JP2004250456A - Dentifrice - Google Patents

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JP2004250456A
JP2004250456A JP2004133387A JP2004133387A JP2004250456A JP 2004250456 A JP2004250456 A JP 2004250456A JP 2004133387 A JP2004133387 A JP 2004133387A JP 2004133387 A JP2004133387 A JP 2004133387A JP 2004250456 A JP2004250456 A JP 2004250456A
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granules
dentifrice
wet
silica granules
silica
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JP4694794B2 (en
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Yoshiyuki Muroi
愛行 室井
Yasuteru Eguchi
泰輝 江口
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Kao Corp
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Kao Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To easily produce a low-cost dentifrice by compounding granules using no binder into the dentifrice. <P>SOLUTION: This dentifrice contains wet-method silica granules with such a granular size that the granules pass through a 30-mesh sieve but does not pass through a 200-mesh sieve. The silica granules have a breaking strength per granule of 30-800 gf/mm<SP>2</SP>and a grinding force with a RDA (radioactive dentine abrasion) value of ≤150. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

本発明は、湿式法シリカ顆粒入り歯磨剤に関し、詳しくは顆粒の審美的効果と口腔内での顆粒の感触により汚れ落とし効果を認識でき、また、この顆粒が口腔内で触知できる程度の強度と大きさを有しているにもかかわらず、歯磨の過程で徐々に崩壊していくために不愉快な異物感を与えない歯磨剤に関する。   The present invention relates to a dentifrice containing wet-processed silica granules, and more specifically, an aesthetic effect of the granules and a touch of the granules in the oral cavity so that the effect of removing dirt can be recognized, and the granules have such strength as to be perceptible in the oral cavity. The present invention relates to a dentifrice that does not give an unpleasant foreign body sensation because it gradually disintegrates in the process of dentifrice, despite having such a size.

顆粒や顆粒状の物質を配合した歯磨剤は従来から知られている。かかる顆粒には、薬剤、酵素剤、研磨剤等の機能性材料を含有させたものや、その審美的効果を目的としたものがある。これら顆粒の結合剤としてはメチルセルロース、カルボキシメチルセルロース等の水溶性結合剤やワックス、エチルセルロース等の水不溶性結合剤が使われてきたが、上記水溶性結合剤を用いた場合、歯磨製造時の混合過程で顆粒が崩壊したりする等の問題があり、また、上記水不溶性結合剤を用いた場合、触知し得る程度に顆粒の硬度と大きさを調整すると、顆粒が口腔内で異物感として捉えられたりする等の問題があった。   Dentifrices containing granules or granular substances have been conventionally known. Such granules include those containing a functional material such as a drug, an enzyme agent, and an abrasive, and those intended for the aesthetic effect thereof. As a binder for these granules, a water-soluble binder such as methylcellulose and carboxymethylcellulose and a water-insoluble binder such as wax and ethylcellulose have been used. In addition, there are problems such as the disintegration of the granules, and when the above water-insoluble binder is used, if the hardness and size of the granules are adjusted to the extent that they can be perceived, the granules are perceived as foreign matter in the oral cavity And other problems.

そこで、本出願人は、先にかかる問題点を解消した歯磨剤として、ゼオライト等の水不溶性粉末材料を水不溶性無機結合剤で結着させて得られる顆粒入りの歯磨剤を提案した(特許文献1)。この歯磨剤は、水不溶性粉末材料を水不溶性結合剤で造粒し、一定の大きさと強度を保持した顆粒を配合したものであるため、口腔内において顆粒を触知でき、効果感を認識できるにもかかわらず、異物感をほとんど感ずることがなく、また、歯を傷つけることなく研磨力が増強されたものである。
特開平1−299211号公報
Accordingly, the present applicant has proposed a dentifrice containing granules obtained by binding a water-insoluble powder material such as zeolite with a water-insoluble inorganic binder as a dentifrice that has solved the above problems (Patent Documents) 1). This dentifrice is made by granulating a water-insoluble powder material with a water-insoluble binder and blending granules having a certain size and strength, so that the granules can be palpated in the oral cavity and the effect can be recognized. Nevertheless, the abrasive force is enhanced without substantially feeling the foreign substance sensation and without damaging the teeth.
JP-A-1-299211

