JP2015124161A - Dentifrice - Google Patents

Dentifrice Download PDF

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JP2015124161A
JP2015124161A JP2013268335A JP2013268335A JP2015124161A JP 2015124161 A JP2015124161 A JP 2015124161A JP 2013268335 A JP2013268335 A JP 2013268335A JP 2013268335 A JP2013268335 A JP 2013268335A JP 2015124161 A JP2015124161 A JP 2015124161A
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granule
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dentifrice
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JP6316586B2 (en
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厚子 千葉
Atsuko Chiba
厚子 千葉
義徳 村上
Yoshinori Murakami
義徳 村上
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Kao Corp
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Kao Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a dentifrice with which dirt on teeth such as dental plaque and stained dirt can be effectively removed over the entire surface of teeth where recesses of various sizes or a narrow gap between curved surfaces exists.SOLUTION: There is provided the dentifrice that contains 5 mass% or more to 40 mass% or less of granules (A) each of which has a particle diameter of 39 μm or more and which have a collapse strength of 15 gf/piece or more to 50 gf/piece or less and are composed of the following granules: (a1) a granule with a particle diameter of 39 μm or more to less than 78 μm, (a2) a granule with a particle diameter of 78 μm or more to less than 116 μm, (a3) a granule with a particle diameter of 116 μm or more to less than 152 μm, (a4) a granule with a particle diameter of 152 μm or more to less than 200 μm, (a5) a granule with a particle diameter of 200 μm or more, the volume ratio (a2/a3) of the content of the granule (a2) and granule (a3) being 0.5 or more to 2 or less, and the volume ratio (a4/a3) of the content of the granule (a4) and granule (a3) being 0.2 or more to 2 or less, and that further contains (B) a polisher.

Description

本発明は、顆粒を含有する歯磨剤に関する。   The present invention relates to a dentifrice containing granules.

従来より、歯磨剤に顆粒を配合することによって、歯の表面や歯と歯の間の汚れ除去能を高められることが知られており、種々の顆粒が用いられている。例えば、特許文献1には、崩壊強度が10〜200g/個、平均粒子径が50〜150μmで、かつ90%粒子径と平均粒子径の差が100μm以下である顆粒を含有する歯磨組成物が記載されている。   Conventionally, it has been known that by adding granules to a dentifrice, the surface of the teeth and the ability to remove dirt between teeth can be enhanced, and various granules are used. For example, Patent Document 1 discloses a dentifrice composition containing granules having a disintegration strength of 10 to 200 g / piece, an average particle size of 50 to 150 μm, and a difference between the 90% particle size and the average particle size of 100 μm or less. Have been described.

国際公開第2006/003989号International Publication No. 2006/003989

こうしたなか、近年における食生活や生活習慣等の変化に伴い、口腔内環境の悪化を引き起こす要因も増大しつつあるため、近心唇面溝、中央隆線及び遠心唇面溝部等、大小様々な凹凸が散在する歯の表面において多種多様の汚れが堅固に付着し、残存しやすい状況下にある。残存した歯の汚れは着色の原因にもなり得るため、口腔内環境を清潔にしつつ白く美しい歯を保つうえで、歯の汚れを十分に除去し得る歯磨剤が益々強く望まれている。   Under these circumstances, with recent changes in eating habits and lifestyle habits, factors causing deterioration of the oral environment are also increasing, so there are various sizes such as the mesial lip groove, central ridge and centrifugal lip groove. A wide variety of stains are firmly attached to the surface of the tooth with unevenness and are likely to remain. Since the remaining tooth stains can cause coloring, a dentifrice that can sufficiently remove the tooth stains is strongly desired in order to keep white and beautiful teeth while keeping the oral environment clean.

しかしながら、特許文献1に記載された顆粒は、比較的硬い上に一定の平均粒径において粒径分布がシャープであるため、通常の歯磨き時間では、歯の表面に存在する一部の凹部や歯茎との境目近傍の歯の表面に、着色汚れが十分に取り除かれずに付着したままとなる。したがって、こうした通常の歯磨き行為によっても、様々な大きさの歯の表面に存在する凹部に起因して残る着色汚れのみならず、歯と歯の間や歯と歯茎の境目のように、曲面と曲面に阻まれた狭小な歯の表面に残る着色汚れをも効率よく除去することが望まれる。   However, since the granule described in Patent Document 1 is relatively hard and has a sharp particle size distribution at a constant average particle size, some of the recesses and gums present on the tooth surface during normal brushing time. The colored dirt remains attached to the surface of the tooth near the boundary without being sufficiently removed. Therefore, even with such normal tooth brushing, not only colored stains remaining due to the concave portions present on the surface of various sizes of teeth, but also curved surfaces such as between teeth and between teeth and gums. It is desirable to efficiently remove colored stains remaining on the surface of a narrow tooth blocked by a curved surface.

こうしたなか、本発明者らにより、歯の表面に残る僅かな着色汚れは、従来の歯磨剤に含有される顆粒では、歯の表面に存在する様々な大きさを有する凹部や曲面と曲面に阻まれた狭小な部位に十分に対応できないために、歯磨後もなお付着したままとなることに起因すると判明した。また、特に特定の大きさを有する凹部に付着した汚れを除去することが困難であることも、大きな要因であることが判明した。   Under these circumstances, the present inventors have confirmed that slight coloring stains remaining on the tooth surface are blocked by concaves, curved surfaces and curved surfaces having various sizes existing in the tooth surface in the granules contained in the conventional dentifrice. It was found that it was caused by the fact that it remained attached even after dentifrice, because it was not able to cope with the narrow and narrow site. In addition, it has been found that the fact that it is difficult to remove the dirt adhering to the concave portion having a specific size is also a major factor.

したがって、本発明は、大小様々な大きさの凹部や曲面と曲面に阻まれた狭小な部位が存在する歯の表面全域にわたり、付着した歯垢や着色汚れ等の汚れを効果的に除去することのできる歯磨剤に関する。   Therefore, the present invention effectively removes dirt such as adhering plaque and colored dirt over the entire surface of the tooth where there are concave portions of various sizes and curved surfaces and narrow portions blocked by curved surfaces. It relates to a dentifrice that can be used.

そこで本発明者らは、特定の粒径範囲にある顆粒が特定の含有量で存在する顆粒、すなわち特定の粒度分布を有する顆粒であって、特定の崩壊強度を有する顆粒を特定量で用いつつ、研磨剤を併用することにより、歯の表面において特に除去することが困難であった特定の大きさを有する凹部に付着した汚れのみならず、近心唇面溝、中央隆線及び遠心唇面溝部等をも含む大小様々な微小な凹部や、歯と歯の間及び歯と歯茎の境目にまで至る歯の表面全域にわたって、歯垢や着色汚れ等の汚れを十分に除去することのできる歯磨剤が得られることを見出した。   Therefore, the present inventors have used a granule in which a granule in a specific particle size range is present in a specific content, that is, a granule having a specific particle size distribution and having a specific disintegration strength in a specific amount. In addition to the dirt adhering to the concave portion having a specific size, which was difficult to remove particularly on the tooth surface by using an abrasive together, the mesial lip groove, the central ridge, and the centrifugal lip face Toothpaste that can sufficiently remove dirt such as plaque and colored stains across the entire surface of the teeth, including small and large concave portions including grooves, etc., and between the teeth and the boundary between the teeth and gums. It was found that an agent can be obtained.

