JP6321951B2 - Process for producing dentifrice granules - Google Patents

Description

  The present invention relates to a method for producing a dentifrice granule and a dentifrice granule.

In recent years, dentifrices containing granules that can effectively remove dental plaque causing causative teeth and periodontal disease and are palpable are known. These granules are substantially spherical agglomerated particles so as not to damage the enamel and gums on the tooth surface, and contain functional materials such as drugs, enzyme agents, and abrasives. There are things that aim at the visual effect.

For example, Patent Document 1 discloses a granule obtained by binding a water-insoluble powder material with a water-insoluble inorganic binder and has a particle size size that passes through a 30-mesh sieve but does not pass through a 200-mesh sieve. A dentifrice containing granules that disintegrate when a load of 0.1 to 10 g per granule is applied is disclosed.
In Patent Document 2, as a method for producing a granule for a dentifrice having a comfortable granule feel without foreign substance feeling, step (1): calcium carbonate and / or silica having an average particle diameter of 0.1 to 100 μm and an average A step of mixing a water-insoluble inorganic binder having a particle size of 7 to 40 nm to prepare a water slurry having a solid content of 50 to 70% by weight, step (2): drying the water slurry obtained in step (1) And the process of obtaining the granule which contains the said water-insoluble inorganic binder 12 to 40 weight% (solid content content conversion) is disclosed.

JP-A-1-299211 JP 2010-70458 A

Conventionally, various water-soluble binders and water-insoluble binders have been used as granule binders. Patent Documents 1 and 2 disclose granules prepared by using a spray-drying method by preparing a slurry comprising a water-insoluble inorganic powder and a water-insoluble inorganic binder, but a dentifrice having sufficient wet disintegration strength. In order to produce the granules for use, it is necessary to use a large amount of the water-insoluble inorganic binder, and there is a problem that the production cost increases.
An object of the present invention is to provide a method for producing a dentifrice granule having excellent wet disintegration strength even with a small amount of a water-insoluble inorganic binder, and a granule obtained thereby.

  The inventors of the present invention are excellent in supplying water-insoluble powder material in a container-rotating granulator as liquid droplets of a water-insoluble inorganic binder containing colloidal silica using a multi-fluid nozzle. It has been found that dentifrice granules having high wet disintegration strength can be produced efficiently.

That is, the present invention provides the following [1] to [2].
[1] A method for producing a dentifrice granule, in which a water-insoluble powder material (A) and a water-insoluble inorganic binder (B) containing colloidal silica are mixed and granulated using a container rotating granulator. A method for producing a granule for dentifrice, wherein a granule is produced by supplying droplets of an aqueous dispersion of a water-insoluble inorganic binder (B) to the water-insoluble powder material (A) using a multi-fluid nozzle. .
[2] Dentifrice granules obtained by the method of [1] above.

  According to the present invention, an efficient production method capable of producing a dentifrice granule having excellent wet disintegration strength even with a smaller amount of a water-insoluble inorganic binder, and a granule obtained by the production method are provided. can do.

[Method for producing granules for dentifrice]
In the method for producing dentifrice granules of the present invention, the water-insoluble powder material (A) and the water-insoluble inorganic binder (B) containing colloidal silica are mixed and granulated using a container rotating granulator. A method for producing a dentifrice granule, wherein a droplet of an aqueous dispersion of a water-insoluble inorganic binder (B) is supplied to the water-insoluble powder material (A) using a multi-fluid nozzle to produce a granule. This is a method for producing a dentifrice granule.

In the present invention, as described above, the water-insoluble powder material (A) is granulated using a container rotating granulator. Therefore, the water-insoluble powder material (A) can be made to flow uniformly, and further, the water-insoluble powder material (A) can be flown by a mixing mechanism involving lifting of the water-insoluble powder material (A) by rotation and sliding / falling by its own weight. The shear force applied to A) is suppressed. Therefore, it can be said that the granulation method using the container rotating granulator is a non-consolidated granulation method.
In Patent Document 2, in the spray drying method, the water-insoluble inorganic powder and the water-insoluble inorganic binder (B) are sprayed together, dried and granulated, so that the water-insoluble inorganic binder (B) evaporates moisture. Accordingly, it is described that there is a tendency to accumulate more on the granule surface. However, in this application, since the aqueous dispersion of the water-insoluble inorganic binder (B) is supplied as droplets using a multi-fluid nozzle, the water-insoluble inorganic binder (B) exists uniformly from the inside to the surface of the granule. Moreover, since it is a non-consolidated production method using a container rotating granulator, a binding force is generated from the inside of the granule as the water evaporates, and the binder (B) is used as a binder throughout the granule. It is considered to function.
Therefore, it is considered that the wet disintegration strength is excellent and the amount of the water-insoluble inorganic binder (B) used can be reduced.
Hereafter, each component used for the method of this invention and a manufacturing method are demonstrated one by one.

