JP3107920B2 - Manufacturing method of dentifrice - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a dentifrice, and more particularly, to a method for producing a dentifrice having good stability without volatilization of perfume components and variations in viscosity.

[0002]

2. Description of the Related Art Toothpastes have been used for many years for the purpose of preventing tooth decay, periodontal disease, bad breath, etc., but the feeling of use is particularly limited in terms of pushability from a dentifrice tube and squeezing on a toothbrush. The appearance at the time, and the quality of the flavor in the mouth are important factors.

In general, dentifrices include abrasives such as dibasic calcium phosphate, binders such as carboxymethylcellulose, wetting agents such as glycerin, fragrance components such as peppermint oil, spearmint oil, and menthol, and surfactants.
It consists of a mixture of sweeteners, preservatives, and the like in water. As an industrial production method, first, a binder is dissolved in a wetting agent and water to form a mucus, and then the slurry contains an abrasive, a fragrance component, A method for obtaining a dentifrice by widely adding a surfactant, a sweetening agent, a preservative, and the like, kneading the mixture, and then defoaming under reduced pressure to obtain a dentifrice has been widely used. Here, the reason for defoaming under reduced pressure at the end is that not only does the appearance deteriorate if air bubbles are contained in the dentifrice,
This is because the aging stability is reduced.

[0004] Recently, various attempts have been made to increase the productivity by making the conventional manufacturing method more efficient. For example, Japanese Patent Publication No. Sho 61-10444 discloses a method in which a fragrance is mixed with other components and then defoamed.
JP-A-11926, JP-A-1-165515 and JP-A-61-236717 describe a method of mixing and defoaming each component of a dentifrice according to a specific method.

[0005] However, in the method described in Japanese Patent Publication No. 61-10444, since the defoaming is performed under reduced pressure after adding the fragrance, a part of the fragrance component having a high vapor pressure volatilizes and the flavor balance is reduced. There was a drawback that it collapsed.
In addition, Japanese Patent Publication No. 61-11925, Japanese Patent Publication No.
The methods described in Japanese Patent No. 1926 and Japanese Patent Application Laid-Open No. 1-165515 also impair the flavor balance due to the same reason as described above, and these methods have a plurality of intermediates in the process, so that the quality of the final product, particularly the viscosity, is controlled. Difficult to do,
There was a problem that the quality was not stable. Further, in the method described in JP-A-61-236717, a binder fine swelling liquid containing a fragrance, a surfactant aqueous solution, and an abrasive slurry obtained by defoaming a premix are mixed. In addition, as in the above-described method, there is a problem that it is difficult to control the quality of the final product, particularly the viscosity, because of having a plurality of intermediates in the process.

[0006]

SUMMARY OF THE INVENTION Accordingly, the present invention provides an excellent flavor without volatilization of the flavor component, preventing the balance of the composition of the flavor component from being lost, and enhancing the flavor without mixing bubbles. And a method for producing a high-quality dentifrice.

[0007]

Under these circumstances, the present inventors have conducted research and found that an abrasive, a binder,
Simultaneous mixing of the wetting agent and water makes it easy to control the mixing conditions of each component and to control the physical properties, especially the viscosity, because there is no production intermediate,
Further, they have found that the addition of a fragrance component after defoaming under reduced pressure can prevent a loss of balance due to volatilization of the fragrance component, and thus completed the present invention.

That is, the present invention relates to a method for producing a dentifrice containing an abrasive, a binder, a humectant, a fragrance component, and water. A method for producing a dentifrice comprising defoaming under reduced pressure and then adding a fragrance component by static mixing.

As the abrasive, binder and wetting agent used in the method of the present invention, various known ones can be blended according to the purpose. As the abrasive, dibasic calcium phosphate (dihydrate And anhydrous), monobasic calcium phosphate, tribasic calcium phosphate, aluminum hydroxide, alumina, calcium carbonate, calcium pyrophosphate, insoluble sodium metaphosphate, silicic anhydride, hydrous silicic acid, aluminum silicate, magnesium phosphate, magnesium carbonate, Examples include calcium sulfate, polymethyl acrylate, bentonite, zeolite, zirconium silicate, synthetic resin, crystallized cellulose and the like. These abrasives are preferably used in such an amount that the compounding amount in the obtained dentifrice is 5 to 80% by weight.