すなわち、本発明は、(A)粒径が39μm以上であって、次の顆粒(a1)〜(a5):
(a1)粒径が39μm以上78μm未満の顆粒
(a2)粒径が78μm以上116μm未満の顆粒
(a3)粒径が116μm以上152μm未満の顆粒
(a4)粒径が152μm以上200μm未満の顆粒
(a5)粒径が200μm以上の顆粒
からなり、顆粒(a2)及び顆粒(a3)の含有量の体積比(a2/a3)が0.5以上2以下であり、顆粒(a4)及び顆粒(a3)の含有量の体積比(a4/a3)が0.2以上2以下であり、かつ崩壊強度が15gf/個以上50gf/個以下である顆粒 5質量%以上40質量%以下、並びに
(B)研磨剤
を含有する歯磨剤に関する。
That is, in the present invention, (A) the particle size is 39 μm or more, and the following granules (a1) to (a5):
(A1) Granule having a particle size of 39 μm or more and less than 78 μm (a2) Granule having a particle size of 78 μm or more and less than 116 μm (a3) Granule having a particle size of 116 μm or more and less than 152 μm (a4) Granule having a particle size of 152 μm or more and less than 200 μm ) It consists of granules having a particle size of 200 μm or more, the volume ratio (a2 / a3) of the contents of granules (a2) and granules (a3) is 0.5 or more and 2 or less, and granules (a4) and granules (a3) 5% by mass or more and 40% by mass or less of granules having a volume ratio (a4 / a3) of 0.2 to 2 and a disintegration strength of 15 to 50 gf / unit, and (B) polishing The present invention relates to a dentifrice containing an agent.

本発明の歯磨剤によれば、従来の顆粒を含有する歯磨剤では取り除くことが困難であった、大小様々な凹部や、歯と歯の間及び歯と歯茎の境目にまで至る歯の表面全域にわたり、通常の歯磨き行為によっても、歯の表面に付着した汚れを十分に除去することができる。   According to the dentifrice of the present invention, it is difficult to remove with a dentifrice containing conventional granules, and the entire surface of the tooth that reaches various gaps between the teeth and between the teeth and the boundary between the teeth and gums, which is difficult to remove. In addition, the dirt adhering to the tooth surface can be sufficiently removed even by a normal brushing action.

実施例1〜2、4〜6で用いた顆粒A1〜A2、A4〜6の粒度分布を示すグラフである。It is a graph which shows the particle size distribution of granule A1-A2 and A4-6 used in Examples 1-2, 4-6. 比較例2〜3、5で用いた顆粒A7〜A8、A11の粒度分布を示すグラフである。It is a graph which shows the particle size distribution of granule A7-A8, A11 used by Comparative Examples 2-3, 5. 汚れ除去性能の評価で用いた汚れモデルとして油性マジックを塗布した顎模型を示す撮影画像である。It is the picked-up image which shows the jaw model which apply | coated the oil-based magic as a dirt model used by evaluation of dirt removal performance. 図2(a)は、実施例4におけるブラッシング後に撮影した顎模型を示す撮影画像であり、図2(b)は、比較例2におけるブラッシング後に撮影した顎模型を示す撮影画像である。2A is a photographed image showing a jaw model photographed after brushing in Example 4, and FIG. 2B is a photographed image showing a jaw model photographed after brushing in Comparative Example 2. ブラッシング前における着色部位の面積、及びブラッシング後における着色部位の面積(汚れ残存面積(mm2))を示すグラフである。It is a graph which shows the area of the coloring site | part before brushing, and the area (stained residual area (mm < 2 >)) of the coloring site | part after brushing.

以下、本発明について詳細に説明する。
本発明の歯磨剤は、(A)粒径が39μm以上であって、次の顆粒(a1)〜(a5):
(a1)粒径が39μm以上78μm未満の顆粒
(a2)粒径が78μm以上116μm未満の顆粒
(a3)粒径が116μm以上152μm未満の顆粒
(a4)粒径が152μm以上200μm未満の顆粒
(a5)粒径が200μm以上の顆粒
からなり、顆粒(a2)及び顆粒(a3)の含有量の体積比(a2/a3)が0.5以上2以下であり、顆粒(a4)及び顆粒(a3)の含有量の体積比(a4/a3)が0.2以上2以下であり、かつ崩壊強度が15gf/個以上50gf/個以下である顆粒 5質量%以上40質量%以下、並びに
(B)研磨剤
を含有する。
Hereinafter, the present invention will be described in detail.
The dentifrice of the present invention has (A) a particle size of 39 μm or more, and the following granules (a1) to (a5):
(A1) Granule having a particle size of 39 μm or more and less than 78 μm (a2) Granule having a particle size of 78 μm or more and less than 116 μm (a3) Granule having a particle size of 116 μm or more and less than 152 μm (a4) Granule having a particle size of 152 μm or more and less than 200 μm ) It consists of granules having a particle size of 200 μm or more, the volume ratio (a2 / a3) of the contents of granules (a2) and granules (a3) is 0.5 or more and 2 or less, and granules (a4) and granules (a3) 5% by mass or more and 40% by mass or less of granules having a volume ratio (a4 / a3) of 0.2 to 2 and a disintegration strength of 15 to 50 gf / unit, and (B) polishing Contains agents.

本発明の歯磨剤は、様々な大きさの顆粒からなる顆粒(A)を含有することにより、従来の顆粒を含有する歯磨剤では十分に除去し得なかった歯の表面における特定の大きさを有する凹部、例えば前歯の表面において視認できる唇面溝等の凹部へ、各顆粒が相互作用をもたらしつつ入り込み、付着する汚れを有効に除去することができる。なかでも、特に歯の表面に存在する幅200μm未満の大きさの凹部は、通常歯ブラシのブリッスル先端の直径が約200μmであって、歯磨剤に含有される粉体の平均粒径が5〜13μmであることから、ブリッスル先端が届きにくく汚れが残存しがちであったところ、本発明の歯磨剤であれば、かかる凹部に強固に付着した汚れをも有効に除去することができる。
なお、本発明の歯磨剤中にかかる顆粒(A)を含有させため、歯磨剤に配合する顆粒を、以下「原料顆粒」とも称する。
The dentifrice of the present invention contains granules (A) composed of granules of various sizes, so that the specific size on the tooth surface that cannot be sufficiently removed by the dentifrice containing conventional granules can be obtained. It is possible to effectively remove dirt adhered to each concave portion, for example, a concave portion such as a lip groove that can be visually recognized on the surface of the front teeth, while allowing each granule to interact. Among them, in particular, a recess having a width of less than 200 μm present on the tooth surface usually has a bristle tip diameter of about 200 μm, and the average particle size of the powder contained in the dentifrice is 5 to 13 μm. Therefore, when the tip of the bristle is difficult to reach and dirt tends to remain, the dentifrice of the present invention can effectively remove even the dirt firmly adhered to the recess.
In addition, since the granule (A) is contained in the dentifrice of the present invention, the granule blended in the dentifrice is hereinafter also referred to as “raw granule”.

顆粒(A)は、全ての粒子の粒径が39μm以上であって、顆粒(a1)〜(a5)からなり、これらの顆粒が特定の含有量を保持している。すなわち、本発明の歯磨剤が含有する顆粒(A)は、特定の粒度分布を有している。具体的には、顆粒(a2)と顆粒(a3)の含有量の体積比(a2/a3)が0.5以上2以下であり、顆粒(a4)と顆粒(a3)の含有量の体積比(a4/a3)が0.2以上2以下である。このような顆粒(A)の粒度分布は、粒径78μm以上200μm未満の顆粒をバランスよく含有する。具体的には、粒径78μm以上200μm未満において、顆粒(a2)、顆粒(a3)、顆粒(a4)を同程度の含有量になるブロードな粒度分布であるか、或いは顆粒(a2)と顆粒(a3)を同程度含み、顆粒(a4)を顆粒(a2)のおよそ半分程度含むブロードな粒度分布であるか、また或いは顆粒(a2)と顆粒(a4)にピークを有しつつ全体にブロードな粒度分布であるため、特に歯ブラシのブリッスルが届きにくい200μm未満の大きさの凹部にも顆粒(a2)〜(a4)が相互作用しながら入り込むことが可能になると考えられる。   The granules (A) have a particle size of 39 μm or more, and are composed of granules (a1) to (a5), and these granules retain a specific content. That is, the granule (A) contained in the dentifrice of the present invention has a specific particle size distribution. Specifically, the volume ratio (a2 / a3) of the content of the granule (a2) and the granule (a3) is 0.5 or more and 2 or less, and the volume ratio of the content of the granule (a4) and the granule (a3) (A4 / a3) is 0.2 or more and 2 or less. The particle size distribution of such granules (A) contains granules having a particle size of 78 μm or more and less than 200 μm in a well-balanced manner. Specifically, it has a broad particle size distribution in which the granule (a2), the granule (a3), and the granule (a4) have the same content in a particle size of 78 μm or more and less than 200 μm, or the granule (a2) and the granule It is a broad particle size distribution containing the same amount of (a3) and about half of the granule (a4) of the granule (a2), or broadly having a peak in the granule (a2) and the granule (a4). Therefore, it is considered that the granules (a2) to (a4) can enter the recesses having a size of less than 200 μm, which is difficult to reach the bristles of the toothbrush, while interacting with each other.

