JP2005179287A - Method for producing dentifrice - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a dentifrice enabling promotion of production efficiency in multiproduct production without impairing quality of flavor, dispersibility, shape-retaining property, stability, or the like, in production of various kinds of dentifrices. <P>SOLUTION: This method for producing the dentifrice is a method for producing two or more kinds of dentifrices each containing a polishing agent, a wetting agent, a foaming agent, a binder, a perfume and water. The method for producing the dentifrice comprises (i) a step for preparing a common base composition containing at least two kinds of agents selected from components contained in common in two or more kinds of dentifrices among the polishing agent, the wetting agent, the foaming agent, the binder, the perfume and water and (ii) a step for adding residual components which are not formulated in the step (i) among components contained in dentifrices produced to the common base composition obtained in the step (i) and mixing the composition with the residual components by low shearing force. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method for producing a dentifrice containing an abrasive, a wetting agent, a foaming agent, a binder, a fragrance, and water.

In general, a dentifrice contains ingredients such as an abrasive, a foaming agent, a wetting agent, a binder, and a fragrance. In order to obtain dentifrice preparations, it is usually necessary to perform uniform dispersion, uniform swelling and the like by combining these components in order to obtain design qualities such as flavor, blended skin, shape retention and cleaning power. Therefore, equipment having sufficient shearing force and mixing force is used for manufacturing.
In addition, dentifrices that are subject to the Pharmaceutical Affairs Law must meet GMP (Good Manufacturing Practice), which is a requirement for manufacturing excellent products with good quality, and one of the requirements is management of production lots. It is necessary to thoroughly. For this reason, dentifrice production facilities are often batch-type facilities that are easy to manage.
However, such a manufacturing facility inevitably requires a labor such as a cleaning operation when performing a product switching operation in a multi-product production process. The labor for this type switching operation takes much more labor than those not subject to the Pharmaceutical Affairs Law, and this deteriorates the total manufacturing efficiency in the multi-type production process.

In order to solve this problem, many proposals have been made to improve the efficiency of the manufacturing process, but no fundamental solution has been achieved.
For example, in Patent Documents 1 to 3, the manufacturing time cycle and the like are shortened by improving the blending order and mixing conditions of a binder, an abrasive, a wetting agent, and the like in a batch blending manufacturing process.
However, since batch cleaning is required for each type change and the frequency does not change, total production efficiency is insufficient.

Moreover, in patent documents 4-6, the improvement of manufacturing efficiency is attempted by continuous production.
However, there is a problem in that it is difficult to quantitatively supply each component and follow-up of lots, there are many small items, and in-line cleaning is required. In this in-line cleaning, in terms of certainty of cleaning, it is often insufficient in terms of sterilization and the like, and it is necessary to disassemble and clean the piping. For this reason, it takes a lot of time for dismantling, cleaning, and assembly when changing the product type, and the total number of days and necessary people is inefficient.

Patent Document 7 describes a method in which the components other than the fragrance component are heated to a high temperature of 40 to 80 ° C. to promote the swelling of the binder, and the fragrance component is statically mixed at 50 ° C. or less after batch mixing. Has been. In this method, the efficiency of the swelling of the binder is improved by batch blending the components excluding the fragrance component at a high temperature.
However, since it is necessary to cool before adding the fragrance component, a heat exchanger that is difficult to dismantle and clean is actually required as a manufacturing facility. Therefore, it is not preferable on GMP.
In addition, the static mixing used at the time of adding the fragrance component theoretically requires a very large number of modules in order to completely disperse the high-viscosity paste and the low-viscosity fragrance component uniformly. For this reason, the total length of the piping is increased, and the actual microscopic uniform dispersion is insufficient. That is, the fragrance component and other components are not easily blended, and the dentifrice is insufficient in terms of quality such as flavor.
Japanese Patent Laid-Open No. 11-171743 JP-A-11-171748 JP-A-11-171747 Japanese Patent No. 1932177 JP-A-1-165515 JP-A-6-9335 Japanese Patent No. 3107920

  The present invention provides a method for producing a dentifrice capable of improving the production efficiency in multi-product production without impairing the quality of flavor, dispersibility, shape retention, stability, etc. in the production of various dentifrices. For the purpose.

