JPS58208209A - Preparation of toothpaste - Google Patents

Abstract

PURPOSE:To obtain a toothpaste of high quality without containing air bubbles, by dispersing a powdery or granular material containing a polishing agent and a binder in a solution containing a wetting agent and water, deaerating the resultant slurry, and allowing the resultant slurry to stand to swell and dissolve the binder particles completely in the slurry. CONSTITUTION:A powdery or granular material containing a polishing agent, e.g. potassium secondary phosphate dihydrate, and a binder having 10-300mum average particle diameter, e.g. sodium carboxymethyl cellulose, or further a perfume is dispersed in a solution containing water and a wetting agent, e.g. glycerol, or further a surfactant, at 5-40 deg.C to form a slurry, which is then deaerated at 10-100mm.Hg (absolute pressure) reduced pressure while the binder is present in the particulate form. The slurry is then allowed to stand to swell and dissolve the binder particles completely in the slurry and give the aimed toothpaste. The time required for the powdery or granular material from the dispersion to the completion of the deaeration is 1-90sec. The resultant toothpaste will not easily deteriorate even for a long term.

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.

Practice +11N! # generally refers to abrasives such as calcium diphosphate, surfactants such as higher alkyl sulfates, wetting agents such as glycerin, and Cal? It is obtained by homogeneously mixing a binder such as oxymethylcellulose sodium, sweeteners, fragrances, medicinal ingredients, etc. with purified water and forming it into a fluid linear shape or a low fluidity dal shape. However, in this case, it is desirable that the manufacturing of toothpaste be efficient and highly productive. Also, bubbles (air) in toothpaste
If air bubbles are mixed in, it not only deteriorates the appearance but also causes a total deterioration in the quality of the toothpaste, so it is required to remove all 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 air bubbles must be removed more strictly during the manufacturing process. There is.

Conventionally, the industrial manufacturing method for toothpaste is to first swell and dissolve a binder in a wetting agent, purified water, etc. At this time, heat is applied as necessary to prepare a viscous swollen solution WL, and then this swelling A widely used method is to mix abrasive powder into a bath liquid, add surfactants, fragrances, medicinal ingredients, etc. to the mixture, homogenize it, and remove air to obtain lf4 toothpaste. However, in this method, the swelling bath solution typically has a poise of 100 to 400 poise (
BH type rotational viscometer, 2 Or, p, m, , 2~3
It is a viscous polymer solution with a high viscosity of The interaction between the abrasive powder and the swelling solution produces p-agglomerates, resulting in extremely high viscosity, which poses the problem of requiring 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 look bad, but the ingredients in the toothpaste will be oxidized, causing deterioration and discoloration, so it is necessary to remove air in toothpaste as much as possible. In the above manufacturing process,
The degassing operation to remove all air typically takes between 20 and 6
This is carried out in parallel with or after the homogenization of each toothpaste component under a vacuum of 0.0 Hg. However, in either case, due to the high viscosity of the thread, it takes a long time for degassing, and it is not possible to completely remove even the smallest air bubbles, and usually 2 to 5 volumes of air bubbles are left in the toothpaste However, even if the air bubbles mixed into the toothpaste are so small as to be 2 to 5 volumes and so minute that they cannot be detected with the naked eye, they can be used for several months to three years. If stored for a long period of time, the air generated by these small amounts of small air bubbles may cause deterioration and discoloration of the ingredients due to chemical reaction, 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 very low because the air) operation is carried out at high viscosity.Therefore, it has been desired to further improve the productivity and to perform the degassing more completely.

