JPS6111925B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for efficiently producing a stable toothpaste that does not contain air bubbles.

Toothpaste generally contains abrasives such as dicalcium phosphate, surfactants such as higher alkyl sulfates, humectants such as glycerin, binders such as sodium carboxymethylcellulose, sweeteners, fragrances, medicinal ingredients, and purified water. It is obtained by homogeneously mixing the toothpaste and forming it into a fluid paste or a gel with low fluidity, but in this case, the production of toothpaste is efficient and highly productive. Something is desired. Note that if air bubbles (air) are mixed into the toothpaste, it not only deteriorates the appearance but also causes a decrease in the quality of the toothpaste, so it is required to remove air bubbles (air) as much as possible. In particular, when it comes to transparent toothpaste, if air bubbles are mixed in, the transparency may be impaired and the appearance may change to translucent or opaque, so it is necessary to remove air bubbles more strictly during the manufacturing process. There is.

Conventionally, the industrial manufacturing method for toothpaste has been to first swell and dissolve a binder in a wetting agent, purified water, etc., then heat as necessary to prepare a viscous swollen solution. Knead the abrasive powder into
A widely used method is to add surfactants, fragrances, medicinal ingredients, etc., homogenize the mixture, and remove air to obtain toothpaste. However, in this method, the swelling solution typically has a high viscosity value of 100 to 400 poise (BH type rotational viscometer, 20 rpm, value after 2 to 3 minutes).
This is a viscous polymer solution with 0.6 to 1.2 times the weight ratio of abrasive powder to this swelling solution. There is a problem that lumps are formed and the viscosity becomes extremely high, which requires a large amount of energy and time to homogenize the components. In addition, as mentioned above, if air gets mixed into toothpaste, it not only looks bad, but also
Since the ingredients in toothpaste are oxidized, resulting in deterioration and discoloration, it is necessary to remove as much air as possible from toothpaste. This is carried out under a vacuum of 20 to 60 mmHg in parallel with or after the homogenization of the toothpaste ingredients. However, in either case, the viscosity of the system is high, so degassing takes a long time, and it is not possible to completely remove even the smallest air bubbles. However, the air bubbles mixed into the toothpaste like this are 2~
Even if it is as small as 5% by volume and is so minute that it cannot be detected with the naked eye, it will keep the toothpaste intact for several months.
If stored for a long period of 3 years, the components will deteriorate due to air oxidation caused by these small amounts of air bubbles.
Discoloration may occur, and in particular, the problem of decreased activity of medicinal ingredients is likely to occur. In this way, the above-mentioned industrial manufacturing method for toothpaste involves kneading abrasive powder into a viscous polymeric swelling solution, breaking the resulting agglomerates and homogenizing them, and removing air. The production efficiency is extremely low since the evaporation process is carried out at high viscosity.Therefore, it has been desired to further improve productivity and to perform deaeration more completely.

Regarding this point, JP-A-52-108031 discloses that a powder mixture consisting of an abrasive, a binder, and a foaming agent and a fragrance are simultaneously introduced into water in a short period of time, and at a speed of 600 rpm or more. We propose a method for producing a toothpaste, which is characterized in that the mixed powder, fragrance, and water are stirred and mixed together at a rotational speed to form a coarse mixture, and the coarse mixture is degassed under reduced pressure. are doing. This method is preferable because it can shorten the manufacturing time of toothpaste and increase productivity compared to conventional methods, but it also reduces the deterioration of the binder due to mechanical shearing under high-speed stirring of 600 rpm or more. Due to the need to prevent this, it is necessary to strictly set manufacturing conditions such as the rotation speed of the stirrer and stirring time depending on the lot of raw materials, especially the binder. There is a problem with degassing under reduced pressure for such materials.
Note that Japanese Patent Publication No. 35-7699 also proposes a method for producing toothpaste, but this method also has problems such as degassing under reduced pressure a highly viscous coarse material in which a binder has swelled and dissolved.