しかしながら、上記歯磨剤に配合されている顆粒は、その製造の際に結合剤を必要とするために高価であるという問題がある。
従って、結合剤を使用しないで製造した顆粒を配合し、かつ上記歯磨剤と同程度又はそれ以上の性能を有する歯磨剤が要望されている。
However, there is a problem that the granules contained in the dentifrice are expensive because a binder is required for the production.
Therefore, there is a need for a dentifrice that incorporates granules produced without using a binder and has the same or better performance as the above dentifrice.

このような実情において、本発明者は鋭意検討を行った結果、湿式法シリカが結合剤なしで顆粒状とすることができ、この顆粒を配合した歯磨剤は口腔内において顆粒を触知でき、効果感を認識できるにもかかわらず、異物感をほとんど感ずることがなく、また、歯を傷つけることなく研磨力が増強されたものであることを見出し本発明を完成するに至った。   Under such circumstances, the present inventors have conducted intensive studies and as a result, the wet process silica can be made into granules without a binder, and the dentifrice containing the granules can palpate the granules in the oral cavity, Despite recognizing the effect, the inventor found that the feeling of foreign matter was hardly felt and the polishing power was enhanced without damaging the teeth, and the present invention was completed.

すなわち、本発明は、30メッシュ篩(JIS規格)を通過するが、200メッシュ篩(JIS規格)を通過しない粒径サイズを有し、1個当りの崩壊強度が30〜800gf/mm2 であり、研磨力がRDA値150以下である湿式法シリカ顆粒を含む歯磨剤を提供するものである。 That is, the present invention has a particle size that passes through a 30-mesh sieve (JIS standard) but does not pass through a 200-mesh sieve (JIS standard), and has a collapse strength per unit of 30 to 800 gf / mm 2 . Another object of the present invention is to provide a dentifrice containing wet-processed silica granules having an abrasive force of 150 or less in RDA value.

本発明で用いる湿式法シリカ顆粒は、30メッシュ篩を通過するが、200メッシュ篩を通過しない粒径サイズ(75〜500μm)であることが必要である。肉眼的に認知し、口腔内で触知するには75μm以上の粒径を必要とし、粒径が500μmを超えると口腔内でのざらつきが強くなり、使用感が悪くなる。また、平均粒径は150〜250μm であるのが好ましい。   The wet-processed silica granules used in the present invention need to have a particle size (75 to 500 μm) that passes through a 30-mesh sieve but does not pass through a 200-mesh sieve. A particle size of 75 μm or more is required to be visually perceived and palpable in the oral cavity. Further, the average particle size is preferably 150 to 250 μm.

湿式法シリカ顆粒の強度(硬さ)は、顆粒1個当り30〜800gf/mm2 で崩壊する強度であるが、40〜500gf/mm2 であることが特に好ましい。シリカ顆粒1個当りの崩壊強度が30gf/mm2 未満の場合、研磨力が十分ではなく、また、800gf/mm2 を超えると、異物としてしか感じられず、ブラッシングによっても全く崩壊しないため、歯のエナメル質を傷つける恐れがある。 Strength of the wet process silica granules (hardness) is a strength decay in granular per 30~800gf / mm 2, particularly preferably 40~500gf / mm 2. If the disintegration strength per silica granule is less than 30 gf / mm 2 , the abrasive power is not sufficient, and if it exceeds 800 gf / mm 2 , it is felt only as a foreign substance and does not disintegrate by brushing at all. May damage the enamel.