As a result of intensive studies, the inventors have previously manufactured a common composition in a plurality of dentifrices, and then can add the remaining components and mix with low shearing force, thereby improving manufacturing efficiency. It has been found that the quality such as flavor, dispersibility, shape retention and stability is not impaired.
That is, the present invention is a method for producing two or more dentifrices containing an abrasive, a wetting agent, a foaming agent, a binder, a fragrance and water,
(I) A common base composition comprising at least two selected from the ingredients commonly contained in the two or more dentifrices among the abrasive, wetting agent, foaming agent, binder, perfume and water. A step of preparing
(Ii) Of the components contained in the dentifrice to be manufactured, the remaining components not blended in (i) above are added to the common base composition obtained in (i) above and mixed with low shearing force. A method for producing a dentifrice comprising the steps of:

  With the method for producing a dentifrice of the present invention, in the production of a plurality of dentifrices, the total production efficiency including the washing switching step is improved without impairing quality such as flavor, dispersibility, shape retention, and stability. be able to.

Below, the manufacturing method of the dentifrice of this invention is demonstrated in detail.
The dentifrice produced by the production method of the present invention is two or more types of dentifrice containing an abrasive, a wetting agent, a foaming agent, a binder, a fragrance, and water.

<Process (i)>
In the production method of the present invention, firstly, from (i) components contained in common among two or more dentifrices to be produced among abrasives, wetting agents, foaming agents, binders, fragrances and water. A step of preparing a common base composition including at least two selected (step (i)) is performed.
The two or more types of dentifrices usually contain at least two or more of a polishing agent, a wetting agent, a foaming agent, a binder, a fragrance, and water as a common component.
The common base composition is composed of at least two, preferably 4 to 6, selected from components commonly contained in two or more different dentifrices, and each component is suitable for its purpose. Blended in balance.

As abrasives, potassium hydrogen phosphate, anhydrous, calcium hydrogen phosphate dihydrate, tertiary calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminum hydroxide, anhydrous silicic acid, aluminum silicate, insoluble sodium metaphosphate , Tertiary magnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, zirconium silicate, polymethyl methacrylate, and other synthetic resins. These can be used alone or in combination of two or more.
As for the compounding quantity of an abrasive | polishing agent, 10-50 mass% is preferable with respect to the total mass of a dentifrice.

Examples of the wetting agent include glycerin, sorbit, propylene glycol, 1,3-butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xylit and the like. These can be used alone or in combination of two or more.
The blending amount of the wetting agent is preferably 5 to 60% by mass with respect to the total mass of the dentifrice.

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

As binder, carrageenan, xanthan gum, sodium polyacrylate, cellulose derivatives such as sodium carboxymethyl cellulose, methyl cellulose, hydroxyethyl cellulose, alginic acid derivatives such as sodium alginate, propylene glycol alginate, gums such as gellan gum, tragacanth gum, caraya gum And synthetic binders such as polyvinyl alcohol, and inorganic viscosity agents such as silica gel, bee gum, laponite, montmorillonite, bentonite and kaolin. These can be used alone or in combination of two or more.
As for the compounding quantity of a binder, 0.1-10 mass% is preferable with respect to the total mass of a dentifrice.

Perfumes 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, absolute Natural fragrance ingredients such as peppermint, absoluteton rose, orange flower; processed fragrance ingredients of these natural fragrance ingredients; menthol, carvone, anethole, cineol, methyl salicylate, cinnamic aldehyde, eugenol, 2-diol, pinene, Known perfume ingredient materials used for oral compositions, such as single perfume ingredients such as octylaldehyde, citral, pregon, carbyl acetate, and anisaldehyde; formulated perfume ingredients such as strawberry flavor and apple flavor can be used. . These can be used alone or in combination of two or more.
The blending amount of the fragrance is preferably 0.1 to 5% by mass with respect to the total mass of the dentifrice.

