JP2003192555A - Dentifrice composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain a dentifrice composition having excellent control effect on foul breath and appearance even after long-term preservation. <P>SOLUTION: This dentifrice composition contains a synthetic amorphous silicate, which comprises zirconium bonded as ZrO<SB>2</SB>to SiO<SB>2</SB>in the ratio of 1.5-3.5 mass % and has diffraction peaks at X-ray diffraction angle 2θ=21-23° (d=4.07-4.09) and 2θ=35-37° (d=2.48-2.50) when fired at 900°C for one hour and pH 8.8-10.5 in 5 mass % slurry, as an abrasive and a copper compound and has excellent compatibility with fluorine. <P>COPYRIGHT: (C)2003,JPO

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dentifrice composition having an excellent effect of suppressing bad breath even after long-term storage and having a good appearance. 2. Description of the Related Art
It is known that water-soluble copper compounds such as copper gluconate and copper citrate have an antibacterial effect, an effect of removing bad breath, and an effect of inhibiting plaque formation, and various dentifrice compositions containing these copper compounds have been proposed. (U.S. Pat. Nos. 3,044,939, 3,565,933, 3,655,868, and 411)
No. 2066, JP-A-56-169519 and JP-A-56-1
No. 69620, No. 61-143317, No. 62-14
2109, JP-A-1-153620, 1-153
622). However, a dentifrice composition containing the above-mentioned copper compound is not sufficiently effective in removing bad breath, and is inferior in stability and appearance during long-term storage. The development of a dentifrice composition having an excellent appearance has been desired. Means for Solving the Problems and Embodiments of the Invention The present inventors have conducted intensive studies to meet the above-mentioned demand, and as a result, a specific abrasive, that is, zirconium has been converted to ZrO _{2 by} SiO _2. X-ray diffraction angle 2θ when baked at 900 ° C. for 1 hour
21 to 23 ° (d = 4.07 to 4.09) and 2θ = 35
A synthetic amorphous silicate having a diffraction peak at ３７37 ° (d = 2.48 to 2.50) and a pH of 5% by mass of the slurry of 8.8 to 10.5 was prepared by adding a copper gluconate or the like. The present inventors have found that a dentifrice composition excellent in bad breath suppression effect and excellent in appearance can be obtained even after long-term storage by using it together with a copper compound, and the present invention has been accomplished. Hereinafter, the present invention will be described in more detail. [0006] The dentifrice composition of the present invention has a zirconium content of Z
X-ray diffraction angle 2θ = 21 to 23 ° (d = 20%) when rO ₂ is bonded to SiO _{2 in} a range of 1.5 to 3.5% (mass percentage, the same applies hereinafter) and fired at 900 ° C. for 1 hour. 4.0
7 to 4.09) and 2θ = 35 to 37 ° (d = 2.48 to
2.50) having a diffraction peak and a 5% slurry p
A synthetic amorphous silicate having H of 8.8 to 10.5 is contained as an abrasive. In this case, a 5% slurry having a pH lower than 8.8 has poor compatibility with fluorine and has a pH of 10.5.
If it is higher, an adverse effect is exerted on the flavor, resulting in a disadvantage that the feeling of use is lowered. The silicate has a primary average particle diameter of 0.01 to 0.5 μm and an aggregated particle diameter of 1.5 to 30 μm.
