JP6807729B2 - Toothpaste granules and dentifrice composition containing them - Google Patents
Toothpaste granules and dentifrice composition containing them Download PDFInfo
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- JP6807729B2 JP6807729B2 JP2016248879A JP2016248879A JP6807729B2 JP 6807729 B2 JP6807729 B2 JP 6807729B2 JP 2016248879 A JP2016248879 A JP 2016248879A JP 2016248879 A JP2016248879 A JP 2016248879A JP 6807729 B2 JP6807729 B2 JP 6807729B2
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- dentifrice
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 229940070802 palmitoyl glutamate Drugs 0.000 description 1
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- 229920001277 pectin Polymers 0.000 description 1
- 208000028169 periodontal disease Diseases 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
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- 229920001296 polysiloxane Polymers 0.000 description 1
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- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
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- 229940071089 sarcosinate Drugs 0.000 description 1
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- 235000010413 sodium alginate Nutrition 0.000 description 1
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- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 description 1
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- 235000019351 sodium silicates Nutrition 0.000 description 1
- UPUIQOIQVMNQAP-UHFFFAOYSA-M sodium;tetradecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCOS([O-])(=O)=O UPUIQOIQVMNQAP-UHFFFAOYSA-M 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
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- 230000008719 thickening Effects 0.000 description 1
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- 230000036346 tooth eruption Effects 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- 239000000080 wetting agent Substances 0.000 description 1
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Description
本発明は、歯磨剤用顆粒及びこれを含有する歯磨剤組成物に関する。 The present invention relates to dentifrice granules and a dentifrice composition containing the same.
歯面に歯垢や着色汚れ等の種々の汚れ（歯垢等）が付着すると、虫歯や歯周病等の原因となり得ることから、こうした歯垢等を効率よく除去し、或いはこれら歯垢等の形成や付着を未然に防止すべく、種々の成分を用いた歯磨剤の技術が開発されている。このようななか、歯磨剤に顆粒を配合することによっても歯垢等の除去能を効果的に高め得ることから、薬剤、酵素剤、研磨剤等の成分を顆粒と併用した歯磨剤や、特定の物性を付与した顆粒を用いた歯磨剤も多々開発されている。 If various stains (plaque, etc.) such as plaque and colored stains adhere to the tooth surface, they may cause tooth decay and periodontal disease. Therefore, such plaque, etc. can be efficiently removed, or these plaques, etc. Techniques for dentifrices using various components have been developed to prevent the formation and adhesion of plaque. Under these circumstances, the ability to remove plaque and the like can be effectively enhanced by adding granules to the dentifrice. Therefore, dentifrices in which components such as chemicals, enzymes, and abrasives are used in combination with the granules, and specific dentifrices Many dentifrices using granules with physical properties have also been developed.
例えば、特許文献１には、特定の成分を含有し、荷重の負荷に対して特有の崩壊挙動を示す歯磨剤用顆粒が開示されており、歯と歯の隙間のような狭小な領域に至るまで、歯垢等の除去効果を高めるとともに、つるつる感や汚れ落ち感の向上も図っている。 For example, Patent Document 1 discloses dentifrice granules containing a specific component and exhibiting a peculiar disintegration behavior with respect to a load, and reach a narrow region such as a gap between teeth. In addition to enhancing the effect of removing plaque, etc., we are also trying to improve the feeling of slipperiness and dirt removal.
一方、歯面に歯垢等が付着するのを未然に防止する技術の開発も試みられている。例えば、特許文献２には、脂肪酸塩を配合した歯面コート剤が開示されており、かかる脂肪酸塩によって歯面コート作用を発揮させ、細菌によって産生される酸から歯面を守り、歯への菌や食べカスの付着防止効果を高めている。 On the other hand, attempts have been made to develop a technique 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, which exerts a tooth surface coating action, protects the tooth surface from acids produced by bacteria, and applies to teeth. It enhances the effect of preventing the adhesion of bacteria and food waste.
しかしながら、特許文献１に記載の技術を用いることによって、一旦歯面に付着した歯垢等を有効に除去し得たとしても、時間が経過するにつれ、或いはその後に飲食等を繰り返すにつれ、再び歯面にこれら歯垢等が形成されるのを充分に回避できないおそれがある。また、仮に特許文献２に記載の技術を用いたとしても、歯面に脂肪酸塩が良好に吸着した状態を維持し、歯面への歯垢等の形成抑制効果を充分に持続させるには、依然として改善を要する状況にある。 However, even if the plaque and the like once adhering to the tooth surface can be effectively removed by using the technique described in Patent Document 1, the teeth are re-emerged as time elapses or as eating and drinking is repeated thereafter. It may not be possible to sufficiently avoid the formation of these plaques and the like on the surface. Further, even if the technique described in Patent Document 2 is used, in order to maintain a state in which fatty acid salts are well adsorbed on the tooth surface and sufficiently maintain the effect of suppressing the formation of plaque or the like on the tooth surface, The situation still needs improvement.
そのため、すでに歯面に堅固に付着した歯垢等に対し、高い除去効果を発揮するだけでなく、かかる歯垢等が再び歯面に形成されるのをも有効に防止することができる技術の実現が強く望まれる。 Therefore, not only is it highly effective in removing plaque and the like that have already adhered firmly to the tooth surface, but it is also possible to effectively prevent such plaque and the like from being formed on the tooth surface again. Realization is strongly desired.
したがって、本発明は、歯面に堅固に付着した歯垢や着色汚れ等（歯垢等）に対し、高い除去効果を発揮するとともに、かかる歯垢等の歯面における形成を有効に抑制することができる歯磨剤用顆粒、及びこれを含有する歯磨剤組成物に関する。 Therefore, the present invention exerts a high removal effect on plaque, colored stains, etc. (dental plaque, etc.) firmly attached to the tooth surface, and effectively suppresses the formation of such plaque on the tooth surface. The present invention relates to dentifrice granules capable of producing dentifrice and a dentifrice composition containing the same.
そこで本発明者は、特定の造粒物に特定の飽和又は不飽和脂肪酸或いはこれらの塩が担持されていながら、特定の平均粒径と崩壊強度を有することにより、すでに歯面に付着した歯垢等の除去効果を高めながら、さらに歯面における歯垢等の形成抑制効果を持続させることのできる歯磨剤用顆粒が得られることを見出した。 Therefore, the present inventor has a specific average particle size and disintegration strength while carrying a specific saturated or unsaturated fatty acid or a salt thereof on a specific granule, so that plaque has already adhered to the tooth surface. It has been found that granules for dentifrice can be obtained, which can enhance the effect of removing plaque and the like and further maintain the effect of suppressing the formation of plaque and the like on the tooth surface.
すなわち、本発明は、次の成分（Ａ）、及び（Ｂ）：
（Ａ）水不溶性粉体材料を含む造粒物、及び
（Ｂ）炭素数１４以上２２以下の、飽和又は不飽和脂肪酸或いはこれらの塩
を含有し、成分（Ａ）に成分（Ｂ）が担持されている顆粒であり、かつ
平均粒径が５０μｍ以上５００μｍ以下であり、崩壊強度が湿潤状態で０．２ｇｆ／個以上３０ｇｆ／個以下である歯磨剤用顆粒に関する。
また、本発明は、上記歯磨剤用顆粒を１質量％以上５０質量％以下含有する歯磨剤組成物に関する。
That is, the present invention describes the following components (A) and (B):
It contains (A) granules containing a water-insoluble powder material, and (B) saturated or unsaturated fatty acids having 14 or more and 22 or less carbon atoms or salts thereof, and the component (B) is supported by the component (A). The present invention relates to granules for dentifrices, which have 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 present invention also relates to a dentifrice composition containing the above-mentioned dentifrice granules in an amount of 1% by mass or more and 50% by mass or less.
本発明の歯磨剤用顆粒によれば、歯面に堅固に付着した歯垢等の除去効果を有効に高めることができるとともに、歯垢等が付着しにくい歯面の状態を充分に維持することができる高い歯垢等の形成抑制効果を発揮することができる。したがって、かかる歯磨剤用顆粒を含有する歯磨剤組成物を用いれば、歯面への歯垢等の再付着を未然に防止することが可能となり、歯面におけるつるつるした感触をも持続させて、良好な使用感をもたらすことができる。
なお、つるつるとした感触とは、歯面を舌でふれたときに、歯垢等が付着しているような感触を得ることなく、歯の表面でなめらかに舌をすべらせることができる感触をいう。
According to the dentifrice granules of the present invention, the effect of removing plaque and the like firmly adhering to the tooth surface can be effectively enhanced, and the state of the tooth surface on which plaque and the like are hard to adhere can be sufficiently maintained. It is possible to exert a high effect of suppressing the formation of plaque and the like. Therefore, by using a dentifrice composition containing such dentifrice granules, it is possible to prevent reattachment of dental plaque or the like to the tooth surface, and the smooth feel on the tooth surface is maintained. It can bring a good feeling of use.
The smooth feel means that when the tooth surface is touched with the tongue, the tongue can be smoothly slid on the surface of the tooth without getting the feeling that plaque or the like is attached. Say.
以下、本発明について詳細に説明する。
本発明の歯磨剤用顆粒は、成分（Ａ）として、水不溶性粉体材料を含む造粒物を含有する。かかる成分（Ａ）の造粒物としては、顆粒状を呈した、粒子又は粉体の集合物や凝集物であればよい。
成分（Ａ）に含まれる水不溶性粉末材料としては、歯の研磨剤として通常用いられる材料が好ましく、具体的には無機材料が好ましい。ここで、「水不溶性」とは、水１００ｇに対する溶解量（２０℃）が１ｇ以下であることを意味する。より具体的には、例えば、軽質炭酸カルシウム、重質炭酸カルシウム、ゼオライト、シリカ、第二リン酸カルシウム、第三リン酸カルシウム、不溶性メタリン酸ナトリウム、水酸化アルミニウム、リン酸マグネシウム、ピロリン酸カルシウム、及び炭酸マグネシウム等から選ばれる１種又は２種以上が挙げられる。
Hereinafter, the present invention will be described in detail.
The dentifrice granule of the present invention contains a granule containing a water-insoluble powder material as the component (A). The granulated product of the component (A) may be an aggregate or agglomerate of particles or powders in the form of granules.
As the water-insoluble powder material contained in the component (A), a material usually used as an abrasive for teeth is preferable, and specifically, an inorganic material is preferable. Here, "water-insoluble" means that the amount dissolved (20 ° C.) in 100 g of water is 1 g or less. More specifically, from, for example, light calcium carbonate, heavy calcium carbonate, zeolite, silica, dicalcium phosphate, tricalcium phosphate, insoluble sodium metaphosphate, aluminum hydroxide, magnesium phosphate, calcium pyrophosphate, magnesium carbonate and the like. One or more selected species may be mentioned.
水不溶性粉末材料の平均粒径は、顆粒崩壊後の歯垢等の除去効果や形成抑制効果を高める観点から、好ましくは０．１μｍ以上であり、より好ましくは０．５μｍ以上である。また、水不溶性粉末材料の平均粒径は、異物感を減じる観点から、好ましくは２０μｍ以下であり、より好ましくは１５μｍ以下であり、さらに好ましくは１０μｍ以下である。そして、水不溶性粉末材料（Ａ）の平均粒径は、好ましくは０．１〜２０μｍであり、より好ましくは０．５〜１５μｍであり、さらに好ましくは０．５〜１０μｍである。平均粒径は、レーザー回折／散乱式粒度分布測定装置により測定することが可能である。 The average particle size 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 size 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. The average particle size of the water-insoluble powder material (A) is preferably 0.1 to 20 μm, more preferably 0.5 to 15 μm, and even more preferably 0.5 to 10 μm. The average particle size can be measured by a laser diffraction / scattering type particle size distribution measuring device.