<Water-insoluble powder material (A)>
As the water-insoluble powder material (A) used in the method of the present invention, those usually used for tooth abrasives are preferred, and specifically, inorganic materials are preferred. Here, “water-insoluble” means that the amount dissolved in 100 g of water at 20 ° C. is 1 g or less.
Specific examples of the water-insoluble powder material (A) include light calcium carbonate, heavy calcium carbonate, zeolite, silica other than colloidal silica, dicalcium phosphate, tricalcium phosphate, insoluble sodium metaphosphate, aluminum hydroxide, magnesium phosphate. , One or more selected from calcium pyrophosphate, magnesium carbonate, and titanium oxide.

  Among these, from the viewpoint of physical properties and cost when granulated, the water-insoluble powder material (A) is selected from light calcium carbonate, heavy calcium carbonate, zeolite, and silica other than colloidal silica, or one or two One or more species are preferred, and one or two species selected from light calcium carbonate and heavy calcium carbonate are preferred.

  The average particle size of the water-insoluble powder material (A) is preferably 0.1 μm or more, more preferably 0.5 μm or more, still more preferably 0.8 μm or more, from the viewpoint of removing dirt on the teeth after granule disintegration. From the viewpoint of suppressing the feeling of foreign matter, it is preferably 20 μm or less, more preferably 16 μm or less, and further preferably 12 μm or less. In addition, the average particle diameter of water-insoluble powder material (A) can be measured by the method as described in an Example.

<Water-insoluble inorganic binder (B)>
The water-insoluble inorganic binder (B) is used for binding the water-insoluble powder material (A) and imparting appropriate strength to the granules. The water-insoluble inorganic binder (B) contains colloidal silica. Thereby, the granule for dentifrice which has moderate wet disintegration strength can be manufactured even if a water-insoluble inorganic binder (B) is a small amount.
From the viewpoint, the content of colloidal silica in the water-insoluble inorganic binder (B) is preferably 50% by mass or more, more preferably 60% by mass or more, still more preferably 80% by mass or more, and still more preferably 90%. It is at least mass%, more preferably 100 mass%.
Examples of the water-insoluble inorganic binder (B) other than colloidal silica include magnesium aluminate metasilicate, synthetic aluminum silicate, and alumina sol.
In the example of the water-insoluble inorganic binder (B), there is a substance containing water such as colloidal silica. In the present invention, the amount of the water-insoluble inorganic binder (B) is the substance excluding water. Means the amount of inorganic binder.

  The amount of the water-insoluble inorganic binder (B) supplied to 100 parts by mass of the water-insoluble powder material (A) is preferably 2 parts by mass or more from the viewpoint of granulating the water-insoluble powder material (A) and improving wet disintegration strength and the like. More preferably 3 parts by mass or more, still more preferably 4 parts by mass or more, still more preferably 5 parts by mass or more, still more preferably 6 parts by mass or more, and preferably 50 parts by mass from the viewpoint of the efficiency of the binder. Or less, more preferably 40 parts by mass or less, still more preferably 30 parts by mass or less, still more preferably 25 parts by mass or less, still more preferably 20 parts by mass or less, still more preferably 18 parts by mass or less, and even more preferably 15 It is below mass parts.

  From the viewpoint of obtaining sufficient wet disintegration strength, the average particle size of the water-insoluble inorganic binder (B) is preferably 1 nm or more, more preferably 3 nm or more, still more preferably 5 nm or more, and preferably 100 nm or less. More preferably, it is 50 nm or less, More preferably, it is 30 nm or less. In addition, an average particle diameter can be measured by the method as described in an Example.

<Dispersion of water-insoluble inorganic binder (B)>
The content of the water-insoluble inorganic binder (B) in the dispersion of the water-insoluble inorganic binder (B) is 5% by mass or more, 10% by mass or more, and 20% by mass from the viewpoint of increasing the binding force as the binder. From the viewpoint of improving the sprayability by the multi-fluid nozzle, it is preferably 60% by mass or less, more preferably 50% by mass or less, 40% by mass or less, and 38% by mass or less.

<Optional component>
In the present invention, a water-insoluble powder material (A) (abrasive) and a water-insoluble inorganic binder (B) (binder) used in the method of the present invention as necessary, within a range not impairing the object of the present invention. ), And other optional components such as water-insoluble organic binders, organic fibers, medicinal ingredients, and colorants can be blended.

