JPS6287507A - Dentifrice agent - Google Patents

Abstract

PURPOSE:A transparent or semitransparent dentifrice agent, obtained by incorporating spherical fine silica gel as a polishing agent with other components and having improved feeling of use and desired polishing property. CONSTITUTION:A dentifrice agent containing spherical fine silica gel, consisting of three-dimensional aggregates of primary particles, having preferably 200-1,000m<2>/g specific surface area measured by the BET method, 0.1-1.5ml/g pore volume, 1.40-1.48 refractive index, <=30mu average particle diameter, <=45% moisture and >=40wt% particles having 2-50mu particle diameter in the particle size distribution thereof as a polishing agent. THe dentifrice agent has soft touch to teeth in use without damaging gums and scarcely causes cracking in polishing agent particles after cleaning teeth with improved cleaning characteristic and good feeling of use. Since the above-mentioned dentifrice agent contains no impurities reactive with fluoride ions, it is capable of thoroughly blending with fluorides to be incorporated at the same time and useful as a dentifrice agent for preventing dental caries.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a dentifrice. In particular, the present invention has excellent usability,
The present invention also relates to a transparent or opaque dentifrice having desired abrasive properties.

[Prior Art] Conventionally, amorphous silica gels such as precipitated silica gels, high-temperature silica gels, and silica aerogels have been blended as abrasives in dentifrices such as toothpastes. In addition, crushed silica xerogel is used as another abrasive. In addition, dibasic calcium phosphate, calcium carbonate, calcium pyrophosphate, insoluble sulfurium metaphosphate, aluminum oxide, resin, and the like are also used.

[Problems to be Solved by the Invention] Toothpaste is used morning and evening, and must not only feel pleasant to use, but also have an excellent cleaning effect through polishing. However, among the above-mentioned abrasives, for example, precipitated silica gel, high-temperature silica gel, silica aerogel, etc. are primary particles or weak combinations of primary particles, so they have poor oral cleaning properties or polishing properties, and are not used as abrasives for tooth brushing. was not satisfactory.

In addition, although conventional crushed silica xerogel has particle hardness sufficient to exhibit a sufficient polishing effect, it contains irregularly shaped and angular particles, which can damage tooth enamel and gums. The toothpaste containing this product did not have an excellent feel when used.

・[Means for solving the problem] The present invention was achieved as a result of various studies in order to eliminate the above-mentioned drawbacks of conventional dentifrices. It is made by blending silica gel as an abrasive. That is, its gist is a dentifrice characterized by containing fine spherical silica gel.

The present invention will be explained in detail below. The abrasive compounded in the dentifrice of the present invention is fine particles of silica gel having a particle shape of a true sphere or a sphere close to a true sphere. In terms of physical properties, it is composed of three-dimensional aggregates of °-order powder particles.
Specific surface 0-1000m2/Cl r by BET method,
Pore volume is 4.0 mQ/qr or less, preferably 0.1 to 1
．． 5mQ/gr.

Refractive index is 1.40-1.48. The average particle size is 30μ or less, the moisture content is 65% or less, preferably 45% or less, and the particle size is 40% or more by weight of 2 to 50μ. .

By controlling the physical properties mentioned above, the polishing power can be controlled from low to high, within a range that gives a nice roughness to the teeth. In general,
As shown in the polishing force test described below, AQab
It is an abrasive material with a small r value that does not easily damage enamel.

Fine silica gel having a spherical shape and the above-mentioned physical properties can be obtained, for example, by the following method.

1. A method in which silica hydrosil, whose pH has been adjusted in advance, is suspended in a medium such as oil that has no affinity with the silica hydrosil, solidified during suspension, washed to remove impurities, and then dried.

2 Spray silica hydrosil into the air to gel it,
Method of drying after washing and removing impurities (Special Publication No. 48-138
No. 34).

The spherical fine silica gel blended into the dentifrice of the present invention may be prepared by any of these methods.

Spherical fine silica gel having the above-mentioned physical properties can be obtained by the various methods described above by finding, through trial and error, micronization conditions for improving the physical properties by 1q.

In the dentifrice of the present invention, in addition to the spherical fine silica gel as the abrasive, the same components as those usually included in known abrasives are blended, and the components to be blended are not limited by the abrasive. .