As water, pure water, ion exchange water, distilled water, or the like can be used.
As for the compounding quantity of water, 5-80 mass% is preferable with respect to the total mass of a dentifrice.

  The method / apparatus for preparing the common base composition is not particularly limited. For example, after 5 components excluding the binder are mixed together, a powdery binder is added, and the mixture is uniformly mixed and swollen. After degassing under a reduced pressure of 001 to 0.010 MPa, it is preferable to finally add a foaming agent in a stationary state and mix under a reduced pressure of 0.001 to 0.010 MPa.

<Process (ii)>
Next, (ii) the common base composition obtained in (i) is divided into two or more, and each of the components contained in the dentifrice to be produced is divided into the divided common base composition, (i) The remaining components not blended in step (i) are added and mixed at a low shearing force (step (ii)).
Here, the remaining components not blended in the step (i) are:
Of the abrasives, wetting agents, foaming agents, binders, fragrances, and water, components not blended in step (i), or components blended in step (i) but not all The remaining amount, and the active ingredient of each dentifrice, and other optional ingredients, for example, flavoring agents characteristic of each dentifrice, preservatives, coloring agents, sweeteners, and other characteristic components. These components can be used alone or in combination of two or more.
Hereinafter, the remaining components blended in step (ii) may be collectively referred to as post-added components.

Active ingredients include sodium monofluorophosphate, sodium fluoride, hinokitiol, cetylpyridinium chloride, benzalkonium chloride, triclosan, chlorhexidine salts, enzymes such as dextranase, amylase, protease, lysozyme, mutanase, chloride Examples include sodium, [epsilon] -aminocaproic acid, tranexamic acid tocopherols, glycyrrhetinic acids, ascorbic acid and its derivatives and salts thereof, herbal medicines, potassium nitrate, duckweed extract, chamomile, oxon and the like.
The amount of the active ingredient is preferably 0.001 to 5% by mass relative to the total mass of the dentifrice.

Examples of the fragrance include the same ones as described above.
Examples of the preservative include methyl p-oxybenzoate, butyl p-oxybenzoate, ethyl p-oxybenzoate, propyl p-oxybenzoate, benzoic acid, sodium benzoate and the like.
Examples of the colorant include food colors and titanium dioxide.
Examples of the sweetener include saccharin sodium, aspartame, stevioside, stevia extract, sucrose, maltose, lactose, perilartine, glycyrrhizin salts, neohesperidyl dihydrochalcone, paramethoxycinnamaldehyde, and the like. The blending amount of the sweetener is preferably 0.1 to 5% by mass with respect to the total mass of the dentifrice.

In the present invention, by mixing the common base composition and these post-added components with a low shearing force, the viscosity is reduced by cutting the binder added and swollen in step (i) or (ii). The quality such as flavor can be ensured without impairing the shape retention, which is an important factor in quality.
Mixing with a low shear force can be performed using a commercially available low shear mixer, high disperser or the like. Among these, a low shear high disperser is preferable because uniform mixing with a low shear force is possible, and the quality is particularly excellent. The low-shear and high-dispersing machine here means, except for a so-called static mixer, preferably a low shear of 3 m / s or less, more preferably 1 m / s or less, and a residence time on the basis of the peripheral speed (linear velocity). The apparatus is preferably capable of ensuring high dispersion and uniform composition in 60 seconds or less, more preferably 30 seconds or less.
Examples of the low shear high disperser include Vibro mixer (manufactured by Chilling Industry Co., Ltd.), hypermelt screw (manufactured by Kobe Steel Co., Ltd.), KRC kneader (Kurimoto Industry Co., Ltd.) and the like.

