JP2008088145A - Method for producing toothpaste - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for effectively producing toothpaste with a reduced amount of bubbles, excellent in uniformity of components, shape-retaining property and gloss of skin, and excellent in flavor in an easy process in a short time. <P>SOLUTION: The invention relates to the method for producing toothpaste comprising: charging organic binder powder into a hopper of a high shearing type inline wet mixing and dispersing equipment (A) provided with a high shearing type mixer part provided with a stator with a comb-shaped ring wall and a rotor with a spiral blade and a comb-shaped ring wall, a hopper part supplying the organic binder powder and a liquid introducing part supplying water or aqueous solution of the moistening agent; continuously supplying the organic binder and water or the aqueous solution of the moistening agent into the mixer to prepare a dispersion of the organic binder in which the organic binder is dispersed in the water or the aqueous solution of the moistening agent; supplying the dispersion to a low shearing type vacuum mixing equipment (B) to obtain the swollen and dissolved liquid of the organic binder; and mixing the remaining materials such as a polishing agent, a perfume, or the like under reduced pressure by using the equipment (B). <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention can efficiently produce toothpastes with less air bubbles, excellent uniformity of components such as organic binders, excellent shape retention and skin gloss, and excellent aroma. The present invention relates to a method for producing toothpaste.

  In the manufacturing method of dentifrice, when it manufactures with the equipment with excessive shear force, a fragrance | flavor and an abrasive | polishing agent are atomized, the fragrance | flavor adsorb | sucked to an abrasive | polishing agent increases, and the smell of a flavor worsens. In addition, cutting of the organic binder occurs, and the shape retention of the toothpaste is deteriorated.

  On the contrary, if it manufactures with the installation whose shear force is too weak, swelling mixing of the organic binder becomes insufficient, and it becomes easy to generate lumps. In order to solve this problem, it is recommended that the swelling mixing of the organic binder is made with a mixing tank equipped with paddle blades, and the mixing of the fragrance and the abrasive is made with a low shear kneader (Patent Document 1; No. 171743). However, this method has a problem that switching washing performance is poor because a step of transferring the swelling aqueous solution to a kneader is included, and the swelling mixture of the binder has a high water activity and thus has a low preservative power.

  Therefore, development of an industrially advantageous method of producing toothpaste that can obtain a toothpaste that is free from the above-described problems, has less air bubbles, is fragrant, and has excellent component uniformity is desired.

Japanese Patent Laid-Open No. 11-171743 US Pat. No. 4,511,256 U.S. Pat. No. 4,729,663 Quadro homepage http: // www. quadro. com / A_resource / 5_caseStudies / 2_ytron / costetics / APYC05_ToothpasteManufacturing. asp

  The present invention has been made in view of the above circumstances, and it is a simple process for toothpaste with few bubbles mixed in, excellent uniformity of ingredients, good shape retention and good skin gloss, and excellent fragrance. An object of the present invention is to provide a method for producing a toothpaste that can be produced efficiently in a short time.

As a result of intensive studies to achieve the above-mentioned object, the present inventor has a high-shear mixer just below the inlet of the organic binder powder, and the powder raw material flowing in from above is the mixer part. A high-shear in-line wet mixing and dispersing device and a low-shear type vacuum mixing device that can wet and disperse the powder at the same time as mixing with the liquid raw material flowing in from the liquid inlet of the same line. When using, that is, producing toothpastes containing abrasives, organic binders, wetting agents, water, fragrances,
(A) A high-shear mixer unit including a stator having a comb-shaped ring wall, spiral blades, and a rotor having a comb-shaped ring wall on the outside thereof, and a powder raw material component are supplied to the mixer unit. A device using the high shear type in-line type wet mixing / dispersing device and the (B) low shear type vacuum mixer equipped with a hopper and a liquid introducing unit for supplying liquid raw material components to the mixer unit. An organic binder powder is introduced into a hopper for supplying the powder raw material, water or a wetting agent aqueous solution is introduced from a liquid introduction unit, and the organic binder powder supplied from the hopper is the liquid. Water or wet so that the average residence time until it comes into contact with the water flowing in from the introduction part or the aqueous wetting agent solution and discharged from the high shear mixer part of the wet mixing and dispersing apparatus is 0.05 to 0.50 seconds. The flow rate of the aqueous solution Then, the organic binder and the water or the wetting agent aqueous solution are continuously supplied into the mixer unit to prepare an organic binder dispersion liquid in which the organic binder is dispersed in the water or the wetting agent aqueous solution. The organic binder dispersion is supplied to a low-shear vacuum mixing device (B) to obtain a swelling solution of the organic binder, and the swelling solution is further reduced under reduced pressure using the device (B). By mixing the remaining powder raw material component containing the abrasive and the remaining liquid raw material component containing the fragrance, there is almost no mixing of bubbles, components such as the organic binder are uniformly dispersed, and the shape retention and It is possible to efficiently produce a toothpaste with excellent condensed skin (skin gloss) and good flavor quality, and according to this production method, for example, there is no need to disperse the binder into water or a wetting agent aqueous solution. It is advantageous for switching cleaning, industrially advantageous and high quality with a simple process. It was found to be capable of producing toothpaste.

  A high shear type in-line wet mixing / dispersing device is proposed in Patent Documents 2 and 3 (US Pat. No. 4,511,256, US Pat. No. 4,729,663). A method of manufacturing a toothpaste using an apparatus has been proposed. In the present invention, a high-quality toothpaste can be easily and easily reduced by performing a specific process using the above apparatuses (A) and (B) on the same line. It has been found that it can be manufactured in time, and this is a new finding of the present inventors.

According to the production method of the present invention,
(1) Since the organic binder is swollen and dispersed with a high shear mixer, the product becomes a uniform swelling liquid without any powder (fish eyes). Moreover, since the number of passes through the high-shear mixer is one, there is no decrease in viscosity due to unnecessary shearing, the shape retention of the final product is good, and the skin texture (skin gloss) is also excellent.
(2) Since the abrasive and the fragrance are mixed with other components in a low shear vacuum mixer, a toothpaste with good flavor quality can be produced without being atomized.
(3) By arranging both equipments (A) and (B) in series, an intermediate product tank is not required, and switching cleaning can be easily performed. Moreover, since it discharges | emits after a liquid contact for a short residence time, there is no piping clogging.
There are advantages such as.

Therefore, the present invention
Claim 1;
A method for producing a toothpaste containing an abrasive, an organic binder, a wetting agent, water, and a fragrance, comprising a stator having comb-shaped ring walls, spiral blades, and a comb-shaped ring wall on the outside thereof High shear type comprising a high shear type mixer unit provided with a rotor, a hopper for supplying organic binder powder to the mixer unit, and a liquid introduction unit for supplying water or a wetting agent aqueous solution to the mixer unit The water or wetting agent in which the organic binder powder is fed into the hopper of the in-line type wet mixing and dispersing apparatus (A), and the organic binder powder supplied from the hopper flows in from the liquid introduction part Adjust the inflow rate of water or the wetting agent aqueous solution so that the average residence time until it comes into contact with the aqueous solution and is discharged from the high-shear mixer of the wet mixing and dispersing device is 0.05 to 0.50 seconds. , Organic binder and water or wet An aqueous binder is continuously fed into the mixer section to prepare an organic binder dispersion in which the organic binder is dispersed in the water or the wetting agent aqueous solution, and then the organic binder dispersion is a low shear type. After being supplied to the vacuum mixing device (B) to obtain a swelling solution of the organic binder, the remaining powder raw material components and flavors containing the abrasive in the swelling solution under reduced pressure using the device (B) A method for producing a toothpaste comprising mixing the remaining liquid raw material components including
Claim 2;
A high shear type in-line type wet mixing and dispersing apparatus (A) has a powder supply hopper and a liquid introduction unit, and a mixer unit in which powder and liquid are supplied and mixed from the hopper and the liquid introduction unit, respectively. In addition, a plurality of spiral blades are attached, a ring wall formed by a large number of comb teeth along the circumferential direction on the outside thereof, and a rotor having a rotating shaft, and a large number along the circumferential direction. And a stator having a ring wall formed of comb teeth, and the powder and liquid supplied from the hopper and the liquid introduction unit are agitated and mixed by blades rotating integrally with the rotation shaft of the rotor. The manufacturing method according to claim 1, wherein the mixture is sheared when passing through a gap between comb teeth of the rotor and the stator and discharged from an outlet provided in the device (A).
Claim 3;
The rotor is provided with an inner ring wall formed of a large number of comb teeth on the outside of the spiral blade, and a ring-shaped gap is formed between the inner ring wall and the inner ring wall. The manufacturing method according to claim 2, wherein an outer ring wall formed of a plurality of comb teeth is provided, and the stator is disposed so as to insert the ring wall into the ring-shaped gap. Method.
Claim 4;
The manufacturing method according to any one of claims 1 to 3, wherein the gaps between the comb teeth of the rotor and the stator are 0.5 to 5 mm, respectively.
Claim 5;
The liquid introduction part of an apparatus (A) is equipped with the pump as an installation which supplies a liquid, and adjusted the inflow speed of the liquid by adjusting the flow volume of this pump, The any one of Claims 1-4 Manufacturing method.
Claim 6;
The manufacturing method according to claim 1, wherein the apparatus (B) is a batch type kneader of a sigma type blade.

  According to the method for producing a toothpaste of the present invention, a toothpaste with less air bubbles, excellent uniformity of ingredients, excellent shape retention and skin gloss, and excellent fragrance can be efficiently produced in a short time. Can be manufactured well.