Furthermore, Japanese Patent Application Laid-Open No. 48-40947 discloses that the liquid medium, the gelling agent, and the abrasive gas are removed.
or a gas-free paste or gel dentifrice consisting of producing a gas-free mixture, producing an essentially gas-free mixture of a synthetic organic cleaning agent and a liquid medium, and mixing these mixtures; However, this method requires a low-efficiency kneading operation in which abrasive powder is kneaded into a high viscosity solution containing a swollen and dissolved binder to homogenize it, a synthetic organic detergent, and a polyhydric alcohol. In order to remove air bubbles in the mixed aqueous solution, operations such as heating and leaving it for a long time will cause the binder to swell and dissolve.Then, the abrasive powder will be kneaded into an extremely highly viscous mixture, and a synthetic organic cleaning agent will be added to the mixture. It is difficult to increase productivity because it uses an operation with low mixing efficiency of mixing a mixture containing . Furthermore, this method is difficult to employ in systems containing a small amount of polyhydric alcohol.

The inventors of the present invention have conducted intensive research on a method to improve the above situation and efficiently mass-produce high-quality toothpaste that does not contain air bubbles, leaves the skin smooth, and does not deteriorate during storage. As a result of aging, abrasive 1
Low viscosity is achieved by mixing preferably 0.5 parts by weight or more of water or a mixed solution of water and a wetting agent based on the weight part, deaerating the mixture, and finally adding a binder dispersed in the wetting agent to swell and dissolve it. The inventors have discovered that the above object can be achieved by homogenizing the ingredients and removing air bubbles in a process that makes it possible to efficiently and reliably mass-produce high-quality toothpaste that does not contain air bubbles. It is ivy.

The present invention will be explained in more detail below.

The method for producing a toothpaste according to the present invention includes mixing preferably 0.5 parts by weight or more of water or a mixed solution of water and a wetting agent with 1 part by weight of the abrasive, deaerating the mixture, and finally dispersing the toothpaste in the wetting agent. It is characterized by swelling and dissolving with the addition of a binder, and as a result, it does not contain air bubbles, resulting in smooth skin with a good appearance and feel, and does not deteriorate even after long-term storage. This makes it possible to efficiently obtain a toothpaste that can stably retain medicinal ingredients.

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Here, as the polishing agent, dibasic calcium phosphate dihydrate and anhydride, tribasic calcium phosphate, calcium carbonate, aluminum hydroxide, alumina, insoluble sodium metaphosphate, calcium pyrophosphate, crystalline silica, amorphous silica, Examples include magnesium carbonate, magnesium phosphate, and synthetic resin powder, and one or more of these can be used. The particle size of these abrasives is not particularly limited, and any suitable particle size may be used depending on the desired polishing effect, but those having an average particle size of 1 to 20 μm are usually used. The hardness is preferably one that does not damage the teeth, and a Mohs hardness of 3 or less is usually used. Further, the amount of abrasive used is not limited, but it can usually be blended in an amount of 20 to 60% (wt%, same hereinafter) of the total toothpaste.

Examples of wetting agents include polyhydric alcohols such as glycerin, propylene glycol, sorbitol, polyethylene glycol, polypropylene glycol, xylitol, maltitol, and lactitol, and one or more of these may be blended. The amount used varies depending on the type of toothpaste, but is usually 5 to 70% of the total toothpaste. In addition, when using glycerin and/or propylene glycol and sorbitol (usually used in an aqueous solution) together, glycerin and/or propylene glycol and a sorbitol aqueous solution (50 to
80% solution) is 1:20 to 1:20 by weight.
The ratio is preferably 10:1, particularly 1:15 to 1:1.

Furthermore, as a binder, cellulose derivatives such as sodium carboxymethylcellulose, methylcellulose, and hydroxyethylcellulose, carrageenan, alkali metal alginates such as sodium alginate, gums such as xanthan gum, gum tragacanth, gum karaya, and gum arabic, polyvinyl alcohol, and polyacrylic acid. Examples include synthetic binders such as sodium and carboxyvinyl polymers that swell and dissolve in water, and one or more of these can be used. In this case, the particle size of these binders is appropriately selected depending on the type, etc. Further, the amount of the binder used is not particularly limited, but is usually 0.3 to 5% of the total toothpaste.

In the present invention, first, water or a mixed solution of water and a wetting agent is mixed with 1 part by weight of the above-mentioned polishing agent, preferably at least 0.5 part by weight, more preferably at least 0.7 part by weight, and then degassed.

