JPS58208208A - Preparation of toothpaste - Google Patents

Abstract

PURPOSE:To obtain a toothpaste having a good appearance without air bubbles nor fear for the deterioration in quality, by incorporating a polishing agent with water or a mixed solution of the water with a wetting agent, deaerating the resultant mixture with stirring under reduced pressure, and adding a binder dispersed in the wetting agent thereto. CONSTITUTION:One pts.wt. polishing agent, e.g. calcium secondary phosphate dihydrate, is incorporated with 0.5pts.wt. or more water or a mixture solution of the water with a wetting agent, e.g. glycerol, and the resultant mixture is then deaerated with stirring under 10-200mm.Hg reduced pressure. One pt.wt. binder, e.g. sodium carboxymethyl cellulose, dispersed in 2-10pts.wt. wetting agent is then swollen and dissolved in the resultant mixture to give the aimed toothpaste without containing air bubbles. The homogenization of the components and removal of the air bubbles can be carried out due to the low viscosity by the above-mentioned method. A perfume and a surfactant can be added to a slurry obtained by incorporating the polishing agent in water, etc.

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 calcium diphosphate, surfactants such as higher alkyl sulfates, wetting agents such as glycerin, binders such as sodium carboxymethylcellulose, sweeteners, fragrances, medicinal ingredients, and purified water. It is obtained by homogeneously mixing and forming into a fluid linear shape or a low fluidity glue shape, but in this case, the production of toothpaste is efficient and highly productive. It is hoped that Further, if air bubbles (air) are mixed in 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, transparent toothpaste (if available)
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 very strictly during the manufacturing process.

Conventionally, the industrial manufacturing method for toothpaste has been to first swell and dissolve a binder in a wetting agent, ice cubes, etc. At this time, heat is applied as necessary to form a viscous swelling solution, and then this swelling solution is A widely used method is to knead abrasive powder, then add surfactants, fragrances, medicinal ingredients, etc. to homogenize it, and then remove air to obtain toothpaste. However, this method requires that the swelling solution is typically a viscous solution with a high viscosity value of 100 to 400 poise (BH type rotational viscosity value after 2 to 3 minutes). When using a polymer solution, the abrasive powder is kneaded in an amount of 0.6 to 1.2 times the weight of the swelling solution, so during this mixing, the interaction between the abrasive powder and the swelling solution causes agglomerates to form. It forms and becomes extremely viscous,
For this reason, there is a problem in that it requires a great deal of energy and time to homogenize the components. In addition, as mentioned above, if air is mixed into toothpaste, it will not only make the toothpaste look bad, but also cause the ingredients in the toothpaste to oxidize and cause deterioration and discoloration, so it is necessary to remove air from the toothpaste as much as possible. In the above manufacturing process, the degassing operation to remove air is typically performed over 20 to 60 m
This is carried out in parallel with or after the homogenization of the toothpaste components under HH vacuum. However, in either case, the viscosity of the system is high, so it takes a long time to degas the system, and it is not possible to completely remove even the smallest bubbles.
5 volumes of air bubbles remain in the toothpaste, but even if the air bubbles mixed into the toothpaste are as small as 2 to 5 volumes and are so minute that they cannot be detected with the naked eye, they still remain in the toothpaste. If toothpaste is stored for a long period of time, from several months to three years, there is a risk of deterioration and discoloration of the ingredients due to air oxidation caused by these small amounts of air bubbles, and the problem of decreased activity of medicinal ingredients is particularly 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, 1. In Japanese Patent Application Laid-Open No. 52-108031, 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
The above mixed powder at a rotation speed of 600 r, pom, or more,
A method for producing a toothpaste is proposed, which is characterized in that a fragrance and water are stirred and mixed together to form a wire-like material, and the wire-like material is degassed under reduced pressure.

This method is a preferable method because it can shorten the manufacturing time of toothpaste and increase productivity compared to conventional methods.
Due to the need to prevent deterioration of the binder due to mechanical shearing under high-speed stirring of 0 r, p, m or more, It is necessary to strictly set manufacturing conditions such as stirring time, and there is also the problem of degassing under reduced pressure a highly viscous braided wire in which the binder has swelled and dissolved. In addition, special public service No. 35-7699
Although the publication also proposes a method for manufacturing toothpaste, this method also has problems such as degassing under reduced pressure a high viscosity braided wire in which the binder has swelled and dissolved.