Hereinafter, the present invention will be described in more detail. The present invention is a method for producing a toothpaste containing an abrasive, an organic binder, a wetting agent, water, and a fragrance,
(A) A high shear mixer unit including a cylindrical stator having a comb-like gap in the circumferential direction, a spiral blade and a cylindrical rotor having a comb-like gap on the outside thereof, Using a high shear type in-line wet mixing / dispersing device having a hopper for supplying powder raw material components to the mixer unit and a liquid introducing unit for supplying liquid raw material components, and (B) a low shear type vacuum mixer The organic binder powder is supplied from the hopper after the organic binder powder is put into the hopper that supplies the powder provided in the apparatus (A), the water or the wetting agent aqueous solution is put from the liquid introduction part. So that the average residence time is 0.05 to 0.50 seconds until it comes into contact with the water flowing in from the liquid introduction part or the aqueous wetting agent and is discharged from the high shear mixer part of the wet mixing and dispersing apparatus. Adjust the inflow rate of water or aqueous wetting agent The organic binder and water or a wetting agent aqueous solution are continuously fed into the mixer section to prepare an organic binder dispersion in which the organic binder is dispersed in the water or the wetting agent aqueous solution. The binder dispersion is supplied to a low shear type vacuum mixing device (B) to obtain a swelling solution of the organic binder, and then the polishing solution is further applied to the swelling solution under reduced pressure using the device (B). The remaining powder raw material component containing scent and the remaining liquid raw material component containing fragrance are mixed.

(1) High shear type in-line type wet mixing and dispersing device The high shear type in-line type wet mixing and dispersing device used in the present invention includes a high shear type mixer having a stator and a rotor, and a powder raw material component in the mixer. A hopper for supplying liquid, a liquid raw material introduction part for supplying liquid raw material components, and preferably a pump as equipment for adjusting the supply time of the raw material components.

  In the high shear type in-line type wet mixing and dispersing apparatus, a liquid raw material component inlet, a powder raw material component supply port, and a discharge port are provided, and a hopper for supplying the powder raw material component is provided in the supply port. A liquid introduction part and a liquid flow path for supplying a liquid raw material component are installed at the component inlet, and the liquid raw material component and the powder raw material component are respectively provided with a rotor and a stator from the inlet and the supply port. A continuous type in which the dispersion liquid mixed under high shear is discharged from the discharge port by being charged into the (high shear type mixer section), contacting in the mixing section, and passing through the gap between the rotor and the stator. It is a mixing device.

  More specifically, the high shear type in-line type wet mixing and dispersing apparatus (A) has a powder supply hopper and a liquid introduction part, and the powder and liquid are respectively supplied from these hopper and liquid introduction part. A rotor having a plurality of spiral blades attached to a mixer unit to be supplied and mixed, a ring wall formed by a large number of comb teeth along the circumferential direction on the outside thereof, and a rotating shaft And a stator having a ring wall formed of a large number of comb teeth along the circumferential direction, and the powder supplied from the hopper and the liquid flowing in from the liquid introduction part are integrated with the rotating shaft of the rotor The mixture is agitated and mixed by rotating blades, and the mixture is sheared when passing through the gap between the rotor and the stator and is discharged from an outlet provided in the device (A). thing In this case, the rotor is provided with an inner ring wall formed of a large number of comb teeth on the outside of the spiral blade, and the inner ring wall is connected to the inner ring wall on the outer side of the inner ring wall. An outer ring wall formed of a large number of comb teeth is provided so as to form a ring-shaped gap between them, and the stator is arranged so that the ring wall is inserted into the ring-shaped gap. In addition, the liquid introduction part is provided with a pump such as a centrifugal pump as equipment for supplying the liquid, and the flow rate of the pump is adjusted to adjust the flow rate of the liquid. It is preferable.

Examples of such an apparatus (A) include a high shear type in-line type wet mixing and dispersing apparatus shown in FIGS.
That is, the apparatus 1 includes a powder supply hopper 2 and a liquid introduction unit 3. A liquid flow path 4 is connected to the liquid introducing portion 3, and a pump 5 is interposed in the flow path, and the supply rate of the liquid flowing through the flow path 4 is adjusted by adjusting the flow rate of the pump 5. Is done. In addition, 6 is a liquid inflow port of the mixer part 10 mentioned later, 7 and 8 are open / close valves, respectively.
A mixer unit 10 includes a rotor 11 and a stator 21. In this case, the rotor 11 has a rotating shaft 12 at the center, and a plurality of spiral blades 13 are attached to the rotating shaft 12. In addition, a circular inner ring wall 15a formed by a large number of comb teeth 14a is provided along the circumferential direction outside the tip of the blade 13, and the inner ring wall 15a is provided outside the inner ring wall 15a. A circular outer ring wall 15b formed of a large number of comb teeth 14b is provided along the circumferential direction so that a circular ring-shaped gap 16 is formed between the rotary shaft 12 and the outer ring wall 15a. The blades 13 and the circular ring walls 15a and 15b rotate integrally with the rotation of. On the other hand, the stator 21 has a diameter that matches the diameter of the ring-shaped gap formed by a large number of comb teeth 24 along the circumferential direction through the intermediate inclined ring wall 23 at the lower peripheral edge of the large-diameter circular ring-shaped substrate 22. A small-diameter circular ring wall 25 having a ring shape is integrally provided, and the ring wall 25 of the stator 21 is disposed so as to be inserted into the ring-shaped gap 16 of the rotor 11.
The powder introduced from the hopper 2 to the mixer unit 10 (on the blade 13) and the liquid introduced from the liquid introduction unit 3 through the liquid inlet 6 into the mixer unit 10 (on the blade 13) are: When the spiral blade 13 that rotates integrally with the rotation of the rotary shaft 12 of the rotor 11 is stirred and mixed to flow toward the inner ring wall 15a and passes through the gaps between the comb teeth 14a, 24, and 14b. And is discharged through the discharge port 26.

The high shear type in-line type wet mixing and dispersing device is a high shear type, and the mixing condition of the mixer (linear velocity at the tip of the circular outer ring wall 15b) is in the range of 15 to 50 m / s, particularly 25 to 40 m / s. It is preferable that If it is less than 15 m / s, the shearing is insufficient and the organic binder is easily damaged, and if it exceeds 50 m / s, the shear is too strong, and the organic binder is cut and the viscosity is likely to decrease. The linear velocity can be calculated by the following method.
Linear velocity (m / s) =
Circumference ratio x number of rotations of rotating shaft (rpm) x diameter of circular outer ring wall tip (m) ÷ 60
Moreover, the rotation speed of the mixer rotating shaft calculated | required from a linear velocity is calculated | required by a following formula.
Number of rotations of rotating shaft (rpm) =
60 ÷ Circumference x Linear velocity (m / s) ÷ Diameter of circular outer ring wall tip (m)
For example, when the mixing condition of a mixer having a circular outer ring wall tip diameter of 0.095 m is indicated by the rotational speed of the rotary shaft, a range of 3,017 to 10,057 rpm, particularly 5,028 to 8,046 rpm is preferable. Become.

  Further, in the high shear type in-line type wet mixing and dispersing apparatus, the gap between the comb-like gaps of the rotor and the stator in the mixer is preferably 0.5 to 5 mm, particularly preferably 1.5 to 3.0 mm. . When the gap interval is narrower than 0.5 mm, shearing of the organic binder becomes strong, resulting in a decrease in viscosity, which may deteriorate the shape retention. If the gap interval is wider than 5 mm, the shearing of the organic binder is weakened, the organic binder is insufficiently dispersed, and there is a case where the shape retention and the skin are deteriorated.

  In the present invention, the paste skin is an evaluation of the gloss of the skin of the dentifrice. Specifically, the dentifrice is put on a straw half paper, and the dentifrice is sandwiched by folding the straw half paper. When the skin gloss on the surface of the dentifrice when it is opened is visually evaluated, a skin with no gloss on the surface of the dentifrice and having a good gloss is evaluated as having good skin. The dentifrice of this dentifrice leads to the ease of spreading of the dentifrice in the mouth.

Specifically, the following apparatus can be used as such a high shear type in-line type wet mixing and dispersing apparatus.
In-line type wet mixing and dispersing equipment Quadroightron XC type, ZC type [Pauleck Co., Ltd.] Quadro Becomix DUO-homogenizer [Berentz]

  As the high shear type in-line type wet mixing and dispersing apparatus used in the present invention, a Ytron ZC type mixer (US Patent No. 4, 511, 256, No. 4, 729, manufactured by Quadro, Canada) is used. 663) is preferably used. Since this machine can instantaneously wet and disperse the organic binder powder with the inflowing liquid, it can be discharged as a uniform swelling liquid without clogging in the piping and without fish eyes.

  In the present invention, when only a low shear type vacuum mixer is used in place of the high shear type in-line type wet mixing and dispersing device, the organic binder can be lumped, the shape retention of toothpaste, the mixed skin When using a high-shear type off-line wet mixing device, the cleaning performance is poor because of off-line, and only a high-shear type one pot is used, and a low-shear type vacuum mixer is not used. In this case, the fragrance of the flavor deteriorates due to the atomization of the abrasive and the fragrance, and in addition, the shape retention is deteriorated due to excessive shearing, and none of the objects of the present invention can be achieved.