In this operation, for example, water is first placed in a tank equipped with a stirring blade that allows the whole to flow, and if necessary, a wetting agent is added and mixed. At this stage, the viscosity is usually less than 1 poise. Next, an abrasive is added and dispersion mixing is performed. In this case, the inside of the tank can be depressurized and degassed from the stage of dispersion and mixing of the abrasive, but the viscosity of the slurry in which the abrasive is dispersed and mixed is water or water and a wetting agent per 1 part by weight of the abrasive. mixed solution of
When the amount is 0.5 parts by weight or more, the air bubbles are usually 20 poise or less at this stage, so air bubbles can be almost completely removed simply by stirring under normal pressure. Note that if the amount of water or a mixed solution of water and a wetting agent is less than 0.5 part by weight per 1 part by weight of the abrasive, air bubbles may not be removed sufficiently. It is preferable that the amount of the mixed solution is 0.5 parts by weight or more.

When the above-described operation of dispersing and mixing the abrasive is performed under normal pressure, it is preferable that the inside of the tank is then placed under reduced pressure, so that air bubbles can be completely removed. In this case, the degree of vacuum is preferably 10 to 200 mmHg (absolute pressure).

In the present invention, the abrasive is first mixed with water or water.
It is dispersed and mixed in a wetting agent mixed solution and degassed to remove air bubbles caused by the abrasive. In addition to the above-mentioned components, surfactants,
Sweeteners, flavors, preservatives, medicinal ingredients, etc. can be incorporated during the above-mentioned operations or in subsequent operations.

In this case, the surfactants include sodium lauryl sulfate, sodium myristyl sulfate, sodium palmityl sulfate, higher fatty acid soap, anionic active agents such as sodium α-olefin sulfonate, lauryl diethanolamide, sucrose fatty acid ester, polyoxyethylene sorbitan. Examples include nonionic active agents such as monolaurate, amphoteric active agents, etc., and one or more of them are usually used in an amount of 0.1 to 7% of the total toothpaste. These surfactants may be mixed with the abrasive in powder form and added to water or a water-wetting agent mixed solution;
More preferably, the abrasive is added to the dispersed slurry. In this case, the surfactant may be added as it is to the abrasive-dispersed slurry, but it is preferable to add a surfactant that has been previously dispersed or dissolved in water or a mixed solution of water and a wetting agent. When a mixed solution of water and a wetting agent is used, the ratio of the wetting agent to 1 part by weight of water is preferably 4 parts by weight or more.

In addition, as a sweetener, saccharin sodium,
Sucrose, maltose, lactose, perillartin, stevioside, glycyrrhizin salts, etc. can be blended in an amount of usually 0.05 to 5%, and these may be dissolved in water or a mixed water-wetting agent solution in advance before dispersing the abrasive, or they may be dissolved in powder or granular form. Leave it mixed with polishing agent,
This may be mixed into water or a water-wetting agent mixed solution, or further may be dissolved and blended into an abrasive dispersion slurry. Furthermore, as fragrances, spearmint oil, peppermint oil, salvia oil, eucalyptus oil, lemon oil, lime oil,
Essential oils such as wintergreen oil, cinnamon oil, other spices, fruit flavors, and l
- Usually 0.1-5% of isolated or synthetic fragrances such as menthol, carvone, anethole, eugenol, etc.
Although it is also possible to mix and disperse these fragrances in the abrasive and the like, it is preferable to mix them into the abrasive dispersed slurry.

In addition, as a preservative, ethyl paraoxybenzoate, butyl paraoxybenzoate, etc. may be added.
Medicinal ingredients include enzymes such as dextranase, retituent enzyme, lysozyme, amylase, and lytic enzyme, antiplasmin agents such as epsilon aminocaproic acid and tranexamic acid, sodium fluoride, sodium monofluorophosphate, and stannous fluoride. Fluorine compounds such as chlorhexidine salts, quaternary ammonium salts, aluminum chlorohydroxylalantoin, glycyrrhetinic acid, chlorophyll, sodium chloride, phosphoric acid compounds, etc. may be blended, and further silica gel, aluminum silica gel, organic acids and their salts, etc. These components can be blended as desired, but depending on their form, solubility in water, etc., for example, in the case of water-insoluble powder, they are mixed with the abrasive, and in the case of water-soluble, they are mixed with the abrasive before dispersion. It can be added to water or a mixed water-wetting agent solution or an abrasive-dispersed slurry, and if it is oily or oil-soluble, it can be mixed with a fragrance or added directly to an abrasive-dispersed slurry.

