JP4937640B2 - Dentifrice manufacturing method and dentifrice manufacturing apparatus - Google Patents

Description

  The present invention relates to a method for producing a dentifrice, a dentifrice, and an apparatus for producing a dentifrice.

In general, a dentifrice contains ingredients such as an abrasive, a foaming agent, a wetting agent, a binder, and a fragrance. And, in order to obtain the flavor, kneaded skin, shape retention, cleaning power, etc., which are the design quality of the dentifrice, it is necessary in manufacturing to ensure uniform dispersion, uniform swelling, etc. by combining the above components It becomes a condition.
Therefore, equipment having sufficient shearing force and kneading force is usually used for production.

In addition, dentifrices that are subject to the Pharmaceutical Affairs Law are required to satisfy GMP (Good Manufacturing Practice), which is a requirement for producing excellent products with good quality.
Therefore, it is necessary to thoroughly manage the production lot, and in many cases, the dentifrice production facility is a batch-type facility that is easy to manage.

However, in such a production facility, in the case of a multi-product production process, it takes time and effort to perform a washing operation or the like when the product is switched.
This labor for changing the product type requires a great deal of labor compared to those that are not subject to the Pharmaceutical Affairs Law, and this is a major factor that deteriorates the total manufacturing efficiency in the multi-product production process.

In order to solve this problem, many proposals for improving the efficiency of the manufacturing process have been made.
For example, in Patent Documents 1 to 3, the production time cycle and the like are shortened by improving the blending order and mixing conditions of a binder, an abrasive, a wetting agent, and the like in a batch blending manufacturing process.
In Patent Documents 4 to 5, manufacturing efficiency is improved by charging and mixing a mixed powder such as an abrasive and a binder mixed in advance into a liquid component.
Moreover, in patent documents 6-8, the improvement of manufacturing efficiency is achieved by continuous production.

Patent Document 9 describes a method of promoting the swelling of the binder by bringing the components excluding the fragrance component to a high temperature of 40 to 80 ° C. and mixing them together, and then statically mixing the fragrance component at 50 ° C. or less. Has been. In this method, the efficiency of swelling of the binder is achieved by batch-mixing the components excluding the fragrance component at a high temperature.
Japanese Patent Laid-Open No. 11-171743 JP-A-11-171748 JP-A-11-171747 JP 52-108031 A JP 58-208209 A Japanese Patent No. 1932177 JP-A-1-165515 JP-A-6-9335 Japanese Patent No. 3107920

However, the proposals in Patent Documents 1 to 3 require batch cleaning for each type change, and the frequency thereof does not change, so that the total manufacturing efficiency is insufficient.
In addition, in the methods of Patent Documents 4 to 5, it takes a long time to add a large amount of powder component, or the powder component is charged in a short time. It is assumed that labor is required for cleaning. Furthermore, a special device for pre-mixing the powder is required, and there is a great concern about the occurrence of lumps due to partial swelling of the binder (decrease in stability).

In addition, the proposals of Patent Documents 6 to 8 have problems in that it is difficult to quantitatively supply each composition component and follow-up lots, there are a large number of small raw materials, and in-line cleaning is necessary.
In this in-line cleaning, the reliability of cleaning is often insufficient in terms of sterilization and the like, and it is necessary to disassemble and clean the piping. For this reason, it takes a lot of time for dismantling, cleaning, assembly, etc. when changing the product type, and the number of days and the required number of people are required.

Furthermore, in the method of Patent Document 9, since it is necessary to cool before adding the fragrance component, actually, a heat exchanger that is difficult to dismantle and clean is provided as a manufacturing facility. Therefore, it is not preferable on GMP.
In addition, the addition of the fragrance component by static mixing theoretically requires a very large number of modules in order to completely and uniformly disperse the high-viscosity paste and the low-viscosity fragrance component. For this reason, the total length of the piping is increased, and in practice, microscopic uniform dispersion is insufficient. Therefore, the perfume component and other components are not easily adapted, and the dentifrice is insufficient in terms of quality such as flavor.

  The present invention has been made in view of the above circumstances, and the quality, such as uniformity, flavor, paste skin, shape retention, stability, etc., in dentifrices is good, as well as production efficiency and cleanability of compounding equipment. It is an object of the present invention to provide an excellent dentifrice production method and dentifrice, and a dentifrice production apparatus.

As a result of intensive studies, the present inventors have completed the present invention in order to solve the above problems.
That is, the present invention is a method for producing a dentifrice by mixing dentifrice raw materials, the raw materials are charged into a stirring tank, a part of the contents in the stirring tank is taken out, and the taken out contents Is mixed with other raw materials charged into the low-shear mixer using a low-shear mixer, and the mixture is returned to the stirring tank to mix the dentifrice raw materials to produce a dentifrice. It is a manufacturing method of the dentifrice characterized by the above-mentioned.
In the method for producing a dentifrice of the present invention, the stirring tank having a rotary stirring blade, and a circulation path for taking out a part of the contents in the stirring tank and returning the taken contents back into the stirring tank again. It is preferable to use the in-line type low shear mixer having a vibration type stirring blade provided in the middle.
Further, in the method for producing a dentifrice of the present invention, a part or all of a liquid raw material containing water and / or a wetting agent is charged into the stirring tank, and an abrasive, a binder, a fragrance, a foaming agent, water and It is preferable to introduce at least one selected from a wetting agent into the stirring tank and / or into the low shear mixer.
Moreover, in the manufacturing method of the dentifrice of this invention, it is preferable that the said abrasive | polishing agent contains disintegrating silica and throws the said abrasive | polishing agent in the said stirring tank.
In the method for producing a dentifrice of the present invention, it is preferable that the fragrance is put into the low shear mixer.
Moreover, in the manufacturing method of the dentifrice of this invention, it is preferable that the linear velocity of the said rotary stirring blade tip shall be 1-5 m / s.
Moreover, in the manufacturing method of the dentifrice of this invention, it is preferable that the maximum speed of the said vibration type stirring blade shall be 0.1-1.2 m / s.
In the method for producing a dentifrice of the present invention, it is preferable that the vibration frequency of the vibration type stirring blade is 5 to 30 s ⁻¹ and the amplitude of the vibration type stirring blade is 2 to 6 mm.
The present invention is a dentifrice produced by the method for producing a dentifrice.
The present invention comprises a stirring tank, a circulation path for taking out the contents in the stirring tank, returning the taken contents back into the stirring tank, and a low shear mixer provided in the middle of the circulation path. An apparatus for producing a dentifrice characterized by comprising:
In the dentifrice production apparatus of the present invention, it is preferable that the low shear mixer is an in-line low shear mixer having a vibrating stirring blade.