湿式シリカ顆粒の研磨力はRDA値(Radioactive Dentine Abrasion values)150以下であることが必要であり、特に100以下であることが好ましい。RDA値が150を超えると歯を必要以上に削る恐れがある。   The polishing power of the wet silica granules needs to be 150 or less, particularly preferably 100 or less, RDA value (Radioactive Dentine Abrasion values). If the RDA value exceeds 150, the teeth may be cut more than necessary.

湿式シリカ顆粒のBET法による比表面積及び細孔容積は、顆粒の崩壊強度、薬効成分及び香料の吸着量を制御する上で、それぞれ150〜450m2/g及び1〜2.5ml/gであることが好ましく、特に好ましくは200〜400m2/g及び1.5〜2.0ml/gである。 The specific surface area and pore volume according to the BET method of the wet silica granules are 150 to 450 m 2 / g and 1 to 2.5 ml / g, respectively, for controlling the disintegration strength of the granules, the medicinal component and the amount of adsorption of the fragrance. It is particularly preferably 200 to 400 m 2 / g and 1.5 to 2.0 ml / g.

本発明で用いる湿式法シリカは沈降法又はゲル法により例えば次のような製造法に従って製造することができる。   The wet silica used in the present invention can be produced by a precipitation method or a gel method, for example, according to the following production method.

(1)予めpHの調整されているシリカヒドロゾルを、これとは非親和性の油のような媒体中に懸濁させ、懸濁中に固化させて、不純物を洗浄除去後、乾燥する方法。
(2)シリカヒドロゾルを空気中に噴霧させてゲル化し、不純物を洗浄除去後、乾燥する方法。
(1) A method in which a silica hydrosol whose pH has been adjusted in advance is suspended in a medium such as an incompatible oil, solidified in the suspension, and impurities are washed and removed, followed by drying. .
(2) A method in which a silica hydrosol is sprayed into the air to form a gel, impurities are removed by washing, and then drying is performed.

本発明の歯磨剤中に配合される湿式法シリカ顆粒はこれらのどの方法によって得られたものであってもよい。   The wet-processed silica granules incorporated in the dentifrice of the present invention may be obtained by any of these methods.

このようにして得られる湿式法シリカ顆粒は、練り歯磨剤、粉歯磨剤など各種歯磨剤に配合できるが、顆粒の審美性を表現できる上で特に練り歯磨剤に配合することが好適である。
顆粒の配合量は歯磨剤中に1〜50重量%とすることが好ましく、3〜30重量%とすることが特に好ましい。
The wet-processed silica granules thus obtained can be blended with various dentifrices such as toothpastes and powdered dentifrices, but it is particularly preferable to blend them with toothpastes in order to express the aesthetics of the granules.
The content of the granules is preferably 1 to 50% by weight, particularly preferably 3 to 30% by weight in the dentifrice.

シリカは比表面積が大きいため、湿式法シリカ顆粒に薬用成分や香料を吸着させて歯磨剤に配合することにより、歯磨き時に崩壊したシリカ片が口腔内に吸着、残留し得るため、薬用成分や香料を徐放させることができる。   Since silica has a large specific surface area, by mixing a medicinal component or a fragrance into wet-process silica granules and blending it into a dentifrice, silica fragments that have collapsed during tooth brushing can be adsorbed and remain in the oral cavity. Can be released slowly.

薬用成分としては口腔領域で使用されるものであればよく、特に限定されるものではないが、例えば虫歯予防剤、抗微生物剤、ビタミン、酵素、抗炎症剤等が挙げられ、具体的にはフッ化ナトリウム、フッ化錫、モノフルオロリン酸ナトリウム、ビタミンE、ビタミンC、デキストラナーゼ、ムタナーゼ、塩化ナトリウム、グリチルレチン酸、アズレン、β−グリチルレチン酸、ジヒドコレステロール、クロルヘキシジン、エピジヒドコレステロール、イソプロピルメチルフェノール、トリクロロカルバニリド、ハロカルバン、ヒノキチオール、アラントイン、トラネキサム酸、プロポリス、塩化セチルピリジニウム等が挙げられ、これらは単独で又は2種以上を組み合わせて使用することができる。   The medicinal component is not particularly limited as long as it is used in the oral region, and examples thereof include a caries preventive agent, an antimicrobial agent, a vitamin, an enzyme, an anti-inflammatory agent, and the like. Sodium fluoride, tin fluoride, sodium monofluorophosphate, vitamin E, vitamin C, dextranase, mutanase, sodium chloride, glycyrrhetinic acid, azulene, β-glycyrrhetinic acid, dihydrocholesterol, chlorhexidine, epidihydrocholesterol, Examples thereof include isopropylmethylphenol, trichlorocarbanilide, halocarban, hinokitiol, allantoin, tranexamic acid, propolis, cetylpyridinium chloride, and the like, and these can be used alone or in combination of two or more.