水不溶性粉末材料の含有量は、段階的な崩壊挙動を付与したり、研磨力を高めたりすることによって、歯垢等の除去効果や形成抑制効果の向上を図る観点から、成分（Ａ）中に、乾燥状態で、好ましくは５０質量％以上であり、より好ましくは６０質量％以上であり、さらに好ましくは７０質量％以上であり、よりさらに好ましくは８０質量％以上であり、好ましくは１００質量％以下であり、或いは成分（Ａ）が後述する無機結合剤を含む場合、好ましくは９５質量％以下であり、より好ましくは９０質量％以下であり、さらに好ましくは８５質量％以下である。そして、水不溶性粉末材料の含有量は、成分（Ａ）が後述する無機結合剤を含む場合において、段階的な崩壊挙動を付与したり、研磨力を高めたりすることによって、歯垢等の除去効果や形成抑制効果の向上を図る観点から、成分（Ａ）中に、好ましくは５０〜９５質量％であり、より好ましくは６０〜９０質量％であり、さらに好ましくは７０〜８５質量％であり、よりさらに好ましくは８０〜８５質量％である。
なお、成分（Ａ）中における、乾燥状態での水不溶性粉末材料の含有量が１００質量％である場合、成分（Ａ）は、後述する無機結合剤が介在することなく、水不溶性粉末材料の粒子又は粉体により形成されてなる顆粒状を呈する凝集物（水不溶性粉末材料の凝集物（ａ１））に相当する。
The content of the water-insoluble powder material is in the component (A) from the viewpoint of improving the effect of removing plaque and the like and the effect of suppressing the formation by imparting a stepwise disintegration behavior and increasing the polishing power. In the 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, and 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 further preferably 85% by mass or less. Then, the content of the water-insoluble powder material is such that when the component (A) contains an inorganic binder described later, plaque and the like are removed by imparting a stepwise disintegration behavior or increasing the polishing power. From the viewpoint of improving the effect and the effect of suppressing formation, the content of 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 80-85% by 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 the water-insoluble powder material without the intervention of an inorganic binder described later. It corresponds to a granular aggregate (aggregate of water-insoluble powder material (a1)) formed of particles or powder.
成分（Ａ）は、さらに無機結合剤を含んでいてもよい。かかる無機結合剤を含む成分（Ａ）は、上記水不溶性粉末材料と無機結合剤とが結合し、成分（Ａ）内に空隙を有しつつ無機結合剤が介在してなり、水不溶性粉末材料の粒子又は粉体により加工又は造粒されてなる顆粒状を呈する造粒物（水不溶性粉末材料と無機結合剤を含有する造粒物（ａ２））に相当する。 The component (A) may further contain an inorganic binder. The component (A) containing such an inorganic binder is a water-insoluble powder material in which the water-insoluble powder material and the inorganic binder are bonded to each other, and the inorganic binder is interposed while having voids in the component (A). Corresponds to a granulated product (granulated product (a2) containing a water-insoluble powder material and an inorganic binder) which is processed or granulated by the particles or powder of the above.
無機結合剤としては、水溶性無機結合剤及び水不溶性無機結合剤から選ばれる１種又は２種以上が挙げられる。水溶性無機結合剤としては、具体的には、珪酸ナトリウム、ポリアクリル酸、粉末セルロースのような加工セルロース類、ポリビニルピロリドン、及びシリコーン等から選ばれる１種又は２種以上が挙げられ、珪酸ナトリウム、粉末セルロースが好ましい。水不溶性無機結合剤としては、具体的には、コロイダルシリカ、メタ珪酸アルミン酸マグネシウム、合成珪酸アルミニウム、珪酸カルシウム、及びアルミナゾル等から選ばれる１種又は２種以上が挙げられ、コロイダルシリカが好ましい。 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 processed celluloses such as sodium silicate, polyacrylic acid and powdered cellulose, polyvinylpyrrolidone, and silicone, and sodium silicate. , Powdered cellulose is preferred. Specific examples of the water-insoluble inorganic binder include one or more selected from colloidal silica, magnesium aluminometasilicate, synthetic aluminum silicate, calcium silicate, and alumina sol, and colloidal silica is preferable.
なかでも、本発明の効果を良好に発揮させる観点から、水溶性無機結合剤を含むことが好ましく、顆粒内に様々な大きさの空隙を散在させつつ、空隙中の水分のｐＨをアルカリ性にして歯垢等の除去効果や形成抑制効果を高める観点、及び歯面におけるつるつる感等の使用感を向上させる観点から、珪酸ナトリウムを含むことがより好ましい。かかる珪酸ナトリウムとしては、メタ珪酸ナトリウム（Ｎａ2ＳｉＯ3）、オルト珪酸ナトリウム（Ｎａ4ＳｉＯ4）、二珪酸ナトリウム（Ｎａ2Ｓｉ2Ｏ5）、四珪酸ナトリウム（Ｎａ2Ｓｉ4Ｏ9）及びそれらの水和物が挙げられる。 Among them, from the viewpoint of satisfactorily exerting the effect of the present invention, it is preferable to contain a water-soluble inorganic binder, and the pH of the water in the voids is made alkaline while the voids of various sizes are scattered in the granules. It is more preferable to contain sodium silicate from the viewpoint of enhancing the effect of removing plaque and the like and the effect of suppressing the formation, and from the viewpoint of improving the feeling of use such as a slippery feeling on the tooth surface. Examples of such sodium silicate 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.
珪酸ナトリウムは、一般にＮａ2Ｏ・ｎＳｉＯ2・ｍＨ2Ｏの分子式で表される。係数ｎ（Ｎａ2Ｏに対するＳｉＯ2の分子比）はモル比と呼ばれ、下記式（Ｉ）で表すことができる。
モル比＝質量比(ＳｉＯ2質量％/Ｎａ2Ｏ質量％)×(Ｎａ2Ｏの分子量/ＳｉＯ2の分子量) ・・・（Ｉ）
珪酸ナトリウムとしては、通常、ＪＩＳ Ｋ１４０８に記載の珪酸ソーダ１号、２号、３号の他、種々のモル比の水ガラスを使用することができるが、なかでも珪酸ソーダ３号がさらに好ましい。
Sodium silicate is generally represented by the molecular formula of Na 2 O, nSiO 2 , mH 2 O. The coefficient n (molecular ratio of SiO 2 to Na 2 O) is called a molar ratio and can be expressed by the following formula (I).
Mol ratio = mass ratio (SiO 2 mass% / Na 2 O mass%) × (Na 2 O molecular weight / SiO 2 molecular weight) ・ ・ ・ (I)
As the sodium silicate, in addition to the sodium silicates No. 1, No. 2 and No. 3 described in JIS K1408, water glass having various molar ratios can be usually used, but sodium silicate No. 3 is more preferable.
珪酸ナトリウムの物性は前記モル比（係数ｎ）によって異なるが、医薬部外品原料規格へ適合させる観点、本発明の効果を良好に発揮させる観点、及び得られる歯磨剤用顆粒のｐＨをアルカリ性にする観点から、前記モル比（係数ｎ）は、好ましくは２．０以上であり、より好ましくは２．４以上であり、さらに好ましくは２．８以上であり、またさらに好ましくは３．０以上であり、好ましくは４．０以下であり、より好ましくは３．５以下であり、さらに好ましくは３．４以下であり、またさらに好ましくは３．３以下である。そして、前記モル比（係数ｎ）は、好ましくは２．０〜４．０であり、より好ましくは２．４〜３．５であり、さらに好ましくは２．８〜３．４であり、またさらに好ましくは３．０〜３．３である。 The physical characteristics of sodium silicate differ depending on the molar ratio (coefficient n), but from the viewpoint of conforming to the quasi-drug raw material standard, from the viewpoint of satisfactorily exerting the effect of the present invention, and making the pH of the obtained dentifrice granules alkaline. From this point of view, the molar ratio (coefficient n) is preferably 2.0 or more, more preferably 2.4 or more, still more preferably 2.8 or more, and even more 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. The molar ratio (coefficient n) is preferably 2.0 to 4.0, more preferably 2.4 to 3.5, and even more preferably 2.8 to 3.4. More preferably, it is 3.0 to 3.3.
成分（Ａ）が無機結合剤を含有する場合、かかる無機結合剤の含有量は、粗大粒子を効果的に抑制する観点、及び本発明の歯磨剤用顆粒の崩壊強度を有効に高める観点から、成分（Ａ）中に、好ましくは３０質量％以下であり、より好ましくは２５質量％以下であり、さらに好ましくは２０質量％以下である。また、無機結合剤の含有量は、成分（Ａ）の製造を容易にする観点から、成分（Ａ）中に、好ましくは１質量％以上であり、より好ましくは２質量％以上であり、さらに好ましくは４質量％以上である。そして無機結合剤の含有量は、成分（Ａ）中に、好ましくは１〜３０質量％であり、より好ましくは２〜２５質量％であり、さらに好ましくは４〜２０質量％である。 When the component (A) contains an inorganic binder, the content of the inorganic binder is determined 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 the component (A), it is preferably 30% by mass or less, more preferably 25% by mass or less, and further preferably 20% by mass or less. Further, the content of the inorganic binder is preferably 1% by mass or more, more preferably 2% by mass or more, and further, from the viewpoint of facilitating the production of the component (A). It is preferably 4% by mass or more. The content of the inorganic binder in the component (A) is preferably 1 to 30% by mass, more preferably 2 to 25% by mass, and further preferably 4 to 20% by mass.
また、無機結合剤として珪酸ナトリウムを用いる場合、上記珪酸ナトリウム（固形分）の含有量は、粗大粒子を効果的に抑制する観点、及び本発明の歯磨剤用顆粒の崩壊強度を有効に高める観点から、成分（Ａ）中に、好ましくは２５質量％以下であり、より好ましくは２０質量％以下であり、さらに好ましくは１８質量％以下である。また、珪酸ナトリウム（固形分）の含有量は、成分（Ａ）の製造を容易にする観点から、成分（Ａ）中に、好ましくは１質量％以上であり、より好ましくは２質量％以上であり、さらに好ましくは４質量％以上である。そして、珪酸ナトリウム（固形分）の含有量は、成分（Ａ）中に、好ましくは１〜２５質量％であり、より好ましくは２〜２０質量％であり、さらに好ましくは４〜１８質量％である。 When sodium silicate is used as the inorganic binder, the content of the sodium silicate (solid content) 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. 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. Further, 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, 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.