FIG. 1 is a process flow diagram showing an example of the manufacturing method of the present invention.
First, in the blending tank 1, two or more kinds of common composition components are mixed to perform step (i) of preparing a common base composition.
Next, step (ii) is performed in which the post-addition component of the dentifrice is added and mixed in the mixer 2 to obtain the dentifrice. Further, after preparing the common base composition without washing the compounding tank 1, the post-addition component of the dentifrice different from the previous one is added in the compounding machine 3, and mixed in the same manner to obtain a dentifrice.
On the other hand, the obtained common base composition is divided into two parts and transferred to the mixers 2 and 3, respectively. In each of the mixers 2 and 3, the post-addition component of each dentifrice is added to each common base composition. In addition, it is also possible to obtain a dentifrice by performing the step (ii) of mixing with a low shear force.
In addition, the number which divides | segments a common base composition can be suitably set according to the number of the types of dentifrice to be manufactured. Moreover, division | segmentation does not need to be equal and can be suitably set according to the quantity of the dentifrice to be manufactured.

  In both the steps (i) and (ii), the addition of equipment such as heating and cooling is eliminated and the heating and cooling time is reduced from the manufacturing time by performing the process at 40 ° C. or lower. preferable.

  Further, even if a vacuum degassing step is added before or after step (ii), or both, the same purpose can be achieved.

With the method for producing a dentifrice of the present invention, in the production of a plurality of dentifrices, the total production efficiency including the washing switching step is improved without impairing quality such as flavor, dispersibility, shape retention, and stability. be able to. That is, conventionally, the entire device has to be cleaned each time the type of dentifrice to be produced is switched. However, in the present invention, it is not necessary to clean the apparatus that performs the step (i) for preparing the common components even if the switching is performed, and only the portion of the apparatus that performs the step (ii) may be cleaned. Therefore, the work associated with the switching work is reduced as a whole, the multi-product manufacturing process is rationalized and labor-saving, and the total manufacturing efficiency is improved.
Furthermore, according to the present invention, it is possible to produce a necessary amount of a plurality of types of dentifrices from a certain amount of common components, and the flexibility in production planning is also improved.

Hereinafter, the present invention will be described in more detail with reference to quality evaluation methods and examples, but is not limited thereto.
<Quality evaluation method>
About the dentifrice manufactured in Examples 1-3 and Comparative Examples 1-2 mentioned later, sensory evaluation was performed according to the following reference | standard. The results are shown in Table 1.
[Flavor]
○: It has a good flavor as a dentifrice and is excellent in use feeling.
X: The flavor balance is lost as a dentifrice, and there is a problem in merchantability.
[Dispersibility]
In step (ii), sampling at 3 or more points from the outlet every time, viscosity (Tokyo Keiki Co., Ltd. BL type viscometer, No. 7 rotor, 20 rpm, 180 seconds), pH, specific gravity (specific gravity cup method) and liquid From the measurement results of the active ingredients by chromatography, the following criteria were used for evaluation.
◎: All items have a runout width of less than 1.5% ○: All items have a runout width of less than 3% ×: Any item has a runout width of 3% or more [shape retention]
Evaluation was performed using a specific method for use as a product.
The tube was placed on a toothbrush and the shape change at that time was evaluated according to the following criteria.
○: The cross-section is maintained in a circular to elliptical shape, and the dentifrice does not flow between the flocked parts.
X: The cross-section is less than the elliptical shape, and the dentifrice flows between the flocked parts.
[Stability]
The tube was filled and stored under the temperature conditions of 5 ° C., 25 ° C., 40 ° C., and 50 ° C., and the state after one month was observed and evaluated according to the following criteria.
○: Under any storage condition, moisture does not ooze out when the dentifrice is taken out from the tube onto the straw half paper.
X: Moisture exudes when the dentifrice is taken out from the tube onto the straw half paper under any or all storage conditions.

