufactured by Mitsui Miike Chemical Co., Ltd.), a high speed mixer (manufactured by Fukae Kogyo Co., Ltd.), a vertical granulator (manufactured by Powrec Co., Ltd.), and Redige Mixers (I) such as mixers (Matsuzaka Giken Co., Ltd.), Proshare mixers (Pacific Kiko Co., Ltd.), etc .; Mixers such as U trough type ribbon blenders (Hosokawa Micron Co., Ltd., model: R-17W) (B); Mixers (c) such as Nauter mixer (manufactured by Hosokawa Micron Corporation). Such a mixer is preferably provided with a jacket from the viewpoint of facilitating temperature adjustment.
Among the mixers, the mixer (b) and the mixer (c) are preferable from the viewpoint of not breaking the granule, and the mixer (b) is preferable from the viewpoint of preventing unnecessary aggregation.

In the case of using the above mixer, the rotation speed may be selected so that the component (A) does not substantially collapse. For example, when a mixer equipped with a stirring blade is used, the fluid number is preferably 2.1 or less from the viewpoint of avoiding the collapse of the component (A).
The Froude number means a value calculated by the following formula (II).
Fluid number (Fr) = V ² / (R × g) (II)
V: Peripheral speed [m / s] at the tip of the stirring blade and crushing blade
R: Rotating radius of stirring blade and crushing blade [m]
g: Gravity acceleration [m / s ² ]

  When using the mixer, the mixing time is preferably 10 minutes or more, more preferably 20 minutes or more, from the viewpoint of satisfactorily penetrating the component (B) until reaching the inside of the component (A). More preferably, it is 30 minutes or more, and from the viewpoint of productivity, it is preferably 60 minutes or less, more preferably 40 minutes or less.

  Moreover, as an apparatus used in step (II), as a mixer other than the above, a continuous apparatus may be used. As such a continuous apparatus, for example, a flexo-mix type (manufactured by POWREC), Examples thereof include a mixer such as a turbulizer (manufactured by Hosokawa Micron Corporation). In addition to the above mixer, a fluidized bed dryer can also be used.

  The component (B) can be added to the apparatus as a solid or as a liquid heated to a temperature higher than the melting point. When added as a liquid, it is preferable to spray it with a nozzle and add it as uniformly as possible. The temperature adjustment may be performed by adjusting the temperature in the apparatus with a jacket or the like provided in the apparatus, or may be performed by adjusting the temperature of the component (B) added in advance.

  The dentifrice composition of the present invention contains 1 to 50% by mass of the dentifrice granules. With such a dentifrice composition, when applied to the oral cavity, it is possible to effectively enhance the effect of removing plaque and the like firmly adhered to the tooth surface, and the state of the tooth surface to which plaque and the like are difficult to adhere. It can be sufficiently maintained to exert the effect of suppressing the formation of high plaque, etc., preventing the reattachment of plaque etc. to the tooth surface, and also maintaining the smooth feel on the tooth surface, high A feeling of use can be imparted.

  The dentifrice composition of the present invention has a content of the dentifrice granule from the viewpoint of enhancing the effect of removing plaque and the like by the granule and exhibiting sufficient anti-plaque formation effect and improving the feeling of use. The content is 1% by mass or more, preferably 3% by mass or more, and more preferably 5% by mass or more. In the dentifrice composition of the present invention, the content of the granule for dentifrice is from the viewpoint of exerting the effect of removing plaque and the like and suppressing the formation without damaging the feeling of foreign matter and without damaging the tooth enamel. , 50% by mass or less, preferably 30% by mass or less, and more preferably 20% by mass or less. Further, the content of the dentifrice granule is 1 to 50% by mass in the dentifrice composition of the present invention, preferably 3 to 30% by mass, more preferably 5 to 20% by mass. %.

