JP5716649B2 - Dentifrice composition - Google Patents

Description

  The present invention has excellent cleaning power against tooth surface stains and provides a satisfactory feeling of cleaning due to a high level of brushing on the tooth surface, and there is no sense of incongruity due to graininess during brushing, and it is collected on a toothbrush. The present invention relates to a dentifrice composition that is easy to extrude from a container when it is used and has excellent liquid separation stability over time.

  The dentifrice composition contains a polishing agent such as calcium phosphate, calcium carbonate, and abrasive silica to provide the basic function of cleaning dirt adhered to the oral cavity surface such as the tooth surface. The amount is set according to the cleaning power of each abrasive. Calcium phosphate and calcium carbonate generally have a relatively low cleaning power, so the amount incorporated into the dentifrice composition is generally 30 to 60% by mass, whereas abrasive silica has a relatively high cleaning power. Often 10 to 25% by mass is blended. In a general commercially available dentifrice composition, the cleaning power is adjusted to a certain range regardless of which abrasive is used, so there is no significant difference in the amount of abrasive that is a solid component. There is a difference of 2-3 times. This leads to a difference in the feeling of use on the tooth surface when brushing the toothpaste, and the composition with a large amount of abrasive is more sensitive to the tooth surface during brushing brushing (feeling of brushing). Tend to occur.

  However, when abrasive silica is used as an abrasive, there is a problem that it is difficult to obtain a high feeling of brushing because the blending amount is set small. On the other hand, abrasives such as calcium carbonate and calcium phosphate tend to increase the sense of brushing due to the large amount of these compounds. However, since the physical properties of calcium ions are likely to elute, they are used due to the influence of calcium ions that elute. There was a problem that there was a feeling of persistence later and the feeling of refreshing was insufficient.

  As a technique for enhancing the brushing feeling with a dentifrice composition containing abrasive silica, a method for obtaining a brushing feeling by increasing the physical acting force of the toothbrush on the tooth surface by blending inorganic or organic granules. Etc. are known. However, with this technology, there may not always be a feeling of sufficient brushing, and if the amount of granules is increased in order to obtain a sufficient feeling of brushing, the grain may feel rough and uncomfortable during brushing. There were some problems (see Patent Documents 1 and 2).

  On the other hand, synthetic layered sodium silicate / magnesium is a kind of synthetic bentonite, that is, a swellable clay mineral. It is known that thickening and shape retention can be obtained by blending into a dentifrice composition like a binder (see Patent Document 3).

  In general, dentifrice compositions have a high molecular weight substance such as sodium alginate, xanthan gum, sodium carboxymethylcellulose, sodium polyacrylate, etc. as a binder to maintain shape retention for easy collection in a toothbrush. About 1% by mass. These binders are involved in the rheological properties of the dentifrice composition and also affect the feeling of use in dentifrice brushing. In general, when the amount of the binder is increased, it tends to be difficult to understand that the abrasive is hitting the tooth surface and cleaning, and this leads to a sufficient satisfaction of cleaning sensibly against the action of brushing teeth. There was no case. On the other hand, if the compounding amount of the binder is reduced, the dentifrice paste in an emulsified dispersion state containing solid particles is deteriorated in stability over time, causing problems such as partial separation of the solution from the change in the emulsification dispersion state. For this reason, it was difficult to achieve both satisfactory cleaning feeling and liquid separation stability.

  In any case, these conventional techniques are excellent in cleaning power against the dirt on the tooth surface, provide a sufficiently satisfactory feeling that the tooth surface is cleaned, and are easy to extrude when picking up a toothbrush. The composition of the present invention and its technical idea of satisfying all of these were not recalled.

JP 2005-68072 A JP 2008-266251 A Special table 2009-519235 gazette

Therefore, the present invention provides a new dentifrice composition having high cleaning power, sufficient brushing feeling during brushing that leads to a feeling of cleaning, and good general characteristics that provide a refreshing feeling after use. It is a technical problem of the invention.
The present invention has been made in view of the above circumstances, and is excellent in cleaning ability of tooth surface stains, provides a sufficient feeling of brushing on the tooth surface, and does not feel uncomfortable due to graininess during brushing, and is collected in a toothbrush. It is an object of the present invention to provide a dentifrice composition that is easy to extrude from a container at the time and excellent in liquid separation stability of a formulation over time.