Regarding this point, Japanese Patent Application Laid-Open No. 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
The mixed powder, fragrance, and water are stirred and mixed with each other at a rotation speed of 00 r, p, m or more to form a wire-like object, and the wire-like object is degassed under reduced pressure. We are proposing a method for producing toothpaste that This method is a preferable method because it can shorten the manufacturing time of toothpaste and increase productivity compared to the conventional method, but it is difficult to cause caking due to mechanical shearing under high-speed stirring of 600 r, p, m3 or more. In order to prevent the deterioration of the agent, it is necessary to strictly set the manufacturing conditions such as the rotation speed of the stirrer and the stirring time according to the loft of the raw materials, especially the binder.
There is also the problem of degassing under reduced pressure a highly viscous braided wire in which the binder has expanded or dissolved in the bath. In addition, special public service
Publication No. 699 also proposes a method for manufacturing toothpaste,
This 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 an essentially gas-free mixture of a synthetic organic cleaning agent and a liquid medium; and mixing the mixtures. A method for manufacturing paste-like or rubber-like toothpaste that does not contain gas has been proposed, but this method involves kneading abrasive powder into a high-viscosity solution containing a swollen solution of a binder. In addition, operations such as heating and leaving for a long time to remove air bubbles in the synthetic organic detergent and polyhydric alcohol mixed water bath solution, and the swelling and dissolution of the binder, Because we use an operation with low mixing efficiency in which a mixture containing synthetic organic detergent is mixed with an extremely high viscosity mixture containing abrasive powder,
It is difficult to increase productivity. Furthermore, this method is difficult to apply to yarns 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, we conducted extensive research into a method for efficiently mass-producing high-quality toothpaste that is smooth on the skin and does not deteriorate during storage. The caking agent is dispersed in a mixed solution containing water to form a slurry, and the caking agent is degassed while it is present in the form of particles in the slurry, and then the degassed slurry is left to stand. By expanding the particles of the agent, it is possible to homogenize the components and remove air bubbles at low viscosity, and it is possible to efficiently and reliably mass-produce high-quality line drawings M that do not contain air bubbles, achieving the above objectives. found that it is achieved,
This is what led to the present invention.

The present invention will be explained in more detail below.

The method for producing a toothpaste according to the present invention includes dispersing a mixed powder containing an abrasive and a binder in a mixed solution containing a wetting agent and water to form a slurry, and adding the binder to the slurry. While the binder particles exist in the form of particles, that is, before the binder particles are completely swollen and dissolved, the binder particles are fully degassed, and then the degassed slurry IJ-grape device is used to completely swell the binder particles. ＠It is a t-% bond to dissolve the line drawing order in the bath, and in this way, do not turn on the deaeration before the binder particles are completely dissolved and swollen, or leave it to caking after degassing. By dissolving and swelling the drug particles, it does not contain air bubbles, resulting in a smooth skin with a good appearance and feeling of use.It also does not deteriorate easily even after long-term storage and stably retains medicinal ingredients. This makes it possible to efficiently obtain a toothpaste that can be used as a toothpaste.

Here, the abrasives used in the preparation of the mixed powder and granule material include tertiary calcium dihydrate and anhydride, tricalcium phosphate, calcium carbonate, aluminum hydroxide, alumina, insoluble sodium memelate, calcium birophosphate, Examples include crystalline silica, amorphous silica, magnesium carbonate, magnesium phosphate, synthetic resin powder, etc., and one or more of these can be used.

The particle size of these abrasives is not particularly limited, and any appropriate particle size may be used depending on the required 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 immerse the tooth in hot water, and a Mohs hardness of 3 or less is usually used. Also, the amount of abrasive used is not limited, but it is usually 20 to 6 of the total #I tooth layer.
0% (1 amount of rice cake, the same applies hereinafter) may be blended.

As a binder, Calxymethyl cellulose (I)
Cellulose derivatives such as Jum, methylcellulose, and hydroxyethylcellulose, carrageenan, alkali metal alginates such as sodium alginate, xanthan gum, and toragakanth gum.