(2) Low-shear type vacuum mixer As the low-shear type vacuum mixer of the device (B), generally used mixers such as anchor type, spiral type and satellite motion (spinning revolution) type are also available. A batch kneader is preferred although it can be used. The mixing condition of the batch kneader is preferably 10 to 50 rpm, particularly 15 to 40 rpm. If it is less than 10 rpm, satisfactory mixing may not be possible, and if it exceeds 50 rpm, there is a problem that air bubbles are mixed in a lot.

  For the batch kneader, blades such as sigma type, zed type, masticator type, spiral type and fishtail type are used (see page 109 for kneading equipment; author: Kenji Hashimoto, published by Science and Technology Research Institute). In particular, a batch type kneader of a sigma type blade is suitable. In other blades (such as a jet type and a masticator type), the overall mixing may be poor, and the flavor quality may deteriorate.

  In the production method of the present invention, first, as the first step, it is preferably placed in a powder supply hopper provided in the apparatus (A) under a temperature condition of 0 ° C. to 60 ° C., more preferably 10 ° C. to 50 ° C. An organic binder is added, water or a wetting agent aqueous solution is added to the liquid introduction part, and the organic binder powder supplied from the powder supply hopper is supplied from the liquid introduction part and is supplied from the liquid raw material inlet. The inflow rate of the wetting agent aqueous solution so that the average residence time until it comes into contact with the inflowing water or the wetting agent aqueous solution and is discharged from the high shear mixer part of the wet mixing and dispersing apparatus is 0.05 to 0.50 seconds. And an organic binder and water or a wetting agent aqueous solution are continuously supplied into the mixer section to prepare an organic binder dispersion in which the organic binder is dispersed in the water or the wetting agent aqueous solution.

  Here, the average residence time refers to the high shear type in-line type wet mixing / dispersing device from the time when the organic binder powder as the powder raw material comes into contact with the water or the wetting agent aqueous solution flowing from the liquid introduction part. It is the average value of the time (residence time) until it is discharged from the high shear mixer part, particularly the lower rotor, and can be calculated by the following method.

Residence time calculation method Residence time = (rotor + stator) capacity / flow rate per unit time Specifically, the rotor + stator capacity of the Quadro Ytron ZC1 type machine used in the examples described later is 171 ml (radius 40 mm, The height is 34 mm), which is a fixed value. Since the flow rate per unit time can be adjusted with a pump, the residence time can be adjusted by adjusting the flow rate, for example, as follows.
Residence time (seconds): 0.01 0.05 0.15 0.50 1.00
Flow rate (ml / s): 17,100 3,420 1,140 342 171
The standard product of the Quadro Ytron ZC1 machine has a sorbite discharge pump capacity of 1,220 ml / second and a water discharge pump capacity of 2,000 ml / second.

  In the present invention, the average residence time until the organic binder powder supplied from the hopper comes into contact with water or the wetting agent aqueous solution and is discharged from the high shear mixer part of the wet mixing and dispersing apparatus is 0.05 to The flow rate of the wetting agent aqueous solution is adjusted to 0.50 seconds, preferably 0.07 to 0.30 seconds, but if it is shorter than 0.05 seconds, the contact time between the powder and the liquid is too short, Since the body is processed by a mixer before it gets wet with the liquid, uniform swelling and dispersion cannot be performed. On the other hand, if it is longer than 0.50 seconds, the organic binder swells before passing through the mixer, and clogs at the rotor outlet.

  The mass of the water or the wetting agent aqueous solution necessary for dispersing and mixing the organic binder powder with a high shear mixer is preferably 5 times or more, particularly 10 times or more, the mass of the organic binder powder. When the amount is less than 5 times, the high-concentration organic binder powder is swelled and dispersed, and the rotor rotation speed of the high shear mixer is increased more than necessary. There is. The supply amount of the water or the wetting agent aqueous solution can be adjusted by the pump provided as the equipment for supplying the liquid as described above, and the supply amount of the organic binder can be adjusted by opening / closing the opening / closing valve 8 of FIG. For example, the supply rate of the organic binder when the pump capacity is 1,500 g / second is preferably 300 g / second or less, particularly 150 g / second or less.

  The binder used in the toothpaste is a raw material that stabilizes the powder and liquid system of the toothpaste (to prevent liquid separation) and provides shape retention. Organic binders and inorganic binders (For example, silica gel, bee gum, laponite, montmorillonite, bentonite, and the like). In the present invention, an organic binder is used as a binder that is put into a powder supply hopper and processed with a high shear mixer. In addition, there is no problem even if the inorganic binder is processed simultaneously with the organic binder with a high shear mixer, but since the inorganic binder does not require a swelling step by high shear, it can be mixed by the apparatus B in the third step. no problem.

  Organic binders include gums such as xanthan gum, tragacanth gum, karaya gum, gum arabic, etc., synthetic polymers such as polyvinyl alcohol, sodium polyacrylate, carboxyvinyl polymer, polyvinylpyrrolidone, carboxymethylcellulose alkali metal salt, methylcellulose, hydroxyethylcellulose , Cellulose derivatives such as sodium carboxymethyl hydroxyethyl cellulose, alginic acid derivatives such as sodium alginate and propylene glycol alginate, carrageenans and the like.

  Further, 95% or more of the organic binder has a particle size of 500 μm or less, preferably 355 μm or less. The particle size of the organic binder can be determined by the amount of the organic binder that passed through 10 g of the organic binder on a rotation tap type sieve shaker, sieved for 15 minutes, and sieved. As the sieve, sieve number 30 (nominal size 500 μm) and sieve number 42 (nominal size 355 μm) are used in JP standards. Here, the particle size of the organic binder being 500 μm or less means that 95% or more of the organic binder was sieved when the above test was performed using sieve number 30. Similarly, the particle size of the organic binder being 350 μm or less means that 95% or more of the organic binder was sieved when the above test was conducted using sieve number 42.

  The compounding amount of the organic binder in the toothpaste can be a normal compounding amount, and 0.1 to 5% by mass of the whole composition is suitable.

  Examples of the inorganic binder include silica gel, bee gum, laponite, montmorillonite, and bentonite. The compounding quantity of the inorganic binder in toothpaste can be made into a normal compounding quantity, and 0.1-10 mass% of the whole composition is suitable.

  In the first step, as the wetting agent, those usually blended in toothpastes can be used, and examples thereof include sorbit, glycerin, xylit, maltite, lactit, propylene glycol, polyethylene glycol, etc., and particularly sorbit and / or glycerin. Are preferably used, and water is particularly preferably used as the solvent. These wetting agents may be used in the first step, or may be partially used in the second step. Further, the entire amount may be used after the second step.

The mixing ratio (mass ratio) of the wetting agent used in the first step and the water used as the solvent is desirably wetting agent / water = 85/15 to 0/100, particularly 70/30 to 20/80. If the water content is less than 15% by mass, problems such as poor dissolution of powdered wetting agents (xylit, sorbit, etc.) in water, poor flow rate due to increased viscosity of highly viscous wetting agents (glycerin, etc.), etc. In addition, if there is no moisture, the organic binder is processed by a high shear mixer while remaining completely unswelled, and swelling starts in a low shear vacuum mixer, so that sufficient swelling and dissolution may not be obtained. Therefore, when using a liquid wetting agent having good fluidity such as propylene glycol or liquid polyethylene glycol in the first step, it may be used as a wetting agent aqueous solution by adding not less than 15% by mass of water. desirable. The water ratio may be 100% by mass, but when using an organic binder having an extremely fast swelling speed, it may be better to control the swelling speed by setting the water content to 80% by mass or less. is there.
Here, the ratio of the wetting agent is a value expressed in a pure amount. For example, in the case of sorbit, it represents the concentration as a powder, and in the case of a 70 mass% sorbite aqueous solution that is used for general purposes, it is expressed as sorbit / water = 70/30.

As described above, the humectant used in the present invention is preferably sorbit and / or glycerin, and these have less influence on the flavor compared to other humectants usually used in dentifrices, and in large amounts. It is preferably used because it can be blended and the dispersibility of the organic binder is good. In addition, sorbite can be prepared by dissolving a high-purity sorbite powder in water to prepare a sorbite solution with a specified concentration, or diluting a general-purpose sorbite solution (for example, 70% by mass solution) to a specified concentration, or using it as it is. good. As for glycerin, high-purity concentrated glycerin or glycerin liquid (for example, 85 mass% liquid) may be diluted to a prescribed concentration or used as it is.
As for the compounding quantity of the wetting agent in a dentifrice, 5-60 mass% of the whole composition is preferable.

  Further, water is preferably used as the solvent, and when producing a wetting agent aqueous solution, a part of the water mixed in the dentifrice is mixed with the wetting agent. The amount of water in the dentifrice is usually preferably 20 to 70% by mass of the entire composition. A part of the organic binder is used as a dispersion medium for the organic binder so as to have the above mixing ratio to prepare an aqueous swelling agent solution, and the remaining water is used for swelling and dissolving after the organic binder is dispersed. In any case, a mixed aqueous solution in which water-soluble raw materials (excluding binder and foaming agent) are dissolved in water as a solvent may be used.

  In the present invention, the organic binder dispersion refers to a liquid in which the organic binder is uniformly dispersed in water or an aqueous wetting agent solution. In the present invention, the organic binder is in a powder state (unswelled). The dispersion liquid in which the state of swelling and dissolution is mixed is shown. About the state of this dispersion liquid, it can confirm by the presence or absence of the unswelled organic binder by the viscosity change immediately after dispersion | distribution by a continuous mixing disperser and time-lapse | temporality, and microscopic observation. According to microscopic observation, the particles can be seen when they are not swollen, and when the particles are swollen and dissolved, the particles disappear and become a transparent liquid.