Examples of the fats and oils that can be used as the water-insoluble organic binder include higher fatty acids such as wax, paraffin, stearic acid, magnesium stearate, calcium stearate, and salts thereof.
Polymers and resins that can be used as water-insoluble organic binders include (i) polysaccharides such as xanthan gum, dextrin, gelatin, and derivatives thereof, (ii) rubber latex, (iii) acrylic acid, acrylic ester , Methacrylic acid, methacrylic acid ester, hydroxymethacrylic acid ester, styrene, vinyl acetate, vinyl pyrrolidone, maleic acid ester, methyl vinyl ether, α-olefin homopolymers, copolymers thereof and the like.
Examples of the organic fiber include cellulose, hemicellulose, lignin, chitin, and the like. Among these, cellulose is particularly preferable from the viewpoint of removing plaque from the granules.

  Medicinal ingredients include caries preventive agents, antimicrobial agents, enzymes, anti-inflammatory agents, etc., specifically sodium fluoride, potassium fluoride, tin fluoride, sodium monofluorophosphate, vitamin E, vitamins C, dextranase, mutanase, sodium chloride and other anti-inflammatory agents; aluminum lactate, azulene, glycyrrhetinic acid, β-glycyrrhetinic acid, allantochlorohydroxyaluminum, lysozyme chloride, epsilon aminocaproic acid, copper chlorophyllin sodium, copper gluconate, acetic acid Antiperceptive agents such as dl-tocopherol and potassium nitrate; anticalculus agents such as sodium tripolyphosphate and ethanehydroxydiphosphonate; plaque formation inhibitors such as zinc compounds, dihydrcholesterol, chlorhexidine, epidihydrcholesterol, iso B pills methylphenol, trichlorocarbanilide, halocarban, hinokitiol, allantoin, tranexamic acid, propolis, benzethonium chloride, cetylpyridinium chloride, fungicides such as triclosan, polyethylene glycol, Tabakoyani removers such as polyvinylpyrrolidone and the like.

Examples of the colorant include titanium oxide and ultramarine blue, and an aesthetic effect can be added by adding these colorants.
The above optional components can be used alone or in combination of two or more.
The content of the optional component is preferably 0 to 3 parts by mass with respect to 100 parts by mass of the total solid content of the water-insoluble powder material (A) and the water-insoluble inorganic binder (B) from the viewpoint of disintegration feeling. -2 mass parts is more preferable, and 0-1 mass% is still more preferable.

<Granulator>
In the present invention, a container rotating granulator is used in order to prevent the granulation from being compressed by giving strong shear to the granule. Since the granules obtained by the non-consolidated manufacturing method are porous, the dispersion of the binder (B) existing inside the granules is easy to dry, and the water-insoluble inorganic binder (B) inside the granules has a binding action. This is thought to be because the granules were strengthened.

(Container rotating granulator)
As the container rotating granulator, a drum granulator and a bread granulator are preferable. The drum granulator is not particularly limited as long as the drum-shaped cylinder rotates and performs processing. A horizontal or slightly inclined drum granulator can also be used. These apparatuses may be either batch type or continuous type.
If the coefficient of wall friction between the powder containing the water-insoluble powder material (A) and the inner wall of the container rotary granulator is small and it is difficult to apply sufficient ascending kinetic force to the powder, Preferably, a plurality of baffles (baffles) for assisting mixing are provided on the inner wall. By providing the baffle plate, it is possible to impart an upward movement to the powder, and the powder mixing property and the solid-liquid mixing property are improved.

  The operating conditions of the container rotating granulator are not particularly limited as long as the water-insoluble powder material (A) in the granulator can be flowed as uniformly as possible and stirred. From the viewpoint of obtaining granules having good disintegration strength and the like, the fluid number defined by the following formula (1) is preferably 0.005 or more, more preferably 0.01 or more, still more preferably 0.05 or more, From the viewpoint of obtaining non-consolidated granules, it is preferably 1.0 or less, more preferably 0.6 or less, and still more preferably 0.4 or less.

Fluid number: Fr = V ² / (R × g) (1)
V: Circumferential speed [m / s]
R: Radius from the center of rotation to the circumference of the rotating object [m]
g: Gravity acceleration [m / s ² ]

  In a drum granulator or a bread granulator in which granulation proceeds by rotation of the main body, V and R are values of the main body, and in a pan granulator equipped with crushing blades. , V and R are the values of the crushing blade.