また、香料としては例えばメントール及びメントールを含む天然物;バジル、カンファー、キャラウェイ、カルダモン、コリアンダー、ゼラニウム、ジンジャー、ローレル、ラベンダー、メース、ナツメグ、ペッパー、ローズ、ローズマリー、タイム、イランイラン、ジャスミン、バニラ、ヒソップ、ラバンジン、オリス、キャロットシード、ダバナ、エレミ、オスマンタスの精油及び抽出物;ボルネオール及びその誘導体;ヘリオトロピン;α−、β−、γ−、δ−イオノン及びこれらの誘導体;チモール、バニリン、エチルバニリン、マルトール並びにエチルマルトール等が挙げられ、これらは単独で又は2種以上を組み合わせて使用することができる。   Examples of fragrances include menthol and natural products containing menthol; basil, camphor, caraway, cardamom, coriander, geranium, ginger, laurel, lavender, mace, nutmeg, pepper, rose, rosemary, thyme, ylang ylang, jasmine. Essential oils and extracts of vanilla, hyssop, lavandin, oris, carrot seed, dabana, eremi, osmantas; borneol and its derivatives; heliotropin; α-, β-, γ-, δ-ionone and their derivatives; thymol, Examples thereof include vanillin, ethyl vanillin, maltol, and ethyl maltol, and these can be used alone or in combination of two or more.

本発明の歯磨剤の調製は常法に従って行われ、通常の歯磨剤に配合される他の成分を配合することができる。例えば粘結剤としては、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、増粘性シリカ、モンモリロナイト、カラギーナン、アルギン酸ナトリウム、グアガム、ペクチンなどが挙げられる。界面活性剤としては、アシルグルタミン酸ナトリウム、アシルサルコシンナトリウム等のアシルアミノ酸の塩類;ラウリルリン酸ナトリウム等のアルキルリン酸の塩類;ショ糖脂肪酸エステル、ソルビタン脂肪酸エステル、ポリオキシエチレン脂肪酸エステル、ポリオキシエチレンポリオキシプロピレンブッロク共重合体などが挙げられる。その他、前記と同様の薬用成分及び香料、湿潤剤、甘味剤、防腐剤等を配合することができる。   Preparation of the dentifrice of the present invention is carried out according to a conventional method, and other components which are added to a usual dentifrice can be added. Examples of the binder include sodium carboxymethylcellulose, sodium polyacrylate, hydroxyethylcellulose, thickening silica, montmorillonite, carrageenan, sodium alginate, guar gum, pectin, and the like. Examples of the surfactant include salts of acyl amino acids such as sodium acylglutamate and sodium acylsarcosine; salts of alkyl phosphoric acids such as sodium lauryl phosphate; sucrose fatty acid esters, sorbitan fatty acid esters, polyoxyethylene fatty acid esters, and polyoxyethylene. And polyoxypropylene block copolymers. In addition, the same medicinal components and flavors, humectants, sweeteners, preservatives, and the like as described above can be added.

本発明の歯磨剤に配合されている顆粒は結合剤を使用しないものであるため、安価にかつ容易に製造することができ、歯磨剤のコストを低減し得る利点がある。   Since the granules contained in the dentifrice of the present invention do not use a binder, they can be easily manufactured at low cost and have an advantage that the cost of the dentifrice can be reduced.