  As a result of intensive studies to achieve the above object, the inventors of the present invention have (A) synthetic layered sodium silicate and magnesium silicate, (B) an average particle size of 50 to 400 μm, and an average disintegration strength of 10 to 10. 200g / piece granule, (C) abrasive silica, and (D) anionic binder are blended, the content of component (B) is 1 to 5% by mass and the content of component (D) is 0. .2 to 0.5% by mass provides high cleaning power for tooth surface stains, excellent brushing feeling, no feeling of roughness after use, good refreshing feeling, and extrusion It has been found that a formulation having good properties and appearance stability can be obtained, and that the mass ratio of (A) / (D) is 5 to 25, the feeling of brushing is further improved.

  It is known that when synthetic layered sodium silicate / magnesium is blended in a dentifrice composition, thickening and shape retention can be obtained in the same manner as a polymer binder. Since the compound has a fine layered structure, the applicant pays attention to the property that when the physical mechanical force is applied, the structure collapses and the viscosity rapidly decreases, unlike the polymer binder. Japanese Patent Application No. 2009-267392 proposed a technique for improving dispersibility during brushing using a dentifrice composition containing synthetic layered sodium silicate / magnesium.

  As a result of further investigation into the blending of the synthetic layered sodium silicate / magnesium into the dentifrice composition, the applicant has found that the synthetic layered sodium silicate / magnesium has increased viscosity and shape retention by blending into the dentifrice composition. However, unlike ordinary binders, it uses the property of drastically lowering the viscosity when applied, and is a combination of synthetic layered sodium silicate / magnesium and specific granules, and abrasive silica. When used in combination, the effect on the tooth surface of inorganic particles that are usually attenuated by a binder such as a general polymer substance during brushing is efficiently and directly transmitted to the tooth surface, which is high. We have developed a technology that leads to cleaning power and a sense of cleanliness, and have made the present invention. According to the present invention, the (A) synthetic layered sodium silicate magnesium and (B) a granule having an appropriate average particle size and average disintegration strength are combined, and (C) abrasive silica and (D) anionic By properly blending the binder, the above-mentioned effects are effectively exhibited, the cleaning power derived from the abrasive silica is sufficiently exhibited, stains attached to the tooth surface can be effectively removed, and the feeling of cleaning A brushing feeling that leads to a satisfactory brushing feeling can be obtained, a refreshing feeling after use can be obtained, and a dentifrice composition with good general characteristics can be provided. In the present invention, a silica-based abrasive such as silicic anhydride is used as an abrasive, and although the blending amount of the abrasive is small compared to calcium phosphate or the like, it has excellent feeling of brushing and feels rough and uncomfortable after use. The refreshing feeling is good and an excellent cleaning power is obtained. Furthermore, by appropriately combining and blending an anionic binder, good extrudability and liquid separation stability, which are general characteristics of a dentifrice, can be ensured as well as the above excellent sensation.

Accordingly, the present invention provides the following dentifrice composition.
[1]
(A) Synthetic layered sodium silicate / magnesium, (B) granules having an average particle size of 50 to 400 μm and an average disintegration strength of 10 to 200 g / piece, (C) abrasive silica, and (D) anions A dentifrice characterized by comprising an adhesive binder, wherein the content of the component (B) is 1 to 5% by mass and the content of the component (D) is 0.2 to 0.5% by mass. Composition.
[2]
(B) component is dicalcium phosphate, tricalcium phosphate, water-insoluble calcium metaphosphate, silica, aluminum hydroxide, magnesium phosphate, bengara, calcium carbonate, calcium pyrophosphate, zeolite, aluminosilicate, magnesium carbonate, zirconosilicate, [1] The dentifrice composition according to [1], wherein the dentifrice composition is a particle obtained by granulating one or more water-insoluble powders selected from calcium sulfate.
[3]
The dentifrice composition according to [1] or [2], wherein the component (D) is one or more anionic binders selected from sodium alginate, sodium polyacrylate, sodium carboxymethylcellulose, xanthan gum, and carrageenan.
[4]
The dentifrice composition according to [1], [2] or [3], wherein (A) / (D) is 5 to 25 by mass ratio.