本発明の歯磨剤用顆粒は、成分（Ｂ）として、炭素数１４以上２２以下の、飽和又は不飽和脂肪酸或いはこれらの塩を含有し、成分（Ａ）に成分（Ｂ）が担持されている。すなわち、成分（Ａ）が水不溶性粉末材料の凝集物（ａ１）であっても、水不溶性粉末材料と無機結合剤を含有する造粒物（ａ２）であっても、かかる成分（Ａ）を形成する粒子間に狭間が存在することから、かかる狭間において成分（Ｂ）が介在するように成分（Ａ）に担持されて、本発明の歯磨剤用顆粒を形成している。そのため、歯磨剤用顆粒中において、成分（Ｂ）を偏在させることなく均一に散在させることができ、また使用時におけるブラッシング等の負荷によって歯磨剤用顆粒が崩壊した際、口腔内で良好に溶融して効率よく均一に歯面へ吸着し、歯垢等が形成又は付着しにくい歯面の状態を充分に維持することができる。さらに、こうした脂肪酸又はその塩により誘発されやすい泡立ちの低下や風味劣化を緩和し、使用感の向上を図ることもできる。 The dentifrice granule of the present invention contains saturated or unsaturated fatty acids having 14 or more and 22 or less carbon atoms or salts thereof as the component (B), and the component (B) is supported by the component (A). .. That is, whether the component (A) is an aggregate (a1) of a water-insoluble powder material or a granule (a2) containing a water-insoluble powder material and an inorganic binder, such a component (A) is used. Since there is a gap between the particles to be formed, the component (B) is supported by the component (A) so as to intervene in the gap to form the dentifrice granule of the present invention. Therefore, the component (B) can be uniformly scattered in the dentifrice granules without being unevenly distributed, and when the dentifrice granules disintegrate due to a load such as brushing during use, the components (B) are satisfactorily melted in the oral cavity. Therefore, it can be efficiently and uniformly adsorbed on the tooth surface, and the state of the tooth surface on which plaque and the like are hard to form or adhere can be sufficiently maintained. Further, it is possible to alleviate the decrease in foaming and the deterioration of flavor which are easily induced by such fatty acids or salts thereof, and to improve the usability.
成分（Ｂ）の炭素数は、使用時におけるブラッシング等の負荷によって歯磨剤用顆粒が崩壊した際に、良好な溶解性を保持する観点から、２２以下であって、好ましくは１８以下であり、より好ましくは１６以下であり、使用時における風味の観点から、１４以上であって、好ましくは１６以上である。 The carbon number of the component (B) is 22 or less, preferably 18 or less, from the viewpoint of maintaining good solubility when the dentifrice granules are disintegrated due to a load such as brushing during use. It is more preferably 16 or less, and from the viewpoint of flavor at the time of use, it is 14 or more, preferably 16 or more.
また、成分（Ｂ）が有する炭化水素基としては、飽和炭化水素基、直鎖炭化水素基、分岐鎖を有する炭化水素基が挙げられ、飽和炭化水素基が好ましく、直鎖飽和炭化水素基がより好ましい。かかる炭化水素基としては、例えば、ミリスチン酸、ペンタデシル酸、パルミチン酸、パルミトレイン酸、ステアリン酸、オレイン酸、リノール酸、リノレン酸等が挙げられ、ミリスチン酸、ペンタデシル酸、パルミチン酸、ステアリン酸が好ましい。なかでも、水への溶解性を確保する観点から、ミリスチン酸、パルミチン酸が好ましく、より風味を良好にする観点から、パルミチン酸が好ましい。 Examples of the hydrocarbon group contained in the component (B) include a saturated hydrocarbon group, a linear hydrocarbon group, and a hydrocarbon group having a branched chain, and a saturated hydrocarbon group is preferable, and a linear saturated hydrocarbon group is preferable. More preferred. Examples of such hydrocarbon groups include myristic acid, pentadecylic acid, palmitic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid and the like, with myristic acid, pentadecylic acid, palmitic acid and stearic acid being preferred. .. Of 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.
なお、成分（Ｂ）として、上記飽和又は不飽和脂肪酸或いはこれらの塩を１種単独で用いてもよく、又は２種以上の飽和又は不飽和脂肪酸或いはこれらの塩を混在させて用いてもよい。 As the component (B), the above-mentioned saturated or unsaturated fatty acids or salts thereof may be used alone, or two or more kinds of saturated or unsaturated fatty acids or salts thereof may be used in combination. ..
成分（Ｂ）の含有量は、成分（Ｂ）を成分（Ａ）に良好に担持させて歯磨剤用顆粒中に均一に散在させる観点、及び歯磨剤用顆粒が崩壊した際における溶融性を確保して歯面への吸着性を高める観点から、成分（Ａ）１００質量部に対し、好ましくは０．１質量部以上であり、より好ましくは４質量部以上であり、さらに好ましくは７質量部以上であり、よりさらに好ましくは１１質量部以上である。また、成分（Ｂ）の含有量は、成分（Ｂ）の成分（Ａ）への担持量が増大するにつれて過度に崩壊強度が高まり、歯磨剤用顆粒の崩壊性までも必要以上に低下してしまうのを回避する観点から、成分（Ａ）１００質量部に対し、好ましくは４０質量部以下であり、より好ましくは３５質量部以下であり、さらに好ましくは３０質量部以下であり、よりさらに好ましくは２５質量部以下である。そして、成分（Ｂ）の含有量は、成分（Ａ）１００質量部に対し、好ましくは０．１〜４０質量部であり、より好ましくは４〜３５質量部であり、さらに好ましくは７〜３０質量部であり、１１〜２５質量部である。 The content of the component (B) ensures that the component (B) is well supported on the component (A) and uniformly scattered in the dentifrice granules, and that the dentifrice granules are meltable when disintegrated. From the viewpoint of enhancing the adsorptivity to the tooth surface, it is preferably 0.1 part 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). The above is more preferably 11 parts by mass or more. In addition, the content of the component (B) excessively increases the disintegration strength as the amount of the component (B) supported on the component (A) increases, and the disintegration property of the dentifrice granules also decreases more than necessary. From the viewpoint of avoiding storage, 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, still more preferably, with respect to 100 parts by mass of the component (A). Is 25 parts by mass or less. The content of the component (B) is preferably 0.1 to 40 parts by mass, more preferably 4 to 35 parts by mass, and further preferably 7 to 30 parts by mass with respect to 100 parts by mass of the component (A). It is a mass part, and is 11 to 25 parts by mass.
また、成分（Ｂ）の含有量は、成分（Ｂ）を成分（Ａ）に良好に担持させて歯磨剤用顆粒中に均一に散在させる観点、及び歯磨剤用顆粒が崩壊した際における溶融性を確保して歯面への吸着性を高める観点から、本発明の歯磨剤顆粒中に、好ましくは１質量％以上であり、より好ましくは４質量％以上であり、さらに好ましくは８質量％以上であり、よりさらに好ましくは１０質量％以上である。また、成分（Ｂ）の含有量は、成分（Ｂ）の成分（Ａ）への担持量が増大するにつれて過度に崩壊強度が高まり、歯磨剤用顆粒の崩壊性までも必要以上に低下してしまうのを回避する観点から、本発明の歯磨剤顆粒中に、好ましくは２５質量％以下であり、より好ましくは２０質量％以下であり、さらに好ましくは１７質量％以下である。そして、成分（Ｂ）の含有量は、本発明の歯磨剤顆粒中に、好ましくは１〜２５質量％であり、より好ましくは４〜２０質量％であり、さらに好ましくは８〜１７質量％であり、よりさらに好ましくは１０〜１７質量％である。 Further, the content of the component (B) is from the viewpoint that the component (B) is well supported on the component (A) and uniformly scattered in the dentifrice granules, and the meltability when the dentifrice granules are disintegrated. In the dentifrice granules of the present invention, preferably 1% by mass or more, more preferably 4% by mass or more, still more preferably 8% by mass or more, from the viewpoint of ensuring the above-mentioned properties and enhancing the adsorptivity to the tooth surface. It is more preferably 10% by mass or more. In addition, the content of the component (B) increases the disintegration strength excessively as the amount of the component (B) carried on the component (A) increases, and the disintegration property of the dentifrice granules also decreases more than necessary. From the viewpoint of avoiding the above, 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 granules of the present invention. 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 granules of the present invention. Yes, and even more preferably 10 to 17% by mass.
本発明の歯磨剤用顆粒は、歯垢形成抑制効果を付与する観点、及び水溶性珪酸塩又はコロイダルシリカによって形成されるネットワーク構造を強化して徐々に崩壊する物性の発現を確保する観点から、さらに珪酸カルシウム、酸化マグネシウム、酸化チタン及び酸化亜鉛から選ばれる１種又は２種以上の結合助剤を含有することが好ましく、酸化亜鉛と他の結合助剤を含むことがさらに好ましい。 The dentifrice granules of the present invention have an effect of suppressing plaque formation, and from the viewpoint of strengthening the network structure formed by water-soluble silicate or colloidal silica to ensure the expression of physical properties that gradually collapse. Further, it is preferable to contain one or more kinds of binding aids selected from calcium silicate, magnesium oxide, titanium oxide and zinc oxide, and it is more preferable to contain zinc oxide and other binding aids.
結合助剤の含有量は、歯垢形成抑制効果と徐々に崩壊する物性を向上する観点から、本発明の歯磨剤用顆粒中に、乾燥状態で好ましくは０．２質量％以上であり、より好ましくは０．５質量％以上であり、さらに好ましくは０．８質量％以上である。また、結合助剤の含有量は、崩壊強度が過剰に高くなることを抑制する観点、本発明の歯磨剤用顆粒を配合した歯磨剤の泡立ちや泡質を向上する観点、及び金属味を抑制する観点から、本発明の歯磨剤用顆粒中に、乾燥状態で好ましくは５質量％以下であり、より好ましくは３質量％以下であり、さらに好ましくは２質量％以下である。また、結合助剤の含有量は、本発明の歯磨剤用顆粒中に、乾燥状態で好ましくは０．２〜５質量％であり、より好ましくは０．５〜３質量％であり、さらに好ましくは０．８〜２質量％である。 The content of the binding aid is preferably 0.2% by mass or more in the dry state in the granules for dentifrice of the present invention from the viewpoint of improving the effect of suppressing plaque formation and the physical properties of gradual disintegration. It is preferably 0.5% by mass or more, and more preferably 0.8% by mass or more. In addition, the content of the binding aid suppresses the disintegration strength from becoming excessively high, the viewpoint of improving the foaming and foam quality of the dentifrice containing the dentifrice granules of the present invention, and suppressing the metallic taste. In the dentifrice granules of the present invention, the amount is preferably 5% by mass or less, more preferably 3% by mass or less, and further preferably 2% by mass or less in a dry state. Further, the content of the binding aid is preferably 0.2 to 5% by mass, more preferably 0.5 to 3% by mass, still more preferably, in the dentifrice granules of the present invention in a dry state. Is 0.8 to 2% by mass.
本発明の歯磨剤用顆粒の平均粒径（μｍ）は、充分な歯垢等の除去効果と形成抑制効果を発揮させる観点、及び良好な研磨力を付与する観点から、５０μｍ以上であって、好ましくは７５μｍ以上であり、より好ましくは１００μｍ以上である。また、本発明の歯磨剤用顆粒の平均粒径（μｍ）は、口腔中での異物感を抑制する観点から、５００μｍ以下であって、好ましくは４５０μｍ以下であり、より好ましくは４００μｍ以下である。そして、歯磨剤用顆粒の平均粒径（μｍ）は、５０μｍ以上５００μｍ以下であって、好ましくは７５〜４５０μｍであり、より好ましくは１００〜４００μｍである。
なお、上記顆粒の平均粒径は、ＪＩＳＺ８８０１−１（２０００年５月２０日制定、２００６年１１月２０日最終改正）規定の２０００、１４００、１０００、７１０、５００、３５５、２５０、１８０、１２５、９０、６３、４５μｍの篩を用いて５分間振動させた後、篩分け法による篩下重量分布について５０％平均径を算出したものを採用する。
The average particle size (μm) of the dentifrice granules of the present invention is 50 μm or more from the viewpoint of exerting a sufficient effect of removing plaque and the like and an effect of suppressing formation, and from the viewpoint of imparting good polishing power. It is preferably 75 μm or more, and more preferably 100 μm or more. The average particle size (μm) of the dentifrice granules of the present invention is 500 μm or less, preferably 450 μm or less, and more preferably 400 μm or less from the viewpoint of suppressing a foreign body sensation in the oral cavity. .. The average particle size (μm) of the dentifrice granules is 50 μm or more and 500 μm or less, preferably 75 to 450 μm, and more preferably 100 to 400 μm.