  The dentifrice composition of the present invention may further contain a binder. Examples of the binder include one or more selected from carboxymethyl cellulose sodium, sodium polyacrylate, hydroxyethyl cellulose, carrageenan, xanthan gum, sodium alginate, guar gum, pectin and the like. The content of the binder is effectively diffused in the oral cavity while dissolving and dispersing the components contained therein, and the effect of removing plaque and the like by the above-mentioned dentifrice granule is effectively exhibited to give a sense of slickness and a feeling of dirt removal. In the dentifrice composition of the present invention, it is preferably 0.1% by mass or more, and more preferably 0.5% by mass from the viewpoint of providing good foaming while enhancing the effect of suppressing the formation of plaque and the like. It is above, More preferably, it is 0.7 mass% or more, Preferably it is 3 mass% or less, More preferably, it is 2 mass% or less. Moreover, the content of the binder is preferably 0.1 to 3% by mass, more preferably 0.5 to 2% by mass, and still more preferably 0.8% in the dentifrice composition of the present invention. 7 to 2% by mass.

  The dentifrice composition of the present invention may further contain a thickener together with the above binder. Examples of the thickener include thickened silica (the amount of oil absorption measured by a method according to JIS K5101-13-3 is 200 to 400 mL / 100 g), montmorillonite, and the like. The content of such a thickener is effectively diffused in the oral cavity while dissolving and dispersing the above components, and effectively exhibits the effect of removing plaque and the like by the above-mentioned dentifrice granules and the effect of suppressing the formation of the tooth surface. In the dentifrice composition of the present invention, it is preferably 3% by mass or more, more preferably 4% by mass or more, and further preferably, from the viewpoint of enhancing the feeling of smoothness and dirt removal and providing good foaming. Is 5% by mass or more, preferably 10% by mass or less, and more preferably 8.5% by mass or less. Moreover, the content of the thickener in the dentifrice of the present invention is preferably 4 to 10 mass%, more preferably 5 to 8.5 mass% in the dentifrice composition of the present invention.

  The dentifrice composition of the present invention preferably further contains a surfactant. This enhances the cleaning effect while providing good foaming, and can sufficiently exert the effect of removing plaque and suppressing the formation of dentifrice granules up to a narrow area such as the gap between teeth. In addition, it is possible to provide a good feeling of use by imparting a feeling of slipping on the tooth surface in the oral cavity after use.

  As such surfactants, anionic surfactants, nonionic surfactants, and zwitterionic surfactants can be used. Examples of the anionic surfactant include alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate; N-acyl sarcosine salts such as sodium N-lauroyl sarcosine and sodium N-myristoyl sarcosine; sodium N-palmitoyl glutamate N-acyl glutamate such as sodium N-methyl-N-acyl taurine, sodium N-methyl-N-acylalanine, sodium α-olefin sulfonate, sodium dioctyl sulfosuccinate and the like.

  Nonionic surfactants include sugar fatty acid esters such as sucrose fatty acid esters; sugar alcohol fatty acid esters such as maltitol fatty acid esters and lactitol fatty acid esters; polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monostearate Oxyethylene sorbitan fatty acid ester; fatty acid diethanolamide such as lauric acid mono or diethanolamide, myristic acid mono or diethanolamide; sorbitan fatty acid ester, fatty acid monoglyceride, polyoxyethylene higher alcohol ether, polyoxyethylene polyoxypropylene copolymer, etc. Can be mentioned.

  As the zwitterionic surfactant, N-alkyldiaminoethylglycine such as N-lauryldiaminoethylglycine, N-myristyldiaminoethylglycine, N-alkyl-N-carboxymethylammonium betaine, 2-alkyl-1-hydroxyethylimidazoline Examples include betaine sodium.

  Among the above surfactants, anionic surfactants are preferred from the viewpoint of imparting good foaming properties and feeling of use in addition to the effect of removing plaque and the like, and the effect of suppressing formation, and alkyl sulfates such as sodium lauryl sulfate. Is more preferable.