次に実施例を挙げて説明するが、本発明はこれらの実施例に限定されるものではない。   Next, the present invention will be described with reference to examples, but the present invention is not limited to these examples.

実施例1
一次粒子径4.0nmのシリカヒドロゾルを空気中に噴霧させてゲル化させ、精製水で洗浄後、乾燥させることにより湿式法シリカ顆粒を製造した。
Example 1
A silica hydrosol having a primary particle size of 4.0 nm was sprayed into the air to gel, washed with purified water, and dried to produce wet-process silica granules.

得られた顆粒は、30メッシュ篩を通過するが、200メッシュ篩を通過しない粒径(平均粒径200μm )を有し、200gf/mm2 の荷重を加えたときに崩壊し、研磨力はRDA値60であり、比表面積は280m2 /gであり、細孔容積は1.90ml/gのものであった。 The resulting granules have a particle size (average particle size 200 μm) that passes through a 30 mesh sieve but does not pass through a 200 mesh sieve, disintegrates when a load of 200 gf / mm 2 is applied, and the abrasive power is RDA The value was 60, the specific surface area was 280 m 2 / g, and the pore volume was 1.90 ml / g.

顆粒の感触を評価するために、製造した顆粒をそのまま表1に示す組成の歯磨剤に配合した。歯磨剤は香料の安定化のために製造後1週間放置した。その後、20人のパネラーにこの歯磨剤を使用してもらい、その直後に顆粒の感触について評価した。ハブラシは通常のラウンドカットハブラシを用いた。顆粒の口腔内の認知度及び顆粒の感触については次のように分類した。なお、顆粒の感触については顆粒を口腔内で認知したパネラーによって評価した。結果を表2に示す。   To evaluate the feel of the granules, the produced granules were directly blended into a dentifrice having the composition shown in Table 1. The dentifrice was left for one week after production for stabilization of the fragrance. Thereafter, 20 panelists were asked to use this dentifrice, and immediately afterwards, the feel of the granules was evaluated. A normal round cut toothbrush was used as the toothbrush. The degree of recognition of the granules in the oral cavity and the feel of the granules were classified as follows. The feel of the granules was evaluated by a panelist who recognized the granules in the oral cavity. Table 2 shows the results.

(顆粒の口腔内の認知度):
1;歯を磨き始めてから磨き終わるまで認知した。
2;歯磨き初期には顆粒を触知したが、歯磨き中に触知できなくなった。
3;顆粒を触知できなかった。
(Recognition of granules in the oral cavity):
1; Recognized from the start of brushing until the end of brushing.
2: Granules were palpable at the beginning of brushing, but could not be felt during brushing.
3: The granules could not be palpated.

(顆粒の感触):
1;良い。
2;やや良い。
3;どちらでもない。
4;やや悪い。
5;悪い。
(Granular feel):
1; good.
2; somewhat good.
3: Neither.
4: Somewhat bad.
5; bad.

Figure 2004250456
Figure 2004250456

Figure 2004250456
Figure 2004250456

試験例
表1に示した歯磨剤(本発明品)と表1に示した歯磨剤において湿式法シリカ顆粒の代わりに粒径10μmの湿式法シリカ15.0重量%を配合した歯磨剤(比較品)について清浄作用を調べた。歯磨剤1gを黒のマジックインキを塗布したガラス板に塗布してブラッシングし、肉眼で見てガラス板上のマジックシンキが完全に除去されたときのブラッシングの回数(試験を10回行ったときの平均)で判定した。ブラッシングの回数は、本発明品は4.7回、比較品は30.5回であった。
Test Example Dentifrice (comparative product) in which 15.0% by weight of wet-process silica having a particle size of 10 μm was blended instead of the wet-process silica granules in the dentifrice shown in Table 1 (the present invention) and the dentifrice shown in Table 1 ) Was tested for cleaning action. 1 g of dentifrice was applied to a glass plate coated with black magic ink and brushed, and the number of times of brushing when the magic sink on the glass plate was completely removed with the naked eye (when the test was performed 10 times) Average). The number of times of brushing was 4.7 for the product of the present invention and 30.5 for the comparative product.