A brief explanation of these includes sodium carboxymethyl cellulose, bitroxyethyl cellulose, algin MjW, carrageenan, gum arabic, binders such as polyvinyl alcohol, wetting agents such as polyethylene glycol, sorbitol, glycerin, propylene glycol, sodium raur sulfate, and dodecyl. Sodium benzenesulfonate, hydrogenated coconut fatty acid monosodium glyceride monosulfate, sodium laurylsulfoneacetate, sodium N-lauroylsarcosinate,
Foaming agents such as N-acylglutamine 1m, lauric acid jetanolamide, sucrose fatty acid ester, essential oils such as peppermint, spearmint, fragrance materials such as Ω-menthol, carvone, eugenol, anethole, etc., saccharinna 1~ A sweetening agent such as sterium, stevioside, neohesberidyldihydrochalconaltin, p-methoxycinnamic aldehyde, etc. can be blended.

In addition, the dentifrice of the present invention also contains mutanase, sorbic acid,
Alexidine, hinokitiol, cetylpyridinium chloride, alkylglycine, alkyldiaminoethylglycine salt, allantoin, ε-aminocaproic acid, tranexamic acid, azulene, vitamin E, water-soluble primary or diphosphate, quaternary ammonium compound, sodium chloride , active ingredients such as crude drug extracts, TiOz as an opaque pigment, etc. can also be blended.

The dentifrice of the present invention contains at least about 1100-100 op.
p, typically about 750-2000 ppm of fluorine. Fluorine-providing compounds include sodium fluoride, stannous fluoride, potassium fluoride, potassium stannous fluoride, sodium hexafluorostannate, and amine fluorides, and can also include mixtures thereof. The most typical examples are sodium fluoride, hexafluoride m! Sodium or a mixture of sodium monofluorophosphate and sodium fluoride can be used.

Dentifrice is about 1100-1ooopp, e.g. about 750-
2000[)m, and especially about 1400-2ooopp
It is preferred to include sodium monofluorophosphate or sodium fluoride or mixtures thereof to provide fluorine, e.g., about 1400-1670 ppm. It is preferable to use a two-component fluoride system of sodium heptanofluoride and sodium fluoride, in which about 30-40% of the fluorine
% (eg, about 30-35%) is provided by sodium fluoride.

Commercially available sodium monofluorophosphate, NaP0
3F varies considerably in purity. Any suitable purity can be used so long as the impurities do not materially adversely affect the desired properties.

Generally, a purity of at least 80% is desirable. For best results, use at least 8
7) Sodium fluorophosphate, preferably at least 90%, with the remainder being primarily impurities or manufacturing by-products such as sodium fluoride and water-soluble sodium phosphate. In other words, the amount of sodium monofluorophosphate used is 12% or more, preferably 12%.
a total fluoride content of more than 7%, a free fluoride ion content of less than 1.5% and preferably less than 1.2%, and a sodium monofluorophosphate content of at least 12%, all calculated as fluoride. Should.

The abrasiveness of the dentifrice of the present invention is evaluated using the following two methods. One of them is Hetferren, J.
Dent, Res., 563-573 (1976,
The American Dental Association (July-August issue)
American Dental As5ocia
The radioactivity polishing value (Radioactivity dentin abrasion value) determined according to the selection method
This is an evaluation based on the brasion value (hereinafter abbreviated as RDA). The details of this method are as follows: 8 human teeth are extracted in advance, radioactive P (phosphorus) with a trade number of 32 is generated in the dentin, held with resin, and 8 times with a brush load of 150 qr. Set each in the continuous polisher. Next, add 25 liters of toothpaste to 5 ounces of tap water.
Add 0 mΩ and mix well, put each slurry into a water tank of a polishing machine, and polish 1000 times. After polishing, 3 mΩ of the slurry was placed in a flat metal mold and dried overnight at 60 to 70'C while circulating air. Radioactivity measurements are performed on the surface of the slurry drying plate thus produced.

Using the same tooth, perform similar measurements on a slurry of 5QmΩ of calcium phosphate 10 gr 10.5% carboxymethyl cellulose aqueous solution, numb the value for each aquarium with the radiation dose for calcium phosphate as 100, and calculate the average value of the 8 values as RAD. value.