μm is preferably used. Further, the one having a BET specific surface area of 5 to 800 m ² / g is preferable. The method for producing the above silicate is not particularly limited. For example, a water-soluble alkali metal silicate is charged in a reaction vessel in advance, and a water-soluble zirconium salt and a mineral acid are added thereto. When the obtained wet cake is dispersed in several times the amount of water and washed, the slurry p
A method of adjusting H can be adopted. The amount of the abrasive in the dentifrice is not necessarily limited, but is usually 1 to 50% (mass percentage, hereinafter the same), preferably 5 to 40% of the whole composition. In the present invention, a water-soluble copper compound is used in combination with the above-mentioned abrasive, whereby an excellent deodorizing effect and appearance can be obtained. In this case, the water-soluble copper compounds include copper gluconate, copper citrate, copper lauroyl sarcosine, copper formate, copper acetate, copper propionate, copper butyrate, copper lactate, copper oxalate, copper phytate, Organic acid copper such as copper tartrate, copper malate, copper succinate, copper malonate, copper maleate, copper benzoate, copper salicylate, copper aspartate, copper glutamate, copper fumarate, copper glycerophosphate, copper chlorophyllin sodium, Examples thereof include inorganic acid copper salts such as copper chloride, copper fluoride, copper sulfate, copper fluorosilicate, copper nitrate, copper fluoroborate, and copper iodate.In particular, organic acid copper, among which copper gluconate is preferably used. You. The amount of the water-soluble copper compound is desirably 0.0001 to 5%, preferably 0.001 to 2%, more preferably 0.05 to 1% of the whole composition. The dentifrice composition of the present invention comprises, in addition to the above silicate and copper compound, an abrasive, a thickener, a binder, a surfactant, a sweetener, a preservative, an active ingredient, a coloring matter, a flavor and the like. Can be blended, and these components can be mixed with water to produce. As the abrasive, it is possible to use in combination with one or more of the following in addition to the above silicate. That is, as such abrasives, silica-based abrasives such as silica gel, precipitated silica, igneous silica, aluminosilicate, zirconosilicate, dibasic calcium phosphate dihydrate, dibasic calcium phosphate anhydrate, calcium pyrophosphate, water Aluminum oxide, alumina, titanium dioxide, crystalline zirconium silicate, polymethyl methacrylate, insoluble calcium metaphosphate, light calcium carbonate, heavy calcium carbonate, magnesium carbonate, tribasic magnesium phosphate, zeolite, zirconium silicate, tribasic calcium phosphate, Examples include hydroxyapatite, fluoroapatite, calcium-deficient apatite, quaternary calcium phosphate, octacalcium phosphate, and synthetic resin-based abrasives. As the thickener, one or more of glycerin, sorbitol, propylene glycol, polyethylene glycol having a molecular weight of 200 to 6000, polyhydric alcohol such as reduced starch saccharified product, and the like can be used. Examples of the binder include xanthan gum, sodium alginate, sodium polyacrylate, propylene glycol alginate, carboxymethyl cellulose, polyvinyl alcohol, hydroxyethyl cellulose, carrageenan, carbopol, guar gum, gelatin, Avicel, montmorillonite, kaolin, bentonite and the like. Inorganic binders and the like. Examples of the surfactant include an anionic surfactant, a cationic surfactant, and a nonionic surfactant. Specific examples thereof include sodium lauryl sulfate, sodium N-lauroyltaurine, N-acyl sarcosinate, α-olefin sulfone. Acid sodium, N-acyl glutamate, 2-
Alkyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, N-acyl taurate,