実施例2〜4
下記表3に示す性状のシリカ顆粒を得て、表4に示す組成の練歯磨剤を調製した。これらの練歯磨は感触、清浄作用ともに良好であった。
Examples 2 to 4
Silica granules having the properties shown in Table 3 below were obtained, and a toothpaste having the composition shown in Table 4 was prepared. These toothpastes were good in both feel and cleansing action.

Figure 2004250456
Figure 2004250456

Figure 2004250456
Figure 2004250456

Claims (5)

30メッシュ篩を通過するが、200メッシュ篩を通過しない粒径サイズを有し、1個当りの崩壊強度が30〜800gf/mm2であり、研磨力がRDA値150以下である湿式法シリカ顆粒を含む歯磨剤。 Wet silica granules having a particle size that passes through a 30-mesh sieve but does not pass through a 200-mesh sieve, have a disintegration strength of 30 to 800 gf / mm 2 , and have an abrasive power of 150 or less RDA value. Dentifrice containing. 湿式法シリカ顆粒のBET法による比表面積が150〜450m2/gである請求項1記載の歯磨剤。 Dentifrice according to claim 1, wherein a BET specific surface area of the wet silica granules is 150~450m 2 / g. 湿式法シリカ顆粒の細孔容積が1〜2.5ml/gである請求項1又は2記載の歯磨剤。   The dentifrice according to claim 1 or 2, wherein the pore volume of the wet process silica granules is 1 to 2.5 ml / g. 湿式法シリカ顆粒の含有量が1〜30重量%である請求項1〜3のいずれかに記載の歯磨剤。   The dentifrice according to any one of claims 1 to 3, wherein the content of the wet-process silica granules is 1 to 30% by weight. 湿式法シリカ顆粒が沈降法又はゲル法により合成されたものである請求項1〜4のいずれかに記載の歯磨剤。   The dentifrice according to any one of claims 1 to 4, wherein the wet method silica granules are synthesized by a precipitation method or a gel method.
JP2004133387A 2004-04-28 2004-04-28 Dentifrice Expired - Fee Related JP4694794B2 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60214725A (en) * 1977-12-20 1985-10-28 ジエー.エム.フーバー コーポレーシヨン Dentifrice composition
JPS6287507A (en) * 1985-10-11 1987-04-22 Fuji Debuison Kagaku Kk Dentifrice agent
JPS62191415A (en) * 1985-12-03 1987-08-21 ユニリ−バ− ナ−ムロ−ゼ ベンノ−トシヤ−プ Amorphous sedimented silica
JPH01299211A (en) * 1988-05-25 1989-12-04 Kao Corp Dentifrice
JPH05186320A (en) * 1991-07-01 1993-07-27 Colgate Palmolive Co Dentifrice having low rda value for giving clean mouth feeling
JPH0912436A (en) * 1995-06-30 1997-01-14 Kao Corp Dentifrice

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60214725A (en) * 1977-12-20 1985-10-28 ジエー.エム.フーバー コーポレーシヨン Dentifrice composition
JPS6287507A (en) * 1985-10-11 1987-04-22 Fuji Debuison Kagaku Kk Dentifrice agent
JPS62191415A (en) * 1985-12-03 1987-08-21 ユニリ−バ− ナ−ムロ−ゼ ベンノ−トシヤ−プ Amorphous sedimented silica
JPH01299211A (en) * 1988-05-25 1989-12-04 Kao Corp Dentifrice
JPH05186320A (en) * 1991-07-01 1993-07-27 Colgate Palmolive Co Dentifrice having low rda value for giving clean mouth feeling
JPH0912436A (en) * 1995-06-30 1997-01-14 Kao Corp Dentifrice

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