  The content of the surfactant is the dentifrice of the present invention from the viewpoint of providing a good flavor while enhancing the cleaning effect and feeling of use by imparting good foaming in addition to the effect of removing plaque and the like and suppressing the formation thereof. In a composition, Preferably it is 0.1 mass% or more, More preferably, it is 0.2 mass% or more. Further, the content of the surfactant is preferably 2.0% by mass or less, more preferably 1.7% by mass in the dentifrice composition of the present invention, from the viewpoint of suppressing the deterioration of the flavor. It is as follows. The surfactant content in the dentifrice composition of the present invention is preferably 0.1 to 2.0% by mass, more preferably 0.2 to 1.7% by mass.

  When the dentifrice composition of the present invention contains an anionic surfactant as a surfactant, the content of the anionic surfactant brings about a good flavor while improving foaming, cleaning effect and feeling of use. From a viewpoint, it is 0.1 mass% or more preferably in the dentifrice composition of this invention, More preferably, it is 0.2 mass% or more. In addition, the content of the anionic surfactant is preferably 2.0% by mass or less, more preferably 1.5% by mass in the dentifrice composition of the present invention, from the viewpoint of suppressing the loss of flavor. % Or less. Furthermore, the content of the anionic surfactant is preferably 0.1 to 2.0% by mass, more preferably 0.2 to 1.5% by mass in the dentifrice composition of the present invention.

  When the dentifrice composition of the present invention contains an alkyl sulfate that is an anionic surfactant as a surfactant, the content of such an alkyl sulfate is good while improving foaming, cleaning effect and feeling of use. From the viewpoint of providing a good flavor, it is preferably 0.05% by mass or more, and more preferably 0.1% by mass or more in the dentifrice composition of the present invention. In addition, the content of the alkyl sulfate is preferably 1% by mass or less, more preferably 0.5% by mass or less, in the dentifrice composition of the present invention, from the viewpoint of suppressing the loss of flavor. is there. Furthermore, the content of the alkyl sulfate is preferably 0.05 to 1% by mass, more preferably 0.1 to 0.5% by mass in the dentifrice composition of the present invention.

  The dentifrice composition of the present invention preferably contains sorbitol. By containing such sorbitol, the above ingredients are dissolved and dispersed to effectively diffuse in the oral cavity, and while effectively exerting the effect of removing plaque and the like, it provides good foaming and flavor, and enhances the feeling of use. be able to.

  The content of sorbitol is preferably 5% by mass or more in the dentifrice composition of the present invention, from the viewpoint of achieving both the effect of removing plaque and the like, the effect of inhibiting the formation and imparting a good feeling of use. Preferably it is 10 mass% or more, More preferably, it is 15 mass% or more, Preferably it is 60 mass% or less, More preferably, it is 50 mass% or less, More preferably, it is 40 mass% or less. Moreover, the content of sorbitol is preferably 5 to 60% by mass, more preferably 10 to 50% by mass, and further preferably 15 to 40% by mass in the dentifrice composition of the present invention.

The dentifrice composition of the present invention may further contain water. The content (water content) of such water is effectively diffused in the oral cavity while dissolving and dispersing the above components, and from the viewpoint of effectively exhibiting the effect of removing plaque such as plaque and the effect of suppressing the formation of granules. In the dentifrice composition, it is preferably 3% by mass or more, more preferably 5% by mass or more, still more preferably 7% by mass or more, preferably 60% by mass or less, more preferably 55% by mass. % Or less, and more preferably 50% by mass or less. Moreover, the content of water is preferably 3 to 60% by mass, more preferably 5 to 55% by mass, and further preferably 7 to 50% by mass in the dentifrice composition of the present invention.
In addition, although this moisture content can also be calculated by calculation from the mix | blended moisture content and the moisture content in the mix | blended component, it can measure with a Karl Fischer moisture meter, for example. As the Karl Fischer moisture meter, for example, a trace moisture measuring device (Hiranuma Sangyo Co., Ltd.) can be used. In this apparatus, 5 g of dentifrice is taken and suspended in 25 g of anhydrous methanol, and 0.02 g of this suspension is fractionated and the amount of water can be measured.