The average particle size of the granules is 2000, 1400, 1000, 710, 500, 355, 250, 180, 125 specified by JISZ8801-1 (established on May 20, 2000, final revision on November 20, 2006). , 90, 63, 45 μm sieves were vibrated for 5 minutes, and then the 50% average diameter was calculated for the weight distribution under the sieve by the sieving method.
本発明の歯磨剤用顆粒の崩壊強度は、湿潤状態で０．２ｇｆ／個以上であって、好ましくは０．５ｇｆ／個以上であり、より好ましくは１ｇｆ／個以上であり、さらに好ましくは３ｇｆ／個以上である。また、本発明の歯磨剤用顆粒の崩壊強度は、使用時におけるブラッシング等の負荷によって歯磨剤用顆粒を良好に崩壊させ、成分（Ｂ）の溶解性を確保して効果的に歯垢等の形成抑制効果を高める観点から、湿潤状態で３０ｇｆ／個以下であって、好ましくは２５ｇｆ／個以下であり、より好ましくは２０ｇｆ／個以下であり、さらに好ましくは１５ｇｆ／個未満である。そして、本発明の歯磨剤用顆粒の崩壊強度は、湿潤状態で０．２ｇｆ／個以上３０ｇｆ／個以下であって、好ましくは０．５〜２５ｇｆ／個であり、より好ましくは１〜２０ｇｆ／個であり、さら好ましくは３ｇｆ／個以上１５ｇｆ／個未満である。
なお、顆粒の湿潤状態での崩壊強度とは、顆粒を歯磨剤組成物に配合した後、水溶液分散させて顆粒を回収した状態で測定した値を意味し、具体的には実施例に記載の方法により測定される。
The disintegration strength of the dentifrice granules of the present invention is 0.2 gf / piece or more, preferably 0.5 gf / piece or more, more preferably 1 gf / piece or more, and further preferably 3 gf in a wet state. / More than one. Further, the disintegration strength of the dentifrice granules of the present invention satisfactorily disintegrates the dentifrice granules due to a load such as brushing during use, ensuring the solubility of the component (B) and effectively removing plaque and the like. From the viewpoint of enhancing the formation inhibitory effect, it 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 in a wet state. The disintegration strength of the dentifrice granules of the present invention is 0.2 gf / piece or more and 30 gf / piece or less, preferably 0.5 to 25 gf / piece, and more preferably 1 to 20 gf / piece in a wet state. The number is, more preferably 3 gf / piece or more 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 blended in a dentifrice composition and then dispersed in an aqueous solution to recover the granules, and specifically described in Examples. Measured by method.
本発明の歯磨剤用顆粒は、予め成分（Ａ）を製造する工程（Ｉ）、及び工程（Ｉ）で得られた成分（Ａ）に成分（Ｂ）を担持させる工程（II）を経ることにより製造することができる。
工程（Ｉ）は、成分（Ａ）の造粒物を製造する工程であり、成分（Ａ）は、水不溶性粉末材料の凝集物（ａ１）、或いは水不溶性粉末材料と無機結合剤を含有する造粒物（ａ２）のいずれであってもよい。また、噴霧乾燥法や転動造粒法のいずれを用いてもよく、装置としては、噴霧乾燥機や撹拌転動造粒機、容器回転型造粒機等を用いることができる。
The dentifrice granule of the present invention undergoes a step (I) of producing the component (A) in advance and a step (II) of supporting the component (B) on the component (A) obtained in the step (I). Can be manufactured by
The step (I) is a step of producing a granulated product of the component (A), and the component (A) contains an aggregate (a1) of a water-insoluble powder material or a water-insoluble powder material and an inorganic binder. It may be any of the granulated products (a2). Further, either the spray drying method or the rolling granulation method may be used, and as the apparatus, a spray drying machine, a stirring rolling granulator, a container rotary granulator, or the like can be used.
工程（Ｉ）の成分（Ａ）の製造方法としては、例えば、特開２０１０−７０４５８号公報及び特開２０１３−１４７４３１号公報、特開２０１４−００１１８６号公報、特開２０１４−０２４８３７号公報等に記載される方法を採用することができる。 Examples of the method for producing the component (A) of the step (I) include JP-A-2010-704858, JP-A-2013-147431, JP-A-2014-001186, JP-A-2014-024837 and the like. The described method can be adopted.
工程（II）は、工程（Ｉ）で得られた成分（Ａ）に成分（Ｂ）を担持させる工程である。かかる工程（II）では、成分（Ａ）において成分（Ｂ）が偏在することなく、成分（Ａ）の内部にいたるまで充分に成分（Ｂ）を担持させる観点から、成分（Ａ）に成分（Ｂ）を加熱混合するのが好ましい。加熱混合における温度は、成分（Ｂ）の融点以上であるのが好ましい。また、加熱混合における混合時間は、成分（Ａ）全体に対して均一に成分（Ｂ）を担持させる観点から、好ましくは５分以上であり、より好ましくは１０分以上であり、生産性の観点から、好ましくは６０分以下であり、より好ましくは４５分以下である。 The step (II) is a step of supporting the component (B) on the component (A) obtained in the step (I). In the step (II), the component (B) is not unevenly distributed in the component (A), and the component (B) is sufficiently supported up to the inside of the component (A). It is preferable to heat and mix B). The temperature in the heating and mixing is preferably equal to or higher than the melting point of the component (B). Further, the mixing time in the heating and 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, and more preferably 45 minutes or less.
工程（II）において用いる装置としては、例えば、ヘンシェルミキサー（三井三池化工機（株）製）、ハイスピードミキサー（深江工業（株）製）、バーチカルグラニュレーター（（株）パウレック製）、レディゲミキサー（松坂技研（株）製）、プロシェアミキサー（太平洋機工（株）製）等の混合機（イ）；Ｕトラフ型リボンブレンダ（ホソカワミクロン株式会社製、型式：Ｒ−１７Ｗ）等の混合機（ロ）；ナウターミキサー（ホソカワミクロン（株）製）等の混合機（ハ）が挙げられる。かかる混合機は、温度調整を容易にする観点から、ジャケットを備えたものであるのが好ましい。
上記混合機のなかでも、顆粒を壊さない観点からは、混合機（ロ）、混合機（ハ）が好ましく、不要な凝集を防ぐ観点からは、混合機（イ）が好ましい。
The devices used in step (II) include, for example, Henshell mixer (manufactured by Mitsui Miike Kakoki Co., Ltd.), high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), vertical granulator (manufactured by Paulek Co., Ltd.), and Ladyge. Mixer (a) such as mixer (manufactured by Matsuzaka Giken Co., Ltd.), Proshare mixer (manufactured by Pacific Kiko Co., Ltd.); mixer such as U trough type ribbon blender (manufactured by Hosokawa Micron Co., Ltd., model: R-17W) (B); Examples thereof include a mixer (c) such as a Nauter mixer (manufactured by Hosokawa Micron Co., Ltd.). Such a mixer is preferably provided with a jacket from the viewpoint of facilitating temperature control.
Among the above mixers, the mixer (b) and the mixer (c) are preferable from the viewpoint of not breaking the granules, and the mixer (a) is preferable from the viewpoint of preventing unnecessary aggregation.
上記混合機を用いる場合、回転数は、成分（Ａ）が実質的に崩壊しない程度の値を選択すればよい。例えば、攪拌翼を備えた混合機を用いる場合、成分（Ａ）の崩壊を回避する観点から、フルード数が２．１以下であるのが好ましい。
なお、フルード数とは、下式（II）にて算出される値を意味する。
フルード数（Ｆｒ）＝Ｖ2／（Ｒ×ｇ）・・・（II）
Ｖ：攪拌翼・解砕翼の先端の周速[ｍ／ｓ]
Ｒ：攪拌翼・解砕翼の回転半径[ｍ]
ｇ：重力加速度[ｍ／ｓ2]
When the above mixer is used, 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 Froude 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 equation (II).
Froude number (Fr) = V 2 / (R × g) ・ ・ ・ (II)
V: Peripheral speed at the tip of stirring blade / crushing blade [m / s]
R: Radius of gyration of stirring blade / crushing blade [m]
g: Gravity acceleration [m / s 2 ]
また、上記混合機を用いる場合、混合時間は、成分（Ａ）の内部にいたるまで成分（Ｂ）を良好に浸透させる観点から、好ましくは１０分以上であり、より好ましくは２０分以上であり、さらに好ましくは３０分以上であり、生産性の観点から、好ましくは６０分以下であり、より好ましくは４０分以下である。 When the above mixer is used, the mixing time is preferably 10 minutes or more, more preferably 20 minutes or more, from the viewpoint of allowing the component (B) to penetrate well into the inside of the component (A). It is more preferably 30 minutes or more, preferably 60 minutes or less, and more preferably 40 minutes or less from the viewpoint of productivity.
また、工程（II）において用いる装置としては、上記以外の混合機として、連続型の装置を用いてもよく、かかる連続型の装置としては、例えば、フレキソミックス型（（株）パウレック製）、タービュライザー（ホソカワミクロン（株）製）等の混合機が挙げられる。さらに、上記混合機のほか、流動層乾燥機を用いることもできる。 Further, as the apparatus used in the step (II), a continuous type apparatus may be used as a mixer other than the above, and examples of such a continuous type apparatus include a flexomix type (manufactured by Paulec Co., Ltd.). Examples thereof include a mixer such as a turbulizer (manufactured by Hosokawa Micron Co., Ltd.). Further, in addition to the above mixer, a fluidized bed dryer can also be used.
成分（Ｂ）は、固体として、或いは融点以上に加温された液体として装置内に添加することができ、液体で添加する場合は、ノズルにて噴霧し、できるだけ均一に添加することが好ましい。温度調整としては、装置が備えるジャケット等により装置内の温度を調整することにより行ってもよく、また、予め添加する成分（Ｂ）の温度を調整することにより行ってもよい。 The component (B) can be added into the apparatus as a solid or as a liquid heated to a temperature higher than the melting point. When the component (B) is added as a liquid, it is preferably sprayed with a nozzle and added as uniformly as possible. The temperature may be adjusted by adjusting the temperature inside the device with a jacket or the like provided in the device, or by adjusting the temperature of the component (B) to be added in advance.
本発明の歯磨剤組成物は、上記歯磨剤用顆粒を１質量％以上５０質量％以下含有する。かかる歯磨剤組成物であれば、口腔内に適用した際、歯面に堅固に付着した歯垢等の除去効果を有効に高めることができるとともに、歯垢等が付着しにくい歯面の状態を充分に維持させて高い歯垢等の形成抑制効果を発揮することができ、歯面への歯垢等の再付着をも未然に防止して、歯面におけるつるつるした感触をも持続させ、高い使用感を付与することができる。 The dentifrice composition of the present invention contains the above-mentioned dentifrice granules in an amount of 1% by mass or more and 50% by mass or less. With such a dentifrice composition, when applied into the oral cavity, the effect of removing plaque and the like firmly adhering to the tooth surface can be effectively enhanced, and the state of the tooth surface on which plaque and the like do not easily adhere can be improved. It can be sufficiently maintained to exert a high effect of suppressing the formation of plaque, etc., prevent reattachment of plaque, etc. to the tooth surface, and maintain a smooth feel on the tooth surface, which is high. It is possible to give a feeling of use.
