JPS5822124B2 - toothpaste composition - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a dentifrice composition containing aluminum hydroxide (alumina trihydrate, mineralogically called gibbsite, hereinafter the same) as an abrasive.

Conventionally, the use of aluminum hydroxide as an abrasive for toothpaste has not been known (Japanese Patent Publication No. 26-4650).

28-3000.3l-5550), and recently it has been proposed to use aluminum hydroxide in combination with an insoluble alkali metal metaphosphate for the purpose of stabilizing fluorine compounds (Japanese Patent Publication No. 44-18600.48-38864). ，
49-495゜5O-5266) However, there are generally not many examples of actually using aluminum hydroxide as an abrasive, and in particular, there are almost no examples of using aluminum hydroxide alone as an abrasive. .

The reason is that conventional aluminum hydroxide has higher abrasive power than commonly used toothpaste abrasives such as dicalcium phosphate dihydrate, calcium pyrophosphate, and insoluble sodium metaphosphate. If used as an abrasive, it may cause tooth abrasion or scratches, and if an aluminum tube is filled with toothpaste that uses aluminum hydroxide as its sole abrasive, the aluminum hydroxide will corrode the aluminum tube, causing the tube to deteriorate. This is because the tube may swell or, in severe cases, may burst, making long-term storage difficult.

In addition, conventional aluminum hydroxide, especially when used alone, has a very poor usability, making it unsuitable for use as a product.Moreover, its low whiteness deteriorates the appearance of toothpaste, making it unsuitable for use as a product. There were problems such as degrading the image.

As a result of various studies conducted by the present inventors to solve these problems, we found that the average particle size (Stokes diameter) of aluminum hydroxide is 5 to 14μ, and the amount of soluble sodium compounds eluted in water when washed with water is oxidized. Slurry〇P obtained by suspending in water at a concentration of 10% by weight, with an attached sodium oxide content calculated as sodium content of 0.02% by weight or less
When using aluminum hydroxide as an abrasive, which has an H of 7 to 9 and a hunter's self-scoring rating of 96 or higher according to the test method specified in JIS P8123-1961, it has a moderate abrasive power, can prevent selective scratches, and has a good usability. It has been found that even when used alone as an abrasive, a toothpaste having excellent properties can be obtained.

In particular, the present inventors found that among the various properties of aluminum hydroxide, the amount of sodium oxide adhesion and the pH of the 10% slurry are factors that have a large influence on the corrosion of aluminum tubes, and that the adhesion of sodium oxide on aluminum hydroxide If the amount exceeds 0.0102% by weight, especially 0.02% by weight.
06% by weight or more, 10% by weight slurry〇PH
If it exceeds 9, aluminum tubes are easily corroded (therefore, the amount of sodium oxide deposited on aluminum hydroxide, which has been conventionally used as an abrasive, is 0.1% by weight).
It has been found that the aluminum tube is significantly corroded because the amount of carbon dioxide is higher than that.

In contrast, if the amount of IJium deposited is 0.02% by weight or less and the pH of the 10% by weight slurry is 9 or less, the aluminum tube will not be corroded. It was discovered that even when this toothpaste is used as a sole abrasive and stored in an aluminum tube, the tube does not corrode and can be stored stably for a long period of time, and there is no off-taste or astringent taste, improving the usability. The inventors have discovered that the above problems can be solved all at once, and have completed the present invention.

The present invention will be explained in detail below.

The dentifrice composition according to the present invention contains aluminum hydroxide as an abrasive, but in the present invention, aluminum hydroxide has an average particle diameter (Stokes diameter) of 5 to
14 μ, the content of attached sodium oxide calculated by converting the amount of soluble sodium compounds eluted into water when washed with water as the amount of sodium oxide is 0.02% by weight or less, and 10% by weight
PH of water slurry is 7-9, JIS P8123
Use a material with a whiteness (Hunter white discoloration) of 96 or higher according to the test method specified in 1961.

When using aluminum hydroxide with this kind of properties, it is possible to obtain a toothpaste that has appropriate abrasiveness, feels very good in use, does not corrode the aluminum tube, and has a good appearance. It was made.