顆粒(A)は、粒径39μm以上78μm未満の大きさの顆粒(a1)を含有する。顆粒(a1)の含有量は、より大きな顆粒(a2)〜(a5)との相互作用により、幅100μm未満の凹部にも入り込み、汚れを除去する観点から、顆粒(A)中に、好ましくは2体積%以上であり、より好ましくは5体積%以上であり、さらに好ましくは10体積%以上である。顆粒(a1)の含有量は、顆粒(a2)〜(a4)の含有量とのバランスを良好に保持して、歯ブラシのブリッスルが届きにくい幅200μm未満の凹部において強固に付着する汚れを除去する観点から、顆粒(A)中に、好ましくは40体積%以下であり、より好ましくは30体積%以下であり、さらに好ましくは20体積%以下である。また、顆粒(a1)の含有量は、好ましくは2〜40体積%であり、より好ましくは5〜30体積%であり、さらに好ましくは10〜20体積%である。   The granules (A) contain granules (a1) having a particle size of 39 μm or more and less than 78 μm. The content of the granule (a1) is preferably in the granule (A) from the viewpoint of entering a recess having a width of less than 100 μm and removing dirt by interaction with the larger granule (a2) to (a5). It is 2 volume% or more, More preferably, it is 5 volume% or more, More preferably, it is 10 volume% or more. The content of the granule (a1) maintains a good balance with the content of the granules (a2) to (a4), and removes the dirt that adheres firmly in the recesses with a width of less than 200 μm that the toothbrush bristle is difficult to reach. From the viewpoint, the content in the granule (A) is preferably 40% by volume or less, more preferably 30% by volume or less, and still more preferably 20% by volume or less. The content of the granule (a1) is preferably 2 to 40% by volume, more preferably 5 to 30% by volume, and still more preferably 10 to 20% by volume.

顆粒(A)は、粒径78μm以上116μm未満の大きさの顆粒(a2)を含有する。顆粒(a2)の含有量は、顆粒(a1)、及び顆粒(a3)〜(a5)との相互作用により、幅150μm未満の凹部にも入り込み汚れを除去する観点から、顆粒(A)中に、好ましくは15体積%以上であり、より好ましくは18体積%以上である。顆粒(a2)の含有量は、顆粒(a3)及び顆粒(a4)の含有量とのバランスを良好に保持して歯ブラシのブリッスルが届きにくい幅200μm未満の凹部において強固に付着する汚れを除去する観点から、顆粒(A)中に、好ましくは40体積%以下であり、より好ましくは35体積%以下である。また、顆粒(a2)の含有量は、好ましくは15〜40体積%であり、より好ましくは18〜35体積%である。   The granule (A) contains a granule (a2) having a particle size of 78 μm or more and less than 116 μm. The content of the granule (a2) is determined in the granule (A) from the viewpoint of removing dirt by entering the concave portion having a width of less than 150 μm by the interaction with the granule (a1) and the granules (a3) to (a5). , Preferably it is 15 volume% or more, More preferably, it is 18 volume% or more. The content of the granule (a2) maintains a good balance between the content of the granule (a3) and the content of the granule (a4), and removes dirt that adheres firmly in the concave portion with a width of less than 200 μm that the bristle of the toothbrush is difficult to reach. From the viewpoint, it is preferably 40% by volume or less, more preferably 35% by volume or less in the granule (A). The content of the granule (a2) is preferably 15 to 40% by volume, more preferably 18 to 35% by volume.

顆粒(A)は、粒径116μm以上152μm未満の大きさの顆粒(a3)を含有する。顆粒(a3)の含有量は、顆粒(a1)〜(a2)、及び顆粒(a4)〜(a5)との相互作用により、幅200μm未満の凹部にも入り込み汚れを除去する観点から、顆粒(A)中に、好ましくは12体積%以上であり、より好ましくは18体積%以上である。
顆粒(a3)の含有量は、顆粒(a2)及び顆粒(a4)の含有量とのバランスを良好に保持して歯ブラシのブリッスルが届きにくい幅200μm未満の凹部において強固に付着する汚れを除去する観点から、顆粒(A)中に、好ましくは40体積%以下であり、より好ましくは32体積%以下である。また、顆粒(a3)の含有量は、好ましくは12〜40体積%であり、より好ましくは18〜32体積%である。
The granule (A) contains a granule (a3) having a particle size of 116 μm or more and less than 152 μm. The content of the granule (a3) is from the viewpoint of removing dirt by entering into a recess having a width of less than 200 μm by interaction with the granules (a1) to (a2) and the granules (a4) to (a5). In A), it is preferably 12% by volume or more, more preferably 18% by volume or more.
The content of the granule (a3) maintains a good balance between the content of the granule (a2) and the content of the granule (a4), and removes dirt that adheres firmly in the concave portion with a width of less than 200 μm that the toothbrush bristle is difficult to reach. From the viewpoint, the content in the granule (A) is preferably 40% by volume or less, more preferably 32% by volume or less. The content of the granule (a3) is preferably 12 to 40% by volume, more preferably 18 to 32% by volume.

顆粒(A)は、粒径152μm以上200μm未満の大きさの顆粒(a4)を含有する。顆粒(a4)の含有量は、幅200μm未満の凹部に顆粒(a2)、顆粒(a3)とともに顆粒(a4)を入り込ませ、かかる凹部における強固に付着する汚れを除去する観点から、顆粒(A)中に、好ましくは5体積%以上であり、より好ましくは8体積%以上であり、好ましくは10体積%以上である。顆粒(a4)の含有量は、顆粒(a2)及び顆粒(a3)の含有量とのバランスを良好に保持して、歯ブラシのブリッスルが届きにくい幅200μm未満の凹部における強固に付着する汚れを除去する観点から、顆粒(A)中に、好ましくは40体積%以下であり、より好ましくは37体積%以下であり、さらに好ましくは25体積%以下であり、よりさらに好ましくは20体積%以下である。また、顆粒(a4)の含有量は、好ましくは5〜40体積%であり、より好ましくは8〜37体積%であり、さらに好ましくは8〜25体積%であり、よりさらに好ましくは10〜20体積%である。   The granule (A) contains a granule (a4) having a particle size of 152 μm or more and less than 200 μm. The content of the granule (a4) is from the viewpoint of allowing the granule (a4) to enter the concave portion having a width of less than 200 μm together with the granule (a2) and the granule (a3), and removing the firmly adhered dirt in the concave portion. ) Is preferably 5% by volume or more, more preferably 8% by volume or more, and preferably 10% by volume or more. The content of the granules (a4) maintains a good balance with the contents of the granules (a2) and granules (a3), and removes the dirt that adheres firmly in the recesses with a width of less than 200 μm that the toothbrush bristle is difficult to reach. From the viewpoint of, in the granule (A), it is preferably 40% by volume or less, more preferably 37% by volume or less, further preferably 25% by volume or less, and still more preferably 20% by volume or less. . The content of the granule (a4) is preferably 5 to 40% by volume, more preferably 8 to 37% by volume, still more preferably 8 to 25% by volume, and still more preferably 10 to 20%. % By volume.