  According to the present invention, the cleaning power and the feeling of brushing on the tooth surface are excellent, and there is no sense of incongruity due to particles, and the extrusion is easy when collected on a toothbrush, and the liquid separation stability of the preparation over time It is possible to provide a dentifrice composition which is excellent in general properties and excellent in properties.

Hereinafter, the present invention will be described in more detail.
The dentifrice composition of the present invention is suitably prepared as a toothpaste for toothpaste, liquid toothpaste, etc., particularly as a toothpaste. (A) Synthetic layered sodium silicate / magnesium, (B) Average particle size A granule having an average disintegration strength of 10 to 200 g / piece, (C) abrasive silica, and (D) an anionic binder is contained.

The component layered sodium silicate / magnesium (A) is a kind of synthetic bentonite (hectorite) which is a layered silicate. Generally, it has a structure in which plate-like crystals having a thickness of about 1 nm and a side of 20 to 100 nm overlap each other in layers. As its constituent components, SiO ₂ : 58.0%, MgO: 25.4%, Na ₂ O: 3.1%, Li ₂ O: 1.0% as approximate mass%, A synthetic clay agent containing water and trace metals. It is a completely synthetic product and is produced by mixing sodium silicate with sodium salt, magnesium salt and lithium salt and reacting them.
The synthetic layered sodium silicate / magnesium component (A) preferably has a viscosity measured using a B-type viscometer of 3,000 to 10,000 mPa · s, particularly 5,000 to 8,000 mPa · s. What is s is more preferable. When the viscosity is less than 3,000 mPa · s, there may be a case where a sufficient brushing feeling cannot be obtained, and when it exceeds 10,000 mPa · s, the composition becomes hard and the extrudability may be impaired.
The viscosity was measured with a B10H viscometer after dispersing 4% of synthetic layered sodium silicate / magnesium in ion-exchanged water and stirring with a stirrer for 30 minutes (rotor No. 5, rotation speed: 20 rpm, (Measurement time: 3 minutes, 25 ° C.)
As such synthetic layered sodium silicate / magnesium, for example, commercially available products such as Laponite D and Laponite DF (both manufactured by Rockwood Additives) can be used.

  The blending amount of the synthetic layered sodium silicate / magnesium is 2 to 8% (mass%, the same applies hereinafter) based on the total amount of the composition from the viewpoints of improvement in cleaning power, improvement in brushing, liquid separation stability and extrusion hardness. ), Especially 4 to 6% is preferable. If it is less than 2%, sufficient cleaning power or feeling of brushing may not be obtained, or liquid separation with time may occur more easily. If it exceeds 8%, the composition becomes hard and the extrudability may be impaired. is there.

  The granule (B) is a particle in which a water-insoluble powder is formed into a granular shape, and a binder may be used for granulation, but in particular, a binder is not used. As water-insoluble powder, dicalcium phosphate, tricalcium phosphate, water-insoluble calcium metaphosphate, silica, aluminum hydroxide, magnesium phosphate, bengara, calcium carbonate, calcium pyrophosphate, zeolite, aluminosilicate, magnesium carbonate, zirconosilicate Inorganic powders such as calcium sulfate and mixtures thereof can be mentioned, and silica granules are particularly preferable.

  As the silica granule, wet method gel method silica and precipitation method silica are suitably used, and the primary particle diameter is about 3 to 15 nm, preferably 4 to 10 nm. For example, a silica gel mass having a primary particle size grown to about 4 to 10 nm by a gel method is washed, dried and then pulverized to classify into silica granules having an average particle size of 50 to 400 μm. A method of preparing granules by spraying in the air and gelling, a method of preparing by agglomeration while suppressing the growth of primary particles by the precipitation method and then growing the primary particle diameter to about 4 to 10 nm, etc. Silica granules can be prepared by these methods. Among them, a method of pulverizing a mass of silica gel prepared by the gel method is preferable because it is simple in production and easy to control the average particle diameter by classification. By preparing by such a method, the granule which has suitable average disintegration strength can be obtained, and a thing with low abrasiveness can be obtained, and a silica granule suitable as (B) component can be obtained.