  ADVANTAGE OF THE INVENTION According to the present invention, a method for producing a dentifrice and a dentifrice having good quality, such as uniformity, flavor, kneaded skin, shape retention, stability, etc. in the dentifrice, and excellent production efficiency and cleanability of the blending equipment. And an apparatus for producing a dentifrice can be provided.

  Hereinafter, the method for producing a dentifrice of the present invention and the device for producing a dentifrice will be described in detail along the procedure with reference to the drawings.

≪Dentifrice manufacturing equipment≫
In the device for producing a dentifrice of the present invention, the agitation tank has a rotary agitation blade, the agitation device attached to a shaft that is rotated by a motor or the like, and the contents (raw material or raw material mixture). ) Is provided with a predetermined container.
Examples of the rotary stirring blade include a propeller blade, a paddle blade, a helical ribbon blade, a screw blade, an anchor blade, and a turbine blade. Among these, it is preferable to use a combination of a paddle blade and an anchor blade attached with a wall surface oyster blade from the standpoint of the cleaning performance and the mixing efficiency of the entire high-viscosity liquid in the stirring vessel.

FIG. 1 shows an embodiment of an apparatus for producing a dentifrice of the present invention.
In FIG. 1, the stirring tank 10 includes a plurality of honey 11 a protruding inside the stirring tank 10 and a blade 11 b with a wall surface oyster blade with a blade 11 b that scrapes the wall surface integrated via a U-shaped shaft 11 c, This is a main compounding tank having a plurality of low-speed rotating type stirring blades 12 and having a raw material inlet 13 and a content outlet 14 at the bottom.
The wall surface wing 11 with wall surface oyster blades and the plurality of low-speed rotation type stirring blades 12 are provided at the same rotation center axis position, but the wall surface oyster is formed by the multi-axis rotation shaft 17 arranged at the center thereof. The blade-attached side wall blade 11 and the plurality of low-speed rotation type stirring blades 12 are configured to be rotatable in the same direction or in the opposite direction individually or both simultaneously.
Either one of the low-speed rotation type stirring blade 12 and the side wall pit 11 with wall surface oyster blades is rotated (at this time, the other is fixed without rotating), or the raw materials are stirred by rotating both of them. Mix. Since mixing efficiency is good, it is preferable to stir and mix the raw materials while rotating both (preferably while rotating in the opposite direction).
Further, the rotational speed of the rotary stirring blade, that is, the low-speed rotation type stirring blade 12 and the wall-side honey-blade 11 with wall surface oyster blades is preferably set on the basis of the linear velocity at the tips of the stirring blade 12 and the wall-side honey-wall-side blade 11. Is 1 to 5 m / s, more preferably 1 to 3 m / s. When the linear velocity is 1 m / s or more, mixing efficiency such as solubility and dispersibility of the raw material is improved. On the other hand, by being 5 m / s or less, mixing of bubbles is suppressed and flavor quality is also improved.

In addition, the said linear velocity is calculated | required from the calculation formula (1) shown below.
Formula (1): U = πND / 60
U: Linear velocity (m / s), N: Number of rotations (rpm), D: Stirring blade diameter (m).

The agitation tank 10 has a circulation path (external circulation line) 36.
The circulation path 36 includes paths 30, 31, 32 composed of pipes connected in series, and a path 33 and a path 34 branched into two from the path 32, and the path 33 is formed in the upper part of the stirring tank 10. The paths 34 are respectively connected to the inner bottom of the stirring tank 10.
Further, the inlet side of the path 30 is connected to the discharge port 14 formed at the bottom of the stirring tank 10 via a pump 39.
In the circulation path 36, a low-shear mixer 20 is provided between the path 31 and the path 32, and the circulation is performed so that the raw material mixture circulates between the low-shear mixer 20 and the stirring tank 10. The path 36 is attached to the stirring tank 10.
Further, in the circulation path 36, the discharge path 35 branches from between the path 30 and the path 31.

In the dentifrice production apparatus of the present invention, the low-shear mixer is preferably an in-line low-shear mixer having a vibrating stirring blade. By being the low shear mixer, the uniform dispersibility when mixing the raw materials is improved, and the mixing efficiency is increased. Moreover, the disintegration of the powder component having a weak particle strength is suppressed, and the quality such as flavor is improved.
Here, the “in-line type” means a type in which a mixer is installed in the middle of a pipe (circulation path or the like) and the contents (raw material or raw material mixture) passing through are continuously stirred.
The low-shear mixer is not agitated by rotation of the stirring blade, but is stirred by vibrating the stirring shaft to which the stirring blade is attached in the longitudinal direction of the stirring shaft (the height direction of the low-shear mixer). It is a blender. Specific examples include mixers disclosed in JP-A-2-293035 and JP-A-2000-157856.
Examples of the vibration type stirring blade include a disk type, a porous disk type, and a spiral type. Of these, the spiral type is preferable in terms of mixing efficiency. By making the stirring blade spiral, the raw material mixture flowing along the spiral flow path is repeatedly “folded” and “stretched” by the vibration of the stirring blade to promote mixing. The stirring blade is more preferably a spiral blade having a hole. By making the holes, a circulation flow is generated, and the mixing efficiency is further increased.