Examples of the binder include carboxymethyl cellulose and salts thereof, methyl cellulose, hydroxyethyl cellulose, carrageenan, sodium polyacrylate, hydroxypropyl cellulose, sodium carboxymethyl hydroxyethyl cellulose, sodium alginate, propylene glycol alginate,
Xanthan gum, tragacanth gum, karaya gum, arabia gum, polyvinyl alcohol, polyvinylpyrrolidone, veegum, laponite and the like can be mentioned. These binders have a compounding amount of 0.1 to 10 in the obtained dentifrice.
It is preferred to use an amount that results in a percentage by weight.

Examples of the humectant include glycerin, sorbitol, propylene glycol, 1,3-butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xylit, maltit, lactit and the like. It is preferable to use these wetting agents in such an amount that the compounding amount in the obtained dentifrice is 5 to 80% by weight.

It is preferable to use water in such an amount that the compounding amount in the obtained dentifrice is 1 to 80% by weight.

In the present invention, the above-mentioned abrasive, binder, wetting agent and water are first mixed simultaneously. In the present invention, simultaneous mixing means abrasive, binder, wetting agent, water and optional components described below, that is, components other than the fragrance component at the same time.
Alternatively, it means that the mixture is continuously administered to a mixer and mixed. In this way, since there is no production intermediate in the process up to this point and the mixing conditions are constant, it is easy to control the physical properties of the dentifrice obtained, especially the viscosity, and it is possible to obtain a high-quality dentifrice. it can.

The mixing temperature of the simultaneous mixing is 40 to 80.
C., especially 45 to 75 C., is preferred. If the temperature is lower than 40 ° C., the binder is difficult to dissolve uniformly, so that the viscosity of the product tends to decrease and there is a problem with stability. Is liable to decrease, causing a problem in stability and also causing coloring.

In the present invention, as a mixer used for the simultaneous mixing, a flow jet mixer (manufactured by Koken Co., Ltd.), a funeki mazeler (manufactured by Tokushu Kika Kogyo Co., Ltd.), a spiral pin mixer (Takai Kikko Co., Ltd.) )), T.I.
K. Motionless Magellar (Special Kika Co., Ltd.)
), A dispersing mixer (manufactured by Akatake Engineering), a tribe blender (manufactured by Ueno Engineering), a Fine Flow Mill (manufactured by Taiheiyo Kiko Co., Ltd.), and the like.

Further, in the present invention, a tooth strengthening agent, a bactericide, a pH adjuster, an enzyme, an anti-inflammatory / blood circulation promoting agent, a surfactant, which are used in ordinary dentifrices at the time of the simultaneous mixing described above. , A sweetener, a preservative, a coloring agent, a coloring agent, and the like can be appropriately compounded.

[0017] Among these components, as a tooth enhancer,
Sodium monofluorophosphate, tin fluoride, sodium fluoride, etc., as bactericides, chlorhexidine salts, cetylpyridinium chloride, triclosan, etc., as pH adjusters, sodium phosphate, etc. Examples of the enzymes include dextranase, amylase, protease, lysozyme, mutanase, and the like.
Hinokitiol, ε-aminocaproic acid, tranexamic acid, allantoins, tocopherols, dihydrocholesterol, glycyrrhetinic acid, glycyrrhizic acid and its salts, glycerophosphate, chlorophyll, water-soluble inorganic phosphate compounds, azulene, chamomile, Toki, Kawaumi, Herbal medicines and the like, and as the surfactant, lauryl sulfate, myristyl sulfate, α-olefin sulfonate, N-acyl amino acid salt, acyl monoglyceride sulfate, soap, fatty acid monoglyceride, fatty acid monoalkanolamide, poly Oxyethylene sorbitan fatty acid esters, polyoxyethylene hydrogenated castor oil, alkyl glycosides, imidazolinium betaines, alkyl betaines, alkyl amide betaines, sulfo betaines, amine oxides and the like. Examples of the sweetener include saccharin sodium, stevioside, thymeatin, asparatylphenylalanine methyl ester, and the like. Preservatives include methyl p-oxybenzoate, ethyl p-oxybenzoate, propyl p-oxybenzoate, and p-oxybenzoate. -Butyl oxybenzoate, sodium benzoate and the like,
Examples of the coloring agents and pigments include edible pigments and titanium dioxide.