The average particle diameter of the granule is 50 to 400 μm, and particularly preferably 60 to 200 μm, since the feeling of brushing is high and there is no sense of incongruity. If the average particle size is less than 50 μm, a sufficient feeling of brushing may not be obtained, and if it is greater than 400 μm, the grainy feeling of graininess may occur during brushing.
The average particle size was measured using a particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., Microtrac particle size distribution meter, dispersion medium: water). The measured value was obtained from the median diameter (d50) using volume average, and this was defined as the average particle diameter.

The average disintegration strength of the granules is 10 to 200 g / piece, particularly 20 to 50 g / piece. When the average disintegration strength is less than 10 g / piece, a sufficient feeling of brushing may not be obtained. When the average disintegration strength is more than 200 g / piece, the grain may have a rough and uncomfortable feeling during brushing.
The average disintegration strength is the value obtained by measuring the automatic breaking strength of 30 granules with a rheometer (Sun Rheometer CR-200D) manufactured by Sun Science Co., Ltd. (this granule disintegrates when one granule is compressed at a speed of 10 mm / min). The value obtained by measuring the load at the time of measurement) was obtained from the average value.

  As the granule having such an average particle diameter and average disintegration strength, a commercially available product can be used. Specific examples of the silica granule include nip gel (manufactured by Tosoh Silica Co., Ltd.), Sorbosil (PQ Corporation) and the like.

  The blending amount of the granule is 1 to 5%, particularly 2 to 4%, based on the total amount of the composition. If it is less than 1%, it is not possible to obtain a sufficient feeling of brushing. If it exceeds 5%, the grainy graininess at the time of use will occur.

(C) Abrasive silica of component is a precipitated silica having abradability, which is different from the silica granule of component (B), and non-silicic acid or 5% or less of zirconium or aluminum is added in the production process. Examples thereof include crystalline silicic anhydride.
As for the average particle diameter of the abrasive silica, the median diameter (d50) using the volume average is preferably 5 to 40 μm, particularly preferably 10 to 30 μm. If the median diameter is less than 5 μm, sufficient polishability cannot be obtained, and if it exceeds 50 μm, there may be a feeling of strangeness (foreign material feeling) during use. The median diameter is a value measured using a particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., Microtrac particle size distribution meter, dispersion medium: water). By using these abrasive silicas, a better refreshing feeling can be obtained after use than calcium carbonate or the like.

  A commercially available product can be used as the abrasive silica, and examples thereof include TIXOSIL 73 (precipitated silica, whose average particle size is 14 μm as a measured median diameter) sold by Rhodia Nikka Co., Ltd.

  The blending amount of the abrasive silica is preferably 10 to 25%, more preferably 14 to 22% of the entire composition. If the blending amount is less than 10%, sufficient cleaning power and a feeling of brushing cannot be obtained, and if it exceeds 25%, the extrusion hardness may become hard.

  Examples of the anionic binder of the component (D) include sodium alginate, sodium polyacrylate, sodium carboxymethylcellulose, xanthan gum, carrageenan, and the like. One of these may be used alone or in combination of two or more. it can. Of these, sodium alginate, sodium polyacrylate, xanthan gum, and carrageenan are preferable, and xanthan gum is more preferable because liquid separation stability is particularly good.

  The compounding quantity of an anionic binder is 0.2 to 0.5% with respect to the composition whole quantity, Preferably it is 0.3 to 0.4%. If it is less than 0.2%, liquid separation occurs. If it exceeds 0.5%, a feeling of brushing is not felt or the extrusion hardness becomes hard.

  Furthermore, in the present invention, the blending ratio of (A) synthetic layered sodium silicate / magnesium and (D) anionic binder, that is, (A) / (D) is 5 to 25, particularly 10 to 18 in mass ratio. It is preferable that such a ratio can further improve the sense of cleanliness. When the blending ratio is less than 5, the sense of cleanliness may not be sufficiently obtained, and when it exceeds 25, the extrusion hardness may become hard or liquid separation may easily occur.

  The dentifrice composition of the present invention has other known components that are usually blended in the dentifrice composition as optional components in addition to the above-described constituents, for example, abrasives other than the component (C), viscous agents, (D ) Other than the components, suitable components such as a binder, a surfactant, a moisturizing agent, and a sweetener, a coloring agent, an antiseptic, a storage stabilizer, a pH adjuster, and a medicinal component are added according to the present invention. It can mix | blend in the range which does not impair an effect, These components and water can be mixed and it can manufacture by a normal method.