  The low-shear mixer 20 is connected to the inlets from the raw material tanks 40 and 50, for example, in FIG. 1, the raw material inlet 21 connected to the raw material tank 40 of the powder component is connected to the low-shear mixer 20. On the bottom side in the height direction, a raw material inlet 22 connected to the raw material tank 50 for the fragrance component is provided in the center in the height direction of the low shear mixer 20.

FIG. 2 is a partial cross-sectional view showing the configuration of the mixing unit 25 in an example of the low shear mixer 20. Hereinafter, description will be given with reference to FIG.
The low shear mixer 20 is configured by stacking a plurality of substantially hollow cylindrical mixing units 25 in the height direction. In this example, ten mixing units 25 are stacked.
In the low shear mixer 20, the mixing units 25, 25 adjacent to each other in the vertical direction are partitioned by a donut plate-like partition plate 25 a. A rod-shaped stirring shaft 24 is provided at the center of the low-shear mixer 20, and a spiral blade-type stirring blade 23 having pores 23a is provided around the stirring shaft 24.
The stirring blades 23 are provided in the respective units 25, and are arranged between separator plates 25a and 25a that separate the mixing units 25.
In this example, the first raw material inlet 21 is provided in the first stage mixing unit 25, and the second second raw material inlet 22 is provided in the fifth stage mixing unit 25. It has been.
At the time of mixing the raw materials, the raw material introduced into the lowermost mixing unit 25 from the stirring tank 10 via the path 30 and the path 31 is moved between the partition plate 25a and the stirring shaft 24 by the vibration of the stirring blade 23. From the gap 32, the mixing unit 25 is pushed up, and the raw materials charged from the raw material charging ports 21 and 22 are sequentially mixed, and further pushed up from the path 32 provided in the uppermost mixing unit 25, A mixture of raw materials is taken out.

  Here, the low-shear mixer is a shear rate with the maximum speed of the vibration type stirring blade preferably 0.1 to 1.2 m / s, more preferably 0.1 to 0.7 m / s. A blender. By setting the maximum speed to 0.1 m / s or more, the uniform dispersibility of powder components such as a binder is improved and the mixing efficiency is increased. On the other hand, by setting it as 1.2 m / s or less, disintegration of the powder component with weak particle strength is suppressed, and flavor quality is improved.

The maximum speed of the vibration type stirring blade can be obtained from the following calculation formula (2).
Formula (2): U = 2πfa
U: Maximum speed of stirring blade (m / s), f: Vibration frequency (s ⁻¹ ), a: Amplitude of stirring blade (m).

In the present invention, the oscillation frequency of the stirring blade of the vibratory preferably be 5～30S ^-1, and more preferably a 10~20s ^-1.
Furthermore, in the present invention, the amplitude of the vibration type stirring blade is preferably 2 to 6 mm, and more preferably 3 to 5 mm.
By setting the vibration frequency and the amplitude to be equal to or greater than the lower limit value of the range, the uniform dispersibility of the powder component such as a binder is improved and the mixing efficiency is increased. On the other hand, by setting it to the upper limit value or less, the collapse of the powder component having a weak particle strength is suppressed, and the flavor quality is improved.
As the in-line type low shear mixer having the vibration type stirring blade, for example, a Vibro mixer (trade name, manufactured by Chilling Industries Co., Ltd.) is preferably used.

At the time of mixing the raw materials, a part of the contents in the stirring tank 10 is taken out from the discharge port 14 at the bottom of the stirring tank 10 by the pump 39 and passes through the path 30 and the path 31 following the discharge port 14 to be a low shear type It is sent to the mixer 20.
The fed raw material is mixed with the raw material introduced from the raw material inlets 21 and 22 by the low shear mixer 20, and this mixture is taken out from the low shear mixer 20 through the path 32.
The end of the path 32 on the stirring tank 10 side is branched into a path 33 and a path 34, the path 33 is connected to the inner upper part of the stirring tank 10, and the path 34 is connected to the inner bottom of the stirring tank 10. The mixture in the path 32 is divided into paths 33 and 34 and is introduced into the stirring tank 10 from above and below the stirring tank 10.
Note that the mixture in the path 32 may be introduced into the stirring tank 10 from either one of the paths 33 and 34.
In addition, the powder component can be directly introduced into the stirring tank 10 mainly from the raw material inlet 13.
One or both of the stirring tank 10 and the low-shear mixer 20 can be used to easily supply a powdery raw material or the like from the raw material inlet 13 or the raw material inlets 21 and 22 by reducing the pressure inside. It can be quickly introduced into the system.
Moreover, the manufactured dentifrice is discharged | emitted out of the system by the discharge path 35 branched between the path | routes 30 and 31. As shown in FIG.

≪Method of manufacturing dentifrice≫
The manufacturing method of the dentifrice of this invention is manufactured using the said dentifrice manufacturing apparatus of this invention as one example of embodiment.
Hereinafter, it demonstrates for every process.

<Step 1>
A part or all of a liquid raw material such as water and a wetting agent is charged into the stirring tank 10 and mixed using a low-speed rotating type stirring blade 12 and a side wall pit 11 with wall surface oyster blades under normal pressure.

<Process 2>
Next, the inside of the manufacturing apparatus system is depressurized.
Thereafter, a part of the content (liquid raw material) mixed in the stirring tank 10 is taken out from the outlet 14 at the bottom of the stirring tank 10 while rotating the stirring blade 12 and the side wall blade 11 with wall surface oyster blades, and is routed by the pump 39. At the same time, the low shear mixer 20 is operated.
Here, a valve is provided at a branch portion of the path 35 branched from the path 30 and the path 31 so that the material is not discharged to the path 35 side during the material circulation.
In this way, the contents are fed from the path 32 to the paths 33 and 34 through the low shear mixer 20 and returned to the stirring tank 10 for circulation.
The pressure in the stirring tank is preferably in the range of 0.001 to 0.090 MPa, more preferably 0.003 to 0.080 MPa.
At the time of introducing the powder component, it is preferable that at least one of the stirring tank 10 and the low shear mixer 20 is reduced in pressure, more preferably both are reduced in pressure, and the entire production apparatus system is reduced in pressure. Is more preferable.