  The mass ratio of the dentifrice granule content to the water content (dentifrice granule / water) in the dentifrice composition of the present invention is good solubility, dispersibility, plaque, etc. From the viewpoint of sufficiently exhibiting the removal effect and the formation suppressing effect, it is preferably 0.02 to 15, more preferably 0.1 to 6, and further preferably 0.15 to 1.

The dentifrice composition of the present invention is a component other than the above, for example, other than sorbitol such as glycerin, propylene glycol, 1,3 butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xylquirit, maltite, lactit, and erythritol. Wetting agents; abrasives; excipients; preservatives; perfumes; medicinal ingredients; coloring agents; and other ingredients commonly used in dentifrices.
In addition, the dentifrice composition of this invention can be manufactured by a conventional method using the said component.

Hereinafter, the present invention will be specifically described based on examples. In addition, unless otherwise indicated in a table | surface, content of each component shows the mass%.
In addition, the average particle diameter of the granule and the disintegration strength in a wet state were measured according to the following methods.

<Measurement of average particle size>
Using sieves of 2000, 1400, 1000, 710, 500, 355, 250, 180, 125, 90, 63, 45 μm of JISZ8801-1 (established on May 20, 2000, final revised on November 20, 2006) Then, a 50% average diameter was calculated for the weight distribution under the sieve according to the sieving method.

<< Measurement of disintegration strength in wet condition >>
2 g of the obtained dentifrice composition was taken and dispersed in 18 mL of ion-exchanged water for 10 minutes, and then granules with a particle size of 190 to 210 μm were taken out from the solution, and a micro compression tester (manufactured by Shimadzu Corporation, MCTM-500) was used. The average value obtained by measuring 10 granules having the particle diameter was obtained and used as the value of the disintegration strength in a wet state.

[Example 1]
Granules were obtained according to the formulation of dentifrice granules shown in Table 1. Specifically, calcium carbonate (Toyo Denka Kogyo Co., Ltd., trade name: Toyo White, average particle size 2-5 μm), colloidal silica (Nissan Chemical Co., Ltd., trade name: Snowtex S), cellulose (Nippon Paper Industries) Chemical Co., Ltd., trade name: KC Flock W-400G) and water were mixed with a disper wing (manufactured by Ashizawa Niro Atomizer Co., Ltd., model: HS-P3) to obtain a water slurry. The obtained water slurry was spray-dried at a blowing temperature of 190 ° C., and classified with a sieve having openings of 90 μm and 500 μm. The granulated product after classification is heated to 100 degrees and charged into a U trough type ribbon blender (model: R-17W, manufactured by Hosokawa Micron Co., Ltd.) having a jacket temperature of 80 degrees. p. Mixing was started at m, fluid number 2.1. Next, after adding palmitic acid at normal temperature (Kao Corporation, Lunac P-95), mixing was performed for 30 minutes to obtain granules.

[Example 2]
Granules were obtained according to the formulation of dentifrice granules shown in Table 1. Specifically, zeolite (Zeo Builder Co., Ltd., trade name: zeolite (powder)), sodium silicate aqueous solution (Fuji Chemical Industry Co., Ltd., trade name: No. 3 sodium silicate, solid content: 55.1%) and water Were mixed with a disper blade (manufactured by Ashizawa Niro Atomizer Co., Ltd., model: HS-P) to obtain a water slurry. The obtained water slurry was spray-dried at a blowing temperature of 190 ° C., and classified with a sieve having an opening of 500 μm. The granulated product after classification is heated to 100 degrees and charged into a U trough type ribbon blender (model: R-17W, manufactured by Hosokawa Micron Co., Ltd.) having a jacket temperature of 80 degrees. p. Mixing was started at m, fluid number 2.1. Next, after adding palmitic acid at normal temperature (Kao Corporation, Lunac P-95), mixing was performed for 30 minutes to obtain granules.