On the other hand, if even one of the above properties is outside the above range, even if the other properties are within the above range, it will not be possible to obtain a toothpaste with sufficiently satisfactory characteristics, and in particular, the usability will be significantly reduced. .

For example, if the average particle diameter is smaller than 5 μm, the polishing power is decreased, and when used, a sticky feeling is imparted, which significantly impairs the feeling of use.

On the other hand, particles with an average particle size larger than 14 μm cause wear and scratches on the teeth, have a poor texture, and are rough, which also impairs the feeling of use.

Further, when the content of attached sodium oxide is more than 0.02% by weight, and when the pH of the 10% by weight slurry is higher than 9, the feeling of use is significantly lowered, and off-taste and astringent taste occur, so that the object of the present invention is not achieved.

Furthermore, if the deposited sodium/lium oxide content is higher than 0.02% by weight, the aluminum tube etc. will be corroded and long-term storage will be hindered.

Also, the whiteness is lower than 96. It spoils the appearance of toothpaste and makes it less palatable.

Aluminum hydroxide with the above properties is used in the compounding method and blending ratio commonly used as an abrasive, and even when aluminum hydroxide with the above properties is used alone as an abrasive, toothpaste with excellent properties cannot be obtained. Obtainable.

However, if necessary, dibasic calcium phosphate dihydrate or anhydrous salt, calcium carbonate, calcium pyrophosphate,
It can also be used in combination with abrasives such as insoluble alkali metal metaphosphates, calcium sulfate, silicon dioxide, etc. Therefore, aluminum hydroxide with the above properties can usually be blended in a proportion of 1 to 70% by weight, but it is particularly effective. 3 from the point of letting
It is preferable to set the blending amount to 0 to 50% by weight.

Other ingredients of the dentifrice composition according to the present invention are the same as those of conventional ones, for example, in the case of toothpaste, sodium salt of carboxymethyl cellulose, sodium salt of hydroxyethyl cellulose, carrageenan, xanthun gum,
Guar gum, locust bean gum, alginate sl
- Binder such as IJum, propylene glycol alginate, polyvinylpyrrolidone (the amount is usually 10% by weight or less, preferably 0.5 to 5% by weight).

), thickeners such as glycerin, sorbitol, propylene glycol, polyethylene glycol (usually 10%
~40% by weight), water-soluble salts of higher fatty acid monoglyceride monosulfates such as thorium salts of monosulfated monoglycerides of coconut oil fatty acids, higher alkyl sulfates such as sodium lauryl sulfate, sodium dodecylbenzene sulfonate, etc. Anionic surfactants such as alkylaryl sulfonates and sodium salts of N-lauroyl sarcosinate, pluronic surfactants, nonionic surfactants such as sucrose fatty acid esters, and other foaming agents (compounding amount usually 0.1 to 10% by weight) , especially 0.
The content is preferably 5 to 5% by weight.

) Furthermore, it can be produced by mixing sweeteners, flavorings, preservatives, fluorine compounds such as sodium stannous fluoride and sodium monofluorophosphate, active ingredients such as enzymes, bactericides, etc. in water. .

Therefore, the dentifrice composition according to the present invention has an average particle size of 5 to 5.
14μ, the adhering sodium oxide content calculated by converting the amount of soluble sodium compounds eluted into water when washed with water as the amount of sodium oxide is 0.02% by weight or less, and the pH of the slurry obtained by suspending it in water at a concentration of 10% by weight is 7. ~9, JIS
By blending aluminum hydroxide as an abrasive with a Hunter Yamaga rating of 96 or higher according to the test method specified in P8123-1961, the polishing power is moderate even when this aluminum hydroxide is used alone as an abrasive. Unlike conventional toothpaste compositions containing aluminum hydroxide, the toothpaste composition does not cause tooth abrasion or scratches and can be expected to sufficiently clean the teeth. It has no taste and has a good texture, and there is no foreign taste or astringent taste.
It tastes good.

In addition, even when the dentifrice composition of the present invention is filled and stored in an aluminum tube, it does not corrode the tube, is durable enough for long-term conservators, and shows almost no deterioration in quality. Furthermore, it has a high degree of whiteness and a good appearance, giving the user a sense of cleanliness.

Next, the effects of the present invention will be specifically explained with reference to Examples.