<Step 3>
Next, from the raw material charging port 13 provided in the stirring tank 10 while maintaining the circulation of the raw material between the stirring tank 10 and the low shear mixer 20 due to the pressure difference with the atmosphere due to the reduced pressure in the manufacturing apparatus system. The powder component 1 is sucked into and mixed with the powder component 2 from the raw material inlet 21 provided in the low shear mixer 20 and the fragrance component from the raw material inlet 22 respectively. By doing so, a plurality of dentifrice raw materials are gradually mixed while circulating between the stirring tank 10 and the low shear mixer 20. The mixing can suppress the formation of lumps of the powder component and suppress the adhesion of dust to the inner surface of the blending tank.
In addition, if a part of the contents in the stirring tank 10 is taken out and mixed with other raw materials in the low shear mixer 20, the other raw materials are put into the contents in the stirring tank 10 with a low shearing force. Thus, the effect of the present invention can be obtained. However, mixing the contents while circulating the contents between the agitation tank 10 and the low shear mixer 20 in this way is possible. It is more preferable from the viewpoint of the effect of the invention.

The raw material mixture passed through the low-shear mixer 20 passes through the path 32 and is sent from the path 33 to the upper part (inner upper part) of the stirring tank 10 and from the path 34 to the lower part (inner bottom part) of the stirring tank 10. It is done. Mixing efficiency can be improved by dividing the upper part and the lower part into the stirring tank 10.
The mixture may be returned to the stirring tank 10 from only one of the paths 33 and 34.

  The powder component 1 may contain a part of or all of other powder components such as an abrasive and a binder; an active ingredient, a preservative, and a colorant.

Thus, the powder component 1 containing the abrasive is preferably sucked into the lower part of the stirring tank 10 (preferably from the bottom surface of the stirring tank 10). By suction-in through the bottom surface of the stirring vessel 10, adhesion of the powder component 1 (preferably abrasive) to the inside of the stirring vessel 10 and formation of lumps of the powder component 1 are suppressed. In addition, dispersibility of abrasive particles and the like is improved, and for example, disintegration when mixing disintegrating silica is suppressed.
The charging method into the stirring tank 10 at this time is not particularly limited, but it is preferable to use a mixing tank bottom nozzle provided at the raw material charging port 13 at the bottom of the mixing tank. Moreover, it can also supply using the submerged addition nozzle shown in FIG.

According to the present invention, particularly when collapsible silica is included as an abrasive, excellent effects such as being able to be stably blended without breaking or collapsing the collapsible silica are obtained.
Here, “disintegrating silica” has an average particle diameter of 0.05 to 2 mm, preferably 0.1 to 1 mm, more preferably 0.2 to 0.5 mm, and an average disintegration strength of 15 to 500 g / It means amorphous silicic acid anhydride particles, preferably 20 to 200 g / piece, more preferably 25 to 100 g / piece. The amorphous silicic acid anhydride can be obtained by a general wet method using water glass, sulfuric acid or the like.
In addition, "average disintegration strength" as used herein means that when a granule disintegrates when one granule is compressed at a speed of 10 mm / min by a Sun Rheometer CR-200D (product name, manufactured by Sun Scientific Co., Ltd.). The average value when the load is repeatedly measured 10 times.
The abrasive can be charged from either the stirring tank 10 or the low shear mixer 20, but is preferably charged into the stirring tank 10 from the viewpoint of production efficiency such as the charging speed of the powder component. Furthermore, it is more preferable to suck in from the bottom surface of the stirring tank 10.

FIG. 3 is a partial cross-sectional view showing an embodiment of an agitation tank equipped with an in-liquid addition nozzle.
The submerged addition nozzle 15 is installed along the inner wall of the stirring tank 10 so that the raw material outlet is located in the lower part of the stirring tank 10 (preferably near the bottom of the stirring tank 10). Then, when the powder component 1 containing an abrasive is sucked in from the raw material accessory tank 16 of the powder component 1, the powder component 1 can be introduced into the agitation tank 10 from its end via the submerged addition nozzle 15. it can.

The powder component 2 should just contain at least one part of the powdery raw material of a dentifrice, and it is preferable to contain a binder especially. Thereby, while suppressing the lumps formation of a powder component, the swelling of the swellable powder raw material in a short time can be promoted.
The powder component 2 may contain a part of the abrasive; a part or the whole amount of other powder components such as active ingredients, preservatives, and colorants.

The powder components 1 and 2 may be a liquid mixture previously dispersed in a liquid raw material.
A part of the powder component excluding the binder, that is, the active ingredient, the preservative, the colorant, and the abrasive may be added and mixed together with the liquid raw material in the stirring tank 10.

  Further, the fragrance component is preferably sucked into the raw material inlet 22. Thereby, a favorable flavor is obtained. In addition, it is difficult to get familiar with the raw material and the fragrance component of the dentifrice having high hydrophilicity. Therefore, it usually takes time to disperse the fragrance component in the raw material mixture, but the fragrance component is introduced from the inlet of the low-shear mixer. Since the stirring is instantaneously performed, efficient dispersion of the fragrance component is facilitated.

<Step 4>
Next, after all the raw materials other than the foaming agent have been put into the system in this way, the stirring in the stirring tank 10 and the operation of the low shear mixer 20 are performed, and the pressure is about 0.001 to 0.010 MPa. The raw material mixture is degassed under reduced pressure.

<Step 5>
Finally, the foaming agent is added from the raw material accessory tank 60 in a stationary state in which stirring is stopped. Thereafter, all the raw materials are stirred and mixed again under a reduced pressure of about 0.001 to 0.010 MPa, and this mixture is sent from the passage 30 to the discharge passage 35 and discharged out of the system for storage and filling. .
In the present invention, as described above, it is preferable to perform vacuum degassing before and after the addition of the foaming agent.