<Multi-fluid nozzle>
In the present invention, the dispersion of the water-insoluble inorganic binder (B) is supplied using a multi-fluid nozzle. By using a multi-fluid nozzle, the droplets can be refined and dispersed, and a large liquid mass that forms coarse particles is less likely to be generated, thereby improving the efficiency of the binder.
A multi-fluid nozzle is a nozzle that mixes and atomizes a liquid and atomizing gas (air, nitrogen, etc.) through an independent flow path to the vicinity of the nozzle tip. Examples include fluid nozzles. Further, the mixing portion of the dispersion of the water-insoluble inorganic binder (B) and the atomizing gas is either an internal mixing type that mixes inside the nozzle tip or an external mixing type that mixes outside the nozzle tip. Also good.

  As such a multi-fluid nozzle, an internally mixed two-fluid nozzle made by Spraying Systems Japan Co., Ltd., Kyoritsu Alloy Manufacturing Co., Ltd., and Ikeuchi Co., Ltd., made by Spraying Systems Japan Co., Ltd., Kyoritsu Co., Ltd. Examples thereof include an external mixed type two-fluid nozzle manufactured by Alloy Seisakusho, manufactured by Atmax Co., Ltd., and an external mixed type four-fluid nozzle manufactured by Fujisaki Electric Co., Ltd.

The droplet diameter of the dispersion of the water-insoluble inorganic binder (B) can be adjusted to a desired range by adjusting the balance between the flow rate of the mixed solution and the flow rate of the atomizing gas. . That is, in order to reduce the droplet diameter, the flow rate of the atomizing gas may be increased with respect to the dispersion liquid having a constant flow rate. What is necessary is just to reduce a flow volume.
For example, when a two-fluid nozzle is used, it is easy to adjust the flow rate of the atomizing gas by adjusting the atomizing pressure of the atomizing gas. The atomizing gas spray pressure is preferably 0.1 MPa or more from the viewpoint of liquid dispersion, and preferably 1.0 MPa or less from the viewpoint of equipment load. Moreover, there is no restriction | limiting in particular as spray pressure of sodium silicate, However, 1.0 MPa or less is preferable from a viewpoint of equipment load, for example.

The average particle size of the droplet diameter of the dispersion of the water-insoluble inorganic binder (B) depends on the production apparatus.
In the case of using a container rotating type mixer, the average number of droplets of the mixed liquid is from the viewpoint of increasing the wet disintegration strength and obtaining a granule having a suitable particle size as a dentifrice granule with high yield because the fluid number is generally low. The diameter is preferably 210 μm or less, more preferably 150 μm or less, and even more preferably 100 μm or less. From the viewpoint of productivity, the diameter is preferably 1 μm or more, more preferably 5 μm or more, still more preferably 10 μm or more, and even more preferably. 20 μm or more.

The smaller the droplet diameter, the lower the flow rate of the liquid mixture and the lower the productivity. For example, by using multiple multi-fluid nozzles and reducing the flow rate per nozzle, maintaining finer droplets However, the addition rate can be increased. One or more multi-fluid nozzles may be used, but two or more and 20 or less can be used.
In addition, the average particle diameter of the droplets of the dispersion liquid is calculated on a volume basis, and is a value measured using, for example, a laser diffraction type particle size distribution measuring apparatus (manufactured by Malvern, Spray Tech). Specifically, it can be measured by the method described in the examples.

The temperature of the dispersion when the dispersion of the water-insoluble inorganic binder (B) is supplied using a multi-fluid nozzle is preferably 5 ° C. or higher, more preferably 10 ° C. or higher, from the viewpoint of spray stability. And preferably 50 ° C. or lower, more preferably 30 ° C. or lower.
The addition rate of the dispersion (solid) of the water-insoluble inorganic binder (B) in the case of using a container rotating mixer is controlled from the viewpoint of suppressing the formation of coarse particles and imparting excellent wet disintegration strength. The amount is preferably 20 parts by weight or less, more preferably 10 parts by weight or less, still more preferably 5 parts by weight or less, and still more preferably 4 parts by weight or less with respect to 100 parts by weight of the insoluble powder material (A). From the viewpoint of productivity, it is preferably 0.3 parts by weight / minute or more, more preferably 0.5 parts by weight / minute or more, and further preferably 1 part by weight / minute. Min. Or more, more preferably 2 parts by mass / min.

  The addition rate of the dispersion (solid content) of the water-insoluble inorganic binder (B) in the case of using a container rotary mixer is controlled from the viewpoint of suppressing the formation of coarse particles and imparting excellent wet disintegration strength. Preferably it is 7 mass parts / min or less with respect to 100 mass parts of insoluble powder material (A), More preferably, it is 5 mass parts / min or less, More preferably, it is 3 mass parts / min or less, More preferably, it is 1.5 masses From the viewpoint of productivity, it is preferably 0.1 parts by weight / minute or more, more preferably 0.3 parts by weight / minute or more, and further preferably 0.5 parts by weight / minute or more.