In the examples below, the average particle diameter is the Stokes diameter, and the adhering sodium oxide content is the p-liquid obtained by soaking aluminum hydroxide in 5 times the weight of warm water at 60 to 70°C for 5 hours, then filtering it. It is the value obtained by converting the amount of alkali obtained by neutralizing with hydrochloric acid into sodium oxide, and 1
The 0 weight % slurry PH is the PH of the slurry obtained by suspending aluminum hydroxide in water at a concentration of 10 weight %, and the whiteness is JIS P8123-1961.
It is a hunter Yamashika according to the measurement method prescribed in .

Experimental Example 1 As an abrasive, aluminum hydroxide having various average particle diameters (Stokes diameter) (deposited sodium oxide content 0.
005-0.015%, pH 7 of 10 wt% slurry,
5 to 9.0, Hunter white discoloration 98 or higher) using the following formulation: aluminum hydroxide 45% by weight colloidal silica 3 sodium lauryl sulfate 1.5 glycerin
20 〃Carboxymethylcellulose 0
．． 8〃Carrageenan 0.2〃Propylene glycol 3〃Fragrance
1 Saccharin
1. A toothpaste with water and balance of 100.0// was produced.

Next, the obtained toothpaste was subjected to RDA method (Journa
1 of Dental Research, 55
, 563 (1977),), and the results shown in FIG. 1 were obtained.

Experimental Example 2 Using aluminum hydroxide with various average particle diameters (Stokes diameter) and whiteness (Hunter Yamaga), Experimental Example 1
A toothpaste with a similar formulation was manufactured.

Next, the preference of these toothpastes was measured using the 5che f fe' pairwise comparison method.

The results are shown in Tables 1 and 2.

In addition, as for the aluminum hydroxide in Table 1, all adhering sodium oxide l) rum content is 0.01% or less and 10% by weight.
A slurry with a pH of 7 to 9 and a Hunter white discoloration of 96 or higher was used, and the aluminum hydroxide in Table 2 had an average particle diameter (Stokes diameter) of about 10μ, an adhering sodium oxide content of 0.01% or less, and a weight of 10%. % Sura' J-p, H
7 to 9 were used.

I adjusted the pH of my toothpaste to about 7.

Experimental Example 3 Using aluminum hydroxide (average particle size (Stokes diameter) 7 to 12μ, Hunter white discoloration 96 or higher) with various adhesion sodium oxide contents and different 10% by weight slurry PH, toothpaste with the following formulation was used. Manufactured.

Aluminum hydroxide 450% by weight Propylene glycol 2.0 Glycerin
20.0 /1 Sodium carboxymethyl cellulose 1.1 Sodium lauryl sulfate
1.5 Satukarin 0.2
Weight % Flavor: 1.0 Preservative: Trace amount of water: Balance: 100.0% Next, these toothpastes were filled into an aluminum tube, sealed tightly, and stored at 50°C.

The degree of corrosion was evaluated from the degree of swelling of the tube due to changes over time, and the results shown in Table 3 were obtained.

Also, a section of aluminum tube (2X 3 cm
) was immersed in a toothpaste having the above composition, the self-potential was measured by comparing it with a saturated Amagi electrode, and then it was polarized to the anode side using a potentiostat, and the results shown in FIG. 2 were obtained.

In addition, in Fig. 2, the amount of Na20 attached is 0.2% for Chunin, the amount of Na20 attached is 0.1% for B, and the amount of Na2O attached is 0.04% for C.
D is the result of toothpaste using aluminum hydroxide with 0.02% Na2 adhesion, and E is the result of toothpaste using dibasic calcium phosphate dihydrate instead of aluminum hydroxide.

The toothpaste using aluminum hydroxide with an adhering Na2O content of 0.02% or less did not have any off-taste or astringent taste, and had a good taste.

Therefore, from the results of 1 or more, the average particle diameter (Stokes diameter)
Aluminum hydroxide is used as an abrasive, and has a pH of 5 to 14μ, a content of attached sodium oxide of 0.02% by weight or less, a pH of 10% by weight slurry of 7 to 9, and a whiteness (Hunter white discoloration) of 96 or more. and.

