WO2006003989A1

WO2006003989A1 - Dentifrice composition

Info

Publication number: WO2006003989A1
Application number: PCT/JP2005/012075
Authority: WO
Inventors: Susumu Hiratsuka; Takaaki Komatsu; Takashi Yamamoto
Original assignee: Lion Corporation
Priority date: 2004-07-06
Filing date: 2005-06-30
Publication date: 2006-01-12
Also published as: KR101169939B1; JPWO2006003989A1; CN1988876B; KR20070028512A; CN1988876A; JP4702561B2

Abstract

A dentifrice composition which comprises (A) heavy calcium carbonate having a mean particle diameter of 5 to 15μm, (B) water-insoluble inorganic granules having a collapse strength of 10 to 200g/granule, a mean particle diameter of 50 to 150μm, and a difference of 100μm or below between 90% particle diameter and mean particle diameter, and (C) a water-soluble polymeric material comprising at least one member selected from Group (a) and at least one member selected from Group (b) at a (b)/(a) mass ratio of 0.25 to 3, Group (a): sodium alginate, sodium carboxymethylcellulose, methylcellulose, hydroxyethylcellulose, Xanthomonas campestris, λ-carrageenan, and straight-chain sodium polyacrylate, and Group (b): gellan gum, agar, κ-carrageenan, ι-carrageenan, gelatin, pectin, and crosslinked sodium polyacrylate, and which has a total content of (a) and (b) of 0.5 to 1.5% by mass based on the whole of the composition.

Description

Dentifrice composition

Technical field

TECHNICAL FIELD [0001] The present invention relates to a dentifrice composition having an appropriate polishing force and having an excellent feeling of use due to a synergistic effect of granule brushing and excellent dentifrice dispersibility.

Background art

[0002] The polishing power of a dentifrice composition is considered to have a correlation with the hardness, particle size, and blending amount of the abrasive used. That is, relatively soft (a Mohs hardness of 2 to 3) Abrasives such as calcium hydrogen phosphate can be incorporated into a dentifrice composition in a relatively large amount. . However, in the case of a relatively hard abrasive such as caustic anhydride (Mohs hardness around 4-6), the particle size can be reduced and only a small amount can be blended.

[0003] On the other hand, the hardness, particle size and blending amount of the abrasive have a great influence on the feeling of use of the dentifrice composition. That is, the feeling of use (a feeling of brushing, dispersibility, etc.) of a dentifrice composition containing an abrasive having a large particle size and a dentifrice composition containing a large amount of abrasive is good. However, the feeling of use of a dentifrice composition containing an abrasive with a small particle size and a dentifrice composition with a small amount of abrasive was required to improve the feeling of use due to poor brushing and dispersibility. . In other words, a dentifrice composition containing a large amount of calcium hydrogen phosphate having a large particle size is a dentifrice composition having an appropriate polishing power and a good feeling of use, whereas an anhydrous case having a small particle size. In the case of adding an acid to the dentifrice composition, it was necessary to consider improving the feeling of use in order to have an appropriate polishing power.

[0004] Until now, measures have been taken to optimize the polishing power of the dentifrice composition and improve the feeling of use at the same time by incorporating specific granules into such a dentifrice composition (Japanese Patent Laid-Open No. 04 243816). JP, 09-12436, JP 10-36236, JP 10-316547). However, with these proposals, the disintegration strength of the blended granule is weak, and the granule disintegrates instantly during brushing. Therefore, it is difficult to maintain a good feeling during use of the toothpaste.

[0005] In addition, when the disintegration strength of the granules is increased (JP 2002-68947 A, JP 2002-2) 55770 gazette, JP 2003-128528 gazette) Although the feeling of use during dentifrice behavior can be maintained, like the abrasive, the particle size of the granule is set in detail to make the abrasive power appropriate. There is a need. In this case, when the particle size is increased or the blending amount is the same as that of the abrasive, a foreign material sensation occurs.