歯磨剤用顆粒の含有量は、かかる顆粒による歯垢等の除去効果を高めるとともに充分な歯垢等の形成抑制効果も発揮し、かつ使用感を向上させる観点から、本発明の歯磨剤組成物中に、１質量％以上であって、好ましくは３質量％以上であり、さらに好ましくは５質量％以上である。歯磨剤用顆粒の含有量は、異物感を感じることなく、また歯のエナメル質を傷つけることなく歯垢等の除去効果と形成抑制効果を発揮させる観点から、本発明の歯磨剤組成物中に、５０質量％以下であって、好ましくは３０質量％以下であり、より好ましくは２０質量％以下である。また、歯磨剤用顆粒の含有量は、本発明の歯磨剤組成物中に、１質量％以上５０質量％以下であって、好ましくは３〜３０質量％であり、より好ましくは５〜２０質量％である。 The content of the dentifrice granules is the dentifrice composition of the present invention from the viewpoint of enhancing the effect of removing plaque and the like by the granules, exhibiting a sufficient effect of suppressing the formation of plaque and the like, and improving the usability. Among them, it is 1% by mass or more, preferably 3% by mass or more, and more preferably 5% by mass or more. The content of the dentifrice granules is contained in the dentifrice composition of the present invention from the viewpoint of exerting the effect of removing plaque and the like and the effect of suppressing the formation without feeling a foreign body sensation 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. The content of the dentifrice granules in the dentifrice composition of the present invention is 1% by mass or more and 50% by mass or less, preferably 3 to 30% by mass, and more preferably 5 to 20% by mass. %.
本発明の歯磨剤組成物は、さらに粘結剤を含有してもよい。かかる粘結剤としては、カルボキシメチルセルロースナトリウム、ポリアクリル酸ナトリウム、ヒドロキシエチルセルロース、カラギーナン、キサンタンガム、アルギン酸ナトリウム、グアガム、及びペクチン等から選ばれる１種又は２種以上が挙げられる。かかる粘結剤の含有量は、含有する成分を溶解・分散させながら口腔内で有効に拡散させ、上記歯磨剤用顆粒による歯垢等の除去効果を有効に発揮させてつるつる感や汚れ落ち感を高め、歯垢等の形成抑制効果も高めながら良好な泡立ちをもたらす観点から、本発明の歯磨剤組成物中に、好ましくは０．１質量％以上であり、より好ましくは０．５質量％以上であり、さらに好ましくは０．７質量％以上であり、好ましくは３質量％以下であり、より好ましくは２質量％以下である。また、粘結剤の含有量は、本発明の歯磨剤組成物中に、好ましくは０．１〜３質量％であり、より好ましくは０．５〜２質量％であり、さらに好ましくは０．７〜２質量％である。 The dentifrice composition of the present invention may further contain a binder. Examples of such a binder include one or more selected from sodium carboxymethyl cellulose, sodium polyacrylate, hydroxyethyl cellulose, carrageenan, xanthan gum, sodium alginate, guagam, pectin and the like. The content of the binder effectively diffuses in the oral cavity while dissolving and dispersing the contained components, and effectively exerts the effect of removing plaque and the like by the above-mentioned dentifrice granules, resulting in a slippery feeling and a feeling of removing stains. In the dentifrice composition of the present invention, it is preferably 0.1% by mass or more, more preferably 0.5% by mass, from the viewpoint of bringing about good foaming while enhancing the effect of suppressing the formation of dental plaque and the like. The above is more preferably 0.7% by mass or more, preferably 3% by mass or less, and more preferably 2% by mass or less. The content of the binder in the dentifrice composition of the present invention is preferably 0.1 to 3% by mass, more preferably 0.5 to 2% by mass, and even more preferably 0. It is 7 to 2% by mass.
本発明の歯磨剤組成物は、さらに上記粘結剤とともに増粘剤を含有してもよい。増粘剤としては、増粘性シリカ（ＪＩＳ Ｋ５１０１−１３−２に準ずる方法により測定される吸油量が、２００〜４００ｍＬ／１００ｇ）、モンモリロナイト等が挙げられる。かかる増粘剤の含有量は、上記成分を溶解・分散させながら口腔内で有効に拡散させ、上記歯磨剤用顆粒による歯垢等の除去効果や形成抑制効果を有効に発揮させて、歯面におけるつるつる感や汚れ落ち感を高め、また良好な泡立ちをもたらす観点から、本発明の歯磨剤組成物中に、好ましくは３質量％以上であり、より好ましくは４質量％以上であり、さらに好ましくは５質量％以上であり、好ましくは１０質量％以下であり、より好ましくは８．５質量％以下である。また、本発明の歯磨剤における増粘剤の含有量は、本発明の歯磨剤組成物中に、好ましくは４〜１０質量％であり、より好ましくは５〜８．５質量％である。 The dentifrice composition of the present invention may further contain a thickener together with the above-mentioned binder. Examples of the thickener include thickening silica (oil absorption amount measured by a method according to JIS K5101-13-2 is 200 to 400 mL / 100 g), montmorillonite and the like. The content of the thickener is such that the above-mentioned components are dissolved and dispersed and effectively diffused in the oral cavity, and the above-mentioned dentifrice granules effectively exert the effect of removing plaque and the like 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, still more preferably, from the viewpoint of enhancing the slippery feeling and the feeling of removing stains 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. The content of the thickener in the dentifrice of the present invention is preferably 4 to 10% by mass, more preferably 5 to 8.5% by mass in the dentifrice composition of the present invention.
本発明の歯磨剤組成物は、さらに界面活性剤を含有するのが好ましい。これにより、良好な泡立ちをもたらしつつ清掃効果を高め、歯と歯の隙間のような狭小な領域に至るまで歯磨剤用顆粒による歯垢等の除去効果や形成抑制効果を十分に及ぼすことができ、使用後の口腔内において歯面につるつるとした感触を付与して良好な使用感をもたらすことができる。 The dentifrice composition of the present invention preferably further contains a surfactant. As a result, the cleaning effect can be enhanced while providing good foaming, and the effect of removing plaque and the like and the effect of suppressing the formation of dentifrice granules can be sufficiently exerted even in a narrow area such as a gap between teeth. , It is possible to give a smooth feel to the tooth surface in the oral cavity after use and bring about a good feeling of use.
かかる界面活性剤としては、アニオン界面活性剤、ノニオン界面活性剤，両性イオン界面活性剤を用いることができる。かかるアニオン界面活性剤としては、例えばラウリル硫酸ナトリウム、ミリスチル硫酸ナトリウム等のアルキル硫酸塩；Ｎ−ラウロイルザルコシン酸ナトリウム、Ｎ−ミリストイルザルコシン酸ナトリウム等のＮ−アシルザルコシン酸塩；Ｎ−パルミトイルグルタミン酸ナトリウム等のＮ−アシルグルタミン酸塩、Ｎ−メチル−Ｎ−アシルタウリンナトリウム、Ｎ−メチル−Ｎ−アシルアラニンナトリウム、α−オレフィンスルホン酸ナトリウム、ジオクチルスルホコハク酸ナトリウム等が挙げられる。 As such a surfactant, an anionic surfactant, a nonionic surfactant, and an amphoteric ion surfactant can be used. Examples of such anionic surfactants include alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate; N-acylsarcosate such as sodium N-lauroyl sarcosinate and sodium N-myristyl sarcosinate; sodium N-palmitoyl glutamate. Such as N-acylglutamate, N-methyl-N-acyltaurine sodium, N-methyl-N-acylalanine sodium, α-olefin sulfonate sodium, sodium dioctyl sulfosuccinate and the like.
ノニオン界面活性剤としては、ショ糖脂肪酸エステル等の糖脂肪酸エステル；マルチトール脂肪酸エステル、ラクチトール脂肪酸エステル等の糖アルコール脂肪酸エステル；ポリオキシエチレンソルビタンモノラウレート、ポリオキシエチレンソルビタンモノステアレート等のポリオキシエチレンソルビタン脂肪酸エステル；ラウリン酸モノ又はジエタノールアミド、ミリスチン酸モノ又はジエタノールアミド等の脂肪酸ジエタノールアミド；ソルビタン脂肪酸エステル、脂肪酸モノグリセライド、ポリオキシエチレン高級アルコールエーテル、ポリオキシエチレンポリオキシプロピレン共重合体等が挙げられる。 Examples of the nonionic surfactant include sugar fatty acid esters such as sucrose fatty acid ester; sugar alcohol fatty acid esters such as maltitol fatty acid ester and lactitol fatty acid ester; polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monostearate and the like. 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.
両性イオン界面活性剤としては、Ｎ−ラウリルジアミノエチルグリシン、Ｎ−ミリスチルジアミノエチルグリシン等のＮ−アルキルジアミノエチルグリシン、Ｎ−アルキル−Ｎ−カルボキシメチルアンモニウムベタイン、２−アルキル−１−ヒドロキシエチルイミダゾリンベタインナトリウム等が挙げられる。 Examples of the amphoteric ion surfactant include N-alkyldiaminoethylglycine such as N-lauryldiaminoethylglycine and N-myristyldiaminoethylglycine, N-alkyl-N-carboxymethylammonium betaine, and 2-alkyl-1-hydroxyethyl imidazoline. Betaine sodium and the like can be mentioned.
上記界面活性剤のなかでも、歯垢等の除去効果や形成抑制効果に加え、良好な発泡性や使用感を付与する観点から、アニオン界面活性剤が好ましく、さらにラウリル硫酸ナトリウム等のアルキル硫酸塩がより好ましい。 Among the above-mentioned surfactants, anionic surfactants are preferable from the viewpoint of imparting good foaming property and usability 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 are further preferable. Is more preferable.
界面活性剤の含有量は、歯垢等の除去効果や形成抑制効果に加え、良好な泡立ちを付与して清掃効果や使用感を高めつつ、良好な風味をもたらす観点から、本発明の歯磨剤組成物中に、好ましくは０．１質量％以上であり、より好ましくは０．２質量％以上である。また、界面活性剤の含有量は、風味が損なわれるのを抑制する観点から、本発明の歯磨剤組成物中に、好ましくは２．０質量％以下であり、より好ましくは１．７質量％以下である。そして、界面活性剤の含有量は、本発明の歯磨剤組成物中に、好ましくは０．１〜２．０質量％であり、より好ましくは０．２〜１．７質量％である。 The content of the surfactant is the dentifrice of the present invention from the viewpoint of providing good foaming to enhance the cleaning effect and usability in addition to the effect of removing plaque and the like and the effect of suppressing the formation, and providing a good flavor. In the composition, it is preferably 0.1% by mass or more, and more preferably 0.2% by 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 content of the surfactant 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.
本発明の歯磨剤組成物が、界面活性剤としてアニオン界面活性剤を含有する場合、かかるアニオン界面活性剤の含有量は、泡立ちの良さや清掃効果や使用感を高めつつ、良好な風味をもたらす観点から、本発明の歯磨剤組成物中に、好ましくは０．１質量％以上であり、より好ましくは０．２質量％以上である。また、アニオン界面活性剤の含有量は、風味が損なわれるのを抑制する観点から、本発明の歯磨剤組成物中に、好ましくは２．０質量％以下であり、より好ましくは１．５質量％以下である。さらに、アニオン界面活性剤の含有量は、本発明の歯磨剤組成物中に、好ましくは０．１〜２．０質量％であり、より好ましくは０．２〜１．５質量％である。 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 enhancing good foaming, cleaning effect and usability. From the viewpoint, it is preferably 0.1% by mass or more, more preferably 0.2% by mass or more in the dentifrice composition of the present invention. Further, 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 deterioration of flavor. % Or less. Further, 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.