  As the abrasive, in addition to the abrasive silica of component (C), other abrasives may be blended. For example, dibasic calcium phosphate dihydrate, dibasic calcium phosphate anhydrate, calcium pyrophosphate, aluminum hydroxide, alumina, titanium dioxide, polymethyl methacrylate, insoluble calcium metaphosphate, light calcium carbonate, heavy calcium carbonate, magnesium carbonate, Examples thereof include tertiary magnesium phosphate, zeolite, zirconium silicate, hydroxyapatite, fluoroapatite, calcium deficient apatite, tertiary calcium phosphate, fourth calcium phosphate, and eighth calcium phosphate. In order to obtain a refreshing feeling after use according to the present invention, it is preferable not to blend an abrasive having a high calcium ion elution property. The blending amount of these abrasives is preferably 0 to 6%, particularly preferably 0 to 2% of the whole composition as long as the effects of the present invention are not hindered.

Examples of the surfactant include an anionic surfactant, an amphoteric surfactant, and a nonionic surfactant. For example, examples of the anionic surfactant include lauryl sulfate, myristyl sulfate, polyoxyethylene alkyl sulfate, N-lauroyl taurine salt, lauroyl sarcosine salt, α-olefin sulfonate and the like. From the above, sodium salt is preferable. Examples of amphoteric surfactants include N-acyl glutamate, 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine, fatty acid amidopropyl betaine, and the fatty acid chain length is 12 to 14 carbon atoms. Those are preferred in terms of solubility. Nonionic surfactants include, for example, polyoxyethylene alkyl ether, alkyl glycoside, sucrose fatty acid ester, alkylol amide, polyoxyethylene sorbitan monostearate, polyoxyethylene polyoxypropylene glycol, fatty acid polyglyceryl, polyoxyethylene hardened castor Oil etc. are mentioned.
In addition, the compounding quantity of these surfactant is 0.5 to 5% of the whole composition normally, Preferably it is 0.8 to 3%.

  As the thickener, for example, polyhydric alcohols such as sorbitol, glycerin, ethylene glycol, propylene glycol, 1,3-butylene glycol, polyethylene glycol, polypropylene glycol, xylitol, maltitol, erythritol, sugar alcohols, etc. may be blended. Good. The blending amount of the thickener is usually 10 to 60%, preferably 20 to 40%.

  As a binder, in addition to the anionic binder of component (D) as necessary, other binders such as non-anionic binders such as hydroxyethylcellulose, methylcellulose, hydroxymethylpropylcellulose, etc. Can be blended. The amount of these binders is 0 to 2%, preferably 0 to 1%.

  Medicinal ingredients include fluorides such as sodium fluoride, potassium fluoride, stannous fluoride, strontium fluoride, sodium monofluorophosphate, chlorhexidine, triclosan, isopropylmethylphenol, cetylpyridinium chloride, benzalkonium chloride, Antibacterial substances such as benzethonium chloride, chlorhexidine salts, sorbate, hinokitiol, azulene sulfonate, degrading enzymes such as dextranase, mutanase, protease, lysozyme, tranexamic acid, epsilon aminocaproic acid, allantoin, glycyrrhizic acid, glycyrrhetinic acid Anti-inflammatory substances such as sodium chloride, potassium nitrate, aluminum lactate, zinc chloride, zinc citrate, strontium chloride, sodium tripolyphosphate, sodium pyrophosphate Chelating compounds such as sodium, zeolite, copper chlorophyllin sodium, chlorophyll, glycerophosphate, various vitamins such as ascorbic acid, tocopherol acetate, pyridoxine, etc., soft sugar beet extract, buckwheat extract, chamomile, clove, rosemary, ugone, safflower, etc. Examples include natural extracts. The compounding quantity of these active ingredients can be made into an effective quantity in the range which does not prevent the effect of this invention.

  Sweeteners include saccharin sodium, aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, perilartin, etc., and preservatives include parabens (paraoxybenzoate) such as butylparaben and ethylparaben. And sodium benzoate.

  As coloring agents, Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green No. 3, mica titanium, titanium oxide and the like.

  Examples of the pH adjuster include citric acid, malic acid, lactic acid, tartaric acid, acetic acid, phosphoric acid, pyrophosphoric acid, glycerophosphoric acid, various salts thereof, sodium hydroxide, and the like. In addition, it is preferable that the dentifrice composition of this invention is adjusted to pH 6-10, especially 7-9.