After preparing the organic binder dispersion liquid in which the organic binder is dispersed in water or an aqueous wetting agent solution by the apparatus (A), this organic binder dispersion liquid is supplied to the apparatus (B) as the second step. The organic binder is swollen and dissolved, and the remaining raw materials are mixed with the organic binder swelling liquid under reduced pressure using the apparatus (B) as step III as described later.
The mixing conditions in the apparatus (B) in the second step are 0 to 50 ° C., preferably 10 to 40 ° C., and 10 to 50 rpm, preferably 15 to 40 rpm, and mixed for 5 to 20 minutes. It is desirable to swell and dissolve the organic binder.

In Step III, after all the remaining raw materials except for the foaming agent are added to the swelling solution of the organic binder obtained in Step II II under reduced pressure using the apparatus (B), 0 to 40 It is preferable to perform defoaming and mixing for 5 to 20 minutes under reduced pressure at a temperature of 10 ° C., preferably 10 to 30 ° C., and 10 to 50 rpm, preferably 15 to 40 rpm. Finally, a foaming agent is added and defoamed and mixed again under the above conditions to obtain a dentifrice composition. In this case, the reduced pressure condition is preferably 1 to 10 kPa, particularly 2 to 8 kPa.
Thus, flavor expression becomes favorable by mixing the remaining raw materials containing a fragrance | flavor, an abrasive | polishing agent, and a foaming agent after organic binder binder swelling dissolution using the apparatus (B) on low shear conditions.

In the manufacture of dentifrices, when fragrances and abrasives are mixed using a continuous mixer in the same manner as organic binders, these raw materials are atomized so that the amount of fragrances adsorbed on the abrasives is reduced. Unlikely, the flavor balance is lost, but after preparing an organic binder dispersion liquid in advance and making it into an organic binder swelling and dissolving liquid, in this step III, a fragrance, an abrasive, etc. are mixed as the remaining raw materials. Thus, the flavor balance can be improved.
Preferably, the fragrance is added before the abrasive and then the abrasive is added. When the fragrance is added after the abrasive, the viscosity of the entire system increases, and the fragrance may be difficult to mix uniformly.

  The remaining raw materials to be added in Step III are known components that are usually used as dentifrice ingredients excluding the raw materials blended in the previous step. For toothpastes, usually abrasives, organic binders, inorganic binders, wetting agents, solvents, fragrances, solubilizers, colorants, preservatives, active ingredients, corrigents, thickeners, sweeteners , PH adjusters, stabilizers, cleaning agents, adsorbents, refreshing agents, foaming agents, etc. are blended, but the remaining raw materials added in the third step are the above-mentioned organic binder, water or It is a component raw material excluding the wetting agent aqueous solution and a raw material not blended in the previous step. Unmixed water and wetting agent are also added in this step.

  As abrasives (powder), 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, tribasic magnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, zirconium silicate, polymethyl methacrylate, other synthetic resins, etc., and these abrasives may be used alone, Two or more kinds may be used in combination. As for the compounding quantity in a dentifrice, it is preferable to use 5-50 mass% of the whole composition.

  As a foaming agent, an anionic surfactant, a nonionic surfactant, and an amphoteric surfactant can be blended. Examples of 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 ester such as ethylene sorbitan monostearate, polyoxyethylene fatty acid ester 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 polyol Dipropylene fatty acid esters. These foaming agents may be used alone or in combination of two or more. As for the compounding quantity in a dentifrice, 0.1-10 mass% of the whole composition 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 fragrance ingredients such as absolute peppermint, absolute rose, orange flower; processed fragrance ingredients of these natural fragrance ingredients; menthol, carvone, anethole, cineol, methyl salicylate, cinnamic aldehyde, eugenol, 3-l-menthoxip Known perfume ingredients used for oral compositions such as bread-1,2-diol, pinene, octylaldehyde, citral, pulegone, calbe acetate, anisaldehyde, etc .; formulated fragrance ingredients such as strawberry flavor and apple flavor A fragrance ingredient material is mentioned. These perfume ingredients may use 1 type and may use 2 or more types together. As for the compounding quantity in a dentifrice, it is preferable to use 0.1-5 mass% of the whole composition.

  Further, the remaining raw materials include active ingredients, inorganic binders, preservatives, colorants, sweeteners, solubilizers, corrigents, thickeners, pH adjusters, stabilizers, detergents, adsorbents, cooling agents. Agents and the like.

  Specifically, as active ingredients, sodium monofluorophosphate, sodium fluoride, hinokitiol, cetylpyridinium chloride, benzalkonium chloride, isopropylmethylphenol, triclosan, chlorhexidine salts, dextranase, amylase, protease, lysozyme, mutanase Enzymes such as sodium chloride, ε-aminocaproic acid, tranexamic acid, tocopherols, glycyrrhetinic acid, ascorbic acid and its derivatives and salts thereof, herbal medicines, potassium nitrate, chamomile, and ougone. The amount of the dentifrice excluding sodium chloride is preferably 0.001 to 5 mass% of the entire composition. As for the compounding quantity in the dentifrice of sodium chloride, 5-25 mass% of the whole composition is preferable.

  Examples of antiseptics include various parabens, nonionic antibacterial agents such as triclosan, cationic antibacterial agents such as benzethonium chloride and cetylpyridinium chloride, sodium benzoate, and essential oils. Examples of the colorant include edible pigments and titanium dioxide.

  Examples of the sweetening agent include saccharin sodium, aspartame, stevioside, stevia extract, maltose, lactose, perilartine, glycyrrhizin salts, neohesperidyl dihydrochalcone, paramethoxycinnamic aldehyde and the like. The compounding amount in the dentifrice is preferably 0.01 to 5% by mass of the entire composition.

  EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In addition, in the following examples, the part of the amount is all parts by mass.

[Example 1]
Toothpaste was obtained by producing 50 kg of the dentifrice composition having the composition shown in Table 1-1 with the equipment shown in FIGS.
Organic shearing agent (0.5 parts of sodium polyacrylate, 0.5 part of xanthan gum, 0.5 part of sodium alginate) and 0.2 part of sodium saccharin as powder raw materials are as shown in FIGS. In-line type wet mixing and dispersing apparatus (QuadroWaitron ZC1 type; manufactured by POWREC Co., Ltd.) into hopper (A) 2 (temperature 25 ° C.), and 25.0 parts of purified water and 20.0 parts of 70% sorbite liquid were added. It put into the liquid introduction part (B) 3 (temperature 25 degreeC). The flow rate of the pump 5 (vortex pump (C) with an inverter) was adjusted to 1,140 ml / s. When the valve (D) 7 is opened and the operation of the pump (C) 5 is started and the liquid flows into the liquid raw material component inlet 6, the valve (E) 8 is opened and the powder raw material of the hopper (A) 2 is increased. It put into the shear mixer (F) 10. The rotation speed of the high shear mixer at this time was set to 6,500 rpm. The high shear mixer 10 is a mixing and dispersing device having a stator 21 and a rotor 11, and has a spiral blade 13 attached to a rotary shaft 12 at the center of the rotor 11. The rotor 11 rotates integrally with the blade 13. By rotating the blades 13 of the rotor 11, the liquid inside the rotor 11 is pushed out and passes through the gaps between the comb teeth 14 a and 14 b of the rotor 11 and the comb teeth 24 of the stator 21. Powder raw materials are mixed and dispersed. In the rotor 11 and the stator 21, the size of the circular inner ring wall 15a formed by the comb teeth 14a is 80 mm, and the size of the circular inner ring wall 15b formed by the comb teeth 14b is 95 mm. The tooth gap spacing was 2.0 mm and the height when the rotor and stator were stacked was 34 mm. At this time, the volume until the powder raw material of the hopper (A) comes into contact with the circular inner ring wall 15a after being put into the liquid is 171 ml. Since the liquid flow rate is set to 1,140 ml / s, the average residence time of the powder raw material of the hopper (A) is 0.15 seconds. In addition, since the rotational speed of the high shear mixer is set to 6,500 rpm, the linear velocity at the tip of the circular outer ring wall is 32.3 m / s. The organic binder dispersion treated by the high shear mixer was put in-line in a low shear type vacuum mixer (effective capacity 60 L kneader, Sigma blade; manufactured by Inoue Seisakusho) equipped with the blade 30 shown in FIG. The mixture was mixed at 34 rpm for 600 seconds to obtain an organic binder swelling solution (temperature 28 ° C.). To this swelling solution, 3.0 parts of propylene glycol was added and mixed at 34 rpm for 120 seconds, and then 1.5 parts of a fragrance was added and mixed at 34 rpm for 300 seconds (temperature 27 ° C.). First, 47.0 parts of calcium hydrogen phosphate / anhydride for dentifrice was added and mixed for 300 seconds at 34 rpm, then the pressure in the vacuum mixer was adjusted to 3 kPa, and kneaded for 600 seconds at a rotation speed of 34 rpm. Was defoamed and mixed at a temperature of 25 ° C. After returning to normal pressure, 1.8 parts of sodium lauryl sulfate was added, the pressure in the vacuum mixer was again set to 3 kPa, kneading was carried out at a rotation speed of 34 rpm for 600 seconds, and second-stage vacuum degassing mixing was performed to prepare a toothpaste. Was prepared (finished temperature 25 ° C.).