The method for producing a dentifrice of the present invention is a method in which a part of the contents in the stirring tank 10 is taken out and returned to the stirring tank 10 through the circulation path 36 as described above, and this circulation is limited to one round. Instead, it may be circulated a plurality of times. Usually, it is preferable to circulate 5 to 10 passes throughout the entire process.
In addition, it is preferable to perform operation which mixes a raw material at 50 degrees C or less, and it is more preferable to carry out at 15-30 degreeC. By setting this temperature, the addition of facilities such as heating and cooling is reduced, and the heating and cooling time can be greatly shortened.

≪ Dentifrice ≫
The dentifrice of this invention is a dentifrice manufactured by the manufacturing method of the dentifrice which is the above-mentioned this invention. The dentifrice of the present invention has good quality such as uniformity, flavor, paste skin, shape retention and stability.
In the dentifrice of the present invention, as described above, liquid raw materials such as wetting agents and water; powder components such as abrasives, binders, active ingredients, preservatives, colorants, sweeteners; An agent is used.

Examples of the wetting agent include glycerin, sorbit, propylene glycol, 1,3-butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xylit and the like. These wetting agents may be used alone or in combination of two or more. It is preferable to use 5 to 60% by mass of the wetting agent in the dentifrice.
It is preferable to use 5 to 80% by mass of water in the amount of dentifrice. In addition, you may use a part of said compounding quantity for raw material accessory preparation.
As abrasives, potassium hydrogen phosphate, anhydrous, calcium hydrogen phosphate dihydrate, tertiary calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminum hydroxide, anhydrous silicic acid, aluminum silicate, insoluble sodium metaphosphate , Tertiary magnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, zirconium silicate, polymethyl methacrylate, and other synthetic resins. Of these, calcium hydrogen phosphate dihydrate and anhydrous silicic acid are preferred. As silicic anhydride, the above collapsible silica is particularly preferable.
These abrasives may be used alone or in combination of two or more. As for the compounding quantity of the abrasive | polishing agent in a dentifrice, it is preferable to use 1-50 mass%.

Examples of binders include carrageenan, xanthan gum, sodium polyacrylate, cellulose derivatives such as sodium carboxymethylcellulose, methylcellulose, and hydroxyethylcellulose; alginic acid derivatives such as sodium alginate and propylene glycol alginate; gums such as gellan gum, tragacanth gum, and caraya gum Synthetic binders such as polyvinyl alcohol; inorganic viscosity agents such as silica gel, bee gum, laponite, montmorillonite, bentonite, kaolin, and the like.
These binders may be used alone or in combination of two or more. It is preferable to use 0.1 to 10% by mass of the binder in the dentifrice.
Furthermore, it is preferable that the binder is preliminarily mixed with other powder components from the viewpoint of swelling efficiency. Among other powder raw materials, silicic anhydride is particularly preferable. In such a case, the mixing ratio of the binder and the other powder component is preferably 1: 0.5 to 1: 4 in terms of the volume ratio of the powder component. By being in this range, the swelling efficiency is further improved.

Active ingredients include sodium monofluorophosphate, sodium fluoride, hinokitiol, cetylpyridinium chloride, benzalkonium chloride, triclosan, chlorhexidine salts, enzymes such as dextranase, amylase, protease, lysozyme, mutanase, chloride Examples thereof include sodium, ε-aminocaproic acid, tranexamic acid tocopherols, glycyrrhetinic acid, ascorbic acid and its derivatives and salts thereof, herbal medicine, potassium nitrate, buckwheat extract, chamomile, oxon and the like. These active ingredients may be used alone or in combination of two or more. As for the compounding quantity of the active ingredient in a dentifrice, 0.001-5 mass% is preferable.
Examples of the preservative include methyl p-oxybenzoate, butyl p-oxybenzoate, ethyl p-oxybenzoate, propyl p-oxybenzoate, benzoic acid, sodium benzoate and the like.
Examples of the colorant include food colors and titanium dioxide.
Examples of the sweetener include saccharin sodium, aspartame, stevioside, stevia extract, sucrose, maltose, lactose, perilartine, glycyrrhizin salts, neohesperidyl dihydrochalcone, paramethoxycinnamic aldehyde and the like. These sweeteners may be used alone or in combination of two or more. As for the compounding quantity of the sweetener in a dentifrice, 0.1-5 mass% is preferable.

  Perfume ingredients include peppermint oil, spearmint oil, anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil , Lime oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, Iris concrete, Natural perfume ingredients such as absolute peppermint, absoluteton rose and orange flower; processed perfume ingredients of these natural perfume ingredients; menthol, carvone, anethole, cineol, methyl salicylate, cinnamic aldehyde, eugenol, 2-diol, pine , Octyl aldehyde, citral, pulegone, Cal beer acetate, separately perfume ingredients, such as anisaldehyde, strawberry flavor, blended fragrance component, such as apple flavor, etc., include known perfume ingredients material used in oral compositions. These perfume ingredients may use 1 type and may use 2 or more types together. The blending amount of the fragrance component in the dentifrice is preferably 0.1 to 5% by mass.