<Dry>
In the present invention, it is preferable to further dry the obtained granules from the viewpoint of improving the wet disintegration strength.

Examples of the drying method include shelf drying, fluidized bed drying, reduced pressure drying, and microwave drying. Among these, from the viewpoint of equipment, shelf drying and fluidized bed drying are preferable.
From the viewpoint of suppressing the disintegration of the granules during drying, a drying method that does not give as much shearing force as possible is preferable. For example, in the batch type, examples include a method of drying with an electric shelf dryer or a hot air dryer, a method of drying in a batch type fluidized bed, and the continuous type includes a fluidized bed, a rotary dryer, a steam tube dryer, and the like. It is done.

The drying temperature can be appropriately determined in consideration of the drying speed, but is preferably 60 ° C. or higher, more preferably 70 ° C. or higher, further preferably 80 ° C. or higher, 90 ° C. or higher, and 100 ° C. or higher. From the viewpoint of heat load, it is preferably 200 ° C. or lower, more preferably 150 ° C. or lower, still more preferably 130 ° C. or lower, and still more preferably 110 ° C. or lower.
The drying time varies depending on the effective amount and amount of the mixed solution used in the production, but is appropriately adjusted so that the wet disintegration strength falls within the preferable range of the present invention. The drying time is preferably 10 minutes or more, more preferably 60 minutes or more, still more preferably 5 hours or more, even more preferably 10 hours or more, still more preferably 15 hours or more, and preferably 48 hours or less, More preferably, it is 24 hours or less, More preferably, it is 20 hours or less. The drying means may be electric drying or fluidized bed drying.
The water content in the resulting granules is preferably 25% by mass or less, more preferably 20% by mass or less, still more preferably 15% by mass or less, and even more preferably 6% by mass or less, from the viewpoint of increasing wet disintegration strength. More preferably, it is 5% by mass or less, still more preferably 4% by mass or less. From the viewpoint of productivity, it is preferably 0.1% by mass or more, more preferably 0.2% by mass or more. The amount of water in the granules can be determined by the method described in the examples.

[Granule for dentifrice]
The dentifrice granules of the present invention can be produced by the production method described above.
The content of the water-insoluble powder material (A) in the dentifrice granules (excluding moisture) produced by the production method of the present invention is preferably 50% by mass or more from the viewpoint of enhancing the disintegration strength and the polishing power. More preferably 60% by mass or more, still more preferably 70% by mass or more, still more preferably 80% by mass or more, still more preferably 85% by mass or more, and preferably 98% by mass or less, more preferably 97% by mass. % Or less, more preferably 96% by mass or less.
In this invention, the calculated value calculated | required from the compounding quantity at the time of granule manufacture can be used for content and mass ratio of each component in the granule for dentifrice. The amount of the water-insoluble inorganic binder (B) is the solid content determined by the method described in the examples.

  In the dentifrice granules (excluding moisture) produced by the production method of the present invention, the content of the water-insoluble inorganic binder (B) is preferably 2% by mass or more from the viewpoint of increasing wet disintegration strength and the like. Preferably it is 3% by mass or more, more preferably 4% by mass or more, still more preferably 5% by mass or more, and from the viewpoint of increasing the efficiency of the binder, preferably 50% by mass or less, more preferably 40% by mass or less, More preferably, it is 30 mass% or less, More preferably, it is 20 mass% or less, More preferably, it is 10 mass% or less.

The preferable amount of the water-insoluble inorganic binder (B) with respect to 100 parts by mass of the water-insoluble powder material (A) in the granule is the same as the aforementioned supply amount.
The water content in the resulting granules is preferably 25% by mass or less, more preferably 20% by mass or less, still more preferably 15% by mass or less, and even more preferably 6% by mass or less, from the viewpoint of increasing wet disintegration strength. More preferably, it is 5% by mass or less, still more preferably 4% by mass or less. From the viewpoint of productivity, it is preferably 0.1% by mass or more, more preferably 0.2% by mass or more. The amount of water in the granules can be determined by the method described in the examples.

  The wet disintegration strength of a dentifrice granule, measured by the method described in the examples described later, can be used when blended with a dentifrice and can feel the granule in the mouth. Therefore, it is preferably 10% or more, more preferably 15% or more, still more preferably 20% or more, still more preferably 31% or more, still more preferably 35% or more, still more preferably 40% or more, and still more preferably From the viewpoint of hardly feeling foreign matter, it is preferably 95% or less, more preferably 90% or less, and still more preferably 85% or less. The wet disintegration strength is increased by increasing the content of the water-insoluble inorganic binder (B) (solid content), decreasing the water content in the granules, or selecting the type of the water-insoluble powder material (A) as appropriate. Can be increased.