In the process of the present invention, the mixture obtained as described above is then defoamed under reduced pressure according to a conventional method. The pressure at this time is 1 to 500 mmHg, especially 10 to 300 mmHg.
mmHg is preferred, and the vacuum deaerator used is Ebara de Mild continuous vacuum deaerator (manufactured by Ebara Corporation), Colma vacuum deaerator (manufactured by Colma), TK
Hibis Dupper (manufactured by Tokushu Kika Kogyo Co., Ltd.) and the like.

After defoaming under reduced pressure, a dentifrice can be obtained by adding a fragrance component. As the fragrance component, various known components can be used depending on the purpose, for example, peppermint oil, spearmint oil, menthol, carvone, anethole, eugenol, methyl salicylate, limonene, ocimene, n-decyl alcohol , Citronellol, α-terpineol, methyl acetate, citronellyl acetate, methyl eugenol, cineole, linalool, ethyl linalool, crocodile, thymol, anise oil, lemon oil, orange oil, sage oil, rosemary oil, cinnamon oil, pimento oil, Cherry oil, perilla oil, winter green oil, clove oil, eucalyptus oil, and the like. It is preferable to use these flavor components in such an amount that the compounding amount in the obtained dentifrice is 0.01 to 10% by weight.

As described above, by adding a flavor component after defoaming under reduced pressure, it is possible to prevent the flavor balance from being lost due to volatilization of a part of the flavor component.

The addition of the fragrance is preferably performed by static mixing. In the present invention, the static mixing means that the degassed mixture and the perfume component are supplied to and mixed with a static mixer having no moving parts such as an agitator or a rotor. As described above, when the fragrance component is added by static mixing, a shearing force applied to the dentifrice is small, so that a binder is not cut and a product excellent in stability without a decrease in viscosity is obtained.

The temperature at which the fragrance component is added is 0 to 50 ° C.
Particularly, 0 to 45 ° C is preferable. If the temperature is lower than 0 ° C., the viscosity increases so rapidly that mixing is difficult. If the temperature is higher than 50 ° C., thermal deterioration of the fragrance component occurs, which is not preferable.

In the present invention, the static mixer used for static mixing of the fragrance component and the mixture defoamed under reduced pressure include a static mixer PSM (manufactured by Petzhold) and a Sulzer mixer (Sulzer Brothers Co., Ltd.).
), High Mixer (Toray Engineering Co., Ltd.)
), Static Mixer (Noritake Co., Ltd.), T.I. K. -ROSS LPD Mixer (manufactured by Tokushu Kika Kogyo Co., Ltd.); K. -ROSS IS
G Mixer (manufactured by Tokushu Kika Kogyo Co., Ltd.), SS type pipe mixer (Koritsu Sangyo Co., Ltd.), mu mixer (Casting Industry Co., Ltd.), Tata Agiter (manufactured by Shimazaki Manufacturing Co., Ltd.), etc. No.

[0024]

According to the production method of the present invention, the fragrance component is not volatilized, so that the composition balance of the fragrance component can be prevented from being destroyed, the flavor is good, the viscosity is not reduced and the dispersion is small, and the storage is stable. A high-quality dentifrice with excellent properties can be obtained.

[0025]

The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.

Example 1 Calcium hydrogen phosphate (abrasive) 20 kg, carboxymethyl cellulose (binder) 0.5 kg, glycerin (wetting agent) 3.4 kg, sorbitol (wetting agent) 12 kg, sodium lauryl sulfate (surfactant) 0.6 kg and 13 kg of water
At a temperature of 60 ° C. (flow jet mixer, manufactured by Koken Co., Ltd.). The obtained paste was continuously degassed under reduced pressure (Ebara de Mild continuous vacuum deaerator, manufactured by Ebara Corporation) at an absolute pressure of 50 mmHg, and then cooled to a temperature of 20 ° C. Next, the obtained paste and a mixture (perfume component) of L-menthol, anethole, carvone, spearmint oil and peppermint oil (perfume component) were mixed at a flow rate ratio (paste: perfume) of 99: 1 with a fixed mixer using a static mixer (Sulzer mixer, Sulzer Brothers). Co., Ltd.) and mixed statically to obtain a dentifrice. Table 1 shows the results of quality evaluation of the obtained dentifrice. In addition, when a total of 30 dentifrices were produced under the same conditions, no air bubbles were mixed in any of the dentifrices, and the dispersion in viscosity was small.