[Example 2]
A toothpaste was prepared in the same manner as in Example 1 except that the capacity (1,140 ml / s) of the centrifugal pump (C) in Example 1 was changed to 3,420 ml / s. The powder residence time at this time was 0.05 seconds.

Example 3
A toothpaste was prepared in the same manner as in Example 1 except that the capacity (1,140 ml / s) of the centrifugal pump (C) in Example 1 was changed to 2,443 ml / s. The powder residence time at this time was 0.07 seconds.

Example 4
A toothpaste was prepared in the same manner as in Example 1 except that the capacity (1,140 ml / s) of the centrifugal pump (C) in Example 1 was changed to 570 ml / s. The powder residence time at this time was 0.30 seconds.

Example 5
A toothpaste was prepared in the same manner as in Example 1 except that the capacity (1,140 ml / s) of the centrifugal pump (C) in Example 1 was changed to 342 ml / s. The powder residence time at this time was 0.50 seconds.

[Comparative Example 1]
A toothpaste was prepared in the same manner as in Example 1, except that the capacity (1,140 ml / s) of the centrifugal pump (C) in Example 1 was changed to 17,100 ml / s. The powder residence time at this time was 0.01 seconds.

[Comparative Example 2]
A toothpaste was prepared in the same manner as in Example 1 except that the capacity (1,140 ml / s) of the centrifugal pump (C) in Example 1 was changed to 171 ml / s. The powder residence time at this time was 1.00 seconds.

[Comparative Example 3]
The high shear type in-line type wet mixing and dispersing apparatus of Example 1 was changed to a low shear type in-line type wet mixing and dispersing apparatus (static mixer; Noritake Company Limited), and a toothpaste was prepared in the same manner as in Example 1. .

[Comparative Example 4] Method by Prior Art (Japanese Patent Laid-Open No. 11-171743) 50 kg of a dentifrice composition having the composition shown in Table 1-1 was prepared by the following method. In a mixing tank equipped with paddle blades, 3.0 parts of propylene glycol and organic binder (0.5 parts of sodium polyacrylate, 0.5 parts of xanthan gum, 0.5 parts of sodium alginate) are stirred for 15 minutes. The organic binder was uniformly dispersed (temperature 22 ° C.). In a mixing tank equipped with paddle blades, 25.0 parts of purified water, 20.0 parts of 70% sorbite liquid and 0.2 part of saccharin sodium were added and mixed for 5 minutes (temperature 24 ° C.). The binder dispersion prepared in advance in the above mixing tank was put into this and swollen and dispersed (temperature 25 ° C.). This swelling liquid was put into a low shear type vacuum mixer (effective capacity 60 L kneader, Sigma blade; manufactured by Inoue Seisakusho), 1.5 parts of a fragrance was added, and mixed at 34 rpm for 5 minutes (temperature 25 ° C.). Furthermore, 47.0 parts of calcium hydrogen phosphate dentifrice for dentifrice was added and mixed at 34 rpm for 5 minutes. This mixture was subjected to first stage vacuum degassing and mixing at a pressure of 3 kPa at 34 rpm for 10 minutes (temperature 23 ° C.). The pressure was returned to normal pressure, 1.8 parts of sodium lauryl sulfate was added, and second-stage vacuum defoaming mixing was performed at a pressure of 3 kPa and 34 rpm for 10 minutes to prepare a toothpaste (finished temperature 23 ° C.).

[Comparative Example 5]
50 kg of the dentifrice composition having the composition shown in Table 1-1 was prepared by the following method.
In a mixing tank equipped with paddle blades, 3.0 parts of propylene glycol and organic binder (0.5 parts of sodium polyacrylate, 0.5 parts of xanthan gum, 0.5 parts of sodium alginate) are stirred for 15 minutes. The organic binder was uniformly dispersed (temperature 20 ° C.). 25.0 parts of purified water, 20.0 parts of 70% sorbite solution and 0.2 part of saccharin sodium are placed in a high shear type wet mixing and dispersing apparatus (200 L universal mixer; manufactured by POWREC) for 5 minutes, agitator 50 rpm, homo Mixing was performed at a mixer of 1,300 rpm (temperature: 25 ° C.). The organic binder dispersion prepared in advance in the mixing tank was added to this and mixed for 10 minutes under the above conditions to swell and dissolve the organic binder (temperature 25 ° C.). To this, 1.5 parts of a fragrance was added and mixed, and further 47.0 parts of calcium hydrogen phosphate / anhydrous dentifrice was added and mixed for 5 minutes under the above conditions. The mixture was kneaded while circulating up and down at a pressure of 3 kPa at an agitator of 50 rpm and a homomixer of 1,300 rpm, and subjected to first stage vacuum degassing and mixing for 10 minutes (temperature 24 ° C.). The pressure was returned to normal pressure, 1.8 parts of sodium lauryl sulfate was added, and a second stage of vacuum defoaming mixing was performed while circulating up and down at a pressure of 3 kPa at an agitator of 50 rpm and a homomixer of 1,300 rpm to prepare a toothpaste ( Finished temperature 24 ° C).

[Comparative Example 6]
50 kg of the dentifrice composition having the composition shown in Table 1-1 was prepared by the following method. In a mixing tank equipped with paddle blades, 3.0 parts of propylene glycol and organic binder (0.5 parts of sodium polyacrylate, 0.5 parts of xanthan gum, 0.5 parts of sodium alginate) are stirred for 15 minutes. The organic binder was uniformly dispersed (temperature 18 ° C.). Put 25.0 parts of purified water, 20.0 parts of 70% sorbite and 0.2 part of saccharin sodium in a low shear type vacuum mixer (effective capacity 60L kneader, Sigma blade; manufactured by Inoue Seisakusho) for 5 minutes at 34 rpm. Mixed (temperature 24 ° C.). To this, an organic binder dispersion prepared in advance in the mixing vessel was added and mixed at 34 rpm for 10 minutes. To this was added 1.5 parts of fragrance, mixed at 34 rpm for 5 minutes, and further 47.0 parts of calcium hydrogen phosphate / anhydrous dentifrice was added and mixed at 34 rpm for 5 minutes (temperature 22 ° C.). This mixture was subjected to first stage vacuum degassing and mixing at a pressure of 3 kPa and 34 rpm for 10 minutes (temperature 21 ° C.). The pressure was returned to normal pressure, 1.8 parts of sodium lauryl sulfate was added, and second-stage vacuum defoaming mixing was performed at a pressure of 3 kPa and 34 rpm for 10 minutes to prepare a toothpaste (finished temperature 21 ° C.).

  The obtained dentifrice composition was evaluated by the following method. The composition of the dentifrice composition in the above Examples and Comparative Examples is shown in Table 1-1, and the dentifrice production conditions and evaluation results are shown in Table 1-2. Furthermore, in Table 1-1, the composition of the dentifrice composition of the Example mentioned later is also shown.

Evaluation method of toothpaste (1) Flavor Take 1g of dentifrice composition on a toothbrush, the flavor when actually brushing teeth is evaluated in the following three stages, each of the eight panelists specializing in flavor, and the evaluation of the dentifrice composition is described above. The average score of 8 people was evaluated in 4 grades.
Evaluation standard of flavor panelists 3 points: Good flavor as a dentifrice and excellent usability.
2 points: The flavor balance is slightly lost as a dentifrice, but there is no problem with the merchantability.
1 point: The balance of flavor is lost as a dentifrice, and there is a problem in merchantability.
Evaluation criteria for dentifrice composition ◎: Evaluation average score of flavor panelists is 2.5 or more ○: Evaluation average score of flavor panelists is 2.0 points or more to less than 2.5 points △: Evaluation average of flavor panelists The score is 1.5 points or more and less than 2.0 points ×: The average evaluation score of the flavor panelists is less than 1.5 points

(2) Shape retention property Clinicaha brush 4-row standard with a normal hardness of the dentifrice composition filled in a tube with a diameter of 8 mm (made by Lion Co., Ltd., hair transplant shape: 4 rows, width 20 mm, vertical 9 mm, high 10 mm), and the penetration into the toothbrush after 1 minute was evaluated in four stages of ◎ to × shown below.
A: The shape of the paste is maintained on the toothbrush,
The penetration into the toothbrush is 1 mm or less. ○: The shape of the paste is slightly broken on the toothbrush.
Soaking into the toothbrush is 1-3mm
Δ: The shape of the paste is broken on the toothbrush,
3-5mm penetration into toothbrush
×: The shape of the paste is completely broken on the toothbrush,
More than 5mm penetration into toothbrush

(3) Condensed skin (skin gloss)
The dentifrice composition filled in a tube having a diameter of 8 mm was extruded 10 cm onto the paper, and the paper was placed on top. In this state, the toothpaste composition is stretched while pushing on the upper paper with a finger, then the upper paper is taken out, and the appearance of the dentifrice composition spread on the paper is divided into three stages as shown below. Eight people evaluated each, and the evaluation of the dentifrice composition was the average score of the above eight people, and was evaluated in the following four stages.
Evaluation criteria of professional panelists 3 points: The surface is uniform, there is no grain (dama), and it is glossy.
2 points: The surface is uniform and there is no grain (dama), but no gloss.
1 point: The surface is uneven and grains (dama) are observed.
Evaluation criteria for dentifrice composition ◎: Evaluation average score of professional panelists is 2.5 or more ○: Evaluation average score of professional panelers is 2.0 or more to less than 2.5 points △: Evaluation average score of professional panelists is 1 .5 points or more and less than 2.0 points ×: Evaluation average score of professional panelists is less than 1.5 points

Moreover, in the said Example and comparative example, evaluation of workability | operativity was evaluated by the following method. The results are shown in Table 1-2.
Evaluation of workability:
(1) Detergency The amount of water required for cleaning the production equipment was evaluated in four stages.
◎: Within 2 times the toothpaste manufacturing pot volume ○: Over 2 times to 4 times the toothpaste manufacturing pot volume △: Over 4 times to 6 times the dentifrice manufacturing pot volume ×: Over 6 times the dentifrice manufacturing pot volume (2 ) Piping clogging The degree of clogging of the rotor outlet was visually evaluated in four stages.
◎: Level with almost no adhesion ○: Level with slight adhesion but can be manufactured continuously △: Level with adhesion and accumulation of deposits becomes impossible ×: With considerable adhesion, continuous production is impossible level

In the table, sodium salt is abbreviated as Na. The number indicating the blending amount represents part by mass (%).