  The average particle size of the dentifrice granules produced by the production method of the present invention is preferably 50 μm or more, more preferably 75 μm or more, still more preferably 100 μm or more, 200 μm or more from the viewpoint of having sufficient polishing power, From the viewpoint of suppressing the feeling of foreign matter in the oral cavity, it is preferably 900 μm or less, more preferably 800 μm or less, still more preferably 500 μm or less, still more preferably 400 μm or less, and even more preferably 320 μm or less. In addition, the average particle diameter of the granule for dentifrice can be measured by the method as described in an Example.

The bulk density of the dentifrice granule produced by the production method of the present invention is preferably 300 g / L or more, more preferably 350 g / L, from the viewpoint of a suitable feeling of use as a dentifrice granule and a suitable wet disintegration strength. L or more, more preferably 400 g / L or more, and preferably 900 g / L or less, more preferably 800 g / L or less, still more preferably 700 g / L or less.
Granules having the above average particle diameter, wet disintegration strength, and the like can be produced by appropriately changing the type, blending amount, and production conditions of the water-insoluble inorganic binder (B).

  In the following examples and comparative examples, “%” is “% by mass” unless otherwise specified, and “parts” is “parts by mass” unless otherwise specified. Each physical property value was measured by the following method.

(1) Water-insoluble inorganic binder (B) Solid content of aqueous dispersion Using a dropper, one drop becomes a droplet having a diameter of about 5 to 10 mm on an aluminum container having a diameter of 11.5 cm. 2.5 g of the sample is sprayed onto the glass as much as possible, and after that, using an infrared moisture meter (FD240, manufactured by Kett Kagaku Kenkyusho Co., Ltd.), the temperature is 105 ° C. in the moisture reference moisture measurement mode, and the conditions of Auto It was calculated by removing the volatilized free water measured in (the measurement was terminated when the amount of change in the measured value was within 0.05% within 30 seconds was regarded as the final measured value).

(2) Water-insoluble inorganic binder (B) Spray dispersion average droplet size of water dispersion Water-insoluble inorganic binder (B) Average droplet size (volume average particle size) of water dispersion is measured by laser diffraction particle size distribution measurement. It measured using the apparatus (The product made by Malvern, Spray Tech). Specifically, a spray nozzle tip is installed at a location 30 cm away from the laser, and the water-insoluble inorganic binder (B) aqueous dispersion is added so that the laser penetrates the center of the spray droplet group perpendicular to the laser. The average droplet size was measured by spraying continuously for 30 seconds.
(3) Method for measuring average particle size of water-insoluble inorganic binder (B) The average particle size of water-insoluble inorganic binder (B) is obtained by using an aqueous dispersion of a water-insoluble inorganic binder and a quartz glass cell having an optical path length of 1 cm. (T-1-UV-10 manufactured by Tosoh Quartz Co., Ltd.), measured using a dynamic light scattering particle size distribution analyzer (manufactured by Otsuka Electronics Co., Ltd., ELS-Z2), and determined by the photon correlation method The autocorrelation function was analyzed by the cumulant method to calculate the average particle size.

(4) Method for measuring average particle diameter of water-insoluble powder material (A) The average particle diameter of the water-insoluble powder material (A) is measured with a laser diffraction / scattering particle size distribution measuring apparatus (LA-920, manufactured by Horiba, Ltd.). The solvent was measured under conditions of ion-exchanged water, a refractive index of 1.2, a circulation rate of 4, and a circulation of 3 min.

(5) Average particle size of granules 2000, 1400, 1000, 710, 500, 355, 250, 180, 125, 90 of JISZ8801-1 (established on May 20, 2000, final revised on November 20, 2006) , 63, and 45 μm, and after shaking for 5 minutes, the 50% average diameter is calculated for the mass distribution under the sieve by the sieving method, and this is used as the average particle diameter. Specifically, 2000, 1400, 1000, 710, 500, 355, 250, 180, 125, 90, 63 of JISZ8801-1 (enacted on May 20, 2000, final amendment on November 20, 2006), Using a 45 μm sieve, stack in order from a sieve with a small mesh on the tray, add 100 g of granules from the top of the top 2000 μm sieve, cover and a low-tap type sieve shaker (manufactured by HEIKO Seisakusho, tapping) 156 times / minute, rolling: 290 times / minute), and after shaking for 5 minutes, the mass of the granules remaining on each sieve and the saucer was measured, and the mass ratio of the granules on each sieve (% ) Is calculated. The mass ratio of the granules on a sieve with a small mesh is added in order from the saucer, and the particle diameter at which the total becomes 50% is taken as the average particle diameter.