Another evaluation method is to use a horizontal reciprocating bushing type polisher, place a slurry of toothpaste sample 259r and 50g of water on an aluminum plate with a smooth surface, apply a load of 200Or, and polish 6000 times. There is a method of measuring the weight loss (hereinafter abbreviated as AΩabr (mg)) of an aluminum plate.

In the case of the dentifrice of the present invention, the use, for example, for adults, for children,
The RDA value ranges from 30 to 400. It is prepared by changing the blending ratio of the abrasive so that the l abr is in the range of 0.1 to 3.0 mC1. Furthermore, the quality of the feeling of use (touch to the teeth, feel on the tongue, etc.) of the dentifrice of the present invention is evaluated by a sensory evaluation method by a plurality of consumer panelists.

[Operations and Effects of the Present Invention] As described above, the dentifrice of the present invention contains spherical silica gel fine particles having specific physical properties as an abrasive. Therefore, when using it, it has a soft texture and does not damage the gums, and even when looking at the abrasive particles after brushing the teeth, there are almost no cracks, compared to the conventional crushing type phosphate and calcium carbonate. Compared to toothpastes containing abrasives made of , alumina, silica, etc., it has better cleaning properties and is extremely comfortable to use. In addition, the silica gel spherical fine particles themselves have a high silica purity of 99% or more, and do not contain impurities that react with fluoride ions such as calcium, so they blend well with the fluoride that is added at the same time to prevent cavities. It is also useful as a toothpaste.

[Examples] Next, the dentifrice of the present invention will be described with reference to Examples, but the present invention is not limited to the following Examples unless the gist thereof is exceeded.

In addition, evaluation of polishing characteristics and feeling of use (polishing) was performed as follows.

1 Evaluation of polishing properties RDA value: Method described in the above volume AΩabr 0 value: Method 2 described in the previous volume Evaluation of feel of use 15 panelists mainly evaluated the texture. The evaluation criteria were as follows.

A: The texture is soft and does not have the roughness of the abrasive.

B: The texture is soft, but the abrasive is a little rough.

C: The polishing agent is a little rough, but it doesn't bother me too much.

D: The abrasive is rough and the usability is poor.

The results of Examples 1 to 5 and Comparative Examples 1 to 2 are shown in Table 1.

A and B are obtained by the second method of producing spherical fine silica gel in the main part.

Each of C has the following physical properties.

(1) Specific surface area (m2/gr) △... by BET method
443 B...763C...671 (2> Pore volume (mg,,'gr) A...0.61 B...0.53C...
・0.46 (3) Refractive index A...1.467 B...1.467C・
...1.467 (/1) Average particle diameter (μ) △...7. OB...5.8 C...8.6 (5) Moisture (%) A...1. OB...2.0 C...1.5 (6) Particle system content A...99 B...99C...9
9 Note 2 Silopure 25 Fine powder silica gel manufactured by Fuji Davison Chemical Co., Ltd. Note 3 PEG #400 (polyethylene glycol, average molecular weight 400) Note 4 Crushed silica gel fine particles A Fine powder silica gel JISA manufactured by Fuji Davison Chemical Co., Ltd. As is clear from the results of Examples 1 to 5 and Comparative Examples 1 to 2, the dentifrice of the present invention using fine spherical silica gel particles as the abrasive has an excellent feeling of use, and
As for the polishing effect, the value of AQabr (mg) is small compared to the RDA value, indicating that it does not damage tooth enamel.

Claims (1)

[Claims] 1. A toothpaste characterized by containing spherical fine silica gel. 2. The dentifrice according to claim 1, wherein the spherical fine silica gel is composed of a three-dimensional aggregate of primary particles. 3 Spherical fine silica gel has a specific surface area of 200 to 1000 m^2/gr and a pore volume of 0.1 to 0.1 by the BET method.
1.5ml/gr, a refractive index of 1.40 to 1.48, an average particle size of 30μ or less, and a water content of 45% or less. 4 Spherical fine silica gel has a particle size distribution of 2 to
The toothpaste according to claim 1, which contains 40% by weight or more of 50μ.