Furthermore, Japanese Patent Application Laid-Open No. 48-40947 discloses that liquid medium,
producing degassed or gas-free mixtures of dulling agents and abrasives, producing essentially gas-free mixtures of synthetic organic cleaning agents and liquid media, and mixing these mixtures; A gas-free method for producing paste-like or glue-like toothpaste has been proposed, but this method involves kneading abrasive powder into a highly viscous solution containing a swollen and dissolved binder to homogenize it. Operations such as heating and leaving for a long time to remove air bubbles in the synthetic organic detergent and polyhydric alcohol mixed aqueous solution, and furthermore, the binder swells and dissolves, and the abrasive powder is added to it. It is difficult to increase productivity because a low mixing efficiency operation is employed in which a mixture containing a synthetic organic (6) detergent is mixed into a kneaded extremely high viscosity mixture. Furthermore, this method is difficult to employ in systems containing a small amount of polyhydric alcohol.

The present inventors have improved the above situation, and there is no inclusion of air bubbles.
For this reason, as a result of extensive research on how to efficiently mass-produce high-quality toothpaste that is smooth on the skin and does not deteriorate during storage, we found that water or water and a wetting agent should be added to 1 part by weight of the abrasive. Preferably 0.5 parts by weight or more of the mixed solution is mixed, degassed, and finally a binder dispersed in a wetting agent is added and swelled and dissolved to homogenize the components and eliminate air bubbles at low viscosity. The present invention was based on the discovery that the above object can be achieved by efficiently and reliably mass producing a high quality toothpaste that is removable and free of air bubbles.

The present invention will be explained in more detail below.

In the method for producing toothpaste according to the present invention, preferably 0.5 parts by weight or more of water or a mixed solution of water and a wetting agent are mixed with 1 part by weight of the abrasive, deaerated, and finally added to the wetting agent. It is characterized by the fact that it swells and dissolves with the force of the dispersed binder, and as a result, it does not contain air bubbles and has a smooth skin with a good appearance and feel while being stored for a long time. This makes it possible to efficiently obtain a toothpaste that is resistant to deterioration even when the toothpaste is in use, and that can stably retain medicinal ingredients.

Here, as the abrasive, calcium diphosphate dihydrate and anhydride, tricalcium phosphate, calcium carbonate, aluminum hydroxide, alumina, insoluble sodium metaphosphate, calcium birophosphate, crystalline silica, amorphous silica, magnesium carbonate, magnesium phosphate,
Synthetic resin powder etc. are mentioned, and these 18 & or 2f
11! or more can be used. The particle size of these abrasives is not particularly limited, and an appropriate particle size can be used depending on the desired polishing effect, but the average particle size is usually 1 to 2.
0 μm is 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 entire toothpaste.

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

Furthermore, as binders, cellulose II 4 bodies such as sodium carboxymethylcellulose, methylcellulose, and hydroxyethylcellulose, carragina/alkali metal alginates such as sodium alginate, xanthan gum, gums such as tora gakanth (9) gum, karaya gum, and gum arabic are used. , polyvinyl alcohol, sodium polyacrylate.

Examples include synthetic binders such as 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. In addition, the amount of binder used is not limited to %, but it is usually 0% of the total toothpaste.
．． It is 3-5%.

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

In this operation, for example, water is first poured into a tank equipped with a stirring blade that allows the entire tank 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 mixed. In this case, it may be possible to reduce the pressure in the cylindrical mold and degas it under reduced pressure from the stage of dispersing and mixing the abrasive, but the viscosity of the slurry in which the abrasive is dispersed and mixed is water or water per 1 part by weight of the abrasive. Mixed solution of wetting agent (10) When the amount is 0.5 parts by weight or more, the bubbles are usually 2° 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 per 1 part by weight of the abrasive is less than 0.5 part by weight, air bubbles may not be removed sufficiently. It is preferable that the amount of the mixed solution is 0.5 part 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 wHg (absolute pressure).

In the present invention, the abrasive is first dispersed and mixed in water or a water-wetting agent mixture solution, and then degassed to remove air bubbles caused by the abrasive. 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, and lumityl sulfate.
IJum, higher fatty acid soap, anionic active agents such as sodium α-olefin sulfonate, nonionic active agents such as lauryl getanolamide, sucrose fatty acid ester, polyoxyethylene sorbitan monolaurate,
Among these are amphoteric activators, one or more of which are usually used in an amount of 1 to 7 qb of the total toothpaste.