Comparative Example 1 In a 100-liter mixing tank (Ajihomomixer, manufactured by Tokushu Kika Kogyo KK), 0.5 kg of carboxymethylcellulose (binder) was dispersed in 3.4 kg of glycerin (wetting agent). Then, add 13 kg of water and 1 sorbitol (wetting agent)
2 kg was added and mixed while heating to 60 ° C. to prepare a mucus. In addition, calcium hydrogen phosphate (abrasive) is added to this mucus.
20 kg and sodium lauryl sulfate (surfactant)
6 kg was added and mixed to obtain a paste. The obtained paste was continuously degassed under reduced pressure (Ebara de Mild continuous vacuum deaerator, manufactured by Ebara Corporation) at an absolute pressure of 50 mmHg, and then cooled to a temperature of 20 ° C. Next, the obtained paste and a mixture (perfume component) of L-menthol, anethole, carvone, spearmint oil and peppermint oil were mixed at a flow rate (paste: perfume component) of 99: 1 with a fixed mixer using a static mixer (Sulzer mixer, Sulzer). (Manufactured by Brothers Inc.) and statically mixed to obtain a dentifrice. Table 1 shows the results of quality evaluation of the obtained dentifrice. When a total of 30 dentifrices were produced under the same conditions, no air bubbles were mixed in any of the dentifrices, but the dispersion in viscosity was large.

Comparative Example 2 Simultaneous mixing was carried out under the same conditions as in Example 1 except that the fragrance component was also mixed simultaneously. Then, defoaming was performed under reduced pressure as in Example 1 to obtain a dentifrice. Table 1 shows the results of quality evaluation of the obtained dentifrice.

(Quality evaluation method) (1) Flavor evaluation Sensory evaluation was performed according to the following criteria. ：: Good flavor as a dentifrice and excellent use feeling. X: As a dentifrice, the balance of flavor was lost, and there was a problem in commercialization.

(2) Measurement of L-Menthol Amount of L-menthol, one of the fragrance components, was determined by gas chromatography. To 10 g of dentifrice, 2 ml of water, 5 ml of ether and 8 g of sodium chloride were added to extract L-menthol into the ether layer, and the obtained supernatant was used as a test solution. The measurement conditions are as follows. Detector: Flame ionization detector Column: 2.6 mm inner diameter, 3 m length glass column Filler: FFAP (5%) Carrier: UniportHP Column temperature: 60 ° C. Carrier gas: helium 40 ml / min Standard substance: diphenyl oxide

(3) Viscosity after 1 day The average value obtained by measuring 5 points of dentifrice 1 day after production with a B8H type viscometer (manufactured by Tokyo Keiki Co., Ltd.) is shown. Rotor: No.7 Number of revolutions: 2.5 rpm Measurement temperature: 25 ° C Measurement time: 1 min

(4) Stability after One Month The state of water separation after one month was visually judged according to the following criteria. ：: No water separation was observed after storage in a tube at 40 ° C. for one month. ×: Separation was observed after filling in a tube and storing at 40 ° C. for one month.

(5) Variation in viscosity after one day The maximum value and the minimum value when the viscosities of 30 dentifrices produced under the same conditions were measured were shown.

[0034]

[Table 1]

As is evident from Table 1, the production method of the present invention has a good flavor without the volatilization of the fragrance component, has a low viscosity decrease and a small variation in viscosity, and has a high viscosity as compared with the conventional method. Quality dentifrice can be obtained.

────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Kazuhiko Hayakawa 2-11-21-203 Nishitakamatsu, Wakayama-shi, Wakayama (56) References JP-A-1-165515 (JP, A) JP-A-51-9735 ( JP, A) (58) Field surveyed (Int. Cl. ⁷ , DB name) A61K 7/16

Claims (2)

(57) [Claims] 1. A method for producing a dentifrice containing an abrasive, a binder, a wetting agent, a fragrance component, and water, the method comprising the steps of:
After simultaneous mixing of binder, wetting agent and water, degassing under reduced pressure,
Next, a fragrance component is added by static mixing, followed by a method for producing a dentifrice. 2. The dentifrice according to claim 1, wherein the abrasive, the binder, the wetting agent and the water are simultaneously mixed at a temperature of 40 to 80 ° C., and the addition of the fragrance component is performed at a temperature of 0 to 50 ° C. Manufacturing method.