Examples include gums such as karaya gum and gum arabic, and synthetic binders such as polyvinyl alcohol, sodium polyacrylate, and calgexivinyl polymer, which swell and dissolve in water. One or more of these may be used. can do. In this case, the particle size of these binders is appropriately selected depending on their type, but in any case, they do not completely swell and dissolve before or during degassing, and if they are left unattended after degassing. The binder should be selected so as not to cause uneven swelling, and therefore the average particle size of the binder is preferably in the range of 10 to 3004 m, most preferably in the range of 30 to 100 m. If the average particle size of the binder is too small, the rate of swelling and dissolution will be too fast, and the binder will completely swell and dissolve before and during degassing, resulting in an extremely high viscosity. If air bubbles are not removed sufficiently and the average particle size of the binder is too large, the binder particles will exist sparsely in the slurry, and when they swell and dissolve after being left to roll, they will become viscous. Since the local concentration of the binder increases significantly, surrounding particles such as abrasives are trapped and aggregated, resulting in uneven swelling due to uneven swelling. When uneven swelling occurs, the texture and gloss of the trout polishing deteriorates, and liquid separation becomes more likely to occur.

Note that the amount of binder used is not particularly limited, but is usually l#
JI11iIiNJ may be blended in a range of 0.3 to 5- of the total JI11iIiNJ.

Further, as wetting agents, glycerin, propylene glycol, sorbitol, polyethylene glycol, polyethylene glycol, xylitol, maltitol, lactitol, etc. may be used, 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 the present invention, the abrasive and the binder are uniformly mixed to prepare a homogeneous mixed powder sound, and the wetting agent is dissolved in water to prepare a mixed solution. Depending on the composition, surfactants, sweeteners, fragrances, preservatives, medicinal ingredients, etc. can be added.

In this case, the surfactant includes sodium lauryl sulfate, sodium myristyl sulfate, sodium noglumityl sulfate, higher fatty acid soap, anionic surfactant such as sodium α-olefin sulfonate, lauryl jetanolamide, sucrose fatty acid ester, Examples include nonionic surfactants such as polyoxy7-ethylene sorbitan monolaurate, and amphoteric surfactants, and one or more of them are usually used in a proportion of 0.1 to 7% of the total toothpaste.

Although these surfactants can be uniformly mixed into the mixed powder or granule as they are, they are preferably dissolved in a mixed solution. Sweeteners include saccharin sodium, sucrose, maltose, lactose,
, stevioside, glycyrrhizin salts, etc. usually 0.0
5 to 5 pieces may be blended, and these may be mixed into the mixed powder or granular material as they are in powder or granule form, or may be dissolved and blended into the mixed solution. In addition, essential oils such as spearmint oil, peppermint oil, salvia oil, eucalyptus oil, lemon oil, lime oil, wintergreen oil, cinnamon oil, other spices, flora flavor, and t-menthol are used. , Cal d? Isolated or synthetic fragrances such as anethole, anethole, and eugenol are usually 0.
It is also possible to mix and disperse these fragrances in the mixed powder or mixed solution, but it is also possible to put them in a separate storage tank and mix the mixed powder and the mixed solution. It is preferable to add and mix at the same time.

Also, is it A as a preservative? laoxybenzoic acid ether,・
Medicinal ingredients include enzymes such as dextranase, lytic enzyme, lysozyme, amylase, bath fungus yeast, anti-plasmin agents such as epsilon aminocaproic acid and tranexamic acid, and sodium fluoride. , sodium monofluorophosphate,
Fluorine compounds such as tin fluoride, chlorhexidine 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. In the case of non-water-bathable powder or granules, it can be mixed into a mixed powder or granule, in the case of water-bathable, it can be mixed in a mixed solution, or in the case of oily or oil-bathable, it can be mixed with a perfume to prepare an oily mixture.

In the present invention, when the mixed powder and granular material, the mixed solution, and an oily mixture containing a fragrance are separately prepared, the oily mixture is mixed to form a slurry, and binder particles are present in this slurry. The slurry is completely degassed while the slurry is in the slurry, and then the degassed slurry is left to swell and dissolve the binder particles.