本発明の歯磨剤組成物が、界面活性剤としてアニオン界面活性剤であるアルキル硫酸塩を含有する場合、かかるアルキル硫酸塩の含有量は、泡立ちの良さや清掃効果や使用感を高めつつ、良好な風味をもたらす観点から、本発明の歯磨剤組成物中に、好ましくは０．０５質量％以上であり、より好ましくは０．１質量％以上である。また、アルキル硫酸塩の含有量は、風味が損なわれるのを抑制する観点から、本発明の歯磨剤組成物中に、好ましくは１質量％以下であり、より好ましくは０．５質量％以下である。さらに、アルキル硫酸塩の含有量は、本発明の歯磨剤組成物中に、好ましくは０．０５〜１質量％であり、より好ましくは０．１〜０．５質量％である。 When the dentifrice composition of the present invention contains an alkyl sulfate as an anionic surfactant as a surfactant, the content of the alkyl sulfate is good while enhancing good foaming, cleaning effect and usability. From the viewpoint of providing a good flavor, it is preferably 0.05% by mass or more, more preferably 0.1% by mass or more in the dentifrice composition of the present invention. Further, 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 deterioration of flavor. is there. Further, 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.
本発明の歯磨剤組成物は、ソルビトールを含有するのが好ましい。かかるソルビトールを含有することにより、上記成分を溶解・分散させて口腔内で有効に拡散させ、歯垢等の除去効果を有効に発揮させながら、良好な泡立ちや風味等をもたらし、使用感を高めることができる。 The dentifrice composition of the present invention preferably contains sorbitol. By containing such sorbitol, the above-mentioned components are dissolved and dispersed and effectively diffused in the oral cavity, and while effectively exerting the effect of removing plaque and the like, good foaming and flavor are brought about, and the usability is enhanced. be able to.
ソルビトールの含有量は、歯垢等の除去効果や形成抑制効果と良好な使用感の付与とを両立させる観点から、本発明の歯磨剤組成物中に、好ましくは５質量％以上であり、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％以上であり、好ましくは６０質量％以下であり、より好ましくは５０質量％以下であり、さらに好ましくは４０質量％以下である。また、ソルビトールの含有量は、本発明の歯磨剤組成物中に、好ましくは５〜６０質量％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１５〜４０質量％である。 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 and the effect of suppressing the formation of the sorbitol and the effect of imparting a good feeling of use. It is preferably 10% by mass or more, more preferably 15% by mass or more, preferably 60% by mass or less, more preferably 50% by mass or less, still more preferably 40% by mass or less. The content of sorbitol in the dentifrice composition of the present invention is preferably 5 to 60% by mass, more preferably 10 to 50% by mass, and further preferably 15 to 40% by mass.
本発明の歯磨剤組成物は、さらに水を含有してもよい。かかる水の含有量（水分量）は、上記成分を溶解・分散させながら口腔内で有効に拡散させ、顆粒による歯垢等の除去効果や形成抑制効果を有効に発揮させる観点から、本発明の歯磨剤組成物中に、好ましくは３質量％以上であり、より好ましくは５質量％以上であり、さらに好ましくは７質量％以上であり、好ましくは６０質量％以下であり、より好ましくは５５質量％以下であり、さらに好ましくは５０質量％以下である。また、水の含有量は、本発明の歯磨剤組成物中に、好ましくは３〜６０質量％であり、より好ましくは５〜５５質量％であり、さらに好ましくは７〜５０質量％である。
なお、かかる水分量は、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 dentifrice composition of the present invention may further contain water. The water content (water content) of the present invention is determined from the viewpoint of effectively diffusing the above components in the oral cavity while dissolving and dispersing them, and effectively exerting the effect of removing dental plaque and the like and the effect of suppressing the formation of the granules. In the dentifrice composition, it is preferably 3% by mass or more, more preferably 5% by mass or more, further preferably 7% by mass or more, preferably 60% by mass or less, and more preferably 55% by mass. % Or less, more preferably 50% by mass or less. The water content in the dentifrice composition of the present invention is preferably 3 to 60% by mass, more preferably 5 to 55% by mass, and even more preferably 7 to 50% by mass.
The water content can be calculated from the water content in the blended water content and the water content in the blended component, but can be measured by, for example, a Karl Fischer titer. As the Karl Fischer titer, for example, a trace moisture measuring device (Hiranuma Sangyo Co., Ltd.) can be used. In this device, 5 g of dentifrice can be taken, suspended in 25 g of anhydrous methanol, and 0.02 g of this suspension can be separated to measure the water content.
また、本発明の歯磨剤組成物中における、歯磨剤用顆粒の含有量と水の含有量との質量比（歯磨剤用顆粒／水）は、良好な溶解性や分散性、及び歯垢等の除去効果や形成抑制効果を充分に発揮させる観点から、好ましくは０．０２〜１５であり、より好ましくは０．１〜６であり、さらに好ましくは０．１５〜１である。 Further, the mass ratio of the content of dentifrice granules to the content of water in the dentifrice composition of the present invention (dentifrice granules / water) has good solubility, dispersibility, plaque and the like. From the viewpoint of sufficiently exerting the effect of removing and suppressing the formation of toothpaste, it is preferably 0.02 to 15, more preferably 0.1 to 6, and even more preferably 0.15 to 1.
本発明の歯磨剤組成物は、上記以外の他の成分、例えばグリセリン、プロピレングリコール、１，３ブチレングリコール、エチレングリコール、ポリエチレングリコール、ポリプロピレングリコール、キシキリット、マルチット、ラクチット、及びエリスリトール等のソルビトール以外の湿潤剤；研磨剤；賦形剤；防腐剤；香料；薬用成分；着色剤；その他一般に歯磨剤において使用されている成分を含有することができる。
なお、本発明の歯磨剤組成物は、上記成分を用い、常法により製造することができる。
The dentifrice composition of the present invention has components other than the above, such as glycerin, propylene glycol, 1,3 butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xikirit, martit, lactite, and sorbitol such as erythritol. Wetting agents; abrasives; excipients; preservatives; fragrances; medicinal ingredients; colorants; and other ingredients commonly used in dentifrices can be included.
The dentifrice composition of the present invention can be produced by a conventional method using the above components.
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、顆粒の平均粒径、及び湿潤状態での崩壊強度は、以下の方法にしたがって測定した。
Hereinafter, the present invention will be specifically described based on examples. Unless otherwise specified in the table, the content of each component indicates mass%.
The average particle size of the granules and the disintegration strength in a wet state were measured according to the following methods.
《平均粒径の測定》
ＪＩＳＺ８８０１−１（２０００年５月２０日制定、２００６年１１月２０日最終改正）規定の２０００、１４００、１０００、７１０、５００、３５５、２５０、１８０、１２５、９０、６３、４５μｍの篩を用いて５分間振動させた後、篩分け法による篩下重量分布について５０％平均径を算出したものを採用した。
<< Measurement of average particle size >>
Using a sieve of 2000, 1400, 1000, 710, 500, 355, 250, 180, 125, 90, 63, 45 μm specified by JISZ8801-1 (established on May 20, 2000, final revision on November 20, 2006). After vibrating for 5 minutes, a 50% average diameter was calculated for the weight distribution under the sieve by the sieving method.
《湿潤状態での崩壊強度の測定》
得られた歯磨剤組成物を２ｇとり、イオン交換水１８ｍＬに１０分間分散させた後、溶液から粒子径１９０〜２１０μｍの顆粒を取り出して、微小圧縮試験機（島津製作所製、ＭＣＴＭ−５００）を用いて該粒子径の顆粒を１０個測定した平均値を求め、湿潤状態での崩壊強度の値とした。
《Measurement of collapse strength in wet state》
After taking 2 g of the obtained dentifrice composition and dispersing it in 18 mL of ion-exchanged water for 10 minutes, granules having a particle size of 190 to 210 μm were taken out from the solution, and a microcompression tester (manufactured by Shimadzu Corporation, MCTM-500) was used. The average value obtained by measuring 10 granules having the particle size was determined and used as the value of the disintegration strength in a wet state.
［実施例１］
表１に示す歯磨剤用顆粒の処方にしたがって、顆粒を得た。具体的には、炭酸カルシウム（東洋電化工業株式会社製、商品名：トヨホワイト、平均粒子径２〜５μｍ）、コロイダルシリカ（日産化学株式会社製、商品名：スノーテックスＳ）、セルロース（日本製紙ケミカル株式会社製、商品名：ＫＣフロック Ｗ−４００Ｇ）及び水を、ディスパー翼（アシザワ・ニロアトマイザー株式会社製、型式：ＨＳ−Ｐ３）で混合し、水スラリーを得た。得られた水スラリーを送風温度１９０℃で噴霧乾燥し、目開きが９０μｍと５００μｍの篩で分級した。分級後の造粒物を１００度に加熱し、ジャケット温度８０度のＵトラフ型リボンブレンダ（ホソカワミクロン株式会社製、型式：Ｒ−１７Ｗ）に投入し、回転数１３０ｒ．ｐ．ｍ、フルード数２．１で混合を開始した。次に常温のパルミチン酸（花王（株）性、ルナックＰ−９５）を投入後、３０分間混合を行い、顆粒を得た。
[Example 1]
Granules were obtained according to the formulation of dentifrice granules shown in Table 1. Specifically, calcium carbonate (manufactured by Toyo Denka Kogyo Co., Ltd., product name: Toyo White, average particle size 2-5 μm), colloidal silica (manufactured by Nissan Chemical Co., Ltd., product name: Snowtex S), cellulose (Nippon Paper Chemicals Co., Ltd.) Chemicals Co., Ltd., trade name: KC Flock W-400G) and water were mixed with a dispenser blade (manufactured by Ashizawa Niro Atomizer Co., Ltd., model: HS-P3) to obtain an aqueous slurry. The obtained water slurry was spray-dried at a blowing temperature of 190 ° C. and classified by a sieve having a mesh size of 90 μm and 500 μm. The granulated product after classification was heated to 100 ° C. and charged into a U-trough type ribbon blender (manufactured by Hosokawa Micron Co., Ltd., model: R-17W) having a jacket temperature of 80 ° C., and the rotation speed was 130 r. p. Mixing was started with m and a Froude number of 2.1. Next, palmitic acid (Kao Corporation, Lunac P-95) at room temperature was added and mixed for 30 minutes to obtain granules.
［実施例２］
表１に示す歯磨剤用顆粒の処方にしたがって、顆粒を得た。具体的には、ゼオライト（ゼオビルダー株式会社製、商品名：ゼオライト（パウダー））、珪酸ナトリウム水溶液（富士化学工業株式会社製、商品名：３号珪酸ソーダ、固形分：５５．１％）及び水を、ディスパー翼（アシザワ・ニロアトマイザー株式会社製、型式：ＨＳ−Ｐ）で混合し、水スラリーを得た。得られた水スラリーを送風温度１９０℃で噴霧乾燥し、目開き５００μｍの篩で分級した。分級後の造粒物を１００度に加熱し、ジャケット温度８０度のＵトラフ型リボンブレンダ（ホソカワミクロン株式会社製、型式：Ｒ−１７Ｗ）に投入し、回転数１３０ｒ．ｐ．ｍ、フルード数２．１で混合を開始した。次に常温のパルミチン酸（花王（株）性、ルナックP−９５）を投入後、３０分間混合を行い、顆粒を得た。
[Example 2]
Granules were obtained according to the formulation of dentifrice granules shown in Table 1. Specifically, zeolite (manufactured by Zeolite Co., Ltd., trade name: zeolite (powder)), aqueous sodium silicate solution (manufactured by Fuji Chemical Industries Co., Ltd., trade name: sodium silicate, solid content: 55.1%) and water. Was mixed with a disper blade (manufactured by Ashizawa Niro Atomizer Co., Ltd., model: HS-P) to obtain an aqueous 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 was heated to 100 ° C. and charged into a U-trough type ribbon blender (manufactured by Hosokawa Micron Co., Ltd., model: R-17W) having a jacket temperature of 80 ° C., and the rotation speed was 130 r. p. Mixing was started with m and a Froude number of 2.1. Next, palmitic acid (Kao Corporation, Lunac P-95) at room temperature was added and mixed for 30 minutes to obtain granules.