In the present invention, when adding a surfactant, fragrance, etc. to the abrasive dispersion slurry, it is preferable to perform the operation under reduced pressure, especially under a reduced pressure of 10 to 100 mmHg (absolute pressure). Even at this stage, the viscosity is usually 25 poise or less and the pressure is reduced, so air bubbles caused by surfactants and the like are reliably removed and no air bubbles are mixed in.
Further, at this stage, there is no restriction on the order in which surfactants, fragrances, etc. are added.

In the present invention, after the above-mentioned operations are carried out, a binder is finally added and the toothpaste is obtained by swelling and dissolving the binder.In this case, the binder has been previously dispersed in a wetting agent. use something In this way, by adding a binder dispersed in a humectant, a toothpaste that is good for the skin can be obtained, but if the binder is added as is, uneven swelling tends to occur;
Unable to obtain good toothpaste. When dispersing the binder in the wetting agent, the ratio is preferably 2 parts by weight or more of the wetting agent to 1 part by weight of the binder. Further, the addition of the binder and the swelling and dissolution may be carried out under normal pressure or reduced pressure, but preferably carried out under reduced pressure.

Although the above operations (abrasive dispersion operation, binder swelling and dissolution operation, etc.) may be performed under heating, they can all be performed at room temperature.

According to the above-mentioned method for manufacturing toothpaste, an abrasive and, if necessary, a surfactant are added to water or a water-wetting agent mixture solution. Since it is possible to disperse and mix granular components containing many air bubbles, air bubbles can be removed easily and quickly.In particular, air bubbles can be removed reliably by removing air bubbles under reduced pressure, and the final viscous Since the inclusion of air bubbles can be prevented before the binder swells and dissolves, the resulting toothpaste does not contain air bubbles. Therefore, the method of the present invention is very advantageous and can be employed in the production of toothpaste with a transparent appearance, and the toothpaste obtained by the method of the present invention does not contain air bubbles, so it can be stored for a long period of time. Deterioration of components due to the presence of air bubbles is prevented. Furthermore, as mentioned above, air bubbles can be easily and quickly removed, without necessarily stirring at high temperatures or applying large shear forces for defoaming.
Since toothpaste can be manufactured, the appearance and stability of the product will be improved. In addition, the air bubbles are released quickly and the slurry can be effectively prevented from foaming or expanding when air bubbles are released, so a mixer with a small capacity can be used and the equipment can be made more compact. can.

Furthermore, according to the method of the present invention, the binder dispersed in the wetting agent is added at the end to swell and dissolve the binder, and the surfactant is added before the binder is added. Therefore, the action of the surfactant improves the hydrophilicity of the abrasive and prevents the formation of aggregates when the binder swells, resulting in a toothpaste with smooth skin, gloss, and texture. in good condition,
It has an excellent appearance.

Next, examples will be shown to specifically explain the present invention.

Example 1 Dibasic calcium phosphate 40% Sorbitol (60% aqueous solution) 30 Glycerin 5 Sodium lauryl sulfate 2 Sodium carboxymethyl cellulose 1.5 Sodium saccharin 0.2 Flavor 1.0 Ethyl paraoxybenzoate 0.01 Water Balance 100.0% Vacuum with a stirring blade that allows total flow Water was placed in a mold stirring tank, and saccharin sodium and ethyl paraoxybenzoate were added thereto and mixed and dissolved. During this time, the mixture was stirred at 25°C for 10 minutes. Furthermore, an aqueous sorbitol solution was added and mixed. At this stage the viscosity is 1
It was below Poise.

Next, dibasic calcium phosphate was added to this aqueous solution and stirred for 5 minutes. At this stage, the viscosity was 30 poise or less, and most of the air bubbles in the powder (dibasic calcium phosphate) were removed during stirring.