(6) Moisture content in dentifrice granules 2 g of a sample was evenly sprayed on an aluminum 11.5 cm diameter container, and then an infrared moisture meter (FD240, manufactured by Kett Science Laboratory Co., Ltd.) was used. Measurement was performed under the same conditions as in 1).

(7) Wet disintegration strength of granules First, the granules having a particle size of 150 to 180 μm are vibrated for 5 minutes using a sieve of 500, 355, 250, 180, 150, 125, 90, 63, 45 μm of JISZ8801-1. Was used as a sample. Next, 15 g of a stainless steel sphere (diameter 4 mm), 3 g of a granule sample, and 30 mL of ion-exchanged water were put into a screw tube (manufactured by Maruemu Co., No. 6) and inverted once. Then, it was left still for 30 minutes, and rotated for 2 minutes 30 seconds at 75 r / min with a tablet wear tester (manufactured by Higaki Medical Science Co., Ltd.).
The obtained granule sample is filtered through a 150 μm sieve, dried at 105 ° C. for 30 minutes, and then cooled to room temperature with a desiccator. The 150 μm sieve is made into a micro-type electromagnetic vibrator (manufactured by Tsutsui Riken Kikai Co., Ltd., micro-type electromagnetic vibratory sieve). The shaker was shaken for 5.5 minutes with an instrument M-2) and then weighed. The value calculated by the following formula was defined as the wet disintegration strength. In addition, wet disintegration strength is so high that the value of wet disintegration strength is large.
Wet disintegration strength (%) = (granule mass remaining on 150 μm sieve ÷ initial sample mass) × 100
(8) Measuring method of bulk density of granule The granule flows into a cylindrical container (diameter: 4 cm) having a volume of 100 mL in advance using a hopper for measuring bulk density specified by JIS K3362: 2008. The bulk density (g / L) was determined by grinding the granules at the top of the container and measuring the mass.

Example 1
7.0 kg of heavy calcium carbonate powder (Calfeine Co., Ltd., Christon SS, average particle size 5 μm) was put into a 75 L drum granulator (diameter 40 cm × L 60 cm) having a baffle plate, and the drum rotation speed was 30 r. p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, colloidal silica aqueous dispersion (Nissan Chemical Co., Ltd., Snowtex S, solid content: 32%, average particle size 22 nm) Using one external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.), 1.0 kg was sprayed and granulated. The addition rate and spray average droplet diameter of the colloidal silica aqueous dispersion were 200 g / min and 65 μm. The granulation operation was performed at 20 ° C.
After spraying the colloidal silica aqueous dispersion, mixing was continued for 1 minute, and then the mixture was discharged from the drum type granulator and dried at 105 ° C. for 19 hours using an electric dryer, and then the physical properties of the granules were evaluated. Production conditions and results are shown in Tables 1 and 2.

Example 2
6.8 kg of heavy calcium carbonate powder (Calfine SS, Cryston SS, average particle size 5 μm) was put into a 75 L drum granulator (diameter 40 cm × L 60 cm) having a baffle plate, and the drum rotation speed was 30 r. p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, colloidal silica aqueous dispersion (Nissan Chemical Co., Ltd., Snowtex S, solid content: 32%, average particle size 22 nm) Using one external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.), 1.2 kg of spray was added and granulated. The addition rate and spray average droplet diameter of the colloidal silica aqueous dispersion were 200 g / min and 65 μm. The granulation operation was performed at 20 ° C.
After spraying the colloidal silica aqueous dispersion, mixing was continued for 1 minute, and then the mixture was discharged from the drum type granulator and dried at 105 ° C. for 19 hours using an electric dryer, and then the physical properties of the granules were evaluated. Production conditions and results are shown in Tables 1 and 2.

Example 3
6.4 kg of heavy calcium carbonate powder (Calfine SS, Cryston SS, average particle size 5 μm) was charged into a 75 L drum granulator (diameter 40 cm × L 60 cm) having a baffle plate, and the drum rotation speed was 30 r. p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, colloidal silica aqueous dispersion (Nissan Chemical Co., Ltd., Snowtex S, solid content: 32%, average particle size 22 nm) Using an external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.), 1.6 kg of spray was added and granulated. The addition rate and spray average droplet diameter of the colloidal silica aqueous dispersion were 200 g / min and 65 μm. The granulation operation was performed at 20 ° C.
After spraying the colloidal silica aqueous dispersion, mixing was continued for 1 minute, and then the mixture was discharged from the drum type granulator and dried at 105 ° C. for 19 hours using an electric dryer, and then the physical properties of the granules were evaluated. Production conditions and results are shown in Tables 1 and 2.