[Example 1]
According to the process flow diagram shown in FIG. 1, a dentifrice was produced by the following procedure.
First, a common base composition including the common composition components listed below was prepared using a unimixer (manufactured by Nippon Paulec Co., Ltd.) as the blending tank 1.
Common composition components: 37.5% by mass of sorbite aqueous solution (wetting agent), 0.19% by mass of sodium saccharin (sweetener), 29.0% by mass of ion-exchanged water, 5% by mass of thickening silica (thickening agent), silica polishing Agent (abrasive) 22.5% by mass, xanthan gum (binder) 0.63% by mass, sodium polyacrylate (binder) 1.0% by mass, propylene glycol 3.1% by mass, sodium lauryl sulfate ( Foaming agent) 1.1% by mass

Next, using the Vibro mixer (Chilling Industry Co., Ltd.) as a mixer 2 for the prepared common base composition, the following post-added components were added at a ratio of common base composition: post-added component = 8: 2. (Mass ratio) was added and continuously mixed at a peripheral speed of 0.2 m / s and a residence time of 30 s to obtain a dentifrice.
Post-addition components: sodium fluoride (active ingredient) 1.05% by mass, ε-aminocaproic acid (active ingredient) 0.15% by mass, tranexamic acid (active ingredient) 0.25% by mass, sodium lauryl sulfate (foaming agent) 3.0 mass%, fragrance component 5.0 mass%, ion-exchanged water 40.55 mass%, sorbite aqueous solution (wetting agent) 50 mass%

  About the obtained dentifrice, the said quality evaluation was performed. The results are shown in Table 1. As a result, it was confirmed that good results were obtained for any of the evaluation items. Among them, particularly good results were obtained in terms of dispersibility.

[Example 2]
A dentifrice having the same composition as in Example 1 was prepared by the following procedure.
First, in Example 1, a common base composition was prepared in the same manner except that it did not contain three components of xanthan gum (binder), sodium polyacrylate (binder), and propylene glycol.
Next, three components of xanthan gum (binding agent), sodium polyacrylate (binding agent), and propylene glycol were added to the after-addition component of Example 1 as a post-addition component, and Vibro Mixer (Cooling Industry Co., Ltd.) ) And continuously mixed at a peripheral speed of 0.4 m / s and a residence time of 30 s to obtain a dentifrice.
About the obtained dentifrice, the said quality evaluation was performed. The results are shown in Table 1. As a result, it was confirmed that good results were obtained for any of the evaluation items. Among them, particularly good results were obtained in terms of dispersibility.

[Example 3]
In Example 1, Example 1 was used except that a KRC kneader (Kurimoto Industry Co., Ltd.) was used instead of the Vibro mixer (Chilling Industry Co., Ltd.) and the mixture was continuously mixed at a peripheral speed of 2 m / s and a residence time of 10 s. A dentifrice was obtained in the same manner.
About the obtained dentifrice, the said quality evaluation was performed. The results are shown in Table 1. As a result, it was confirmed that good results were obtained for any of the evaluation items.

[Comparative Example 1]
In Example 1, a high shear type disperser (T / K homomic line flow (manufactured by Tokushu Kika Kogyo Co., Ltd.) was used instead of the Vibro mixer (Cooling Industry Co., Ltd.), and the peripheral speed was 12 m / s, A dentifrice was obtained in the same manner as in Example 1 except that the mixture was continuously mixed for a residence time of 5 s.
About the obtained dentifrice, the said quality evaluation was performed. As a result, since the shearing force at the time of mixing was strong, the effect of the binder was not sufficiently exhibited, and the shape retaining property could not be maintained, resulting in poor stability.

It is a process flow figure showing an example of a manufacturing method of the present invention.

Explanation of symbols

1 ... Mixing tank, 2 ... Mixer, 3 ... Mixer

Claims (1)

A method for producing two or more dentifrices containing an abrasive, a wetting agent, a foaming agent, a binder, a fragrance and water,
(I) A common base composition comprising at least two selected from the ingredients commonly contained in the two or more dentifrices among the abrasive, wetting agent, foaming agent, binder, perfume and water. A step of preparing
(Ii) Of the components contained in the dentifrice to be manufactured, the remaining components not blended in (i) above are added to the common base composition obtained in (i) above and mixed with low shearing force. A method for producing a dentifrice comprising the steps of:

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