顆粒(A)は、粒径200μm以上の大きさの顆粒(a5)を含有する。顆粒(a5)の含有量は、歯ブラシのブリッスルの応力を受けて、顆粒(a1)〜(a4)を幅200μm未満の凹部まで有効に到達させる観点から、顆粒(A)中に、好ましくは0.5体積%以上であり、より好ましくは1体積%以上である、顆粒(a5)の含有量は、歯ブラシのブリッスルが届きにくい幅200μm未満の凹部における汚れを除去しうる顆粒(a1)〜(a4)の含有量とのバランスを確保する観点、及び為害性を抑制する観点から、顆粒(A)中に、好ましくは40体積%以下であり、より好ましくは35体積%以下である。また、顆粒(a5)の含有量は、好ましくは0.5〜40体積%であり、より好ましくは1〜35体積%である。   The granule (A) contains a granule (a5) having a particle size of 200 μm or more. The content of the granules (a5) is preferably 0 in the granules (A) from the viewpoint of effectively reaching the granules (a1) to (a4) to the recesses with a width of less than 200 μm under the stress of the toothbrush bristle. The content of the granule (a5) is 5% by volume or more, more preferably 1% by volume or more. The content of the granules (a1) to (a1) to (a1) to (a1) to (a1) From the viewpoint of securing a balance with the content of a4) and from the viewpoint of suppressing harmful effects, the content in the granule (A) is preferably 40% by volume or less, more preferably 35% by volume or less. Moreover, content of a granule (a5) becomes like this. Preferably it is 0.5-40 volume%, More preferably, it is 1-35 volume%.

顆粒(a2)及び顆粒(a3)の含有量の体積比(a2/a3)は、歯の表面に多く存在する幅100μm以下の凹部に付着した汚れまで効果的に除去し、さらに唇面溝等の深い凹部に付着した汚れをも除去する観点から、0.5以上であって、好ましくは0.8以上であり、2以下であって、好ましくは1.5以下であり、より好ましくは1.2以下である。このように顆粒(a2)と顆粒(a3)の含有量の体積比(a2/a3)が1:2〜2:1、すなわちこれらの顆粒が同程度の量であることにより、歯磨き後の汚れ除去性能を視覚により実感することができる。また、顆粒(a2)及び顆粒(a3)の含有量の体積比(a2/a3)は、0.5以上2以下であって、好ましくは0.8〜1.5であり、より好ましくは0.8〜1.2である。   The volume ratio (a2 / a3) of the content of the granules (a2) and granules (a3) effectively removes dirt adhering to the recesses with a width of 100 μm or less present on the surface of the tooth, and further, the lip groove, etc. From the standpoint of removing dirt adhering to deep concave portions of the film, it is 0.5 or more, preferably 0.8 or more, 2 or less, preferably 1.5 or less, more preferably 1 .2 or less. Thus, the volume ratio (a2 / a3) of the content of the granule (a2) and the granule (a3) is 1: 2 to 2: 1, that is, the amount of these granules is the same amount, so that the dirt after brushing The removal performance can be felt visually. The volume ratio (a2 / a3) of the content of the granules (a2) and granules (a3) is 0.5 or more and 2 or less, preferably 0.8 to 1.5, more preferably 0. .8 to 1.2.

なお、本発明の顆粒(A)は、崩壊強度が15gf/個以上の崩壊しにくい顆粒であることから、幅100μm以下の凹部には、100μm以下の径のこれらの顆粒が集合して入り込むことにより、かかる凹部に付着した汚れに一定の圧力をかけながら除去することができると考えられる。   In addition, since the granule (A) of the present invention is a granule that is not easily disintegrated having a disintegration strength of 15 gf / piece or more, these granules having a diameter of 100 μm or less gather and enter into a recess having a width of 100 μm or less. Thus, it is considered that the dirt attached to the concave portion can be removed while applying a certain pressure.

顆粒(a4)及び顆粒(a3)の含有量の体積比(a4/a3)は、歯の表面に多く存在し、しかも歯ブラシのブリッスルが届きにくい幅200μm未満の凹部に付着した汚れまで効果的に除去し、さらに唇面溝等の深い凹部に付着した汚れをも除去する観点から、0.2以上であって、好ましくは0.25以上であり、より好ましくは0.3以上であり、2以下であって、好ましくは1.2以下であり、より好ましくは1以下である。また、顆粒(a4)及び顆粒(a3)の含有量の体積比(a4/a3)は、0.2以上2以下であって、好ましくは0.25〜1.2であり、より好ましくは0.3〜1である。   The volume ratio (a4 / a3) of the content of the granules (a4) and granules (a3) is abundant on the surface of the teeth and is effective even for dirt adhering to a recess having a width of less than 200 μm that is difficult for the toothbrush bristle to reach. From the viewpoint of removing and further removing dirt adhering to deep recesses such as lip grooves, it is 0.2 or more, preferably 0.25 or more, more preferably 0.3 or more, 2 Or less, preferably 1.2 or less, more preferably 1 or less. The volume ratio (a4 / a3) of the content of the granules (a4) and the granules (a3) is 0.2 or more and 2 or less, preferably 0.25 to 1.2, more preferably 0. .3-1.

顆粒(a1)及び顆粒(a3)の含有量の体積比(a1/a3)は、幅100μm以下の凹部に入り込む顆粒(a1)と、かかる凹部に顆粒(a1)を押し込むと考えられる顆粒(a3)とのバランスを確保する観点から、好ましくは0.1以上であり、より好ましくは0.5以上であり、好ましくは1.5以下であり、より好ましくは1以下である。また、顆粒(a1)及び顆粒(a3)の含有量の体積比(a1/a3)は、好ましくは0.1〜1.5であり、より好ましくは0.5〜1である。   The volume ratio (a1 / a3) of the content of the granule (a1) and the granule (a3) is as follows: a granule (a1) that enters a recess having a width of 100 μm or less, and a granule (a3) that is considered to push the granule (a1) into the recess From the viewpoint of securing a balance with (), it is preferably 0.1 or more, more preferably 0.5 or more, preferably 1.5 or less, more preferably 1 or less. The volume ratio (a1 / a3) of the content of the granules (a1) and granules (a3) is preferably 0.1 to 1.5, more preferably 0.5 to 1.

なお、顆粒(A)及び顆粒(A)を得るために配合される原料顆粒の粒度分布は、レーザ回折/散乱式粒子径分布測定によるものであり、歯磨組成物中に含有される顆粒(A)の場合には、歯磨き剤をイオン交換水により10質量%に希釈した水溶液を用いて測定し、原料顆粒の場合には、イオン交換水により5質量%に希釈した水溶液を用いて測定する。より具体的には、顆粒(A)が含有される歯磨組成物をイオン交換水により10質量%に希釈した水溶液(又は原料顆粒をイオン交換水により5質量%に希釈した水溶液)を、ミキサー(ROTARY MIXER NPC-20、NISSIN社製)により、75回転/分、水平方向回転、2時間の条件で顆粒を分散させる。次いで、顆粒(A)が含有される分散後の歯磨組成物を希釈して得た水溶液(又は原料顆粒を分散した水溶液)を、室温(25℃)で1日保存する。かかる保存後の水溶液を、再度上記ミキサーにより10分間分散させた後、当該水溶液を用いて、レーザ回折/散乱式粒度分布測定装置(Partica LA-950V2、HORIBA社製)にて、屈折率:1.54、循環速度(目盛:2)、撹拌速度(目盛:3)の条件で測定する。   In addition, the particle size distribution of the raw material granule mix | blended in order to obtain a granule (A) and a granule (A) is based on the laser diffraction / scattering type particle size distribution measurement, and the granule (A In the case of), the dentifrice is measured using an aqueous solution diluted to 10% by mass with ion-exchanged water, and in the case of raw material granules, it is measured using an aqueous solution diluted to 5% by mass with ion-exchanged water. More specifically, an aqueous solution obtained by diluting a dentifrice composition containing granules (A) to 10% by mass with ion-exchanged water (or an aqueous solution in which raw material granules are diluted to 5% by mass with ion-exchanged water) is mixed with a mixer ( ROTARY MIXER NPC-20 (manufactured by NISSIN) is used to disperse the granules under conditions of 75 rotations / minute, horizontal rotation, 2 hours. Next, an aqueous solution (or an aqueous solution in which the raw material granules are dispersed) obtained by diluting the dispersed dentifrice composition containing the granules (A) is stored at room temperature (25 ° C.) for 1 day. The aqueous solution after storage was again dispersed for 10 minutes by the mixer, and then the aqueous solution was used to measure a refractive index of 1 with a laser diffraction / scattering particle size distribution analyzer (Partica LA-950V2, manufactured by HORIBA). .54, measured under conditions of circulation rate (scale: 2), stirring speed (scale: 3).