The abrasiveness is moderate (in Figure 1, the RDA value that represents the abrasive force is in the range of 80 to 160 is the most appropriate range. If it is less than 80, the abrasive force is too small, and if it is thicker than 160, the abrasive force is too low. It is said that if the tooth is too thick, the tooth tends to be easily scraped.

) It does not cause scratches, has a very good usability, does not have a sticky or rough feel, and has no unpleasant taste.
It had no astringent taste, had the same appearance as conventional dibasic calcium phosphate toothpaste, and was found to have excellent performance as a toothpaste.

On the other hand, those using aluminum hydroxide outside the above-mentioned characteristic range had particularly poor usability and were very problematic when used alone as an abrasive.

In addition, in particular, the results of Experimental Example 3 show that when aluminum hydroxide with a deposited oxidized I-IJ content of 0.02% by weight or less is used, almost no corrosion of the aluminum tube occurs; In fact, from the electrochemical measurement results shown in Figure 2, a rapid increase in polarization current was observed even when the polarization potential (△E) was increased, similar to the stable dicalcium phosphate/dihydrate toothpaste that does not easily cause corrosion. It was found that it was stable against aluminum.

On the other hand, when aluminum hydroxide is used with a content of more than 0.02% by weight of attached oxidized I-IJ, corrosion of the aluminum tube progresses rapidly, and electrochemical measurements show that the attached sodium oxide content is 0.02% by weight. When the amount exceeds 0.02% by weight, an increase in polarization current is observed while the polarization potential is low, and it has been found that aluminum tubes are easily corroded. The toothpaste of the present invention using aluminum did not corrode the aluminum tube and was found to be highly stable.

Examples are shown below.

Example 1 Aluminum hydroxide (average particle size 45.0% by weight8.
1μ, whiteness 98, Na2O content 0.007% by weight, 10% by weight slurry pH 8,2) Nruvit liquid 30. On propylene glycol 2. o Carboxymethyl cellulose 1.1 Sodium saccharin 0.2 Sodium lauryl sulfate 1.5 Flavoring
1.0〃Preservative Trace amount of water Balance 100.0/
/ Example 2 Aluminum hydroxide (average particle size 20.0% by weight10.
0μ・Whiteness 98, Na20 content 0.01% by weight, 10% by weight - Slurry pH 8,3) Dibasic calcium phosphate dihydrate 20. Ott Glycerin 25,0//Hydroxyethylcellulose 1,3 Sodium Saccharin 0.1 Sodium Lauryl Sulfate 1. o Flavor
1.0〃Preservative Trace amount of water Balance■ Cノ 0.0 〃 Example 3 Aluminum hydroxide (average particle size: 40.0% by weight, particle size: 12.0% by weight)
1 μ, whiteness 99, Na2O content 0.008% by weight, 10 weight slurry pH 7,9) Silicic anhydride 3.0 Glycerin
10.07/Sorbit solution
10.0//Carboxine methylcellulose 0.5 Sodium carrageenan 0.5% by weight Saccharin 0.2 Sodium lauryl sulfate 160 Sucrose monolaurate
0.5 fragrance
1.0 Preservative Trace amount of water Nokurance 1oo
, on All of the toothpastes of Examples 1 to 3 are extremely stable, with no change in quality even when stored at 50°C for 3 months in aluminum tubes and plastic tubes.
The usability was also good.

[Brief explanation of the drawing]

Figure 1 shows the average particle diameter and polishing force (R) of aluminum hydroxide.
Figure 2 is a graph showing the relationship between the polarization potential and polarization current when a section of aluminum tube is immersed in toothpaste using aluminum hydroxide as an abrasive with various adhering sodium oxide contents. It is a graph showing the relationship between.

Claims (1)

[Claims] 1. An abrasive with an average particle size of 5 to 14μ, which oxidizes the amount of soluble sodium compounds dissolved in water when washed with water.
- The adhering sodium oxide content calculated as the amount of IJum is 0.02% by weight or less, the pH of the slurry obtained by suspending it in water at a concentration of 10% by weight is 7 to 9, JIS P8123
-Hunter's score is 9 according to the test method specified in 1961.
A dentifrice composition comprising aluminum hydroxide having an aluminum hydroxide of 6 or more. 2. The dentifrice composition according to claim 1, which is filled into an aluminum tube.