[0006] Heavy calcium carbonate is a relatively inexpensive abrasive, and its use has cost merit, but it is an abrasive that is relatively hard with a Mohs hardness of around 3 to 4, so it is suitable for polishing. In order to set a dentifrice composition having strength, it was necessary to reduce the particle size and to reduce the blending amount. Therefore, a dentifrice composition containing heavy calcium carbonate as an abrasive has been required to improve the feeling of use due to poor feeling of brushing and dispersibility. Disclosure of the invention

Problems to be solved by the invention

[0007] The present invention has been made in response to a strong demand, and an object of the present invention is to provide a heavy calcium carbonate-containing toothpaste composition having an appropriate polishing power and good usability. Means for solving the problem

[0008] As a result of intensive studies to achieve the above object, the present inventor combined heavy calcium carbonate with an average particle diameter controlled to 5 to 15 m as an abrasive so as to obtain an appropriate polishing force. Water-insoluble inorganic granules having a disintegration strength of 10 to 200 gZ, an average particle size of 50 to 150 111, and a difference between the 90% particle size and the average particle size of 100 m or less. In addition, it can give a brushing feeling to the dentifrice, and at least one water-soluble polymer substance selected from the group (a) below and at least one kind selected from the group (b) below. By blending with a water-soluble polymer substance at a specific mass ratio and the total blending amount within a specific range, the dispersibility of the dentifrice is improved, and the brushing feeling of the dentifrice is further improved. Therefore, it has an appropriate polishing force and has a good feeling of use such as toothpaste dispersibility, brushing feeling and foreign body feeling, and toothpaste behavior. It was found that a dentifrice composition having a good feeling in use can be obtained.

Therefore, the present invention provides

(A) Heavy calcium carbonate with an average particle size of 5 to 15 μm

(B) 10-200 gZ disintegration strength, 50-150 111 average particle size, and 90% particles Water-insoluble inorganic granules whose difference between the diameter and the average particle diameter is 100 μm or less

(C) Mass ratio of at least one water-soluble polymer substance selected from the following (a) group power and at least one water-soluble polymer substance selected from the following (b) group: (b) Group Z (a ) Group = 0.2--3 Water-soluble polymeric substances

Group (a) water-soluble polymeric substances: sodium alginate, sodium carboxymethyl cellulose, methyl cellulose, hydroxyethyl cellulose, xanthan gum, λ-power lagin, nan, linear sodium polyacrylate

(b) Group of water-soluble polymer substances: dillanglan gum, agar, κ-powered laginane, _t carrageenan, gelatin, pectin, cross-linked sodium polyacrylate

Characterized in that 0.5 to 1.5% by mass of the total amount of the water-soluble polymer materials of group (a) and group (b) of component (C) is combined. Dentifrice composition

I will provide a.

The invention's effect

[0010] The dentifrice composition of the present invention has an appropriate polishing power and has an excellent feeling of use due to a synergistic effect of the brushing feeling of granules and excellent dentifrice dispersibility.

BEST MODE FOR CARRYING OUT THE INVENTION

[0011] The dentifrice composition of the present invention comprises (A) heavy calcium carbonate, (B) water-insoluble inorganic granules, and (C) a water-soluble polymer substance.

Here, as the heavy calcium carbonate of component (A) to be blended as an abrasive, those having an average particle size of 5 to 15 m, preferably 7 to 13 μm are used. If the average particle size is too small, the tooth cleaning effect, which is the basic function of the dentifrice, cannot be sufficiently obtained, and the excellent feeling of use cannot be obtained due to poor dispersibility of the toothpaste. If the average particle size is too large, an unpleasant sensation may cause discomfort and the polishing power may be too high.

The average particle diameter is a value measured with a Microtrac particle size distribution analyzer (Model 7995 10, Type SRA, manufactured by Nikkiso Co., Ltd.), and is a value measured by adjusting the turbidity (dV value) of the specimen to 0.5. is there.

[0013] (A) The amount of calcium carbonate component, the total composition of 5-50% (wt ^_0/0, the same below), it is desirable particularly from 15% to 45%. If the blending amount is less than 5%, the dentifrice In some cases, the basic function of cleaning the teeth cannot be sufficiently obtained, and the dispersibility of the toothpaste is deteriorated, so that an excellent feeling of use cannot be obtained. If the blending amount exceeds 50%, the polishing power of the dentifrice may become excessively high as well as causing discomfort if a foreign body is felt.