To celebrate this with a drawing, 1 in the figure is a powder mixer;
An abrasive, a viscous paste, and if necessary, a surfactant and other powders are mixed for a predetermined period of time to prepare a homogeneous mixed powder. 2 is a stirring tank in which a wetting agent and, if necessary, a sweetening agent are dissolved in water to prepare an fC mixed solution. 3 is also a stirring tank in which fragrances and other oily components are mixed as necessary to prepare an oily mixture. Next, the mixed powder and granular material is continuously fed to the solid-liquid continuous mixer 7 at a predetermined ratio by the constant electric feeder 4 for powder, and the mixed solution and oily mixture by the ponders 5 and 6, respectively. to prepare a slurry in which the mixed powder and granular material and the oily mixture are dispersed in the mixed solution. Next, this slurry is passed through a deaerator 8 to deaerate the air, and then left to stand.

Here, as the liquid continuous dispersion machine 7, commercially available devices such as a fluff mixer manufactured by Takarakoki Co., Ltd., a flow jet mixer manufactured by Kouken Co., Ltd., and a Hun Exhaust Mazeller manufactured by Tokushu Kika Kogyo Co., Ltd. are used. City can. - Also, a vacuum continuous defoaming machine is suitable for the defoaming machine 8, and CORNg
Passator made by LL MACHINK COMPANY, F
RYMA-Mashinen AGJI! j free-
A commercially available device such as a vacuum foamer of type rVE can be used. In addition, when using the same liquid continuous mixer 7 capable of defoaming under reduced pressure, the use of the defoaming machine 8 can be omitted by performing solid-liquid mixing and degassing at the same time.

In addition, in the solid-liquid mixing process in which a slurry is prepared by dispersing mixed powder and granules in a mixed solution, and a fragrance or an oily mixture containing a fragrance prepared separately from these if necessary, the same liquid dispersion mixing temperature is If the temperature is low, the binder particles will not sufficiently swell and dissolve even when heated after degassing, resulting in a low viscosity of the toothpaste and a tendency for liquid separation to occur during storage.

On the other hand, if the dispersion mixing temperature is too high, the adhesion force on the surface of particles of powder components such as binders and abrasives becomes strong, causing agglomeration of particles, and clumps are likely to occur. In this respect, the solid-liquid dispersion mixing temperature is particularly preferably in the range of 5 to 40°C, and the average particle size of the binder is 10 to 300 μm.
In the case of using the same, the temperature is preferably 51 to 40°C, most preferably 15 to 30°C.

As a result of intensive research on the swelling and dissolution rate of binders, the present inventors found that in order to make the binder exist in particulate form during the liquid dispersion and degassing operations, the binder particle size and It was discovered that there is an optimum range for the dispersion temperature, and that the swelling and dissolution rate of the binder depends on its particle size at a constant temperature, regardless of the type of binder. By producing toothpaste with an average particle size of the binder of 10 to 300 μm and a solid-liquid dispersion mixing temperature in the range of 5 to 40°C, the binder remains particulate during the same liquid dispersion and degassing operations. However, after degassing, it swells and dissolves uniformly when left to stand, producing a stable toothpaste that does not contain air bubbles and has good texture and gloss.

In this case, the time for dispersion and mixing of the same liquid is
By using a liquid continuous mixer, the deaeration time can be set to 91 to 60 seconds, and by using the vacuum continuous defoaming machine described above, the degassing time can be set to 1 to 30 seconds. By performing the liquid dispersion and deaeration for about 1 to 90 seconds in total, the binder is not completely swollen and dissolved during this process.
After degassing, the binder can be present in particulate form. In addition, during the solid-liquid dispersion and degassing operations, the binder exists in the slurry in the form of particles without swelling or dissolving in the bath. The viscosity is 500 to 2000 poise, but the viscosity can be lowered to about 5 to 20 poise, making it possible to homogenize the components and deaeration quickly and reliably. Quality A toothpaste can be manufactured with high productivity. Note that bubbles and air in the slurry can be removed reliably and with degassing.