Sucrose fatty acid ester, alkylol amide, polyoxyethylene sorbitan monostearate, pluronic, decaglyceryl laurate and the like. As sweeteners, sodium saccharin,
As preservatives such as aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, perillartin,
Examples thereof include parabens such as butylparaben and ethylparaben, paraoxybenzoic acid esters, and sodium benzoate. Various active ingredients include fluorides such as sodium fluoride, potassium fluoride, stannous fluoride, strontium fluoride and sodium monofluorophosphate, and water-soluble compounds such as potassium and sodium orthophosphates. Phosphate compounds, allantoinchlorohydroxyaluminum, hinokitiol, ascorbic acid, lysozyme chloride, glycyrrhizic acid and salts thereof, sodium chloride, tranexamic acid, epsilon aminocaproic acid, dl-tocopherol acetate, dihydrocholesterol, α-bisabolol, isopropylmethylphenol, chlorhexidine Salts, triclosan, biosol, cetylpyridinium chloride, azulene, glycyrrhetin, glycyrrhetinic acid,
Chelating phosphate compounds such as sodium copper chlorophyllin, chlorophyll, glycerophosphate, aluminum lactate, strontium chloride, potassium nitrate, berberine, hydroxamic acid and its derivatives, sodium tripolyphosphate, zeolite, methoxyethylene, maleic anhydride copolymer, polyvinylpyrrolidone , Epidihydrocholesterine, benzethonium chloride, sodium chloride,
Extracts such as dihydrocholesterol, trichlorocarbanilide, zinc citrate, soft oyster extract, oak extract, chamomile, clove, rosemary, red gourd, safflower and the like can be mentioned. Examples of the flavor include l-menthol, carvone, anethole, cineole, methyl salicylate, limonene, ethyl butyrate, eugenol, thymol,
Perfume ingredients such as cinnamaldehyde or derivatives thereof,
Essential oil components such as peppermint and spearmint are exemplified,
Examples of the colorant include Blue No. 1, Yellow No. 4, Green No. 3, and the like. [0022] The amounts of these components can be set as usual within a range not to impair the effects of the present invention. EFFECT OF THE INVENTION The dentifrice composition of the present invention has an excellent effect of suppressing bad breath even after long-term storage, and has a good appearance. EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples. In the following examples,% indicates mass percentage. Examples 1-3 and Comparative Examples 1-4 Toothpaste compositions having the formulations shown in Table 1 were prepared according to a conventional method. The appearance and deodorization rate of the obtained toothpaste composition were evaluated by the following methods. The abrasives A to F used are as shown in Table 2. Table 1 shows the results. <Test Method> Appearance: A toothpaste composition was filled in a tube, and this was heated to 40 ° C.
After storing for one month in a thermostat adjusted to the above, the degree of discoloration of this composition was compared with that stored at −5 ° C. according to the following evaluation criteria. Discoloration evaluation point 3 points: no discoloration is observed compared to the product stored at -5 ° C 2 points: discoloration is slightly observed compared to the product stored at -5 ° C 1 point: discoloration compared to the product stored at -5 ° C Evaluation of deodorizing power in which 1.5 ml of a 0.1 M phosphate buffer solution and 0.5 ml of a 2000-fold diluted solution of a sample (composition) were placed in a test tube having a content of 20 ml, and a 2 ppm methyl mercaptan ethanol aqueous solution was added. 