These surfactants are mixed with abrasives in powder form,
Although it may be added to water or a water-wetting agent mixed solution, it is more preferable to add it to a slurry in which the abrasive is dispersed in water or a water-wetting agent mixed solution. In this case, the surfactant is one of the ingredients in the abrasive dispersion slurry! However, it is preferable to add a wetting agent that has been previously dispersed or dissolved in water or a mixed solution of water and a wetting agent. In addition, when using a mixed solution of water and a wetting agent,
The ratio of the wetting agent to 1 part by weight of water is preferably 4 parts by weight or more.

In addition, sweeteners such as saccharin sodium, sea-crose, maltose, lactose, perillartine, stevioside, and glycyrrhizin salts are usually used at 0.05 to 5
These may be dissolved in water or a water-wetting agent mixed solution before dispersing the abrasive, or they may be mixed with the powdery abrasive and mixed with water or a water-wetting agent mixed solution. The polishing agent may be mixed into the abrasive dispersion slurry, or may be dissolved and blended into the abrasive dispersion slurry. Furthermore, as fragrances, essential oils such as spearmint oil, varmint oil, salvia oil, eucalyptus oil, lemon oil, lime oil, wintergreen oil, and nnamon oil, and other spices,
Fruit Fusino 9-1 and isolated or synthetic fragrances such as vct-menthol, carvone, anethole, eugenol, etc. can be blended in an amount of usually 0.1 to 5%, and these fragrances can also be dispersed and mixed in an abrasive, etc. Although possible, it is preferably mixed into the abrasive dispersion slurry.

In addition, as a preservative, ethyl dioxybenzoate, i
Butyl 47 oxybenzoate, etc. may be blended, and medicinal ingredients include enzymes such as dextranase, lytic enzyme, lysozyme, a(13) mylase, and lytic enzyme, anti-plasmin agents such as epsilon aminocaproic acid and tranexamic acid, and fluorocarbons. Sodium chloride, sodium monofluorophosphate, difluoride
Fluorine compounds such as tin, chlorhexinone salts, quaternary ammonium salts, aluminum chlorohydroxylalantoin, glycyrrhetinic acid, chlorophyll, sodium chloride, phosphoric acid compounds, etc. may be blended, and silica gel, aluminum silica dal, organic acids and their salts, etc. may be blended as desired, but these ingredients may vary depending on their form,
Depending on the solubility in water, for example, in the case of water-insoluble powder, it is mixed with the abrasive, and in the case of water-soluble, it is added to the water before dispersing the abrasive, or to the water-wetting agent mixed solution or abrasive dispersion slurry. death,
Furthermore, if it is oily or oil-soluble, it can be mixed with perfume or added directly to the abrasive dispersion slurry.

In the present invention, when adding surfactants, fragrances, etc. to the abrasive dispersion slurry, the operation is carried out under reduced pressure, especially at
It is preferable to carry out under reduced pressure of ~100 mmHg (absolute pressure), and the viscosity is usually 2! 'i) Since the size is less than 1e and the pressure is reduced, air bubbles caused by surfactants and the like are reliably removed and no air bubbles are mixed in.

- Also, in this stage number, there is no restriction on the order in which surfactants, fragrances, etc. are added.

In the present invention, after the above-mentioned operations are performed, a binder is finally added, and the toothpaste is obtained by swelling and dissolving the binder. In this case, the binder is previously dispersed in a wetting agent. Use. In this way, by adding a binder dispersed in a humectant, a toothpaste that is good for the skin can be obtained.
If only one part of the binder is added, uneven swelling tends to occur and a good toothpaste cannot be obtained. 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 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 producing toothpaste, an abrasive and, if necessary, a surfactant are added to water or a mixed water-wetting agent solution. Since it is possible to disperse and mix powdery components containing many air bubbles, air bubbles can be removed easily and quickly.
In particular, by removing air bubbles under reduced pressure, air bubbles can be removed reliably and air bubbles can be prevented from being mixed in until the final binder swelling and dissolving process, so the resulting toothpaste does not contain air bubbles. It is something. Therefore, the method of the present invention can be very advantageously employed in the production of toothpaste with a transparent appearance, and since the toothpaste obtained by the method of the present invention does not contain air bubbles, air bubbles remain even after long-term storage. This prevents deterioration of the components due to Furthermore, as mentioned above, air bubbles are removed quickly and toothpaste can be produced without necessarily stirring at high temperatures or applying large shear forces to remove air bubbles, which improves the appearance and stability of the product. improves.