本発明の歯磨剤における顆粒(A)は、少なくとも平均粒径50μm以上120μm未満の原料顆粒(x)と、原料顆粒(x)よりも平均粒径が大きい原料顆粒(y)とを含む2種以上の原料顆粒を配合して得ることが好ましい。原料顆粒(y)の平均粒径は、顆粒(A)における顆粒(a2)、(a3)、(a4)の含有量のバランスの観点から、好ましくは120μm以上200μm以下であり、より好ましくは130〜160μmである。原料顆粒(x)の平均粒径は、同様の観点から、50μm以上120μm未満であって、好ましくは60〜120μmであり、より好ましくは60〜100μmである。
原料顆粒(x)と原料顆粒(y)の配合量の質量比(x/y)は、好ましくは0.5〜2であり、より好ましくは0.7〜1.5である。
The granule (A) in the dentifrice of the present invention includes at least two raw material granules (x) having an average particle size of 50 μm or more and less than 120 μm and raw material granules (y) having an average particle size larger than that of the raw material granules (x). It is preferable to obtain by blending the above raw material granules. The average particle diameter of the raw material granules (y) is preferably 120 μm or more and 200 μm or less, more preferably 130 from the viewpoint of the balance of the contents of the granules (a2), (a3), and (a4) in the granules (A). ˜160 μm. From the same viewpoint, the average particle size of the raw material granules (x) is 50 μm or more and less than 120 μm, preferably 60 to 120 μm, more preferably 60 to 100 μm.
The mass ratio (x / y) of the blending amount of the raw material granules (x) and the raw material granules (y) is preferably 0.5 to 2, more preferably 0.7 to 1.5.

本発明の歯磨剤において、顆粒(A)の崩壊強度は、歯の表面の幅200μm以下の凹部における強固に付着した汚れを除去する観点から、15gf/個以上であって、好ましくは20gf/個以上であり、より好ましくは25gf/個以上であり、顆粒による異物感や為害性を抑制する観点から、50gf/個以下であって、好ましくは40gf/個以下であり、より好ましくは35gf/個以下である。   In the dentifrice of the present invention, the disintegration strength of the granule (A) is 15 gf / piece or more, preferably 20 gf / piece, from the viewpoint of removing strongly adhered dirt in the recess having a width of 200 μm or less on the tooth surface. More preferably, it is 25 gf / piece or more, and from the viewpoint of suppressing foreign matter sensation and harmfulness due to granules, it is 50 gf / piece or less, preferably 40 gf / piece or less, more preferably 35 gf / piece. It is as follows.

本発明における顆粒(A)の崩壊強度とは、乾燥状態で測定したときの値であって、歯磨組成物中から10個〜20個の顆粒(A)を取り出し、圧縮試験機(島津製作所、MCTM−500)を用いて、粒径(180〜200μm)の顆粒を荷重速度1.51gf/秒で圧縮して崩壊したときの荷重を顆粒ごとに測定し、求めた平均値である。なお、本発明で用いる顆粒(A)において、乾燥状態における崩壊強度と湿潤状態における崩壊強度とは同じ値である。   The disintegration strength of the granules (A) in the present invention is a value when measured in a dry state, and 10 to 20 granules (A) are taken out from the dentifrice composition, and a compression tester (Shimadzu Corporation, MCTM-500) is a mean value obtained by measuring the load of each granule having a particle size (180 to 200 μm) at a load rate of 1.51 gf / sec and measuring the collapse for each granule. In the granule (A) used in the present invention, the disintegration strength in the dry state and the disintegration strength in the wet state are the same value.

本発明における顆粒(A)は、粒径39μm以上の粒子であって、かかる粒径はレーザ回折/散乱式粒子径分布測定によるものである一方、同様にレーザ回折/散乱式粒子径分布測定による粒径39μm未満の大きさの粒子は、後述する研磨剤(B)に相当する。   The granule (A) in the present invention is a particle having a particle size of 39 μm or more, and the particle size is determined by laser diffraction / scattering particle size distribution measurement, and similarly by laser diffraction / scattering particle size distribution measurement. Particles having a particle size of less than 39 μm correspond to an abrasive (B) described later.

本発明の歯磨剤における顆粒(A)の含有量は、歯ブラシのブリッスルが届きにくい幅200μm未満の凹部に顆粒(a1)〜(a4)を有効に入り込ませ、これらの凹部に付着している汚れを効果的に除去する観点から、本発明の歯磨剤中に5質量%以上であって、好ましくは7質量%以上であり、より好ましくは10質量%以上である。本発明の歯磨剤における顆粒(A)の含有量は、粉っぽさの発現や、構造粘性による口腔内における歯磨剤の分散性の低下を防止する観点から、本発明の歯磨剤中に40質量%以下であって、好ましくは35質量%以下であり、より好ましくは30質量%以下である。   The content of the granules (A) in the dentifrice of the present invention is such that the granules (a1) to (a4) are effectively allowed to enter the recesses having a width of less than 200 μm that are difficult to reach the bristle of the toothbrush, and the stains adhering to these recesses From the viewpoint of effectively removing the amount, the dentifrice of the present invention contains 5% by mass or more, preferably 7% by mass or more, and more preferably 10% by mass or more. The content of the granule (A) in the dentifrice of the present invention is 40 in the dentifrice of the present invention from the viewpoint of preventing the expression of powderiness and the decrease in dispersibility of the dentifrice in the oral cavity due to structural viscosity. It is not more than mass%, preferably not more than 35 mass%, more preferably not more than 30 mass%.

顆粒(A)は、上記含有量の顆粒(a1)〜(a5)からなり、かつ上記崩壊強度を有するものであれば、材質や造粒方法等は特に制限されず、顆粒(A)、或いは各顆粒(a1)〜(a5)として、転動造粒、押し出し造粒、圧縮造粒、破砕造粒、撹拌造粒、流動層造粒、噴霧乾燥造粒、溶融凝固造粒等の公知の方法を用いて造粒した顆粒を用いることができる。具体的には、例えば、炭酸カルシウム、シリカ、水酸化アルミニウム、ゼオライト等の研磨性紛体を、ワックス、パラフィン、ステアリン酸等の無機結合剤を用いて結着させることにより得られる顆粒;結合剤を用いない炭酸カルシウム微粒子を凝集させたり複合化させたりすることにより得られる顆粒;シリカを凝集させるゲル法、沈降法等の湿式法又は噴霧造粒法により得られる顆粒が挙げられる。   The granule (A) is not particularly limited as long as it is composed of the granules (a1) to (a5) having the above contents and has the above-described disintegration strength, and the granules (A) or As each granule (a1) to (a5), known as rolling granulation, extrusion granulation, compression granulation, crushing granulation, stirring granulation, fluidized bed granulation, spray drying granulation, melt solidification granulation, etc. Granules granulated using the method can be used. Specifically, for example, granules obtained by binding an abrasive powder such as calcium carbonate, silica, aluminum hydroxide, and zeolite using an inorganic binder such as wax, paraffin, and stearic acid; Granules obtained by agglomerating or complexing calcium carbonate fine particles that are not used; granules obtained by a wet method such as a gel method or a sedimentation method for agglomerating silica, or a spray granulation method.

顆粒(A)における粒度分布の調整方法としては、各粒径範囲にある顆粒に分粒し、分粒した顆粒を適宜混合することにより得ることができる。また、粒度分布の異なる顆粒を2種以上混合することによっても得ることができる。   As a method for adjusting the particle size distribution in the granule (A), it can be obtained by sizing into granules in each particle size range and appropriately mixing the sized granules. It can also be obtained by mixing two or more types of granules having different particle size distributions.