[Example 3]
According to the formulation of dentifrice granules shown in Table 1, calcium carbonate and zinc oxide were mixed, and granules were obtained by a rolling granulator. Specifically, both raw materials were mixed in the apparatus (equipment: Newgramachine SEG850 type), and granulated by adding 15% purified water to the powder during granulation. After completion of the granulation step, it was dried for about 20 to 30 minutes in a dryer (equipment: rotary kiln). The collapse hardness of the granulated product was 15 to 18 g / piece. In addition, the granulated material removed the granulated material of 50 micrometers or less with the electric sieve. The granulated product after classification is heated to 100 degrees and charged into a U trough type ribbon blender (model: R-17W, manufactured by Hosokawa Micron Co., Ltd.) having a jacket temperature of 80 degrees. p. Mixing was started at m, fluid number 2.1. Next, after adding palmitic acid at normal temperature (Kao Corporation, Lunac P-95), mixing was performed for 30 minutes to obtain granules.

[Examples 4 to 11]
Granules were obtained according to the formulation of dentifrice granules shown in Table 1. Specifically, heavy calcium carbonate (trade name: ACE-25, average particle diameter of about 3 μm, manufactured by Calfine Co., Ltd.) was introduced into a 75 L drum granulator (φ40 cm × L60 cm) having a baffle plate. , Drum rotation speed 30r. p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, sodium silicate (manufactured by Fuji Chemical Industry Co., Ltd., trade name: No. 3 sodium silicate: Na ₂ .3SiO ₂ solution, solid content 38.5 %, Diluted with 3 times the amount of water or less, 25 ° C.) using one external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.) and granulated. The batch size is 10 kg. The addition rate of the aqueous sodium silicate solution was 3.3 mL / min.
After spraying the sodium silicate aqueous solution, mixing was continued for 1 minute, then discharged from the drum granulator, dried at 120 ° C. for 20 hours using an electric shelf dryer, and then a U trough ribbon blender with a jacket temperature of 80 ° C. ( The material (B) was added to Hosokawa Micron Corporation, model: R-17W), and mixed for 3 minutes at a rotation speed of 130 rpm and a fluid number of 2.1 to obtain granules.

[Comparative Examples 1-2]
According to the formulation of the dentifrice granules shown in Table 1, granules were obtained in the same manner as in Example 4 except that the component (B) was not used.

[Comparative Example 3]
According to the formulation of dentifrice granules shown in Table 1, granules were obtained in the same manner as in Example 4 except that lauric acid was used instead of palmitic acid.

  Using each obtained granule, the biofilm formation inhibition rate (%) was determined according to the following method, and the flavor was also evaluated.

<Biofilm formation inhibition rate (%)>
A HAp substrate (APP-100, PEN, manufactured by HOYA Corporation) was used as a sample substrate, and was mirror-polished with sandpaper having a grindstone size of 40 μm, 12 μm, and 3 μm, and then deashed with a 1N HCl solution for 1 minute at room temperature. On the surface of the sample substrate, 87 parts by mass of the glycerin dispersion solution is applied to 13 parts by mass of each granule obtained in Examples 1 to 11 and Comparative Examples 1 to 3, and then the sample substrate is ionized. Washed with exchange water for 10 seconds. In Comparative Example 2, it was allowed to act as 86 parts by mass of the glycerin dispersion and 1 part by mass of palmitic acid with respect to 13 parts by mass of the granules.

Next, each sample substrate after washing was immersed in a 5% sucrose solution of saliva supernatant (centrifuged at 3000 rpm for 10 minutes at room temperature) and allowed to stand for 24 hours under anaerobic conditions at 37 ° C. Thereafter, the plate was washed with ion-exchanged water for 5 minutes, immersed in plaque staining solution for 5 minutes, and then washed twice with ion-exchanged water for 5 minutes. 500 μL of 1N NaOH was added to the dried sample substrate to extract the dye, and the absorbance at λ = 540 nm was measured. Calculate the dye extraction rate in each sample substrate when the absorbance of the untreated substrate (control substrate) that did not act anything was set to 100, calculate the biofilm formation inhibition rate according to the following formula (X), An average value obtained by repeating the same operation five times was taken as a measured value.
The results are shown in FIG.
Biofilm formation inhibition rate (%)
= (1- (absorbance of sample substrate) / absorbance of control substrate) × 100 (X)