Product name (manufacturer)
* 1 Kimika Argin I-3 (Kimika)
* 2 GENUVISCO type PJ-JPE (CP Kelco Japan)
* 3 Rheological 250H (Nippon Pure Chemicals)
* 4 Sunrose F10LC (Nippon Paper Chemicals)
* 5 Monato Gum DA (Dainippon Pharmaceutical)
* 6 Tokushir (Tokuyama)
* 7 70% sorbite solution (Towa Kasei Kogyo)
* 8 85% glycerin solution (Sakamoto Pharmaceutical)
* 9 Adeka propylene glycol (Asahi Denka)
* 10 Xylit (Towa Kasei Kogyo)
* 11 PEG # 400 (Lion)
* 12 Tixosil43 (Rhodia)
* 13 Calcium hydrogen phosphate for dentifrice (Tosoh Akzo)
* 14 Heavy calcium carbonate (Bihoku powdering industry)
* 15 Heidilite-210 (Showa Denko)
* 16 Taipei CR-50 (Ishihara Sangyo)
* 17 Saccharin sodium (Daito Chemical Industry)
* 18 ALSCOPE LN-90P (Toho Chemical Industry)
* 19 Soypon SLP (Kawaken Fine Chemical)

From the above results, the residence time of the organic binder powder of the high shear mixer of the apparatus (A) is preferably 0.05 to 0.50 seconds, and particularly preferably 0.07 seconds to 0.30 seconds. all right. At 0.01 seconds, the shape retention and the skin were poor, and at 1.00 seconds, piping clogging occurred.
The combination of the device (A) and the device (B) is preferably a combination of a high shear in-line wet mixing and dispersing device and a low shear vacuum mixer, and instead of the high shear in-line wet mixing and dispersing device of the device (A), a low shear When the dentifrice composition was produced with an in-line type wet mixing / dispersing device, the shape retention and the skin were poor, and when the dentifrice composition was produced with a high shear off-line type wet mixing / dispersing device, the detergency was poor. In addition, when the dentifrice composition was produced with a high shear type one pot, the flavor quality was poor, and when the dentifrice composition was produced with a low shear type one pot, the shape retention and the skin were deteriorated.

Example 6
Toothpaste was obtained by producing 50 kg of the dentifrice composition having the composition shown in Table 1-1 with the equipment shown in FIGS.
The organic binder (0.8 parts of carrageenan, 1.2 parts of carboxymethylcellulose sodium) and 0.15 parts of saccharin sodium and 0.4 parts of titanium dioxide as powder raw materials are of high shear type as shown in FIGS. Put it in the hopper (A) 2 of an in-line type wet mixing and dispersing device (QuadroWaitron ZC1 type; manufactured by Pauleck Co., Ltd.) (temperature 15 ° C.), and add 30.0 parts of 85% aqueous glycerin solution to the liquid introduction part (B) (Temperature 40 ° C.). The flow rate of the pump 5 (vortex pump (C) with an inverter) was adjusted to 1,140 ml / s. When the valve (D) 7 is opened and the operation of the pump (C) 5 is started and the liquid flows into the liquid raw material component inlet 6, the valve (E) 8 is opened and the powder raw material of the hopper (A) 2 is increased. It put into the shear mixer (F) 10. The rotation speed of the high shear mixer at this time was set to 6,500 rpm. The high shear mixer 10 is a mixing and dispersing device having a stator 21 and a rotor 11, and has a spiral blade 13 attached to a rotary shaft 12 at the center of the rotor 11. The rotor 11 rotates integrally with the blade 13. By rotating the blades 13 of the rotor 11, the liquid inside the rotor 11 is pushed out and passes through the gaps between the comb teeth 14 a and 14 b of the rotor 11 and the comb teeth 24 of the stator 21. Powder raw materials are mixed and dispersed. In the rotor 11 and the stator 21, the size of the circular inner ring wall 15a formed by the comb teeth 14a is 80 mm, and the size of the circular inner ring wall 15b formed by the comb teeth 14b is 95 mm. The tooth gap spacing was 2.0 mm and the height when the rotor and stator were stacked was 34 mm. At this time, the volume until the powder raw material of the hopper (A) comes into contact with the circular inner ring wall 15a after being put into the liquid is 171 ml. Since the liquid flow rate is set to 1,140 ml / s, the average residence time of the powder raw material of the hopper (A) is 0.15 seconds. Moreover, since the rotational speed of the high shear mixer is set to 6,500 rpm, the linear velocity at the tip of the circular outer ring wall is 32.3 m / s. The organic binder dispersion treated by the high shear mixer was put in-line in a low shear type vacuum mixer (effective capacity 60 L kneader, Sigma blade; manufactured by Inoue Seisakusho) equipped with the blade 30 shown in FIG. The mixture was mixed at 34 rpm for 600 seconds to obtain an organic binder swelling solution (temperature 35 ° C.). 44.75 parts of purified water was added to this swollen solution, and after mixing for 120 seconds at 34 rpm, 1.2 parts of fragrance was added and mixed for 300 seconds at 34 rpm (temperature 28 ° C.). To this, 20.0 parts of silicic acid anhydride was added and mixed at 34 rpm for 300 seconds. Then, the pressure in the vacuum mixer was adjusted to 3 kPa, kneaded at a rotation speed of 34 rpm for 600 seconds, and first-stage vacuum degassing mixing was performed. (Temperature 26 ° C.). After returning to normal pressure, 1.5 parts of sodium lauryl sulfate is added, the pressure in the vacuum mixer is set again to 3 kPa, kneading at a rotation speed of 34 rpm for 600 seconds, and second-stage vacuum degassing and mixing are performed. Dentifrice was prepared (finished temperature 26 ° C.).

Example 7
A toothpaste was prepared in the same manner as in Example 6 except that the gap between the rotor and stator comb teeth was changed to 0.3 mm.

Example 8
A toothpaste was prepared in the same manner as in Example 6 except that the gap between the rotor and stator comb teeth was changed to 0.5 mm.

Example 9
A toothpaste was prepared in the same manner as in Example 6 except that the gap between the rotor and stator comb teeth was changed to 1.5 mm.

Example 10
A toothpaste was prepared in the same manner as in Example 6 except that the gap between the rotor and stator comb teeth was changed to 3.0 mm.

Example 11
A toothpaste was prepared in the same manner as in Example 6 except that the gap between the rotor and stator comb teeth was changed to 5.0 mm.

Example 12
A toothpaste was prepared in the same manner as in Example 6 except that the gap between the rotor and stator comb teeth was changed to 7.0 mm.

  About the toothpaste obtained in Examples 6-12, it carried out similarly to Example 1, and evaluated the shape retention property and the paste skin. The production conditions and evaluation results are as shown in Table 2.

  From the above results, the inter-tooth distance between the rotor and the stator of the high shear mixer is preferably 0.5 to 5.0 mm, and particularly preferably 1.5 to 3.0 mm. Compared to the case where the comb tooth interval is 0.5 to 5.0 mm, when the comb tooth interval is 0.3 mm, the mixer shearing force is strong, so the viscosity is lowered and the shape retention is slightly reduced. Since the shearing of the mixer was weak, the dispersibility of the organic binder was slightly affected, and the shape-retaining property and the skin were slightly deteriorated.