The slurry obtained through the solid-liquid dispersion and degassing operations described above has air bubbles removed. Binder particles are present in this slurry, but when left to stand, the binder swells over time and becomes linear or glue-like (9), thereby producing a toothpaste. . Note that the temperature at which the slurry is left is not particularly limited, but room temperature is usually sufficient.

According to the above-mentioned method for producing fc drawings, it is possible to disperse and mix powdery components with low viscosity and many bubbles, so that bubbles can be easily and quickly removed, and in particular, bubbles can be removed under reduced pressure. In particular, the removal of air bubbles is ensured, so that the toothpaste obtained is free of air bubbles. In fact, the method of the present invention can be very advantageously 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 time. Deterioration of components due to the presence of air bubbles is prevented. Furthermore, as mentioned above, air bubbles can be removed easily and quickly, and it is not necessary to stir at high temperatures or apply large shear forces to remove air bubbles, so manufacturing can be carried out efficiently and products can be Improves appearance and stability.

f. According to the present invention, the skin is clean, has good luster and texture, and has an excellent appearance! It is possible to obtain a tooth layer.

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

[Example 1] Calcium/umium diphosphate 45 Sodium thilauryl sulfate 2.0 Sodium calxexymethylcellulose 1.0 (average particle size 100~
150μm) Glycerin 25 Satucharin Sodium 0.2 Flavor
1.0M water
Remaining 100.0% Calcium diphosphate, sodium laurate, and sodium chloride 7-methyl cellulose having an average particle size of 100 to 150 μm were mixed in a ribbon mixer to prepare a mixed powder. Separately, saccharin sodium t-g was dissolved in purified water, and glycerin was mixed thereto to prepare a mixed solution v4 at a temperature of 20°C.

Next, the mixed powder, mixed solution, and fragrance are each continuously fed at a predetermined ratio using a powder metering feeder and a metering pump to the same liquid continuous grazing machine (flash mixer manufactured by Hogyokuki Co., Ltd.). did. At this time, the throughput of the solid-liquid continuous disperser was 500 + (f/hr, and the temperature was 20°C.
The slurry prepared by a continuous liquid dispersion machine contains particulate binder (Kalichi xynonalcellulose sodium), and the slurry is passed through a continuous defoaming machine (Pazator, manufactured by Coronel), which is reduced to a vacuum level. , a bubble-free slurry was obtained.

The binder in this slurry was still particulate, but when left at room temperature, the binder quickly swelled and dissolved uniformly.
This resulted in a toothpaste that did not contain air bubbles, was smooth on the skin, and was stable.

In addition, in the above manufacturing method, when solid-liquid continuous dispersion is performed at a temperature of 2°C, the binder does not swell and dissolve sufficiently even if heated to 30°C after defoaming, resulting in The viscosity of the tamarind was low, and liquid separation occurred after 3 months. Furthermore, when continuous dispersion of the same liquid was carried out at 45°C, agglomeration of particles occurred, which significantly adhered to the inside of the continuous solid dispersion machine. [Example 2] Amorphous silica 19.8% lauryl (IIIE Sodium acid 1.5 Carrageenan (average particle size 10-30 μm) 1.0 Glycerin 25.0 Sorbitol (60
-Aqueous solution) 50.8 Sacchulin sodium 0.2 Flavor
0.8100.0* Amorphous silica, sodium lauryl sulfate and average particle size 1
Carrageenan of 0 to 30 μm was mixed in a luxury mixer to prepare mixed powder 1c. Separately, a mixed solution was prepared by mixing glycerin, sorbitol, and purified water, and dissolving saccharin sodium therein.

Next, the mixed powder and granular material, the mixed solution, and the fragrance were continuously supplied at predetermined ratios to a solid-liquid continuous dispersion machine (Flownoet mixer manufactured by Kouken Co., Ltd.) using a powder metering feeder and a metering pump, respectively. At this time, the pressure inside the solid-liquid continuous disperser was reduced to maintain a degree of vacuum of 30 to 60 mHg, the treatment time was 1000 kg/hr, and the treatment temperature was 10°C.