As a foaming agent, an anionic surfactant, a nonionic surfactant, and an amphoteric surfactant can be blended.
Anionic surfactants include sodium alkyl sulfates such as sodium lauryl sulfate, sodium N-lauroyl sarcosinate, sodium N-acyl sarcosinate such as sodium N-myristoyl sarcosinate, sodium dodecylbenzenesulfonate, hydrogenated coconut fatty acid monoglyceride N-acyl glutamate such as sodium monosulfate, sodium lauryl sulfoacetate, sodium N-palmitoyl glutamate, sodium N-methyl-N-acyl taurate, sodium N-methyl-N-acylalanine, sodium α-olefin sulfonate, etc. Can be mentioned.
Nonionic surfactants include sugar fatty acid esters such as sucrose fatty acid ester, maltose fatty acid ester and lactose fatty acid ester, sugar alcohol fatty acid esters such as maltitol fatty acid ester and lactitol fatty acid ester, polyoxyethylene sorbitan monolaurate, polyoxy Polyoxyethylene sorbitan fatty acid esters such as ethylene sorbitan monostearate, polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil, fatty acid mono or diethanolamide such as lauric acid mono or diethanolamide, myristic acid mono or diethanolamide, sorbitan Fatty acid ester, polyoxyethylene higher alcohol ether, polyoxyethylene polyoxypropylene copolymer, polyoxyethylene Like polyoxypropylene fatty acid esters.
These foaming agents may be used alone or in combination of two or more. As for the compounding quantity of the foaming agent in a dentifrice, 0.1-10 mass% is preferable.

  ADVANTAGE OF THE INVENTION According to the present invention, a method for producing a dentifrice and a dentifrice having good quality, such as uniformity, flavor, kneaded skin, shape retention, stability, etc. in the dentifrice, and excellent production efficiency and cleanability of the blending equipment. And an apparatus for producing a dentifrice can be provided.

In addition, since the binder can be blended stably by mixing with a low shearing force, there is no decrease in viscosity, and there is no loss of shape retention, which is an important factor in quality. Is obtained.
Further, by mixing the powder component in the liquid raw material, dust adhesion of the powder component such as the abrasive and the binder to the inner surface of the stirring tank can be suppressed, so that the cleaning property is improved.

  Hereinafter, the present invention will be described in more detail using examples, but the present invention is not limited to these examples. Further, “parts” and “%” in the examples are solid contents excluding water unless otherwise specified, and indicate mass parts and mass%, respectively.

Example 1
The dentifrice of the composition 1 which consists of the raw material listed below was manufactured using the manufacturing apparatus shown in FIG. 1, FIG.
A vibro mixer (manufactured by Chilling Industries Co., Ltd.) was used as the low shear type high dispersion machine 20 added to the external circulation path 36, and a sine pump (manufactured by Tokushu Kika Kogyo Co., Ltd.) was used as the pump 39 for external circulation. .
First, after the liquid raw material was mixed in the stirring tank 10 at normal pressure, the inside of the system was reduced to 0.070 MPa, external circulation was performed by the pump 39, and the vibromixer was operated at 1 m / s.
The above speed represents the maximum speed of the vibrating stirring blade 23, and the frequency and amplitude at that time were set to 26 s ⁻¹ and 6 mm, respectively.
Powder component 1 containing a silica abrasive from a raw material inlet 13 provided at the bottom of the stirring tank 10, powder component 2 from a raw material inlet 21 of the first stage of a Vibro mixer (of the previous 10 stages), a fragrance The components were charged from the raw material inlet 22 at the fifth stage.
Thereafter, defoaming was performed under a reduced pressure of 0.004 MPa, and finally, the foaming agent was added in a stationary state from the raw material tank 60 at the top of the stirring tank 10 arranged as shown in FIG. To prepare a dentifrice.
The dentifrice was produced by setting other production conditions to the following conditions.
Compounding scale: 200 kg.
Linear velocity at the tips of the stirring blade 12 and the side wall honey 11 with a wall oyster blade: 2 m / s.
Mixing time after adding liquid ingredients: 10 minutes.
Addition time of powder component 1, powder component 2, and perfume component: 15 minutes.
Defoaming time under reduced pressure: 10 minutes.
Defoaming (mixing) time after adding blowing agent: 10 minutes.

≪ Dentifrice composition 1≫
The compositional component amounts (in%) of the following raw materials indicate the content in the dentifrice formulation.
<Liquid raw material>
70% sorbite aqueous solution (wetting agent, trade name “70% sorbite solution”, manufactured by Towa Kasei Kogyo) 35.00%, ion-exchanged water 27.94%.
<Powder component 1>
Sodium fluoride (active ingredient, trade name “Fucca Soda”, manufactured by Stella Chemifa) 0.21%, saccharin sodium (sweetener, trade name “Saccharin sodium”, manufactured by Daiwa Kasei) 0.15%, silica abrasive (abrasive, product) Name “Amorphous Silicic Anhydride”, manufactured by Taki Chemical Co., Ltd. 18.00%, sodium lauryl sulfate (foaming agent, trade name “NIKKOL SLS”, manufactured by Nikko Chemicals) 0.90%, collapsible silica (characterizing agent) Silicic anhydride; trade name “SOLBOSIL”, manufactured by Crossfield) 1.50%.
<Powder component 2>
Thickening silica (thickener, trade name “White Carbon T”, manufactured by Tokuyama) 4.00%, xanthan gum (binder, trade name “Monartum gum DA”, manufactured by Kelco) 0.50%, sodium polyacrylate ( Binder, trade name “Leogic 250H” manufactured by Nippon Pure Chemical Co., Ltd.) 0.80%.
<Foaming agent>
Sodium lauroyl sarcosinate (foaming agent, trade name “Soipon SLP”, manufactured by Kawaken Fine Chemicals) 0.90%.
<Perfume ingredients>
Fragrance component mixture (fragrance A described in Table 4 of JP-A-2005-247786) 1.00%.

(Example 2)
In Example 1, the powder component 1 was charged using the submerged addition nozzle 15 (FIG. 3) extended to the vicinity of the lower part of the stirring tank 10, under the same production conditions as in Example 1. A dentifrice was produced.

(Comparative Example 1)
In Example 1, the mixer 20 provided in the middle of the external circulation path 36 is a high-shear disperser (TK homomic line flow, special machine industry, Ltd.) with a peripheral speed (linear velocity at the tip of the stirring blade) of 10 m / s. A dentifrice was produced under the same production conditions as in Example 1 except that the mixture was changed to).