本発明の歯磨剤は、顆粒(A)以外に研磨剤(B)を含有する。研磨剤(B)は、顆粒(A)以外の粒径39μm未満の顆粒や粒子、すなわち粒径39μm未満の粉体や造粒物であり、例えば、研磨性シリカ、炭酸カルシウム、ゼオライト、リン酸カルシウム、ポリエチレン粉末、ナイロン粉末、及びポリプロピレン粉末等から選ばれる1種又は2種以上が挙げられる。なかでも、研磨剤(B)は、味及び清掃性の観点から、研磨性シリカ、及び炭酸カルシウムから選ばれる1種又は2種以上が好ましい。   The dentifrice of the present invention contains an abrasive (B) in addition to the granules (A). The abrasive (B) is a granule or particle having a particle size of less than 39 μm other than the granule (A), that is, a powder or granulated product having a particle size of less than 39 μm. For example, abrasive silica, calcium carbonate, zeolite, calcium phosphate, Examples thereof include one or more selected from polyethylene powder, nylon powder, polypropylene powder, and the like. Among these, the abrasive (B) is preferably one or more selected from abrasive silica and calcium carbonate from the viewpoints of taste and cleanability.

顆粒(A)と研磨剤(B)の含有量の合計は、清掃性能と使用感の観点から、本発明の歯磨剤中に、好ましくは8質量%以上であり、より好ましくは15質量%以上であり、好ましくは50質量%以下であり、より好ましくは45質量%以下であり、さらに好ましくは40質量%以下である。   The total content of the granule (A) and the abrasive (B) is preferably 8% by mass or more, more preferably 15% by mass or more in the dentifrice of the present invention, from the viewpoint of cleaning performance and usability. Preferably, it is 50 mass% or less, More preferably, it is 45 mass% or less, More preferably, it is 40 mass% or less.

水の含有量は、剤形等に応じて適宜設定することができるが、顆粒(A)やその他の成分の分散性を高め、特定の大きさを有する凹部のみならず、大小様々な微小な凹部や、歯と歯の間及び歯と歯茎の境目にまで至る歯の表面全域にわたり、付着汚れ除去効果を十分に発揮させる観点から、本発明の歯磨剤中に、好ましくは0質量%を超え、より好ましくは10質量%以上であり、さらに好ましくは15質量%以上である。水の含有量は、ブラッシングによって負荷される荷重を顆粒(A)に効率的に伝達し、良好に崩壊させる観点から、本発明の歯磨剤中に、好ましくは60質量%以下であり、より好ましくは50質量%以下である。また、水の含有量は、本発明の歯磨剤中に、好ましくは0質量%を超え60質量%以下であり、より好ましくは10〜50質量%であり、さらに好ましくは15〜50質量%である。   The water content can be appropriately set according to the dosage form, etc., but it increases the dispersibility of the granules (A) and other components, and not only the recesses having a specific size, but also small and large sizes. In the dentifrice of the present invention, it preferably exceeds 0% by mass from the viewpoint of sufficiently exerting the effect of removing adhering stains over the entire surface of the tooth extending from the recess, between the teeth and to the boundary between the teeth and the gums. More preferably, it is 10 mass% or more, More preferably, it is 15 mass% or more. The water content is preferably 60% by mass or less, more preferably in the dentifrice of the present invention, from the viewpoint of efficiently transmitting the load applied by brushing to the granules (A) and causing good disintegration. Is 50 mass% or less. The water content in the dentifrice of the present invention is preferably more than 0% by mass and 60% by mass or less, more preferably 10-50% by mass, and further preferably 15-50% by mass. is there.

本発明の歯磨剤中における水の含有量(水分量)は、配合した水分量及び配合した成分中の水分量から計算によって算出することもできるが、例えばカールフィッシャー水分計で測定することができる。カールフィッシャー水分計としては、例えば、微量水分測定装置(平沼産業(株))を用いることができる。この装置では、歯磨剤を5gとり、無水メタノール25gに懸濁させ、この懸濁液0.02gを分取して水分量を測定することができる。   The water content (moisture content) in the dentifrice of the present invention can be calculated from the blended moisture content and the moisture content in the blended component, but can be measured, for example, with a Karl Fischer moisture meter. . 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.

本発明の歯磨剤には、本発明の効果を阻害しない範囲で、上記成分のほか、例えば、アルギン酸ナトリウム、カルボキシメチルセルロースナトリウム、カラギーナン、キサンタンガム等の粘結剤;グリセリン、ソルビトール、プロピレングリコール、キシリトール、マルチトール、ラクチトール、エリスリトール等の湿潤剤;サッカリンナトリウム、アスパルテーム等の甘味剤;リン酸、クエン酸、リンゴ酸及びこれらの塩等のpH調整剤;N−アシルグルタミン酸塩やN−ラウロイルサルコシンナトリウム等のN−アシルアミノ酸塩、アルキル硫酸エステル塩、ポリオキシアルキルリン酸塩等のアニオン界面活性剤;ショ糖脂肪酸エステル、ポリオキシエチレン硬化ヒマシ油、ポリグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル等のノニオン界面活性剤やその他の界面活性剤;フッ化ナトリウム、フッ化カリウム、フッ化スズ、モノフルオロリン酸ナトリウム、モノフルオロリン酸カリウム等のフッ化物;β−グリチルレチン酸又はその塩、トコフェロール、トリクロサン、及びイソプロピルメチルフェノール等の油溶性有効成分;パラオキシ安息香酸エチル等の防腐剤;香料等を適宜含有させることができる。   In the dentifrice of the present invention, in addition to the above components, for example, a binder such as sodium alginate, sodium carboxymethylcellulose, carrageenan, xanthan gum; glycerin, sorbitol, propylene glycol, xylitol, Wetting agents such as maltitol, lactitol, erythritol; sweeteners such as saccharin sodium and aspartame; pH adjusters such as phosphoric acid, citric acid, malic acid and their salts; N-acyl glutamate and sodium N-lauroyl sarcosine Anionic surfactants such as N-acyl amino acid salt, alkyl sulfate ester salt, polyoxyalkyl phosphate salt; sucrose fatty acid ester, polyoxyethylene hydrogenated castor oil, polyglycerin fatty acid ester, sorbitan fatty acid ester, etc. Nonionic surfactants and other surfactants; fluorides such as sodium fluoride, potassium fluoride, tin fluoride, sodium monofluorophosphate, potassium monofluorophosphate; β-glycyrrhetinic acid or salts thereof, tocopherol, triclosan And oil-soluble active ingredients such as isopropylmethylphenol; preservatives such as ethyl paraoxybenzoate;

本発明の歯磨剤は、ゲル歯磨、練り歯磨、粉歯磨などの各種歯磨剤とすることができる。なかでも、特定の大きさを有する凹部のみならず、大小様々な微小な凹部や、歯と歯の間及び歯と歯茎の境目にまで至る歯の表面全域にわたり、付着汚れを有効に除去する顆粒(A)の効果を十分に享受する観点から、ゲル歯磨、練り歯磨剤とすることが好適である。   The dentifrice of the present invention can be various dentifrices such as gel dentifrice, toothpaste and powder dentifrice. Above all, not only concaves with a specific size, but also fine concaves of various sizes and granules that effectively remove attached dirt over the entire tooth surface between teeth and between the teeth and gums. From the viewpoint of fully enjoying the effect of (A), it is preferable to use gel dentifrice and toothpaste.

以下、本発明について、実施例に基づき具体的に説明する。なお、表中に特に示さない限り、各成分の含有量は質量%を示す。
なお、以下の方法にしたがって、各測定を行なった。
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%.
Each measurement was performed according to the following method.

《原料顆粒及び顆粒(A)の崩壊強度の測定》
180〜200μmの顆粒を10個〜20個抽出し、微小圧縮試験機(島津製作所、MCTM―500)を用いて、荷重速度1.51gf/秒で圧縮して崩壊したときの荷重を顆粒ごとに測定し、平均値を求めた。
<< Measurement of Collapse Strength of Raw Granules and Granules (A) >>
Extract 10 to 20 granules of 180 to 200 μm and use a micro-compression tester (Shimadzu Corporation, MCTM-500) to compress the load at a load speed of 1.51 gf / sec. The average value was obtained by measurement.