Perfumes are peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime Oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, iris concrete, absolute peppermint Natural fragrances such as absolute rose and orange flower, and fragrances processed by these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder fragrance, etc.), and , Menthol, carvone, anethole, cineol, salicylic acid , Cinnamic aldehyde, eugenol, 3-1-menthoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone, menthyl acetate, N-substituted-paramentane-3-carboxamide, pinene, octyl Acetaldehyde, citral, pregon, calbeetoacetate, anisaldehyde, ethyl acetate, ethyl butyrate, allylcyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, hexanal, ethyl alcohol, propyl Alcohol, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cycloten, furfural, trimethylpyrazine, ethyl lactate, methyl lactate , Flavors such as ethyl thioacetate, strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mix flavor, tropical fruit flavor, etc., dentifrice The well-known fragrance | flavor raw material used for a composition can be used, It is not limited to the fragrance | flavor of an Example.
Moreover, although a compounding quantity is not specifically limited, It is preferable to use said fragrance | flavor raw material 0.000001 to 1% in a formulation composition. Moreover, as a fragrance | flavor for perfume using the said fragrance | flavor raw material, it is preferable to use 0.1 to 2.0% in a dentifrice composition.

  The material for the dentifrice composition container is not particularly limited, and a container used for a dentifrice composition can be used. Specifically, plastic containers such as polyethylene, polypropylene, polyethylene terephthalate, and nylon, and laminate containers composed of these plastics and aluminum foil can be used.

  EXAMPLES Hereinafter, although an experimental example, an Example, and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples, the blending amount is mass%.

[Experimental Example 1]
Dentifrice compositions (toothpastes) having the compositions shown in Tables 1 and 2 were prepared by the following method and filled into a laminate tube having a diameter of 26 mm and a mouth inner diameter of 8 mm. The obtained dentifrice composition was evaluated by the following methods for cleaning power, feeling of brushing, uncomfortable feeling, ease of extrusion, and liquid separation stability. The results are shown in Tables 1 and 2.

Preparation of test dentifrice composition:
The preparation of the dentifrice composition was prepared by dissolving a water-soluble substance such as saccharin sodium and sodium fluoride in purified water, adding sorbitol, and then adding the component (A) component layered sodium silicate / magnesium to the dispersion. Separately, a liquid in which an anionic binder of component (D) was dispersed in propylene glycol was added and stirred. Then, a fragrance | flavor, the abrasive silica of (C) component, the granule of (B) component, and also sodium lauryl sulfate were added, and it stirred under reduced pressure (5.3 kPa), and obtained the dentifrice composition. A unimixer (FM-SR-25, manufactured by POWEX CORPORATION) was used for the production. In addition, the dentifrice composition of the comparative example was prepared similarly to the above.

The ingredients used in the preparation of these dentifrice compositions were synthetic layered sodium silicate / magnesium (Laponite D, manufactured by Rockwood Additives, viscosity ^* ; 6,660 mPa · s), granules (trade names Nipgel, Tosoh Silica Co., Ltd., AY grade silica granules, average particle size and average disintegration strength are as shown in the table.), Xanthan gum (Monato Gum DA, manufactured by Dainippon Sumitomo Pharma Co., Ltd.), sodium alginate (Kimika Algin I-3, Kimika Co., Ltd.), carrageenan (CP Kelco Co., Ltd.), sodium polyacrylate (Rheojic 250H, Nippon Pure Chemicals Co., Ltd.), abrasive silica (TIXOSIL 73 manufactured by Rhodia Co., Ltd.), average particle size 14 μm ), Propylene glycol, sorbit (70% aqueous solution), saccharin sodium, sodium fluoride As for other components such as thorium, titanium oxide, sodium lauryl sulfate, and purified water, standard products of the Quasi-drug Raw Material Standard 2006 were used. About the component whose form is aqueous solution, all showed the compounding quantity of pure part conversion also including the table | surface. The fragrance | flavor created and mix | blended the fragrance | flavor A-fragrance | flavor I shown in Table 3 using the flavor composition shown in Tables 4-9.
*; Using a B10H type viscometer (TVB10H type viscometer, Toki Sangyo Co., Ltd.), rotor No. 5, rotation speed: 20 rpm, measurement time: viscosity of 4% synthetic layered sodium silicate / magnesium silicate aqueous solution (using ion-exchanged water) measured at 25 ° C. for 3 minutes.