(Example 3)
The dentifrice of the composition 2 which consists of the raw material listed below was manufactured using the manufacturing apparatus shown in FIG. 1, FIG. However, a stirring tank having a volume of 20 L was used.
A vibro mixer (manufactured by Chilling Industries Co., Ltd.) was used as the low shear type high dispersion machine 20 added to the external circulation path 36, and a sine pump (manufactured by Tokushu Kika Kogyo Co., Ltd.) was used as the pump 39 for external circulation. . In addition, it mix | blended so that the compounding quantity (mixing scale) of all the raw materials might be set to 20 kg in total.
First, a 70% sorbite aqueous solution, ion-exchanged water, sodium monofluorophosphate, and sodium saccharin are added to the stirring tank 10, and the linear velocity at the tip of the stirring blade 12 and the wall-shaped oyster blade-attached blade 11 is 3 m / at normal pressure. After mixing for 3 minutes at a rotational speed of s, the system is depressurized to 0.020 MPa, external circulation is performed by the pump 39 at 10 L / m, and the vibrator mixer is operated with a vibration frequency of 20 s ⁻¹ , an amplitude of 3 mm, a vibration type The stirring blade 23 was operated at a maximum speed of 0.4 m / s.
While maintaining the system at a reduced pressure of 0.020 MPa and continuously stirring the inside of the stirring tank 10, thickening silica (thickening agent), sodium carboxymethylcellulose (viscosity) from the raw material inlet 13 provided at the bottom of the stirring tank 10. The binder was added in 2 minutes.
After completion of the charging, the system is maintained at a reduced pressure of 0.020 MPa, and while stirring the stirring tank 10 continuously, calcium hydrogen diphosphate and collapsible silica are charged from the raw material charging port 13 and at the same time the perfume component is vibrated. The material was introduced from the raw material inlet 22 at the fifth stage of the mixer. All the raw materials were charged in 3 minutes.
Thereafter, defoaming was performed for 6 minutes under a reduced pressure of 0.004 MPa, and finally sodium lauryl sulfate was added in a stationary state from the raw material tank 60 at the top of the stirring tank 10 arranged as shown in FIG. Under reduced pressure for 6 minutes to produce a dentifrice.
The operation of the stirring tank 10 and the vibro mixer was continued from the start time to the end of all steps.

≪ Dentifrice composition 2≫
The compositional component amounts (in%) of the following raw materials indicate the content in the dentifrice formulation.
70% sorbite aqueous solution (wetting agent, trade name “70% sorbite solution”, manufactured by Towa Kasei Kogyo) 35.00%.
Ion exchange water 17.85%.
Sodium monofluorophosphate (active ingredient, trade name “SODIUM MONOFLUOROPHOSPHATE DENIFRICE GRADE, POWDER”, manufactured by Rhodia) 0.50%.
Saccharin sodium (sweetener, trade name “Saccharin Sodium”, manufactured by Daiwa Kasei) 0.15%.
Thickening silica (Thickener, trade name “White Carbon T”, manufactured by Tokuyama) 1.50%,
Sodium carboxymethylcellulose (binding agent, trade name “CMC-1220”, manufactured by Daicel Chemical Industries) 1.20%.
Calcium hydrogen diphosphate (abrasive, trade name “calcium hydrogen phosphate dihydrate for dentifrice”, manufactured by Tosoh Finechem Co., Ltd.) 40.00%.
Disintegrating silica (characterizing agent, silicic anhydride; trade name “SOLBOSIL”, manufactured by Crossfield) 1.50%.
Fragrance component mixture (fragrance A described in Table 4 of JP-A-2005-247786) 1.00%.
Sodium lauryl sulfate (foaming agent, trade name “NIKKOL SLS”, manufactured by Nikko Chemicals) 1.30%.

(Comparative Example 2)
In Example 3, the mixer 20 provided in the middle of the external circulation path 36 is a high shear type disperser (TK homomic line flow, manufactured by Tokushu Kika Kogyo Co., Ltd.) having a linear velocity at the tip of the stirring blade of 7 m / s. A dentifrice was produced under the same production conditions as in Example 3 except that the mixture was mixed.
In addition, the fragrance | flavor component was also thrown in from the inlet provided in the middle of the external circulation path 36 similarly to Example 3. FIG.

(Comparative Example 3)
In Example 3, a dentifrice was produced under the same production conditions as in Example 3 except that all the raw materials including the fragrance were charged into the stirring tank 10.
In addition, the fragrance | flavor component was supplied from the raw material accessory tank 60 of the stirring tank 10 arrange | positioned as shown in FIG.

<Quality and manufacturability evaluation 1>
The quality, flavor, shape retention, stability, kneaded skin, and disintegration of silica particles were evaluated by the following evaluation methods.
For manufacturability, dust adhesion to the inner surface of the mixing tank (visual observation) and the mixing time were evaluated.
The results of quality and manufacturability evaluation are shown in Table 1.

[Flavor]
The sensory evaluation (4 expert panelists) evaluated.
○: It has a good flavor as a dentifrice and is excellent in use feeling.
X: Flavor balance is lost as a dentifrice, and there is a problem in merchantability.

[Shape retention]
The following criteria evaluated the shape change when the dentifrice discharged | emitted from the tube which is a concrete method at the time of using as a product was put on a toothbrush.
○: The cross-section of the dentifrice maintains a circular shape to an elliptical shape, and no kneading flows between the flocked portions.
X: The cross-section of dentifrice collapses rather than an ellipse, and kneading flows between flocked parts.

[Stability]
The dentifrice was filled in the tube and stored at 5 ° C., 25 ° C., 40 ° C., and 50 ° C., and the stability after one month was evaluated according to the following criteria.
○: Moisture does not ooze out when kneaded from the tube onto the straw half paper.
X: Moisture exudes when kneading from the tube onto the straw half paper.

[Kneaded skin]
After filling the dentifrice into the tube, the surface state of the kneaded on the straw half paper was visually observed and evaluated according to the following criteria.
○: The texture of the surface is fine.
X: The texture of the kneaded surface is rough and lumps or the like are confirmed.