《原料顆粒の粒度分布及び含有量(体積%)の測定》
原料顆粒をイオン交換水により5質量%に希釈した水溶液を用いて測定した。原料顆粒をイオン交換水により5質量%に希釈した水溶液を、ミキサー(ROTARY MIXER NPC-20、NISSIN社製)により、75回転/分、水平方向回転、2時間の条件で顆粒を分散させた。次いで、顆粒を分散した水溶液を、室温(25℃)で1日保存した。かかる保存後の水溶液を、再度上記ミキサーにより10分間分散させた後、当該水溶液を用いて、レーザ回折/散乱式粒度分布測定装置(Partica LA-950V2、HORIBA社製)にて、屈折率:1.54、循環速度(目盛:2)、撹拌速度(目盛:3)の条件で測定した。なお、溶媒としてはイオン交換水を用いた。
<< Measurement of particle size distribution and content (volume%) of raw material granules >>
It measured using the aqueous solution which diluted the raw material granule with ion-exchange water to 5 mass%. An aqueous solution obtained by diluting the raw material granules with ion-exchanged water to 5% by mass was dispersed with a mixer (ROTARY MIXER NPC-20, manufactured by NISSIN) under conditions of 75 rotations / minute, horizontal rotation, and 2 hours. Next, the aqueous solution in which the granules were dispersed was stored at room temperature (25 ° C.) for 1 day. The aqueous solution after storage was again dispersed for 10 minutes by the mixer, and then the aqueous solution was used to measure a refractive index of 1 with a laser diffraction / scattering particle size distribution analyzer (Partica LA-950V2, manufactured by HORIBA). .54, circulation rate (scale: 2), stirring speed (scale: 3). In addition, ion-exchange water was used as a solvent.

《顆粒(A)の粒度分布及び含有量(体積%)の測定の測定》
(ii)粒度分布、平均粒子径及び量の測定:得られた粉体及び顆粒(A)を、レーザ回折/散乱式粒子径分布測定装置(Partica LA-950V2、HORIBA社製)を用いて、屈折率:1.54、循環速度(目盛:2)、撹拌速度(目盛:3)の条件で測定した。溶媒としてはイオン交換水を用いた。
なお、本発明において、レーザ回折/散乱式粒子分布測定装置により測定された粒度分布から、各粒径の範囲の顆粒(a1)〜(a5)の含有量(体積%)を計算した。具体的には、レーザ回折により測定された各粒径の範囲について、各粒径の範囲の含有量を合計することにより顆粒(a1)〜(a5)の量を計算した。例えば、レーザ回折による、粒径39μm以上45μm未満の顆粒が0.5体積%、45μm以上51μm未満の顆粒が2.5体積%、51μm以上59μm未満の顆粒が3.0体積%、59μ以上68μm未満の顆粒が3.2体積%、68μm以上78μm未満の顆粒が3.5体積%である場合には、顆粒(a1)の含有量は、0.5体積%+2.5体積%+3.0体積%+3.2体積%+3.5体積%であり、計算結果は12.7体積%となる。
<< Measurement of particle size distribution and content (volume%) measurement of granules (A) >>
(Ii) Measurement of particle size distribution, average particle size and amount: The obtained powder and granule (A) were measured using a laser diffraction / scattering particle size distribution measuring device (Partica LA-950V2, manufactured by HORIBA). The measurement was performed under the conditions of refractive index: 1.54, circulation speed (scale: 2), and stirring speed (scale: 3). Ion exchange water was used as the solvent.
In the present invention, the content (volume%) of granules (a1) to (a5) in the range of each particle size was calculated from the particle size distribution measured by a laser diffraction / scattering particle distribution measuring device. Specifically, the amount of granules (a1) to (a5) was calculated by summing the contents of each particle size range for each particle size range measured by laser diffraction. For example, 0.5% by volume of granules having a particle size of 39 μm or more and less than 45 μm, 2.5% by volume of granules having a particle size of 45 μm or more and less than 51 μm, 3.0% by volume of granules having a particle size of 51 μm or more but less than 59 μm, The content of the granule (a1) is 0.5% by volume + 2.5% by volume + 3.0% when the less than 3.2% by volume and the less than 68 μm to less than 78 μm is 3.5% by volume. Volume% + 3.2% by volume + 3.5% by volume, and the calculation result is 12.7% by volume.

[調製例1:顆粒(A)の調製]
原料顆粒として、表1に示す顆粒1〜6を用い、表2に示す処方に従って顆粒(A1)〜顆粒(A11)を調製した。なお、表2における各顆粒1〜7の配合量は、合計(質量部)を基準とする質量部で示す。
[Preparation Example 1: Preparation of granules (A)]
Granules (A1) to (A11) were prepared according to the formulation shown in Table 2 using granules 1 to 6 shown in Table 1 as raw material granules. In addition, the compounding quantity of each granule 1-7 in Table 2 is shown by the mass part on the basis of the sum total (mass part).

[実施例1〜6、比較例1〜5]
製造例1で得られた顆粒を用い、表4に示す処方(合計100質量%とする含有量(質量%)で示す)にしたがって、各歯磨剤を製造した。次いで、得られた歯磨剤を用い、下記方法にしたがって、顆粒の粒度分布及び含有量(体積%)を測定し、汚れ除去性能の評価を行った。
顆粒の粒度分布及び含有量(体積%)の結果を表3に示し、汚れ除去性能の評価結果を表4に示す。
[Examples 1-6, Comparative Examples 1-5]
Using the granules obtained in Production Example 1, each dentifrice was produced according to the formulation shown in Table 4 (indicated by the content (mass%) to be 100 mass% in total). Subsequently, using the obtained dentifrice, according to the following method, the particle size distribution and content (volume%) of the granule were measured, and the soil removal performance was evaluated.
The results of the particle size distribution and content (% by volume) of the granules are shown in Table 3, and the evaluation results of the dirt removal performance are shown in Table 4.

また、実施例1〜2、4〜6で用いた顆粒A1〜A2、A4〜6の粒度分布のグラフを図1に示し、比較例2〜3、5で用いた顆粒A7〜A8、A11の粒度分布のグラフを図2に示す。
さらに、汚れ除去性能の評価で用いた汚れモデルとして油性マジック(マッキーケア:ゼブラ製)を塗布した顎模型の撮影画像を図3に示すとともに、ブラッシング後に撮影した顎模型の撮影画像を図4に示す(図4(a):実施例4、図4(b):比較例2)
また、ブラッシング前における着色部位の面積、及びブラッシング後における着色部位の面積(汚れ残存面積(mm2)のグラフを図5に示す。
Moreover, the graph of the particle size distribution of granule A1-A2, A4-6 used in Examples 1-2, 4-6 is shown in FIG. 1, and granules A7-A8, A11 used in Comparative Examples 2-3, 5 are shown in FIG. A graph of the particle size distribution is shown in FIG.
Further, FIG. 3 shows a photographed image of a jaw model coated with oil-based magic (Mackey Care: manufactured by Zebra) as a dirt model used in the evaluation of dirt removal performance, and FIG. 4 shows a photographed image of the jaw model photographed after brushing. (FIG. 4 (a): Example 4, FIG. 4 (b): Comparative example 2)
Further, FIG. 5 shows a graph of the area of the colored portion before brushing and the area of the colored portion after brushing (dirt remaining area (mm 2 )).

[歯磨剤における汚れ除去性能の評価]
顎模型(スタディモデル:SRP用顎模型:D16FE−500H(GSF)−QF Nissin製)を用い、上下前歯4本(計8本)の表面に、汚れモデルとして油性マジック(マッキーケア:ゼブラ製)を塗布し、5分間自然乾燥させた。
次いで、得られた各歯磨剤1gを歯ブラシ(チェックスタンダード:花王製)にとり、約200g重の荷重にて1歯につき10秒間、歯科衛生士の手でブラッシングを行い、下記方法にしたがって、汚れ残存面積(mm2)を算出して汚れ除去性能の評価の指標とした。
[Evaluation of dirt removal performance of dentifrice]
Using a jaw model (Study model: SRP jaw model: D16FE-500H (GSF) -QF made by Nissin), oily magic (Mackey Care: made by Zebra) Was applied and allowed to air dry for 5 minutes.
Next, 1 g of each obtained dentifrice is taken on a toothbrush (Check Standard: manufactured by Kao), brushed by the hand of a dental hygienist for 10 seconds per tooth under a load of about 200 g, and dirt remains according to the following method. The area (mm 2 ) was calculated and used as an index for evaluating the dirt removal performance.