Example 4
6.4 kg of light calcium carbonate powder (Toyo Denka Kogyo Co., Ltd., Toyo White, average particle size of 6 μm) was put into a 75 L drum granulator (diameter 40 cm × L 60 cm) with a baffle plate, and the drum rotation speed was 30 r. . p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, colloidal silica aqueous dispersion (Nissan Chemical Co., Ltd., Snowtex S, solid content: 32%, average particle size 22 nm) Using an external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.), 1.6 kg of spray was added and granulated. The addition rate and spray average droplet diameter of the colloidal silica aqueous dispersion were 200 g / min and 65 μm. The granulation operation was performed at 20 ° C.
After spraying the colloidal silica aqueous dispersion, mixing was continued for 1 minute, and then the mixture was discharged from the drum type granulator and dried at 105 ° C. for 19 hours using an electric dryer, and then the physical properties of the granules were evaluated. Production conditions and results are shown in Tables 1 and 2.

Example 5
5.2 kg of light calcium carbonate powder (Toyo Denka Kogyo Co., Ltd., Toyo White, average particle size of 6 μm) was put into a 75 L drum granulator (diameter 40 cm × L 60 cm) with a baffle plate, and the drum rotation speed was 30 r. . p. While mixing under the conditions of m / fluid number 0.2 / drum angle 12.6 °, colloidal silica aqueous dispersion (Nissan Chemical Co., Ltd., Snowtex S, solid content: 32%, average particle size 22 nm) Using one external mixing type two-fluid nozzle (manufactured by Atmax Co., Ltd.), 2.8 kg was sprayed and granulated. The addition rate and spray average droplet diameter of the colloidal silica aqueous dispersion were 200 g / min and 65 μm. The granulation operation was performed at 20 ° C.
After spraying the colloidal silica aqueous dispersion, mixing was continued for 1 minute, and then the mixture was discharged from the drum type granulator and dried at 105 ° C. for 19 hours using an electric dryer, and then the physical properties of the granules were evaluated. Production conditions and results are shown in Tables 1 and 2.

Comparative Example 1
Light calcium carbonate powder 42.9 kg (Toyo Denka Kogyo Co., Ltd., Toyo White, average particle size 6 μm), colloidal silica aqueous dispersion (Nissan Chemical Co., Ltd., Snowtex S, solid content: 32%, average particle size 22 nm ) 33.5kg, ion-exchanged water 23.6kg was charged into the 100L blending layer and mixed with a disperse blade (model: HS-P3, manufactured by Serizawa Nitrotomizer Co., Ltd.) to prepare a water slurry (solid content 52.5%). did.
The obtained water slurry was spray-dried at a blowing temperature of 190 ° C. to produce granules. Production conditions and results are shown in Tables 1 and 2.

Evaluation Results From comparison between Examples 1 to 5 and Comparative Example 1, it is found that the granules obtained by the production method of the present invention have excellent wet disintegration strength with a small amount of water-insoluble inorganic binder.

  According to the method for producing a dentifrice granule of the present invention, a dentifrice granule having excellent wet disintegration strength can be produced.

Claims (4)

A method for producing a dentifrice granule in which a water-insoluble powder material (A) and a water-insoluble inorganic binder (B) containing colloidal silica are mixed and granulated using a container rotating granulator,
Using a multi-fluid nozzle, supply droplets of an aqueous dispersion of a water-insoluble inorganic binder (B) to the water-insoluble powder material (A) to produce granules,
The container rotary granulator is a bread granulator or a drum granulator,
The average particle size of the droplets is 150 μm or less,
The manufacturing method of the granule for dentifrice whose quantity of this water-insoluble inorganic binder (B) is 2-50 mass parts with respect to 100 mass parts of this water-insoluble powder material (A).   The method for producing a dentifrice granule according to claim 1, wherein the amount of the water-insoluble inorganic binder (B) is 2 to 18 parts by mass with respect to 100 parts by mass of the water-insoluble powder material (A).   The dentifrice granule according to claim 1 or 2, wherein the water-insoluble powder material (A) is one or more selected from light calcium carbonate, heavy calcium carbonate, zeolite, and silica excluding colloidal silica. Manufacturing method.   The method for producing a dentifrice granule according to any one of claims 1 to 3, wherein the obtained granule is further dried.