Next, the inside of the stirring tank was pumped 700mm using a vacuum pump.
After creating a vacuum of Hg (absolute pressure 60 mmHg), perfume was added and stirred for 3 minutes, and sodium lauryl sulfate was further added and stirred for 5 minutes. At this stage the viscosity is 10
It was less than a poise, and both defoaming and mixing were performed well and easily.

Finally, sodium carboxymethyl cellulose moistened with glycerin was added under vacuum at an absolute pressure of 60 mmHg with stirring to cause swelling and dissolution to produce a toothpaste.

The obtained toothpaste did not contain air bubbles, had good texture and gloss, and was smooth and stable on the skin.

According to the method described above, since the abrasive and surfactant are mixed with a low viscosity, the air bubbles in the powder are released quickly, and there is no foaming of the slurry or expansion of the slurry due to the inclusion of air bubbles. Unlike conventional devices, it was not necessary to make the device volume twice the volume of toothpaste, and a volume of about 1.2 times was sufficient. Also,
No special operations such as stirring at high temperatures are required to remove air bubbles, reducing production time.
It was also advantageous from the standpoint of stability in the quality of the toothpaste.

Example 2 Glycerin 27% Calcium silicate 20 Sodium carboxymethylcellulose 0.6 Sodium saccharin 0.2 Sorbitol (70% aqueous solution) 40 Dye solution (1% aqueous) 0.2 Fragrance 1.2 Sodium lauryl sulfate 2.0 Ethyl paraoxybenzoate 0.01 Pure water Balance 100.0% High Ethyl paraoxybenzoate and saccharin sodium were dissolved in pure water in a stirring tank for viscosity, and an aqueous sorbitol solution, glycerin, and a dye solution were added and mixed. Calcium silicate was added to the solution and stirred for 5 minutes. Next, the inside of the stirring tank was evacuated (absolute pressure 30 to 100 mmHg), and fragrance and sodium lauryl sulfate, which had been previously mixed with an aqueous glycerin solution (80%) at a weight ratio of 4:1, were added and mixed.

Finally, while maintaining the vacuum state, sodium carboxymethylcellulose, which had been dispersed in 100% glycerin at a weight ratio of 5:1, was added and allowed to swell and dissolve to produce a toothpaste.

The obtained toothpaste did not contain air bubbles, had a visually transparent appearance, had good texture and gloss, was smooth on the skin, and was stable.

In terms of appearance, transparent toothpaste like this
Although the presence of air bubbles is undesirable, in conventional manufacturing methods, degassing is performed at a high viscosity of 300 poise or more after the binder has swelled.
Complete deaeration was difficult. However, according to this method, since calcium silicate and sodium lauryl sulfate containing many air bubbles are mixed and dispersed in low-viscosity water and polyhydric alcohol, air bubbles can be removed easily and reliably, and in a short period of time. It was possible to completely degas in time.

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Claims (1)

[Claims] 1. A polishing agent is mixed with water or a mixed solution of water and a wetting agent, deaerated, and finally a binder dispersed in the wetting agent is added to swell and dissolve. A method for producing toothpaste that does not contain air bubbles. 2. The method according to claim 1, wherein 1 part by weight of the abrasive is mixed with 0.5 part by weight or more of water or a mixed solution of water and a wetting agent. 3. The method according to claim 1 or 2, wherein the abrasive is mixed with water or a mixed solution of water and a wetting agent under reduced pressure of 10 to 200 mmHg absolute and degassed. 4. The method according to claim 1 or 2, wherein the abrasive is mixed with water or a mixed solution of water and a wetting agent under normal pressure, and then stirred and degassed under reduced pressure of 10 to 200 mmHg. 5. The method according to any one of claims 1 to 4, wherein a fragrance and a surfactant are added to a slurry obtained by mixing an abrasive with water or a mixed solution of water and a wetting agent. 6 Add fragrance and surfactant to the slurry at an absolute pressure of 10~
The method according to claim 5, wherein the mixture is added under reduced pressure of 100 mmHg. 7 Claims 1 to 6 in which 1 part by weight of a binder is dispersed in 2 to 10 parts by weight of a wetting agent
The method described in any of the sections. 8. The method according to any one of claims 1 to 7, wherein the binder dispersed in the wetting agent is added under reduced pressure to swell and dissolve.