《汚れ残存面積(mm2)の算出方法》
ブラッシングした後、顎模型の歯8本を取り外し、水洗いした後に、紙タオル(エリエール プロワイプ ソフトタオル)を用いて歯の表面に残存する水分及び歯磨剤を除去した。
次いで、デジタルカメラによりブラッシング後の顎模型を撮影した画像を元に、画像解析ソフト「WinROOF」(三谷商事株式会社)を用いて着色部位の面積を求め、汚れ残存面積(mm2)とした。かかる汚れ残存面積(mm2)の値が小さいほど、汚れ除去性能が高いことを意味する。
なお、予めブラッシング前における各顎模型をデジタルカメラで撮影し、各顎模型間で着色面積に差がないことを確認した。
<< Calculation method of residual area of dirt (mm 2 ) >>
After brushing, 8 teeth of the jaw model were removed, washed with water, and then water and dentifrice remaining on the tooth surface were removed using a paper towel (Erière Prowipe soft towel).
Next, based on an image obtained by photographing the jaw model after brushing with a digital camera, the area of the colored portion was obtained using image analysis software “WinROOF” (Mitani Corporation), and was defined as the remaining area (mm 2 ). It means that the smaller the value of the remaining area (mm 2 ), the higher the dirt removal performance.
In addition, each jaw model before brushing was image | photographed with the digital camera previously, and it confirmed that there was no difference in a coloring area between each jaw model.

上記結果によれば、実施例1〜6の歯磨剤は、比較例1〜5の歯磨剤に比して、汚れ除去能が高いことがわかる。   According to the said result, it turns out that the dentifrice of Examples 1-6 has high dirt removal ability compared with the dentifrice of Comparative Examples 1-5.

得られた顆粒A1〜A6を用い、下記に示す処方にしたがって、実施例1と同様にして各歯磨剤を得た。   Each dentifrice was obtained like Example 1 using the obtained granule A1-A6 according to the prescription shown below.

[実施例7〜12]

顆粒A1〜A6 各々10
カルボキシメチルセルロースナトリウム 1.0
キサンタンガム 0.2
カラギーナン 0.1
ラウリル硫酸ナトリウム 1.5
プロピレングリコール 5.0
ソルビトール液(70%) 23.0
増粘性シリカ 7.0
研磨性シリカ 15.0
リンゴ酸 1.1
リン酸一水素二ナトリウム・12水和物 0.5
水酸化カリウム 0.73
水酸化ナトリウム 0.11
フッ化ナトリウム 0.21
モノステアリン酸ポリオキシエチレンソルビタン 0.3
サッカリンナトリウム 0.13
酸化チタン 0.3
香料 1.0
精製水 残部
[Examples 7 to 12]

Granules A1 to A6 each 10
Sodium carboxymethylcellulose 1.0
Xanthan gum 0.2
Carrageenan 0.1
Sodium lauryl sulfate 1.5
Propylene glycol 5.0
Sorbitol solution (70%) 23.0
Thickening silica 7.0
Abrasive silica 15.0
Malic acid 1.1
Disodium monohydrogen phosphate 12 hydrate 0.5
Potassium hydroxide 0.73
Sodium hydroxide 0.11
Sodium fluoride 0.21
Polyoxyethylene sorbitan monostearate 0.3
Saccharin sodium 0.13
Titanium oxide 0.3
Fragrance 1.0
Purified water balance

Claims (6)

(A)粒径が39μm以上であって、次の顆粒(a1)〜(a5):
(a1)粒径が39μm以上78μm未満の顆粒
(a2)粒径が78μm以上116μm未満の顆粒
(a3)粒径が116μm以上152μm未満の顆粒
(a4)粒径が152μm以上200μm未満の顆粒
(a5)粒径が200μm以上の顆粒
からなり、顆粒(a2)及び顆粒(a3)の含有量の体積比(a2/a3)が0.5以上2以下であり、顆粒(a4)及び顆粒(a3)の含有量の体積比(a4/a3)が0.2以上2以下であり、かつ崩壊強度が15gf/個以上50gf/個以下である顆粒 5質量%以上40質量%以下、並びに
(B)研磨剤
を含有する歯磨剤。
(A) The particle size is 39 μm or more, and the following granules (a1) to (a5):
(A1) Granule having a particle size of 39 μm or more and less than 78 μm (a2) Granule having a particle size of 78 μm or more and less than 116 μm (a3) Granule having a particle size of 116 μm or more and less than 152 μm (a4) Granule having a particle size of 152 μm or more and less than 200 μm ) It consists of granules having a particle size of 200 μm or more, the volume ratio (a2 / a3) of the contents of granules (a2) and granules (a3) is 0.5 or more and 2 or less, and granules (a4) and granules (a3) 5% by mass or more and 40% by mass or less of granules having a volume ratio (a4 / a3) of 0.2 to 2 and a disintegration strength of 15 to 50 gf / unit, and (B) polishing Dentifrice containing an agent.
顆粒(a3)の含有量が、顆粒(A)中に12体積%以上40体積%以下である請求項1に記載の歯磨剤。   The dentifrice of Claim 1 whose content of a granule (a3) is 12 volume% or more and 40 volume% or less in a granule (A). 顆粒(A)と研磨剤(B)の含有量の合計が、7質量%以上50質量%以下である請求項1又は2に記載の歯磨剤。   The dentifrice of Claim 1 or 2 whose sum total of content of a granule (A) and abrasive | polishing agent (B) is 7 to 50 mass%. 顆粒(a1)及び顆粒(a3)の含有量の体積比(a1/a3)が、0.1以上1.5以下である請求項1〜3のいずれか1項に記載の歯磨剤。   The dentifrice of any one of Claims 1-3 whose volume ratio (a1 / a3) of content of a granule (a1) and a granule (a3) is 0.1 or more and 1.5 or less. 顆粒(A)が、少なくとも平均粒径50μm以上120μm未満の原料顆粒(x)と、原料顆粒(x)よりも平均粒径が大きい原料顆粒(y)を含む2種以上の原料顆粒を配合して得られる請求項1〜4のいずれか1項に記載の歯磨剤。   The granule (A) is composed of at least two raw material granules including a raw material granule (x) having an average particle size of 50 μm or more and less than 120 μm and a raw material granule (y) having an average particle size larger than that of the raw material granule (x). The dentifrice of any one of Claims 1-4 obtained by these. 原料顆粒(y)の平均粒径が、120μm以上200μm以下である請求項1〜5のいずれか1項に記載の歯磨剤。   The dentifrice according to any one of claims 1 to 5, wherein the raw material granules (y) have an average particle size of 120 µm or more and 200 µm or less.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01299211A (en) * 1988-05-25 1989-12-04 Kao Corp Dentifrice
JPH04243816A (en) * 1991-01-28 1992-08-31 Kao Corp Granule agent and composition for oral cavity containing the same agent
JP2007126421A (en) * 2005-11-07 2007-05-24 Kao Corp Composition for oral cavity application
JP2010275260A (en) * 2009-05-29 2010-12-09 Kao Corp Toothpaste
JP2011011998A (en) * 2009-06-30 2011-01-20 Kao Corp Granule for dentifrice
JP2011121916A (en) * 2009-12-11 2011-06-23 Kao Corp Dentifrice composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01299211A (en) * 1988-05-25 1989-12-04 Kao Corp Dentifrice
JPH04243816A (en) * 1991-01-28 1992-08-31 Kao Corp Granule agent and composition for oral cavity containing the same agent
JP2007126421A (en) * 2005-11-07 2007-05-24 Kao Corp Composition for oral cavity application
JP2010275260A (en) * 2009-05-29 2010-12-09 Kao Corp Toothpaste
JP2011011998A (en) * 2009-06-30 2011-01-20 Kao Corp Granule for dentifrice
JP2011121916A (en) * 2009-12-11 2011-06-23 Kao Corp Dentifrice composition

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