The slurry prepared by the solid-liquid continuous dispersion machine had air bubbles removed and particles of the binder (carrageenan) were present immediately after preparation, but it was left at room temperature for about 10 minutes. As a result, the binder was dissolved at an expansion rate of f/4, and a transparent line #1 layer containing no air bubbles, having a smooth skin, and being stable was obtained.

[Example 3] Calcium carbonate 46 Sodium α-olefin sulfonate 2.0 Sodium alginate (
Average particle size 250-300 μm) 1.1 Sorbitol (60-aqueous solution) 30 Saccharin sodium 0.2 Flavor
1.0*m water
Remaining 100.04 Calcium carbonate, sodium α-olefin sulfonate, and sodium alginate having an average particle size of 250 to 300 μm were mixed in a Henschel mixer to prepare a mixed powder. Separately, a mixed bath solution in which saccharin sodium was dissolved in purified water and sorbitol was mixed therein was subjected to NI.

Next, the mixed powder and granules, mixed solution, and fragrance were each fed into the same liquid continuous dispersion machine (Fun Ekima Zeller manufactured by Tokushu Kika Kogyo Co., Ltd.) at a predetermined mixing ratio using a powder feeder and a metering pump. Next. At this time, the throughput of the solid-liquid continuous disperser is 8
00kl? /hr and the temperature was 40°C. The slurry prepared by this liquid continuous dispersion machine contains a binder (sodium alginate) in the form of particles, and then this slurry is mixed with the binder in the form of particles for 40 minutes. Freema VE type continuous defoaming machine (FRYMA-Maahlnen A) decompressed to a vacuum degree of ~50 smHH
(manufactured by Q) was passed through the slurry to obtain a slurry containing no air bubbles.

The binder in this slurry was still particulate, so when it was left at room temperature, the binder completely expanded after about 10 minutes.
4 Knead 111 that dissolves and contains air bubbles for smooth and stable skin
11 layers were obtained.

Note that the passage time from the solid-liquid continuous dispersion machine to the continuous defoaming machine was about 30 seconds.

In addition, in the above production method, when the average particle size of sodium alginate is set to 3-5 μm, swelling and dissolution of the binder proceeds immediately after the liquid passes through the continuous dispersion machine, resulting in a significant increase in the viscosity of the slurry. However, it was not possible to completely remove air bubbles using a continuous deaerator.

Furthermore, the average particle size of sodium alginate is 350 to 40
If it is set to 0 μm, swelling of the binder iMtr etc. will occur,
Ren's skin has deteriorated.

[Brief explanation of the drawing]

The drawing is a flow sheet illustrating one embodiment of the invention. 1... Powder mixer, 2, 3... Stirrer, 7... Same-liquid continuous dispersion machine, 8... Defoaming machine. 8

Claims (1)

[Claims] 1. Dispersing mixed powder and granular material containing an abrasive and a binder in a mixed solution containing a wetting agent and water to form a slurry,
Deaeration is performed while the binder is present in the form of particles in the slurry, and the deaerated slurry is then left to completely swell and dissolve the binder particles. A method for producing toothpaste that does not contain 2. The method according to claim 1, wherein a surfactant is mixed into the mixed solution. 3. The method according to claim 1 or 2, wherein the fragrance is dispersed in the mixed solution together with the mixed powder and granules. 4. The binder has an average particle size of io to 300 Am, and the temperature when dispersing the mixed powder and granular material in the mixed solution is 5.
The method according to any one of claims 1 to 3, wherein the temperature is 40°C. 5. The method according to any one of claims 1 to 5, wherein the time from dispersing the mixed powder and granular material in the mixed solution to completing the deaeration of the slurry is 1 to 90 seconds.