  The average particle size of the granules used was 50% particle size (median diameter (d50 using volume average)) measured by a particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., Microtrac particle size distribution meter, dispersion medium: water). The average disintegration strength of the granules was determined by measuring the automatic breaking strength of 30 granules using a rheometer (Sun Rheometer CR-200D) manufactured by Sun Science Co., Ltd. The value obtained by measuring the load when the granule disintegrates when compressed in step 1).

The container used in the following evaluation was a laminated tube (Dai Nippon Printing Co., Ltd.) having a diameter of 26 mm and a mouth inner diameter of 8 mm, and the layer structure was LDPE55 / PET12 / LDPE20 / white LDPE60 / EMAA20 / from the outermost layer. AL10 / EMAA30 / LDPE20 / LLDPE30, and thickness is 257 μm. The abbreviations are as follows, and the numerical values indicate the thickness (μm) of each layer.
LDPE: Low density polyethylene White LDPE: White low density polyethylene LLDPE: Linear low density polyethylene AL: Aluminum PET: Polyethylene terephthalate EMAA: Copolymer resin of ethylene / methacrylic acid

(1) Cleaning power evaluation test method (1-1): Stain-attached hydroxyapatite pellet preparation method Hydroxyapatite pellet surface (Pentax, diameter 7 mm x thickness 3.5 mm) was treated with sand blasting and neutral Washed with an ultrasonic cleaner in an aqueous detergent solution. The surface was etched with a 30% phosphoric acid aqueous solution (10 minutes), washed with water, naturally dried, and then the Lab value (L0) of the pellet before adhesion of tannin iron stain was measured. For the above pellets, an operation of repeatedly dipping in 0.5% albumin aqueous solution → tannin extract → 0.6% iron (III) ammonium citrate aqueous solution for 1 hour was repeated 50 times and air-dried at room temperature for 1 day. Washed with running water and air-dried again to produce colored pellets. In addition, tannin extract liquid, boiled ion exchange water 1200ml, Japanese tea (brand: Oimatsu) 50g, black tea (Brisk tea bag (trade name), manufactured by Lipton), instant coffee (Nescafe (trade name) ), Nestlé Japan Co., Ltd.) 12 g was added and allowed to stand overnight, and Japanese tea and black tea were removed by filtration. The color of the surface of the produced colored pellet was measured, and the value was defined as L1.

(1-2) Evaluation Method for Stain Removal Effect The dentifrice composition having the composition shown in Tables 1 and 2 was diluted with twice the amount of ion-exchanged water to prepare a dentifrice dispersion. The tannin-iron stain-attached hydroxyapatite pellets produced by the above method were immersed in a toothpaste dispersion, and set in an automatic polishing tester (loading 250 g) with a flat-cut toothbrush (trade name: PC CLINICA, manufactured by Lion Corporation). After brushing, the Lab value (L2) of the pellets after brushing was measured. The tannin iron stain removal rate was calculated from the following formula, and the tannin iron stain removal rate was evaluated according to the following criteria.
Tannin iron stain removal rate (%) = [(L2-L1) / (L0-L1)] × 100
Evaluation criteria for cleaning power (stain removal effect) ◎: Tannin iron stain removal rate of 50% or more ○: Tannin iron stain removal rate of 40% or more and less than 50% △: Tannin iron stain removal rate of 30% or more and less than 40% ×: Tannin iron Stain removal rate less than 30%

(2) Evaluation method of brushing feeling Using about 10 subjects, about 1 g of the dentifrice composition was placed on a toothbrush with a brush head width of 10 mm and a length of 20 mm, and the brushing feeling when brushed was expressed as “ "I feel a sense of wiping", "I feel a feeling of wiping", "I don't feel a lot of wiping feeling", and "I don't feel wiping feeling". Among the answers, 4 points are “I feel a lot of brushing”, 3 points are “I feel a lot of brushing”, 2 points are “I don't feel a lot of brushing”, “I don't feel a lot of brushing” As a score, the brushing feeling was evaluated from the average score of 10 people according to the following criteria.
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 1.0 points More than 2.0 points