5 ml was added, the mixture was immediately closed with a rubber stopper, lightly stirred, and shaken in a 37 ° C. constant temperature bath for 6 minutes. Thereafter, 10 ml of the head space of the test tube was collected with a gas tight syringe and injected into a gas chromatograph. The deodorization rate was determined from the following equation. Deodorization rate = [(CS) / C] × 100 (%) C: methyl mercaptan area of control S: methyl mercaptan area of sample [Table 2] Example 4 Abrasive A 15% Copper Gluconate 0.3 Sodium Bicarbonate 0.6 Sodium Tripolyphosphate 3 Sodium Fluoride 0.21 Fragrance 1 Propylene Glycol 3 85% Glycerin 30 Carboxymethyl Cellulose 1.2 Triclosan 0.5 sodium lauryl sulfate 1.2 saccharin sodium 0.1 purified water balance total 100.0% [0030] example 5 abrasive A 15% copper gluconate 0.3 sodium 0.6 sodium tripolyphosphate bicarbonate 3 Sodium fluoride 0.21 Fragrance 1 Propylene glycol 3 85% glycerin 30 Gellan gum 0.3 Carboxymethyl cellulose 0.8 Sodium lauryl sulfate 1.2 Saccharin sodium 0.1 Lauroyl sarcosine sodium 0.2 Purified water balance [Example 6] Abrasive B 18% Copper gluconate 0.3 Sodium bicarbonate 0.6 Sodium tripolyphosphate 3 Sodium fluoride 0.21 Fragrance 1 Propylene glycol 3 70% sorbite solution 30 carboxymethylcellulose 1.4 lauryl 1.5 saccharin sodium 0.1 sodium lauroyl sarcosinate 0.2 purified water balance total 100.0% sodium sulfate [0032] example 7 abrasive B 18% copper gluconate 0.3 sodium bicarbonate 0.6 sodium tripolyphosphate 3 sodium fluoride 0.21 perfume 1 propylene glycol 3 70% sorbitol solution 20 Pluronic 15 saccharin sodium 0.1 sodium lauroyl sarcosinate 0.2 purified water balance total 100.0% [0 Example 8 Abrasive C 18% Copper Gluconate 0.5 Sodium Bicarbonate 0.3 Sodium Tripolyphosphate 1.0 Sodium Fluoride 0.21 Fragrance 1 Propylene Glycol 3 70% Sorbit Solution 30 Xanthan Gum 0.6 sodium 0.5 sodium lauryl sulfate alginate 1.5 saccharin sodium 0.1 sodium lauroyl sarcosinate 0.2 purified water balance total 100.0% [0034] example 9 abrasive C 18% copper gluconate 0.5 carbonate Sodium hydrogen 0.3 Sodium tripolyphosphate 1.0 Sodium fluoride 0.21 Fragrance 1 Propylene glycol 3 70% sorbite solution 30 Xanthan gum 0.6 Iota carrageenan 0.5 Sodium lauryl sulfate 1.5 Sodium saccharin 0.1 Lauroyl Turkey Shin sodium 0.2 Purified water balance Total 100.0% [0035] Example 10 abrasive A 15% copper gluconate 0.5 Sodium fluoride 0.21 Perfume 1 Propylene glycol 3 85% glycerine 30 carboxy methylcellulose 1.2 saccharin sodium 0.1 0.01 triclosan 0.3 purified water balance total 100.0% lauryl sodium 1.2 cetylpyridinium chloride sulfate [0036] example 11 abrasive B 18% copper gluconate 0 0.5 sodium fluoride 0.21 fragrance 1 propylene glycol 3 85% glycerin 30 xanthan gum 0.6 iotacarrageenan 0.5 xylitol 10 sodium lauryl sulfate 1.0 lauryl sarcosine sodium 0.2 myristate diethanolamide 1.2 copper chloride B Villingen sodium 0.15 Purified water balance Total 100.0% [0037] Example 12 abrasive C 18% copper gluconate 0.5 Sodium fluoride 0.21 Perfume 1 Propylene glycol 3 70% sorbitol solution 30 xanthan gum 0.6 sodium alginate 0.5 sodium saccharin 0.1 sodium lauryl sulfate 1.5 sodium lauryl sarcosine 0.2 isopropylmethylphenol 0.1 benzethonium chloride 0.01 purified water balance total 100.0%

   ────────────────────────────────────────────────── ─── Continuation of front page    F-term (reference) 4C083 AB282 AB312 AB371 AB372                       AB471 AB472 AC122 AC132                       AC301 AC302 AC472 AC642                       AC662 AC692 AC782 AC812                       AC862 AC931 AC932 AD052                       AD272 AD302 AD352 BB41                       CC41 DD22 DD27 DD39 DD41                       EE01 EE34 EE36 FF01

Claims (1)

Claims: 1. An X-ray diffraction angle 2θ when zirconium is bonded as ZrO ₂ to SiO _{2 in} a range of 1.5 to 3.5 mass% with respect to SiO _{2 and} fired at 900 ° C. for 1 hour = 21-23 °
(D = 4.07 to 4.09) and 2θ = 35 to 37 ° (d
= 2.48-2.50) and a synthetic amorphous silicate having a pH of 8.8-10.5 having a diffraction peak at 5% by mass of a slurry as an abrasive, and a copper compound containing A dentifrice composition having excellent compatibility with fluorine, characterized by containing.