[0014] As the heavy calcium carbonate used in the present invention, commercially available heavy calcium carbonate can be used, and examples are shown below, but the manufacturer, commodity, and grade are limited thereto. It is not something.

Heavy calcium carbonate [Heavy calcium carbonate RTT—21 (Bihoku Powder Co., Ltd .: average particle size 7-10 / ζ πι), Heavy calcium carbonate RTT—69 (China: Average particle size 8-13 / ζ πι), Whiteon F (manufactured by Shiraishi Calcium Co., Ltd .: average particle size 11-15 m)]

The component (B) blended in the present invention has a disintegration strength of 10 to 200 gZ, an average particle size of 50 to 150 μm, and a difference between the 90% particle size and the average particle size of 100 μm. m or less water-insoluble inorganic granules. As the water-insoluble inorganic granules, those produced by various methods can be used. For example, water-insoluble inorganic agglomerates are produced by pulverizing or water-insoluble inorganic powders are mixed with water to form a slurry and pressure. It can be granulated, dried and formed into granules. Other production methods include a compression molding method, an extrusion molding method, a spray drying method, a sintering method, and the like. The water-insoluble inorganic granules to be blended in the present invention are those produced by any method. Although it can be used, it was produced by the method of pulverizing the water-insoluble inorganic agglomerates described above, the method of adding water to a water-insoluble inorganic powder to form a slurry, granulating and drying by applying pressure. Granules are preferred.

[0016] Here, in the case of producing granules by a method of pulverizing the water-insoluble inorganic agglomerate, adding water to a water-insoluble inorganic powder to form a slurry, and applying pressure to granulate and dry, granules are dried. Examples of the agglomerates and water-insoluble inorganic powders include dicalcium phosphate, triphosphate, insoluble calcium metaphosphate, anhydrous caustic acid, aluminum hydroxide, magnesium phosphate, bengara, calcium carbonate (heavy Or light calcium carbonate), calcium pyrophosphate, zeolite, aluminosilicate, magnesium carbonate, zirconosilicate, calcium sulfate, titanium oxide, aluminum oxide, and mixtures of these. The main water-insoluble inorganic powders that occupy 70% by mass or more and 100% by mass or less of the water-insoluble inorganic granule, especially the anhydrous zeal and zola Those bets, selected calcium carbonate mosquito ゝ al The water-insoluble inorganic powder occupying 0 mass% or more and less than 30 mass% of the water-insoluble inorganic granule is particularly titanium oxide or aluminum oxide. Is preferred.

[0017] As the water-insoluble inorganic agglomerates and water-insoluble inorganic powders used in the present invention, commercially available water-insoluble inorganic powders can be used, and examples are shown below. And the grade is not limited to this.

Caustic anhydride [Keic anhydride RTK-133 (manufactured by Taki Chemical Co., Ltd.), Toxeal (manufactured by Tokuyama Co., Ltd.)] Zeolite [COLITE- P (manufactured by COSMO), Toyobuilder (manufactured by Tosohichi Co., Ltd.), Shilton B (Mizusawa (Made by Chemical Industries)

Calcium carbonate (heavy) [Heavy calcium carbonate RTT-21 (manufactured by Bihoku Powder Chemical Co., Ltd.), heavy calcium carbonate RTT-69 (manufactured in China), Whiteon F (manufactured by Shiraishi Calcium Co., Ltd.)]

Calcium carbonate (light) [Poakaru N (manufactured by Shiroishi Calcium)]

[0018] In addition, the water-insoluble inorganic granules are adsorbed on the surface and blended with organic and inorganic surface coating agents and medicinal components, colorants, fragrance components and other excipients generally used in dentifrice. Monkey.