<Evaluation of flavor>
The flavors of the granules obtained in Examples 4 and 9 to 11 and Comparative Examples 1 and 3 were evaluated by one panelist. For this evaluation, a sample prepared at the time of calculating the biofilm formation inhibition rate was used, and 5 mL of this was included, brushed with a toothbrush (check, manufactured by Kao Corporation), rinsed with water, and flavored ( The presence or absence of oil flavor derived from fatty acids was subjected to sensory evaluation.
As an evaluation standard, point evaluation based on 5 levels of 1 to 5 was adopted. It shows that it is so favorable that the value of this point is large.
The results are shown in Table 2.

  From the results of Table 1 and FIG. 1, Comparative Example 1 in which component (B) was not supported on component (A), Comparative Example 2 in which component (B) was allowed to act independently of granules, and Component (B) It turns out that the granule of Examples 1-11 is excellent in the biofilm formation inhibitory effect compared with the comparative example 3 which made the component (A) carry | support lauric acid (carbon number 12) instead of.

  Moreover, from the results of Table 2, Comparative Examples 1 and 3 felt an oil flavor derived from fatty acids when left in the mouth, and uncomfortable feeling remained, while Examples 4 and 9 to 11 had an oil flavor derived from fatty acids. It can be seen that the taste of zinc and zinc is hardly felt, the taste is good, and the feeling of use is high.

[Example 12]
According to the formulation of dentifrice granules shown in Table 3, granules were obtained in the same manner as in Example 4. Using the obtained granules, a dentifrice was produced according to the formulation of the dentifrice composition shown in Table 3, and the plaque formation inhibition rate (%) was determined according to the following method, and the feeling of use was also evaluated. .

[Comparative Examples 4 to 5]
According to the formulation of dentifrice granules shown in Table 3, granules were obtained in the same manner as in Comparative Example 1. Using the obtained granules, a dentifrice was produced according to the formulation of the dentifrice composition shown in Table 3, and the plaque formation inhibition rate (%) was determined according to the following method, and the feeling of use was also evaluated. .

<In vitro biofilm formation inhibition rate (%)>
A HAp substrate (APP-100, PEN, manufactured by HOYA Corporation) was used as a sample substrate, and was mirror-polished with sandpaper having a grindstone size of 40 μm, 12 μm, and 3 μm, and then deashed with a 1N HCl solution for 1 minute at room temperature. About 1 g of the dentifrice obtained in Example 12 and Comparative Examples 4 to 5 was allowed to act on the surface of this sample substrate for 1 minute, and then the sample substrate was washed with ion-exchanged water for 10 seconds.

Next, the washed sample substrate was immersed in a 5% sucrose solution of saliva supernatant (centrifuged at 3000 rpm for 10 minutes at room temperature) and allowed to stand under anaerobic conditions at 37 ° C. for 24 hours. Thereafter, the plate was washed with ion-exchanged water for 5 minutes, immersed in plaque staining solution for 5 minutes, and then washed twice with ion-exchanged water for 5 minutes. 500 μL of 1N NaOH was added to the dried substrate to extract the dye, and the absorbance at λ = 540 nm was measured. Calculate the dye extraction rate in each sample substrate when the absorbance of an untreated substrate (control substrate) that did not act on was 100, and calculate the biofilm formation inhibition rate according to the above formula (X), An average value obtained by repeating the same operation five times was taken as a measured value.
The results are shown in Table 2 and FIG.