(3) Discomfort Evaluation Method Using about 10 subjects, about 1 g of the dentifrice composition was placed on a toothbrush with a brush head width of 10 mm and a length of 20 mm, and the rough discomfort when brushing was “not felt discomfort”, “ Answers were obtained in four stages: “I feel almost uncomfortable”, “I feel somewhat uncomfortable”, and “I feel uncomfortable”. Of these answers, an average of 10 people gave 4 points for “I don't feel discomfort”, 3 points for “I feel almost no discomfort”, 2 points for “I feel a little discomfort”, and 1 point for “I feel discomfort” From the point, the rough and uncomfortable feeling was evaluated according to the following criteria.
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 1.0 points More than 2.0 points

(4) Evaluation of ease of extrusion After 50 g of the dentifrice composition was filled in the laminate tube and each composition was stored at 50 ° C. for 1 month, a 10 cm dentifrice composition was extruded onto a straw half paper, and the extrusion was easy. Was evaluated according to the following four levels.
4 points: When extruding with a fingertip, the kneading occurs at a stretch of 10 cm or more.
3 points: When extruded with a fingertip, it is extruded at a stretch and a length of 5 cm or more and less than 10 cm is produced.
The
2 points: When extruding with fingertips, it extrudes at a stretch and has a length of 2 cm or more and less than 5 cm.
.
1 point: When extruding with a fingertip, it extrudes at a stretch and kneads come out with a length of less than 2 cm.
The average value of the three evaluation points was determined, and the degree of ease of extrusion was determined in the following four stages. The samples with も の and ○ were judged to be dentifrice compositions with excellent ease of extruding the formulation at 50 ° C storage.
◎: 3.5 points or more and 4.0 points or less ○: 3.0 points or more and less than 3.5 points △: 2.0 points or more and less than 3.0 points ×: Less than 2.0 points

(5) Evaluation method of liquid separation stability 50 g of the dentifrice composition was filled in the above laminate tube, each of the three compositions was stored at 50 ° C. for 1 month, and then the 10 cm dentifrice composition was extruded onto a straw half paper to obtain a liquid. Separation stability was evaluated in the following four stages.
◎: No liquid separation ○: Little liquid separation (less than 1 mm)
Δ: Some liquid separation (1 mm or more and less than 5 mm)
X: There is liquid separation (5 mm or more)

＊純分換算した値を示した。

* Values converted to pure content are shown.

＊純分換算した値を示した。

* Values converted to pure content are shown.

  From the results in Tables 1 and 2, the synthetic layered sodium silicate / magnesium or specific granule is inferior in the sense of brushing, whereas inadequate granule is inferior in the sense of brushing or incongruity. In addition, the dentifrice composition of the present invention is excellent in the cleaning power against the dirt on the tooth surface, and it is possible to obtain an actual feeling that the tooth surface is cleaned from the feeling of brushing the tooth surface, and there is no sense of incongruity of the grain, It was easy to extrude when collected in a toothbrush, and the liquid separation stability of the preparation over time was good, and it had excellent quality that satisfied all.

Claims (4)

  (A) Synthetic layered sodium silicate / magnesium, (B) granules having an average particle size of 50 to 400 μm and an average disintegration strength of 10 to 200 g / piece, (C) abrasive silica, and (D) anions A dentifrice characterized by comprising an adhesive binder, wherein the content of the component (B) is 1 to 5% by mass and the content of the component (D) is 0.2 to 0.5% by mass. Composition.   (B) component is dicalcium phosphate, tricalcium phosphate, water-insoluble calcium metaphosphate, silica, aluminum hydroxide, magnesium phosphate, bengara, calcium carbonate, calcium pyrophosphate, zeolite, aluminosilicate, magnesium carbonate, zirconosilicate, The dentifrice composition according to claim 1, wherein the dentifrice composition is a particle formed by granulating one or more water-insoluble powders selected from calcium sulfate.   The dentifrice composition according to claim 1 or 2, wherein the component (D) is one or more anionic binders selected from sodium alginate, sodium polyacrylate, sodium carboxymethylcellulose, xanthan gum, and carrageenan.   The dentifrice composition according to claim 1, 2 or 3, wherein (A) / (D) is 5 to 25 by mass ratio.