Commercially available products can be used as the water-insoluble inorganic granules used in the present invention. Examples are shown below, but the manufacturer, products, and grades are not limited thereto. Caustic anhydride granules [BFG-50 (INEOS), Micropearl (Rhodia)] Zeolite granules [COLITE-G (COSMO)]

Calcium carbonate granules [NL-K100 (New Lime Research)]

[0019] As described above, the water-insoluble inorganic granules used in the present invention have a disintegration strength of 10 to 200 gZ, preferably 20 to LOOgZ. Granules with a disintegration strength of less than 10gZ may not have an excellent feeling of use due to the disintegration at the start of brushing, and condylar particles with a disintegration strength of more than 200gZ may cause foreign body sensation and discomfort in the oral cavity. . When the disintegration strength is 20 to: LOOgZ, a very excellent feeling of use is obtained from the beginning of dentifrice, and the feeling of use lasts throughout the dentifrice action, so this is a preferable range.

[0020] It should be noted that the disintegration strength is the measured value of the automatic breaking strength of 30 granules (the load when the granules disintegrate when one granule is compressed under the conditions of a plunger diameter of 10 mm and a compression speed of lOmmZ. The measured value. ) Average value.

[0021] The water-insoluble inorganic granule has an average particle size of 50 to 150 µm, preferably an average particle size of 80 to 120 µm. Granules with an average particle size of less than 50 μm do not give a good feeling of use, and granules with an average particle size of more than 150 m may cause a foreign body sensation or discomfort in the oral cavity. When the average particle size is 80 to 120 m, a very excellent feeling of use with no foreign matter or discomfort is obtained from the beginning to the end of dentifrice.

[0022] Further, the water-insoluble inorganic granule has a difference between the 90% particle size and the average particle size of 100 μm or less, and preferably the difference between the 90% particle size and the average particle size is 70 μm. m or less. The difference between the 90% particle size and the average particle size is a factor that has a large influence on the particle size distribution of the granules, and in the case of granules whose difference between the 90% particle size and the average particle size exceeds 100 m, May cause a foreign body sensation or discomfort. When the difference between the 90% particle size and the average particle size is 70 μm or less, it is preferable that a feeling of foreign matter and discomfort are completely eliminated from the beginning to the end of dentifrice. The lower limit of the difference between the 90% particle size and the average particle size is 0 μm or more.

[0023] The average particle diameter and the 90% particle diameter are measured values (m) measured using a microtrack particle size distribution measuring apparatus, that is, an apparatus using a particle size distribution measuring method based on the laser diffraction diffraction method. In the present invention, it is a measurement value measured by adjusting the turbidity (dV value) of the sample to 0.5 using a Model7995-10, Type SRA manufactured by Nikkiso Co., Ltd.

[0024] It is desirable that the water-insoluble inorganic granules used in the present invention have low physical abrasiveness. The RDA (Radioactive Dentin Abrasion) value for evaluating the abrasiveness of the granules is 30 or less, particularly 0 to 15. Preferably there is. If the RDA value exceeds 30, the polishing power of the dentifrice may become too high depending on the amount of granules.

[0025] The blending amount of the water-insoluble inorganic granules of the component (B) is preferably 0.1 to 20%, particularly preferably 0.5 to 10% of the entire composition. If the blending amount is less than 0.1%, an excellent feeling of use may not be obtained. If the blending amount exceeds 20%, a foreign body sensation or discomfort may occur in the oral cavity.

[0026] Further, in the present invention, as component (C), group (a) (sodium alginate, carboxymethyl) Cellulose sodium, methenorescenellose, hydroxyethyl cellulose, xanthan gum, λ-carrageenan, linear sodium polyacrylate) At least one water-soluble polymer selected from group (b) (Gilan gum, agar) , Κ-carrageenan, _t -carrageenan, gelatin, pectin, cross-linked sodium polyacrylate) and a mass ratio of (b) group to (b) group is 0. Mix in the range of 25-3.

[0027] The water-soluble polymer substance of group (a) in this case is generally a viscous solution in the form of an aqueous solution having a water-soluble polymer substance concentration of 1% and a propylene glycol concentration of 3%. It is a water-soluble polymeric substance that does not have gelling ability, and is sodium alginate, sodium carboxymethyl cellulose, methyl cellulose, hydroxyethyl cellulose, λ-force laginan, linear sodium polyacrylate, and at least one selected from xanthan gum. It is a seed. Preferably, at least selected from sodium alginate, sodium carboxymethylcellulose, and xanthan gum in that they do not inhibit the effect of the water-soluble polymer substance of group (b) that has a great influence on the feeling of use of the dentifrice composition (especially dentifrice dispersibility). One type.