Example 13
Toothpaste was obtained by producing 50 kg of the dentifrice composition having the composition shown in Table 1-1 with the equipment shown in FIGS.
A high shear type in-line wet mixing / dispersing device (quadro) as shown in FIGS. 1 to 4 is used for organic binder (0.7 part of sodium alginate, 0.7 part of xanthan gum) and 0.05 part of saccharin sodium as powder raw materials. Waitron ZC1 type (manufactured by POWREC Co., Ltd.) was placed in hopper (A) 2 (temperature 32 ° C.), and 21.95 parts of purified water was placed in liquid introduction portion (B) 3 (temperature 28 ° C.). The flow rate of the pump 5 (vortex pump (C) with an inverter) was adjusted to 1,140 ml / s. When the valve (D) 7 is opened and the operation of the pump (C) 5 is started and the liquid flows into the liquid raw material component inlet 6, the valve (E) 8 is opened and the powder raw material of the hopper (A) 2 is increased. It put into the shear mixer (F) 10. The rotation speed of the high shear mixer at this time was set to 6,500 rpm. The high shear mixer 10 is a mixing and dispersing device having a stator 21 and a rotor 11, and has a spiral blade 13 attached to a rotary shaft 12 at the center of the rotor 11. The rotor 11 rotates integrally with the blade 13. By rotating the blades 13 of the rotor 11, the liquid inside the rotor 11 is pushed out and passes through the gaps between the comb teeth 14 a and 14 b of the rotor 11 and the comb teeth 24 of the stator 21. Powder raw materials are mixed and dispersed. In the rotor 11 and the stator 21, the size of the circular inner ring wall 15a formed by the comb teeth 14a is 80 mm, and the size of the circular inner ring wall 15b formed by the comb teeth 14b is 95 mm. The tooth gap spacing was 2.0 mm and the height when the rotor and stator were stacked was 34 mm. At this time, the volume until the powder raw material of the hopper (A) comes into contact with the circular inner ring wall 15a after being put into the liquid is 171 ml. Since the liquid flow rate is set to 1,140 ml / s, the average residence time of the powder raw material of the hopper (A) is 0.15 seconds. In addition, since the rotational speed of the high shear mixer is set to 6,500 rpm, the linear velocity at the tip of the circular outer ring wall is 32.3 m / s. The organic binder dispersion treated by the high shear mixer was put in-line in a low shear type vacuum mixer (effective capacity 60 L kneader, Sigma blade; manufactured by Inoue Seisakusho) equipped with the blade 30 shown in FIG. The mixture was mixed at 34 rpm for 600 seconds to obtain an organic binder swelling solution (temperature: 40 ° C.). To this swelling solution, 25.0 parts of 70% sorbite aqueous solution, 4.0 parts of silica gel and 5.0 parts of xylit were mixed, mixed at 34 rpm for 120 seconds, and then added with 1.8 parts of fragrance, and then at 34 rpm for 300 seconds. Mixed (temperature 30 ° C.). To this, 40.0 parts of calcium carbonate was added, and after mixing at 34 rpm for 300 seconds, the pressure in the vacuum mixer was set to 3 kPa, kneaded at a rotational speed of 34 rpm for 600 seconds, and first-stage vacuum degassing mixing was performed. (Temperature 29 ° C). After returning to normal pressure, 0.8 parts of sodium lauryl sulfate is added, the pressure in the vacuum mixer is again set to 3 kPa, kneading is carried out at a rotational speed of 34 rpm for 600 seconds, and the second stage of vacuum degassing and mixing is performed. Dentifrice was prepared (finished temperature 28 ° C.).

Example 14
A toothpaste was prepared in the same manner as in Example 13 except that the blade of the vacuum mixer was changed to a jet type.

Example 15
A toothpaste was prepared in the same manner as in Example 13, except that the blade of the vacuum mixer was changed to a masticator type.

  About the toothpaste obtained in Examples 13-15, flavor variation was evaluated by the method shown below. Manufacturing conditions and evaluation results are as shown in Table 3.

Evaluation method of flavor variation Eight flavor panelists judge the toothpaste 1g sampled from 6 locations in the front, front right, front left, back left, back center, back right and back left of the toothpaste manufacturing pot. The degree of odor variation was sensorially evaluated in three stages.
◎: When all six samples are recognized as equivalent ○: 1-2 samples in 6 samples are different, but the difference is small △: 1-2 samples in 6 samples are recognized, and the difference is large Case ×: When 6 or fewer samples are recognized as equivalent

  For the overall mixing of the dentifrice composition, a sigma type is the best as a blade of a low shear vacuum mixer, and in the case of a zet type or a masticator type, there was some variation in flavor depending on the site inside the low shear vacuum mixer.

Example 16
50 kg of a dentifrice composition having the composition shown in Table 1-1 was produced with the equipment shown in FIGS.
High shear type in-line wet mixing and dispersing apparatus as shown in FIGS. 1 to 4 containing organic binder (0.6 part sodium polyacrylate, 0.6 part xanthan gum) and 0.16 part sodium saccharin as powder raw materials (Quadroightron ZC1 type; manufactured by Paulek Co., Ltd.) in a hopper (A) 2 (temperature: 10 ° C.), and 10.0 parts of purified water and 22.0 parts of 85% aqueous glycerin solution are added to the liquid introduction part (B) (Temperature 15 ° C.). The flow rate of the pump 5 (vortex pump (C) with an inverter) was adjusted to 1,140 ml / s. When the valve (D) 7 is opened and the operation of the pump (C) 5 is started and the liquid flows into the liquid raw material component inlet 6, the valve (E) 8 is opened and the powder raw material of the hopper (A) 2 is increased. It put into the shear mixer (F) 10. The rotation speed of the high shear mixer at this time was set to 6,500 rpm. The high shear mixer 10 is a mixing and dispersing device having a stator 21 and a rotor 11, and has a spiral blade 13 attached to a rotary shaft 12 at the center of the rotor 11. The rotor 11 rotates integrally with the blade 13. By rotating the blades 13 of the rotor 11, the liquid inside the rotor 11 is pushed out and passes through the gaps between the comb teeth 14 a and 14 b of the rotor 11 and the comb teeth 24 of the stator 21. Powder raw materials are mixed and dispersed. In the rotor 11 and the stator 21, the size of the circular inner ring wall 15a formed by the comb teeth 14a is 80 mm, and the size of the circular inner ring wall 15b formed by the comb teeth 14b is 95 mm. The tooth gap spacing was 2.0 mm and the height when the rotor and stator were stacked was 34 mm. At this time, the volume until the powder raw material of the hopper (A) comes into contact with the circular inner ring wall 15a after being put into the liquid is 171 ml. Since the liquid flow rate is set to 1,140 ml / s, the average residence time of the powder raw material of the hopper (A) is 0.15 seconds. In addition, since the rotational speed of the high shear mixer is set to 6,500 rpm, the linear velocity at the tip of the circular outer ring wall is 32.3 m / s. The organic binder dispersion treated by the high shear mixer was put in-line in a low shear type vacuum mixer (effective capacity 60 L kneader, Sigma blade; manufactured by Inoue Seisakusho) equipped with the blade 30 shown in FIG. The mixture was mixed at 34 rpm for 600 seconds to obtain an organic binder swelling solution (temperature 17 ° C.). To this swelling solution, 18.14 parts of purified water and 1.0 part of polyethylene glycol were added and mixed at 34 rpm for 120 seconds, and then 1.0 part of fragrance was added and mixed at 34 rpm for 300 seconds (temperature 18 ° C.). . After adding 45.0 parts of aluminum hydroxide and mixing at 34 rpm for 300 seconds, the pressure in the vacuum mixer was set to 3 kPa, kneading was carried out for 600 seconds at a rotation speed of 34 rpm, and first-stage vacuum degassing mixing was performed. (Temperature 17 ° C.). After returning to normal pressure, 1.2 parts of sodium lauryl sulfate and 0.3 part of sodium N-lauroyl sarcosinate were added, the pressure in the vacuum mixer was again adjusted to 3 kPa, kneaded at a rotational speed of 34 rpm for 600 seconds, Two-stage vacuum defoaming mixing was performed to prepare a toothpaste (finished temperature 16 ° C.).

Example 17
A toothpaste was prepared in the same manner as in Example 16 except that the rotation speed of the high shear mixer was changed to 2,011 rpm. In this case, the linear velocity at the tip of the circular outer ring wall of the high shear mixer is 10.0 m / s.

Example 18
A toothpaste was prepared in the same manner as in Example 16 except that the rotation speed of the high shear mixer was changed to 3,017 rpm. In this case, the linear velocity at the tip of the circular outer ring wall of the high shear mixer is 15.0 m / s.

Example 19
A toothpaste was prepared in the same manner as in Example 16 except that the rotation speed of the high shear mixer was changed to 5,028 rpm. In this case, the linear velocity at the tip of the circular outer ring wall of the high shear mixer is 25.0 m / s.

Example 20
A toothpaste was prepared in the same manner as in Example 16 except that the rotational speed of the high shear mixer was changed to 8,046 rpm. In this case, the linear velocity at the tip of the circular outer ring wall of the high shear mixer is 40.0 m / s.

Example 21
A toothpaste was prepared in the same manner as in Example 16 except that the rotation speed of the high shear mixer was changed to 10,057 rpm. In this case, the linear velocity at the tip of the circular outer ring wall of the high shear mixer is 50.0 m / s.

[Example 22]
A toothpaste was prepared in the same manner as in Example 16 except that the number of revolutions of the high shear mixer was changed to 12,068 rpm. In this case, the linear velocity at the tip of the circular outer ring wall of the high shear mixer is 60.0 m / s.

  About the toothpaste prepared in Examples 16-22, it carried out similarly to Example 1, and evaluated the shape retention property and the paste skin. Table 4 shows the manufacturing conditions and the quality evaluation results of the dentifrice.

  The linear velocity at the tip of the circular outer ring wall of the high shear mixer was good from 15.0 to 50.0 m / s, particularly from 25.0 to 40.0 m / s. Compared with the case where the linear velocity is 15.0 to 50.0 m / s, at the linear velocity 10.0 m / s, since the organic binder has low shear, non-swelled organic binder is seen, and the skin is stretched. In addition, the shape-retaining property was slightly poor, and at a linear velocity of 60.0 m / s, the shear was strong, resulting in a decrease in viscosity due to the cutting of the organic binder, and the shape-retaining property was slightly low.