《Plate formation inhibition rate in human test (%)》
Using the dentifrice obtained in Example 12 and Comparative Example 4, a human test was conducted on five subjects according to the following method.
First, a dental hygienist performed tooth surface cleaning (empty brush, scaling) of each subject. Next, after 2 hours or more had elapsed, the dental hygienist performed each subject's tooth surface cleaning for 2 minutes using the dentifrice obtained in Example 12. Next, after stopping brushing for 24 hours, the observation sites were the maxillary left and mandibular right of No. 6, the maxillary right and mandibular left of No. 1 and No. 4, and each tooth's near-distal cheek side corner 2 points, cheek side center The amount of plaque in each part was measured with a total of 36 points, 1 point, 2 points on the lingual side near-distal cheek side and 1 point on the lingual side. The measurement is performed after the dental hygienist stains each subject's plaque, applying a measure of 1mm unit, reading to what height of the gingival margin is stained in 0.5mm unit, the amount of plaque adhesion Was measured. Next, based on the obtained value, the plaque formation inhibition rate was calculated according to the following formula (Y).
After about one week from such measurement, according to the same method, the amount of plaque adhesion was measured using the dentifrice obtained in Comparative Example 4, and the plaque formation inhibition rate was determined according to the following formula (Y). Calculated. The above human test was conducted on a total of 5 subjects, and the average value of each plaque formation inhibition rate was used as an evaluation index.
The results are shown in FIG.
Plaque formation inhibition rate (%) = (plaque formation amount when using dentifrice (mm) / plaque formation amount when empty brushing (mm)) x 100 ... (Y)

<< Evaluation of feeling of use >>
Using the dentifrices obtained in Example 12 and Comparative Examples 4 to 5, the flavor was evaluated by one panelist. Specifically, 1 g of each dentifrice is applied to the tooth surface, brushed with a toothbrush (Check, manufactured by Kao Corporation), then rinsed with water, and the tooth surface is evaluated by a point evaluation of 1 to 5 levels. Evaluation of the smooth feeling and the sustainability, and the flavor (presence or absence of fatty acid-derived oil flavor). Higher values indicate better results.
The results are shown in Table 3.

From the results of Table 3 and FIG. 3, compared to Comparative Example 4 in which component (B) was allowed to act independently of granules, and Comparative Example 5 in which component (B) was not supported on component (A), It can be seen that the dentifrice of Example 12 has a high plaque formation inhibitory effect and can maintain a smooth feel on the tooth surface.
Also, with regard to the feeling of use, in Comparative Example 4, the oil flavor derived from fatty acid was felt after squeezing the mouth, and in comparison with the flavor remaining until later in Example 12, the oil flavor derived from fatty acid was used. It can also be seen that it does not feel zinc and has a good flavor and is excellent in use.

Claims (8)

The following components (A) and (B):
(A) A granulated product containing a water-insoluble powder material, and (B) a saturated or unsaturated fatty acid having 14 to 22 carbon atoms or a salt thereof, and the component (B) is carried on the component (A). A dentifrice granule having an average particle size of 50 μm or more and 500 μm or less and a disintegration strength of 0.2 gf / piece or more and 30 gf / piece or less in a wet state.   The dentifrice granule according to claim 1, wherein the content of the water-insoluble powder material in the component (A) is 50% by mass or more and 95% by mass or less.   The dentifrice granule according to claim 1 or 2, wherein the component (A) contains 1 to 30% by mass of an inorganic binder.   The component (A) is one or two or more types of agglomerated material selected from the aggregate (a1) of the water-insoluble powder material and the granulated material (a2) containing the water-insoluble powder material and the inorganic binder. The granule for dentifrice of any one of Claims 1-3.   The dentifrice granule according to any one of claims 1 to 4, wherein the content of the component (B) is 0.1 to 40 parts by mass with respect to 100 parts by mass of the component (A).   A dentifrice composition containing 1% by mass or more and 50% by mass or less of the dentifrice granules according to any one of claims 1 to 5.   The dentifrice composition of Claim 6 containing a binder.   The dentifrice composition according to claim 6 or 7, wherein the content of sorbitol is 5% by mass or more and 60% by mass or less.