[Disintegration of silica particles]
After the preparation of the dentifrice is diluted with 5 times the amount of ion-exchanged water, it is disintegrated after preparation with a particle size distribution meter (Laser diffraction / scattering type particle size distribution analyzer LA-920, manufactured by Horiba, Ltd.). The volume average particle diameter of the silica particles was measured and evaluated according to the following criteria.
<Definition of comparison value with bulk average particle size>
Comparison value (%) with volume average particle size base material = y / x × 100
x: average particle diameter of the disintegrating silica base material, y: average particle diameter of the disintegrating silica in the kneaded mixture after preparation.
○: The comparison value of the volume average particle diameter is 90% or more compared with the original material.
(Triangle | delta): The comparison value of a volume average particle diameter is 70% or more and less than 90% compared with a raw material.
X: The comparison value of a volume average particle diameter is less than 70% compared with a raw material.

<Quality and manufacturability evaluation 2>
For Example 3 and Comparative Examples 2-3, the quality of the dentifrice (flavor, shape retention, stability, paste skin, disintegration of silica particles) was evaluated by the same evaluation method as the above evaluation method. .
In addition, regarding the manufacturability, after the fragrance component is introduced from the raw material inlet 22 in the fifth stage of the vibro mixer, the time until all of the fragrance component is caught in the liquid from the liquid surface of the raw material mixture (visual observation, hereinafter referred to as “fragrance”). The time when the components are familiar ”is indicated), and the blending time is evaluated.
The results of quality and manufacturability evaluation are shown in Table 2.

As is clear from the results in Tables 1 and 2, the production method of the present invention and Examples 1, 2 and 3 using the production apparatus are good in quality items, and the productivity is also good. It was excellent.
On the other hand, Comparative Example 1 and Comparative Example 2 using a high shearing type disperser were inferior in flavor, shape retention, and disintegration quality of silica particles.
Moreover, in the manufacture of the dentifrice of composition 2, in Comparative Example 3 in which all the raw materials were put into the stirring tank, the time for blending the fragrance component and the blending time were longer than those in Example 3 and Comparative Example 2, resulting in high productivity. It was inferior.
From the above, according to the present invention, the method for producing a dentifrice that has good uniformity, flavor, paste skin, shape retention, stability, etc. in the dentifrice, and excellent in production efficiency and cleanability of the blending equipment, and It was confirmed that a dentifrice and an apparatus for producing a dentifrice can be provided.

It is a partial sectional side view which shows one Embodiment of the manufacturing apparatus of the dentifrice of this invention. It is a partial side sectional view showing an example of an embodiment of a low shear type mixer used in the present invention. It is a partial sectional side view which shows one embodiment of the stirring tank provided with the submerged addition nozzle.

Explanation of symbols

10 Mixing tank
11 Side wall with wall oyster wing
11a Honey
11b wing
11cU-shaped shaft
12 Stirring blade
13 Raw material inlet
14 Discharge port
15 Nozzle for addition in liquid
16 Raw material tank
17 Rotating shaft
20 Low shear mixer
21 Raw material inlet
22 Raw material inlet
23 Stirring blade
23a pore
24 Stirring shaft
25 mixing units
25a separator
30 routes
31 routes
32 routes
33 routes
34 routes
35 discharge channel
36 Circuit
39 Pump
40 Raw material tank
49 Pump
50 Raw material tank
60 Raw material tank

Claims (7)

A method for producing a dentifrice by mixing dentifrice ingredients,
A stirring tank having a rotary stirring blade;
A circuit for taking out the contents in the stirring tank and returning the taken-out contents back into the stirring tank;
An in-line type mixer having a vibration type stirring blade provided in the middle of the circulation path and having a maximum speed represented by the following formula of 0.1 to 1.2 m / s,
The raw material is charged into the stirring tank, a part of the contents in the stirring tank is taken out, the taken-out contents are mixed with the fragrance charged into the mixer using the mixer, and the mixture is mixed with the mixture. A method for producing a dentifrice, characterized in that the dentifrice is produced by mixing the raw materials of the dentifrice by returning to the stirring tank.
Maximum speed of stirring blade (m / s) = 2πfa
f: vibration frequency (s ⁻¹ ), a: amplitude of stirring blade (m) In the manufacturing method of the dentifrice of Claim 1,
A part or all of a liquid raw material containing water and / or a wetting agent is charged into the stirring tank,
A method for producing a dentifrice, wherein at least one selected from an abrasive, a binder, a foaming agent, water and a wetting agent is charged into the agitation tank and / or into the mixer.   3. The method for producing a dentifrice according to claim 2, wherein the abrasive contains disintegrating silica, and the abrasive is introduced into the stirring tank. In the manufacturing method of the dentifrice of Claim 2 or 3,
A method for producing a dentifrice, wherein the binder and another powder component are premixed at a volume ratio of the powder component (binder: other powder component) at 1: 0.5 to 1: 4. The method for producing a dentifrice according to any one of claims 1 to 4, wherein the rotary stirring blade tip has a linear velocity represented by the following formula of 1 to 5 m / s. .
Linear velocity (m / s) = πND / 60
N: number of revolutions (rpm), D: stirring blade diameter (m) In the manufacturing method of the dentifrice as described in any one of Claims 1-5,
A method for producing a dentifrice, wherein the vibration frequency of the vibration type stirring blade is 5 to 30 s ⁻¹ and the amplitude of the vibration type stirring blade is 2 to 6 mm. A stirring tank having a rotary stirring blade;
A circuit for taking out the contents in the stirring tank and returning the taken-out contents back into the stirring tank;
A dentifrice comprising an in-line mixer having a vibrating stirring blade provided in the middle of the circulation path and having a maximum speed of 0.1 to 1.2 m / s represented by the following formula: Agent manufacturing equipment.
Maximum speed of stirring blade (m / s) = 2πfa
f: vibration frequency (s ⁻¹ ), a: amplitude of stirring blade (m)

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