[0028] In addition, the water-soluble polymer substance in group (b) is generally a water-soluble polymer substance having a gelling ability in an aqueous solution having a water-soluble polymer substance concentration of 1% and a propylene glycol concentration of 3%. It is a high molecular weight substance, and is at least one selected from dielan gum, agar, κ-strength laginan, _t- strength laginan, gelatin, pectin, and cross-linked sodium polyacrylate. Preferably, in terms of the feeling of use of the dentifrice composition (especially the dentifrice dispersibility), it is at least one selected from kappa laginane and cross-linked sodium polyacrylate.

[0029] It should be noted that xanthan gum is a water-soluble polymer substance having a gelling ability in the state of an aqueous solution having a water-soluble polymer substance concentration of 1% and a propylene glycol concentration of 3%. It is rich in elasticity and, as is clear from the results of the experimental examples described later, shows different results from the water-soluble polymer substance in group (b), and was classified as a water-soluble polymer substance in group (a).

[0030] As the water-soluble polymer substance used in the present invention, commercially available water-soluble polymer substances can be used, and examples are shown below, but the manufacturer, product, and grade are limited thereto. It is not a thing. (a) group of water-soluble polymeric substances;

Sodium alginate [(Kimi force Algin (made by Kimiki Co., Ltd .: Viscosity (2% · 25 ° C · BL type · Νο. 3 · 1 2rpm) 2500-3500mPa 's), Duck Algin (Kibun Food Chemifa Co., Ltd .: Viscosity ( 2% · 25 ° C · BL type · No. 3 · 12rpm) 2500 to 3500mPa · s)]

Sodium carboxymethylcellulose [CMC Daicel (Daicel Chemical Industries, Ltd .: Viscosity (2% · 25. · Type · Νο. 2-20rpm) 100 ~ 1500mPa-s, etherity degree 0.8 ~ 1.5), Ernest Gum (Daicel Engineering Co., Ltd .: Viscosity (1% · 25 ° C · BH type · No. 2 · 20rpm) 100 ~ 1000mPa's, degree of etherification 1.5 or more), Sunrose F10LC (Nippon Paper Industries, Ltd.) : Viscosity (2% '25 ° C 'BH type · Νο. 5' 20rpm) 30-60mPa's, degree of etherification 0.5-1.0), Serogen (Daiichi Kogyo Seiyaku Co., Ltd .: Viscosity (1% '25 ° C 'BH type · Νο. 2- 20rpm) 100 ~ 1000mPa's, etherification degree 1.0 or more)]

Methylcellulose [(Metros SM (manufactured by Shin-Etsu Chemical Co., Ltd .: Viscosity (2% · 20 ° C · BH type · No. 2-20rpm) 150 ~ 4000mPa-s)]

Hydroxyethyl cellulose [HEC Daicel (Daicel Chemical Industries, Ltd .: Viscosity (1% · 25. C, BH type · Νο. 3, 30rpm) 2400 to 3000mPa, s, methoxykyl group 26.0 to 33.0% )

]

Lambda Nansen [GENUVISCOtypeCSM-2 (CP Kelco: Viscosity (2% · 25 ° C · BH type · 型 ο. 3-20rpm) 1000 ~ 4000mPa-s)]

Linear sodium polyacrylate [Alonbis S (Nippon Pure Chemicals Co., Ltd .: Viscosity (2% · 25 ° C · BH type • No. 2-20rpm) 100 ~ 2000mPa-s)]

Xanthan gum [Monato Gum DA (CP Kelco: Viscosity (pharmaceutical additive standard) 1300 to 1700mPa.s), Keldent (CP Kelco: Viscosity (medicine supplement) 1200 to 1700mPa.s)]

(b) group of water-soluble polymeric substances;