［実施例３］
表１に示す歯磨剤用顆粒の処方にしたがって、炭酸カルシウムと酸化亜鉛を混合し、転動造粒機により顆粒を得た。具体的には、両原料を装置内（機器：ニューグラマシン ＳＥＧ８５０型）で混合し、造粒時に粉体に対して１５％の精製水を加えて造粒を行った。造粒工程終了後、乾燥機内（機器：ロータリーキルン）で２０〜３０分程度乾燥させた。造粒物の崩壊硬度はいずれも１５〜１８ｇ／個であった。なお、造粒物は電動篩機により５０μｍ以下の造粒物を除去した。分級後の造粒物を１００度に加熱し、ジャケット温度８０度のＵトラフ型リボンブレンダ（ホソカワミクロン株式会社製、型式：Ｒ−１７Ｗ）に投入し、回転数１３０ｒ．ｐ．ｍ、フルード数２．１で混合を開始した。次に常温のパルミチン酸（花王（株）性、ルナックP−９５）を投入後、３０分間混合を行い、顆粒を得た。
[Example 3]
Calcium carbonate and zinc oxide were mixed according to the formulation of dentifrice granules shown in Table 1, and granules were obtained by a rolling granulator. Specifically, both raw materials were mixed in an apparatus (equipment: New Gramachine SEG850 type), and 15% purified water was added to the powder at the time of granulation to perform granulation. After the granulation process was completed, it was dried in a dryer (equipment: rotary kiln) for about 20 to 30 minutes. The disintegration hardness of the granules was 15 to 18 g / piece. As for the granulated product, the granulated product having a size of 50 μm or less was removed by an electric sieve machine. The granulated product after classification was heated to 100 ° C. and charged into a U-trough type ribbon blender (manufactured by Hosokawa Micron Co., Ltd., model: R-17W) having a jacket temperature of 80 ° C., and the rotation speed was 130 r. p. Mixing was started with m and a Froude number of 2.1. Next, palmitic acid (Kao Corporation, Lunac P-95) at room temperature was added and mixed for 30 minutes to obtain granules.
［実施例４〜１１］
表１に示す歯磨剤用顆粒の処方にしたがって、顆粒を得た。具体的には、重質炭酸カルシウム（株式会社カルファイン製、商品名：ＡＣＥ−２５、平均粒子径約３μｍ）を、邪魔板を有した７５Ｌドラム型造粒機（φ４０ｃｍ×Ｌ６０ｃｍ）に投入し、ドラム回転数３０ｒ．ｐ．ｍ／フルード数０．２／ドラム角度１２．６°の条件で混合しながら珪酸ナトリウム（富士化学工業株式会社製、商品名：３号珪酸ソーダ：Ｎａ2・３ＳｉＯ2溶液、固形分３８．５％、３倍量以下の水にて希釈、２５℃）を外部混合型二流体ノズル１個（株式会社アトマックス製）を用いて噴霧添加し、造粒した。なお、バッチサイズは１０ｋｇである。珪酸ナトリウム水溶液の添加速度は、３．３ｍＬ／分であった。
珪酸ナトリウム水溶液噴霧後に１分間混合を継続した後、ドラム型造粒機から排出し、電気式棚乾燥機を用いて１２０℃で２０時間乾燥した後、ジャケット温度８０℃のUトラフ型リボンブレンダー（ホソカワミクロン株式会社製、型式：Ｒ−１７Ｗ）に成分（Ｂ）と共に投入し、回転数１３０ｒ.ｐ.ｍ、フルード数２．１で３分混合し顆粒を得た。
[Examples 4 to 11]
Granules were obtained according to the formulation of dentifrice granules shown in Table 1. Specifically, heavy calcium carbonate (manufactured by Calfine Co., Ltd., trade name: ACE-25, average particle diameter of about 3 μm) is put into a 75 L drum type granulator (φ40 cm × L60 cm) having a baffle plate. , Drum rotation speed 30r. p. m / Froude number 0.2 / drum angle 12.6 ° of sodium silicate with mixing under conditions of (Fuji Chemical Industry Co., Ltd., trade name: No. 3 sodium silicate: Na 2 · 3SiO 2 solution, solid content 38.5 %, Diluted with 3 times or less of water, 25 ° C.) was spray-added using one external mixing type two-fluid nozzle (manufactured by Atmax, Inc.) to granulate. The batch size is 10 kg. The addition rate of the sodium silicate aqueous solution was 3.3 mL / min.
After spraying the sodium silicate aqueous solution and continuing mixing for 1 minute, it is discharged from the drum type granulator, dried at 120 ° C. for 20 hours using an electric shelf dryer, and then a U trough type ribbon blender having a jacket temperature of 80 ° C. It was added to Hosokawa Micron Co., Ltd., model: R-17W) together with the component (B), and mixed at a rotation speed of 130 rpm and a Froude number of 2.1 for 3 minutes to obtain granules.
［比較例１〜２］
表１に示す歯磨剤用顆粒の処方にしたがい、成分（Ｂ）を用いなかった以外、実施例４と同様にして、顆粒を得た。
[Comparative Examples 1-2]
Granules were obtained in the same manner as in Example 4 according to the formulation of the dentifrice granules shown in Table 1, except that the component (B) was not used.
［比較例３］
表１に示す歯磨剤用顆粒の処方にしたがい、パルミチン酸の代わりにラウリン酸を用いた以外、実施例４と同様にして、顆粒を得た。
[Comparative Example 3]
Granules were obtained in the same manner as in Example 4, except that lauric acid was used instead of palmitic acid according to the formulation of the dentifrice granules shown in Table 1.
得られた各顆粒を用い、下記方法にしたがって、バイオフィルム形成抑制率（％）を求め、また風味の評価も行った。 Using each of the obtained granules, the biofilm formation inhibition rate (%) was determined according to the following method, and the flavor was also evaluated.
《バイオフィルム形成抑制率（％）》
ＨＡｐ基板（ＡＰＰ−１００、ＰＥＮ、ＨＯＹＡ株式会社製）を試料基板とし、砥石サイズ４０μｍ、１２μｍ、３μｍ のサンドペーパーで鏡面研磨処理した後に１Ｎ ＨＣｌ溶液にて室温で１分脱灰させた。この試料基板の表面に、実施例１〜１１及び比較例１〜３で得られた各顆粒１３質量部に対し、グリセリン分散溶液８７質量部をのせて１分間作用させ、次に試料基板をイオン交換水で１０秒間洗浄した。なお、比較例２では、顆粒１３質量部に対し、グリセリン分散溶液８６質量部、及びパルミチン酸１質量部として作用させた。
<< Biofilm formation suppression rate (%) >>
Using a HAp substrate (APP-100, PEN, manufactured by HOYA Corporation) as a sample substrate, it was mirror-polished with sandpaper having a grindstone size of 40 μm, 12 μm, and 3 μm, and then decalcified with a 1N HCl solution at room temperature for 1 minute. On the surface of this sample substrate, 87 parts by mass of the glycerin dispersion solution was placed on 13 parts by mass of each of the granules obtained in Examples 1 to 11 and Comparative Examples 1 to 3 and allowed to act for 1 minute, and then the sample substrate was ionized. Washed with replacement water for 10 seconds. In Comparative Example 2, 13 parts by mass of the granules were allowed to act as 86 parts by mass of the glycerin dispersion solution and 1 part by mass of palmitic acid.
次いで、洗浄後の各試料基板を唾液上清（室温条件下において３０００ｒｐｍ １０分遠心分離処理）の５％スクロース液に浸漬させ、３７℃の嫌気性条件下において２４時間静置させた。その後、イオン交換水で５分間振とう洗浄し、歯垢染色液に５分浸漬させた後、イオン交換水による５分間振とう洗浄を２回行った。乾燥後の試料基板に１Ｎ ＮａＯＨ ５００μＬを添加して色素を抽出し、λ＝５４０ｎｍの吸光度を測定した。何も作用させなかった未処理の基板（コントロール基板）の吸光度を１００とした場合の各試料基板における色素抽出率を算出し、下記式（Ｘ）にしたがって、バイオフィルム形成抑制率を算出し、同じ操作を５回繰り返した平均値を測定値とした。
結果を図１及び表１に示す。
バイオフィルム形成抑制率（％）
＝(１−（試料基板の吸光度）／コントロール基板の吸光度)×１００・・・（Ｘ）
Next, each sample substrate after washing was immersed in a 5% sucrose solution of saliva supernatant (centrifugation treatment at 3000 rpm for 10 minutes under room temperature conditions), and allowed to stand for 24 hours under anaerobic conditions at 37 ° C. Then, it was shake-washed with ion-exchanged water for 5 minutes, immersed in a plaque stain for 5 minutes, and then shake-washed with ion-exchanged water for 5 minutes twice. 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. The dye extraction rate in each sample substrate was calculated when the absorbance of the untreated substrate (control substrate) on which nothing was applied was set to 100, and the biofilm formation suppression rate was calculated according to the following formula (X). The average value obtained by repeating the same operation 5 times was used as the measured value.
The results are shown in FIG. 1 and Table 1.
Biofilm formation inhibition rate (%)
= (1- (absorbance of sample substrate) / absorbance of control substrate) × 100 ... (X)
《風味の評価》
実施例４、９〜１１及び比較例１、３で得られた顆粒について、１名のパネラーにより風味の評価を行った。かかる評価には、バイオフィルム形成抑制率の算出の際に作製した試料を用い、これを５ｍＬ含漱し、歯ブラシ（チェック、花王株式会社製）を用いてブラッシングした後、水で漱ぎ、風味（脂肪酸由来の油風味の有無）を官能評価した。
評価基準としては、１〜５の５段階によるポイント評価を採用した。かかるポイントの値が大きい程、良好な結果であることを示す。
結果を表２に示す。
《Evaluation of flavor》
The granules obtained in Examples 4, 9 to 11 and Comparative Examples 1 and 3 were evaluated for flavor by one panelist. For this evaluation, the sample prepared when calculating the biofilm formation inhibition rate was used, 5 mL of this was rinsed, brushed with a toothbrush (Check, manufactured by Kao Corporation), rinsed with water, and flavored (). The presence or absence of fatty acid-derived oil flavor) was sensorimetrically evaluated.
As an evaluation standard, a point evaluation based on 5 grades of 1 to 5 was adopted. The larger the value of such points, the better the result.
The results are shown in Table 2.
表１及び図１の結果より、成分（Ａ）に成分（Ｂ）を担持させなかった比較例１、顆粒とは独立して成分（Ｂ）を作用させた比較例２、及び成分（Ｂ）の代わりにラウリン酸（炭素数１２）を成分（Ａ）に担持させた比較例３に比して、実施例１〜１１の顆粒は、バイオフィルム形成抑制効果に優れることがわかる。 From the results of Table 1 and FIG. 1, Comparative Example 1 in which the component (B) was not supported on the component (A), Comparative Example 2 in which the component (B) was allowed to act independently of the granules, and the component (B). It can be seen that the granules of Examples 1 to 11 are superior in the biofilm formation inhibitory effect as compared with Comparative Example 3 in which lauric acid (12 carbon atoms) is supported on the component (A) instead of.