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 into a connoir. 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 Vc# agglomerates when the binder swells, so the resulting toothpaste has smooth skin, shine, and texture. It has a good appearance and good appearance.

(17) Next, examples will be shown to specifically explain the present invention. [Example 1] Calcium diphosphate 40%
Sorbitol (60% aqueous solution) 30 Glycerin 5 Sodium lauryl sulfate 2 Sodium carboxymethylcellulose 1.5 Sodium saccharin 0.2 Flavor
1.0 ethyl oxybenzoate 0.01
100.0% Water was placed in a vacuum stirring tank equipped with stirring blades that allowed total flow, and sodium saccharin and ethyl paraoxybenzoate were added 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 was less than 1 poise.

Next, calcium diphosphate was added to this aqueous solution and stirred for 5 minutes. At this stage, the viscosity should be less than 30 poise.
Also, most of the air bubbles in the powder (calcium diphosphate (18)) were removed during stirring.

Next, the inside of the stirring tank was heated to 700+o with a vacuum and J5 horn.
After creating a vacuum of +Hg (absolute pressure 60 mmHg),
Add fragrance and stir for 3 minutes, then add sodium lauryl sulfate.1. and stirred for 5 minutes. At this stage the viscosity is 10
Degassing and mixing were carried out well and easily at no more than poise.

Finally, sodium carboxymethyl cellulose moistened with glycerin was added under vacuum at an absolute pressure of 60 ranHg with stirring to swell and dissolve, thereby producing a toothpaste.

The obtained toothpaste did not contain air bubbles, had good texture and gloss, and was clean 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 air bubbles.
For this reason, as with conventional devices, the device volume is 2 times the actual toothbrushing volume.
There was no need to double the volume; approximately 1.2 times the volume was sufficient. In addition, since special operations such as stirring at high temperatures are not required to remove air bubbles, manufacturing time is shortened.
It was also advantageous from the viewpoint of stability of toothpaste quality.

[Example 2] Glycerin 27% Calcium silicate 20 Caldequin methyl cellulose sodium 0.6 Satucharin sodium 0.2 Sorbitol (
70 cIb aqueous solution) 40 Dye solution (1 aqueous) 0.2 Fragrance 1.2 Sodium lauryl sulfate 2.0 Ethyl laoxybenzoate 0.01
Ethyl paraoxybenzoate and sodium saccharin were dissolved in pure water in a stirring tank for high 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, evacuate the stirring tank to an absolute pressure of 30 to 100 wHg.
), fragrance and sodium lauryl 4fLrIk, which had been mixed in advance with an aqueous glycerin solution (80%) in a weight ratio of 4:1, were added and mixed.

Finally, while maintaining the vacuum state, sodium chloride methylcellulose, which had been dispersed in 1001 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 such transparent toothpaste, the presence of air bubbles is not good for the appearance, but in conventional manufacturing methods, the high viscosity of 300 voids or more after swelling of the binder prevents them from being released. Complete deaeration was difficult because air was being operated. However, according to this method, calcium silicate and sodium lauryl sulfate containing many air bubbles can be mixed with low viscosity water.
Because it is mixed and dispersed in polyhydric alcohol, bubbles can be removed easily and reliably, and moreover, it can be completely degassed in a short period of time.

(21)

Claims (1)

[Claims] 1. Mixing an abrasive with water or a mixed solution of water and a wetting agent,
After degassing, the viscosity is finally dispersed in the wetting agent. A method for producing a bubble-free toothpaste characterized by adding a binder and swelling and dissolving the toothpaste. 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 the 7 liquids of water or a mixed bath of water and a wetting agent. A method according to claim 1 or 2. 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 a reduced pressure of 10 to 200 mHg. Method. 5. A reduced pressure of 100 ■Hg according to claims 1 to 4, in which 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. The method according to claim 5, further comprising mixing. 7. The method according to any one of 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. 8. The method according to any one of claims 1 to 7, which comprises dispersing in a wetting agent and adding a caking agent under reduced pressure to cause swelling and dissolution.