Jielan gum [(G-100 (Kibun Food Chemifa Corporation: Jelly strength (JIS K-6503) 100-750g)]

Agar [Inager (Ina Foods Co., Ltd .: Jelly strength CFIS K-6503) 200-800g)] Kappa Lagnan [GENUGELtvpeWR (CP Kerco: Viscosity (2% · 25 ° C · BH type · No. 7. 20rpm) 4000 ~ 15000mPa-s)]

i—Carrageenan [GENUVISCO RBK— 19 (manufactured by Kelco: Viscosity (1% '25 ° ○ ': 6 H type · Νο. l-60rpm) 20-60mPa-s)]

Gelatin [Natsubi Gelatin (manufactured by Futsubishi: Jelly strength (JIS K-6503) 225-250g)] Pectin [GENUpectinLM-85AS (CP Kelco: Genoré strength (Cotrol method 0339- 01, Copenhagen Pectin) 19-23% SAG)]

Cross-linked sodium polyacrylate [Rheology 250H (Nippon Pure Chemicals Co., Ltd .: Viscosity (0.5%-25 ° C · BH type · No. 5 · 20rpm) 7500 to 11 OOOmPa · s)]

[0031] The method for preparing the aqueous polymer solution and the method for measuring the viscosity when measuring the above-described viscosity are as follows.

6. Disperse water-soluble polymer in propylene glycol equivalent to 7%, and add purified water of each set temperature to each concentration in this dispersion at a time, in a constant temperature water bath set to each temperature. Then, use a propeller stirrer (3 blades, 25mm long with 2 blades) and stir at 1500 rpm for 10 minutes to prepare a water-soluble polymer aqueous solution.

After the adjustment, measure the viscosity after 3 minutes at each rotational speed using the viscometer of each model and the rotor of each rotor number exactly 1 minute later.

The order in which the measurement conditions are described is (concentration of aqueous solution, measurement temperature, viscometer type, rotor number, rotation speed).

[0032] The jelly strength and gel strength described above are measured values using a rheometer CR-200D manufactured by Sun Scientific.

[0033] In addition to the water-soluble polymer substance in group (b), another water-soluble polymer substance that has been subjected to gelation treatment such as heating, addition of a metal salt, pH adjustment, etc. It can be used as a water-soluble polymer substance belonging to It is also possible to use other water-soluble polymer substances as the water-soluble polymer substance in the group (a) that do not have the same gelling function as the water-soluble polymer substance in the group (a).

[0034] In the present invention, at least one water-soluble polymer substance in group (a) and at least one water-soluble polymer substance in group (b) are used in combination. (b) Group mass ratio ((b) Group Z (Group a)) is set between 0.25 and 3, preferably between 0.3 and 2 It is desirable. When the mass ratio of the (b) group to the (a) group is less than 0.25, the dispersibility of the dentifrice composition is reduced and an excellent feeling of use cannot be obtained, and when it exceeds 3, the (b) group Gelling ability, which is a characteristic of water-soluble high-molecular substances, affects the properties immediately after the preparation of the dentifrice composition, and easily causes water separation. When the mass ratio of the group (b) to the group (a) is between 0.3 and 2, it is more preferable because the influence of other compounding ingredients is extremely small on the feeling and stability of the dentifrice composition. It becomes a range.

[0035] In addition, as a method for evaluating the water separation phenomenon in the properties immediately after the manufacture of the above dentifrice composition, a tube laminated with aluminum foil, a plastic multilayer tube, a pump dispenser, a bottle container, etc. are filled. Extrude the toothpaste composition immediately after production onto straw half paper (Oji Paper Co., Ltd.) for about 15 cm, and after 1 minute, use a method to check for liquid oozing from the back side of the straw half paper. Is evaluated as a “water separation phenomenon”.