また、表２の結果より、比較例１、３は口に含んだ際に脂肪酸由来の油風味を感じ、不快感が後に残った一方、実施例４、９〜１１では、脂肪酸由来の油風味や亜鉛味がほとんど感じられず、良好な風味を呈し、高い使用感をもたらすことがわかる。 In addition, from the results in Table 2, Comparative Examples 1 and 3 felt a fatty acid-derived oil flavor when they were taken in the mouth, and the discomfort remained afterwards, while in Examples 4, 9 to 11, the fatty acid-derived oil flavor was left. It can be seen that almost no zinc or zinc taste is felt, a good flavor is exhibited, and a high usability is brought about.
［実施例１２］
表３に示す歯磨剤用顆粒の処方にしたがい、実施例４と同様にして顆粒を得た。得られた顆粒を用い、表３に示す歯磨剤組成物の処方にしたがって、歯磨剤を製造し、下記方法にしたがって、歯垢形成抑制率（％）を求め、また使用感の評価も行った。
[Example 12]
Granules were obtained in the same manner as in Example 4 according to the formulation of the dentifrice granules shown in Table 3. Using the obtained granules, a dentifrice was produced according to the formulation of the dentifrice composition shown in Table 3, the plaque formation inhibition rate (%) was determined according to the following method, and the usability was also evaluated. ..
［比較例４〜５］
表３に示す歯磨剤用顆粒の処方にしたがい、比較例１と同様にして顆粒を得た。得られた顆粒を用い、表３に示す歯磨剤組成物の処方にしたがって、歯磨剤を製造し、下記方法にしたがって、歯垢形成抑制率（％）を求め、また使用感の評価も行った。
[Comparative Examples 4 to 5]
Granules were obtained in the same manner as in Comparative Example 1 according to the formulation of the dentifrice granules shown in Table 3. Using the obtained granules, a dentifrice was produced according to the formulation of the dentifrice composition shown in Table 3, the plaque formation inhibition rate (%) was determined according to the following method, and the usability was also evaluated. ..
《in vitroでのバイオフィルム形成抑制率（％）》
ＨＡｐ基板（ＡＰＰ−１００、ＰＥＮ、ＨＯＹＡ株式会社製）を試料基板とし、砥石サイズ４０μｍ、１２μｍ、３μｍ のサンドペーパーで鏡面研磨処理した後に１Ｎ ＨＣｌ溶液にて室温で１分脱灰させた。この試料基板の表面に、実施例１２および比較例４〜５で得られた歯磨剤を約１ｇのせて１分間作用させ、次に試料基板をイオン交換水で１０秒間洗浄した。
<< In vitro biofilm formation inhibition rate (%) >>
Using a HAp substrate (APP-100, PEN, manufactured by HOYA Corporation) as a sample substrate, it was mirror-polished with sandpaper having a grindstone size of 40 μm, 12 μm, and 3 μm, and then decalcified with a 1N HCl solution at room temperature for 1 minute. About 1 g of the dentifrice obtained in Example 12 and Comparative Examples 4 to 5 was placed on the surface of the sample substrate and allowed to act for 1 minute, and then the sample substrate was washed with ion-exchanged water for 10 seconds.
次いで、洗浄後の試料基板を唾液上清（室温条件下において３０００ｒｐｍ １０分遠心分離処理）の５％スクロース液に浸漬させ、３７℃の嫌気性条件下において２４時間静置させた。その後、イオン交換水で５分間振とう洗浄し、歯垢染色液に５分浸漬させた後、イオン交換水による５分間振とう洗浄を２回行った。乾燥後の基板に１Ｎ ＮａＯＨ ５００μＬを添加して色素を抽出し、λ＝５４０ｎｍの吸光度を測定した。何も作用させなかった未処理の基板（コントロール基板）の吸光度を１００とした場合の各試料基板における色素抽出率を算出し、上記式（Ｘ）にしたがって、バイオフィルム形成抑制率を算出し、同じ操作を５回繰り返した平均値を測定値とした。
結果を表２及び図２に示す。
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 for 24 hours under anaerobic conditions at 37 ° C. Then, it was shake-washed with ion-exchanged water for 5 minutes, immersed in a plaque stain for 5 minutes, and then shake-washed with ion-exchanged water for 5 minutes twice. 500 μL of 1N NaOH was added to the dried substrate to extract the dye, and the absorbance at λ = 540 nm was measured. The dye extraction rate in each sample substrate was calculated when the absorbance of the untreated substrate (control substrate) on which nothing was applied was set to 100, and the biofilm formation suppression rate was calculated according to the above formula (X). The average value obtained by repeating the same operation 5 times was used as the measured value.
The results are shown in Table 2 and FIG.
《ヒト試験での歯垢形成抑制率（％）》
実施例１２、比較例４で得られた歯磨剤を用い、以下の方法にしたがって、被験者５名によるヒト試験を行った。
まず、歯科衛生士が各被験者の歯面清掃（空ブラシ、スケーリング）を行った。次に、２時間以上経過した後、歯科衛生士が実施例１２で得られた歯磨剤を用い、各被験者歯面清掃を２分間行った。次いで２４時間ブラッシングを停止した後、観察部位を上顎左と下顎右の６番、上顎右と下顎左の１番、４番とし、各歯の近遠心頬側隅角部２点、頬側中央１点、舌側近遠心頬側隅角部２点、舌側中央１点の合計３６点とし、各々の部位の歯垢量を計測した。測定は歯科衛生士が各被験者の歯垢を染色した後に行い、１ｍｍ単位のメジャーを当てて、歯肉辺縁より何ｍｍの高さまで染色されているかを０．５ｍｍ単位で読み取り、歯垢付着量を測定した。次いで、得られた値を元に、下記式（Ｙ）にしたがって、歯垢形成抑制率を算出した。
かかる測定から１週間前後空けた後、同様の方法にしたがって、比較例４で得られた歯磨剤を用いて歯垢付着量を測定し、下記式（Ｙ）にしたがって、歯垢形成抑制率を算出した。上記のヒト試験を計５名の被験者に対して行い、各々の歯垢形成抑制率の平均値を評価の指標とした。
結果を図３に示す。
歯垢形成抑制率（％）＝(歯磨剤使用時の歯垢形成量（ｍｍ）／空ブラッシング時の 歯垢形成量（ｍｍ）)×１００・・・（Ｙ）
《Plaque formation inhibition rate (%) in human test》
Using the dentifrices obtained in Example 12 and Comparative Example 4, a human test was conducted by 5 subjects according to the following method.
First, a dental hygienist cleaned the tooth surface of each subject (empty brush, scaling). Next, after 2 hours or more, a dental hygienist cleaned the tooth surface of each subject for 2 minutes using the dentifrice obtained in Example 12. Next, after stopping brushing for 24 hours, the observation sites were maxillary left and mandibular right No. 6, maxillary right and mandibular left No. 1 and 4, and each tooth was mesio-distal buccal corner 2 points and buccal center. A total of 36 points, 1 point, 2 points on the lingual mesio-distal buccal corner, and 1 point on the center of the lingual side, were used, and the amount of dentition in each part was measured. The measurement is performed after the dental hygienist stains the plaque of each subject, and a measure of 1 mm unit is applied to read the height of the stain from the gingival margin in 0.5 mm units, and the amount of plaque adhered. Was measured. Then, 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, the amount of plaque adhesion was measured using the dentifrice obtained in Comparative Example 4 according to the same method, 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 suppression rate (%) = (plaque formation amount when using dentifrice (mm) / plaque formation amount when empty brushing (mm)) x 100 ... (Y)
《使用感の評価》
実施例１２、比較例４〜５で得られた歯磨剤を用い、１名のパネラーにより風味の評価を行った。具体的には、各歯磨剤１ｇを歯面に塗布し、歯ブラシ（チェック、花王株式会社製）を用いてブラッシングした後に口を水で漱ぎ、１〜５の５段階によるポイント評価により、歯面におけるつるつる感及びその持続性と、香味（脂肪酸由来の油風味の有無）の評価を行った。数値が高い程、良好な結果であることを示す。
結果を表３に示す。
《Evaluation of usability》
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), the mouth is rinsed with water, and the tooth surface is evaluated by points from 1 to 5 on a 5-point scale. The slippery feeling and its persistence, and the flavor (presence or absence of oil flavor derived from fatty acid) were evaluated. The higher the number, the better the result.
The results are shown in Table 3.
表３及び図３の結果より、顆粒とは独立して成分（Ｂ）を作用させた比較例４、及び成分（Ａ）に成分（Ｂ）を担持させなかった比較例５に比して、実施例１２の歯磨剤は、高い歯垢形成抑制効果を示すとともに、歯面におけるつるつるとした感触を良好に持続できることがわかる。
また、使用感についても、比較例４では、口を漱いだ後に脂肪酸由来の油風味が感じられ、後にまでその風味が残ったのに比して、実施例１２では、脂肪酸由来の油風味や亜鉛味が感じられず、良好な香味を呈し、使用感に優れることもわかる。
From the results of Table 3 and FIG. 3, compared with Comparative Example 4 in which the component (B) was allowed to act independently of the granules, and Comparative Example 5 in which the component (B) was not supported on the component (A). It can be seen that the dentifrice of Example 12 exhibits a high effect of suppressing plaque formation and can maintain a smooth feel on the tooth surface satisfactorily.
Regarding the feeling of use, in Comparative Example 4, the oil flavor derived from fatty acid was felt after rinsing the mouth, and the flavor remained until later, whereas in Example 12, the oil flavor derived from fatty acid was felt. It can also be seen that it does not have a zinc or zinc taste, exhibits a good flavor, and is excellent in usability.
Claims (8)
（Ａ）水不溶性粉体材料、並びに珪酸ナトリウム及び／又は酸化亜鉛を含む造粒物、及び
（Ｂ）炭素数１４以上２２以下の、飽和又は不飽和脂肪酸或いはこれらの塩
を含有し、成分（Ａ）に成分（Ｂ）が担持されている顆粒であり、かつ
平均粒径が５０μｍ以上５００μｍ以下であり、崩壊強度が湿潤状態で０．２ｇｆ／個以上３０ｇｆ／個以下である歯磨剤用顆粒。 The following components (A) and (B):
Contains (A) water-insoluble powder material , granules containing sodium silicate and / or zinc oxide , and (B) saturated or unsaturated fatty acids having 14 or more and 22 or less carbon atoms or salts thereof, and components ( Granules for dentifrices in which the component (B) is carried in A), the average particle size is 50 μm or more and 500 μm or less, and the disintegration strength is 0.2 gf / piece or more and 30 gf / piece or less in a wet state. ..
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| JPH0621053B2 (en) * | 1988-05-25 | 1994-03-23 | 花王株式会社 | Toothpaste |
| JP3514777B2 (en) * | 1991-01-25 | 2004-03-31 | 花王株式会社 | Oral composition |
| EP1383476A1 (en) * | 2001-04-24 | 2004-01-28 | Specialty Minerals (Michigan) Inc. | Fluoride compatible calcium carbonate |
| JP5627074B2 (en) * | 2009-12-11 | 2014-11-19 | 花王株式会社 | Dentifrice composition |
| JP6006499B2 (en) * | 2012-01-31 | 2016-10-12 | 花王株式会社 | Dentifrice |
| JP6139994B2 (en) * | 2012-06-20 | 2017-05-31 | 花王株式会社 | Process for producing dentifrice granules |
| JP5961456B2 (en) * | 2012-06-20 | 2016-08-02 | 花王株式会社 | Process for producing dentifrice granules |
| JP6387288B2 (en) * | 2013-11-25 | 2018-09-05 | 花王株式会社 | Dentifrice granules |
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