Example 23
50 kg of a dentifrice composition having the composition shown in Table 1-1 was produced with the equipment shown in FIGS.
A high shear type in-line as shown in FIGS. 1 to 4 is an organic binder (0.4 parts of sodium alginate, 0.8 parts of carrageenan, 1.2 parts of carboxymethylcellulose) and 0.25 parts of sodium saccharin as powder raw materials. Into a hopper (A) 2 of a type wet mixing and dispersing apparatus (quadro waitron ZC1 type; manufactured by POWREC Co., Ltd.) (temperature 30 ° C.), and 25.0 parts of 70% sorbite aqueous solution and 34.55 parts of purified water are introduced into the liquid. Into part (B) 3 (temperature 24 ° C.). The flow rate of the pump 5 (vortex pump (C) with an inverter) was adjusted to 1,140 ml / s. When the valve (D) 7 is opened and the operation of the pump (C) 5 is started and the liquid flows into the liquid raw material component inlet 6, the valve (E) 8 is opened and the powder raw material of the hopper (A) 2 is increased. It put into the shear mixer (F) 10. The rotation speed of the high shear mixer at this time was set to 6,500 rpm. The high shear mixer 10 is a mixing and dispersing device having a stator 21 and a rotor 11, and has a spiral blade 13 attached to a rotary shaft 12 at the center of the rotor 11. The rotor 11 rotates integrally with the blade 13. By rotating the blades 13 of the rotor 11, the liquid inside the rotor 11 is pushed out and passes through the gaps between the comb teeth 14 a and 14 b of the rotor 11 and the comb teeth 24 of the stator 21. Powder raw materials are mixed and dispersed. In the rotor 11 and the stator 21, the size of the circular inner ring wall 15a formed by the comb teeth 14a is 80 mm, and the size of the circular inner ring wall 15b formed by the comb teeth 14b is 95 mm. The tooth gap spacing was 2.0 mm and the height when the rotor and stator were stacked was 34 mm. At this time, the volume until the powder raw material of the hopper (A) comes into contact with the circular inner ring wall 15a after being put into the liquid is 171 ml. Since the liquid flow rate is set to 1,140 ml / s, the average residence time of the powder raw material of the hopper (A) is 0.15 seconds. In addition, since the rotational speed of the high shear mixer is set to 6,500 rpm, the linear velocity at the tip of the circular outer ring wall is 32.3 m / s. The organic binder dispersion treated by the high shear mixer was put in-line in a low shear type vacuum mixer (effective capacity 60 L kneader, Sigma blade; manufactured by Inoue Seisakusho) equipped with the blade 30 shown in FIG. The mixture was mixed at 34 rpm for 600 seconds to obtain an organic binder swelling solution (temperature 28 ° C.). After adding 25.0 parts of 85% glycerin aqueous solution to this swelling solution and mixing at 34 rpm for 120 seconds, 0.8 part of fragrance was added and mixed at 34 rpm for 300 seconds (temperature 29 ° C.). To this, 11.0 parts of silicic acid anhydride was added, mixed at 34 rpm for 300 seconds, the pressure in the vacuum mixer was set to 3 kPa, kneaded at a rotation speed of 34 rpm for 600 seconds, and first-stage vacuum degassing mixing was performed. (Temperature 28 ° C.). After returning to normal pressure, 1.0 part of sodium lauryl sulfate is added, the pressure in the vacuum mixer is again set to 3 kPa, kneading at a rotation speed of 34 rpm for 600 seconds, and second-stage vacuum degassing mixing is performed. Dentifrice was prepared (finished temperature 28 ° C.).

Example 24
A toothpaste was prepared in the same manner as in Example 23 except that the blade rotation speed of the low shear vacuum mixer was changed to 5 rpm.

Example 25
A toothpaste was prepared in the same manner as in Example 23 except that the blade rotation speed of the low shear vacuum mixer was changed to 10 rpm.

Example 26
A toothpaste was prepared in the same manner as in Example 23 except that the blade rotation speed of the low shear vacuum mixer was changed to 15 rpm.

Example 27
A toothpaste was prepared in the same manner as in Example 23 except that the blade rotation speed of the low shear vacuum mixer was changed to 40 rpm.

Example 28
A toothpaste was prepared in the same manner as in Example 23 except that the blade rotation speed of the low shear vacuum mixer was changed to 50 rpm.

Example 29
A toothpaste was prepared in the same manner as in Example 23 except that the blade rotation speed of the low shear vacuum mixer was changed to 60 rpm.

  About Examples 23-29, it was carried out similarly to Example 13, and the flavor variation and the bubble mixing shown below were evaluated. Production conditions and evaluation results are shown in Table 5.

Evaluation of mixing of bubbles A dentifrice composition filled in a tube having a diameter of 8 mm was extruded 10 cm onto paper, and the paper was placed on top. In this state, the toothpaste composition is stretched while pushing on the upper paper with a finger, then the upper paper is taken out, and the appearance of the dentifrice composition spread on the paper is divided into three stages as shown below. Eight people evaluated each, and the evaluation of the dentifrice composition was the average score of the above eight people, and was evaluated in the following four stages.
Evaluation criteria for professional panelists 3 points: No bubbles on the surface.
2 points: There are a few bubbles on the surface.
1 point: There are many bubbles on the surface.
Evaluation criteria for dentifrice composition ◎: Evaluation average score of professional panelists is 2.5 or more ○: Evaluation average score of professional panelers is 2.0 or more to less than 2.5 points △: Evaluation average score of professional panelists is 1 .5 points or more and less than 2.0 points ×: Evaluation average score of professional panelists is less than 1.5 points

  The blade rotation speed of the low shear vacuum mixer is preferably 10 to 50 rpm, and particularly preferably 15 to 40 rpm. Compared to the case where the rotational speed is 10 to 50 rpm, the toothpaste sampled from 6 locations of the low-shear vacuum mixer showed a slight variation in flavor at the rotational speed of 5 rpm, and a slight mixing of bubbles was seen at the rotational speed of 60 rpm. .

It is the schematic of a high shear type in-line type wet-mixing dispersion apparatus (QuadroWaitron ZC1 type | mold; Paulec Co., Ltd. product). It is an enlarged view of the mixer part of the same figure. It is a schematic plan view of a rotor. It is a schematic bottom view of a stator. The blade of a low shear type vacuum mixing apparatus is shown, (A) is a plan view, and (B) is a side view.

Explanation of symbols

1 High shear type in-line wet mixing and dispersing equipment (A)
2 Powder supply hopper 3 Liquid introduction part 4 Liquid flow path 5 Pump 6 Liquid inflow port 7 Open / close valve 8 Open / close valve 10 Mixer part 11 Rotor 12 Rotating shaft 13 Blade 14a Comb tooth 14b Comb tooth 15a Inner ring wall 15b Outside Ring wall 16 Ring-shaped gap 21 Stator 22 Large-diameter circular ring-shaped substrate 23 Intermediate inclined ring wall 24 Comb teeth 25 Small-diameter circular ring wall 26 Discharge port

Claims (6)

  A method for producing a toothpaste containing an abrasive, an organic binder, a wetting agent, water, and a fragrance, comprising a stator having comb-shaped ring walls, spiral blades, and a comb-shaped ring wall on the outside thereof High shear type comprising a high shear type mixer unit provided with a rotor, a hopper for supplying organic binder powder to the mixer unit, and a liquid introduction unit for supplying water or a wetting agent aqueous solution to the mixer unit The water or wetting agent in which the organic binder powder is fed into the hopper of the in-line type wet mixing and dispersing apparatus (A), and the organic binder powder supplied from the hopper flows in from the liquid introduction part Adjust the inflow rate of water or the wetting agent aqueous solution so that the average residence time until it comes into contact with the aqueous solution and is discharged from the high-shear mixer of the wet mixing and dispersing device is 0.05 to 0.50 seconds. , Organic binder and water or wet An aqueous binder is continuously fed into the mixer section to prepare an organic binder dispersion in which the organic binder is dispersed in the water or the wetting agent aqueous solution, and then the organic binder dispersion is a low shear type. After being supplied to the vacuum mixing device (B) to obtain a swelling solution of the organic binder, the remaining powder raw material components and flavors containing the abrasive in the swelling solution under reduced pressure using the device (B) A method for producing a toothpaste comprising mixing the remaining liquid raw material components including   A high shear type in-line type wet mixing and dispersing apparatus (A) has a powder supply hopper and a liquid introduction unit, and a mixer unit in which powder and liquid are supplied and mixed from the hopper and the liquid introduction unit, respectively. In addition, a plurality of spiral blades are attached, a ring wall formed by a large number of comb teeth along the circumferential direction on the outside thereof, and a rotor having a rotating shaft, and a large number along the circumferential direction. And a stator having a ring wall formed of comb teeth, and the powder and liquid supplied from the hopper and the liquid introduction unit are agitated and mixed by blades rotating integrally with the rotation shaft of the rotor. The manufacturing method according to claim 1, wherein the mixture is sheared when passing through a gap between comb teeth of the rotor and the stator and discharged from an outlet provided in the device (A).   The rotor is provided with an inner ring wall formed of a large number of comb teeth on the outside of the spiral blade, and a ring-shaped gap is formed between the inner ring wall and the inner ring wall. The manufacturing method according to claim 2, wherein an outer ring wall formed of a plurality of comb teeth is provided, and the stator is disposed so as to insert the ring wall into the ring-shaped gap. Method.   The manufacturing method according to any one of claims 1 to 3, wherein the gaps between the comb teeth of the rotor and the stator are 0.5 to 5 mm, respectively.   The liquid introduction part of an apparatus (A) is provided with a pump as equipment which supplies a liquid, and adjusted the inflow speed of the liquid by adjusting the flow volume of this pump, The any one of Claims 1-4 Manufacturing method.   The manufacturing method according to claim 1, wherein the apparatus (B) is a batch type kneader of a sigma type blade.

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