[0036] The total amount of the water-soluble polymer substances in the groups (a) and (b) is 0.5 to 1.5% of the entire composition, preferably 0.9 to 1.4. %. When the total amount of water-soluble polymer substances in groups (a) and (b) is less than 0.5%, water separation easily occurs in the properties immediately after the dentifrice composition is manufactured, and 1.5% If it exceeds 1, the dispersibility of the dentifrice composition decreases, and an excellent feeling of use cannot be obtained. When the total amount of water-soluble polymer substances is between 0.9 and 1.4%, the influence of other compounding ingredients on the feel and stability of the dentifrice composition is extremely small. This is a more preferable range.

[0037] The dentifrice composition of the present invention can be prepared into a dentifrice such as a toothpaste, a liquid dentifrice, and a moisturized dentifrice, and various base components used depending on the dosage form can be blended. it can. For example, abrasives other than heavy calcium carbonate, binders other than those described above, thickeners, foaming agents, sweeteners, fragrances and the like can be formulated at ordinary doses within the range that does not interfere with the effects of the present invention.

[0038] As the abrasive, other than heavy calcium carbonate, an abrasive usually blended in a dentifrice composition can be used. Specifically, an anhydrous carboxylic acid type such as silica gel, precipitated silica, aluminosilicate, zirconosilicate, etc. Abrasives, light calcium carbonate, dibasic calcium phosphate dihydrate and anhydrous, calcium pyrophosphate, aluminum hydroxide, alumina, magnesium carbonate, tribasic magnesium phosphate, zeolite, zeolite zelate, triphosphate Karsiu , Hydroxyapatite, quaternary calcium phosphate, synthetic resin abrasives, and the like. The blending amount of these abrasives is preferably 10 to 60% of the entire dentifrice composition as a total amount including heavy calcium carbonate as the component (A).

[0039] In addition, the binder is not limited to the effects of the present invention, and other than the above water-soluble polymer substance, for example, an inorganic binder such as a thickening anhydride, bee gum, or labonite. At least one can be added. These blending amounts are preferably 0.01 to 10% of the entire composition.

[0040] As the thickening agent, at least one polyhydric alcohol such as glycerin, sorbit, ethylene glycol, propylene glycol, polyethylene glycol, polypropylene glycol, xylitol, manolecitol, and ratathitol can be blended (mixing amount is usually 1 to 1). 45%, particularly suitable 2-40%).

[0041] Examples of the foaming agent include sodium lauryl sulfate, sodium myristyl sulfate, sodium N-lauroyl sarcosinate, sodium N-myristol sarcosinate, sodium dodecylbenzene sulfonate, hydrogenated coconut fatty acid monoglyceride sodium monosulfate, lauryl sulfo Anionic surfactants such as sodium acetate, sodium α-olefin sulfonate, Ν-acyl glutamate such as sodium palmitoylglutarate, Ν-methyl Ν-acyl taurate such as sodium taurate, Cationic surfactants, sucrose fatty acid esters such as sucrose fatty acid ester and maltose fatty acid ester, sugar alcohol fatty acid esters such as maltitol fatty acid ester and latator fatty acid ester, alkylol amide, Polyoxyethylene sorbitan fatty acid esters such as oxyethylene sorbitan monostearate, polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil, fatty acid ethanolamides such as lauric acid mono- or diethanolamide, sorbitan fatty acid esters, polyoxyethylene higher alcohols Ether, polyoxyethylene polyoxypropylene copolymer, polyoxyethylene polyoxypropylene fatty acid ester, polyglycerin fatty acid ester Non-ionic surfactants such as pull mouth nick, 2-alkyl-Ν-carboxymethyl -Ν-Hydroxyethyl imidazolium betaine, Ν-lauryldiaminoethylglycine, Ν-myristyldiaminoethylglycine, etc. Ν-alkyldiaminoethylglycine or あるいは—At least one amphoteric surfactant such as sodium alkyl-1-hydroxyethylimidazoline betaine Seeds can be blended. The blending amount of the foaming agent is preferably 0.1 to 4% of the entire composition.

[0042] Examples of the fragrance ingredients include menthol, anethole, carvone, eugenol, limonene, n-decyl alcohol, citronellol, hi-TV neol, citronellyl acetate, cineol, linalool, ethyllinalool, ヮ -lin, timonore, Perfume such as spearmint oil, peno-mint oil, lemon oil, orange oil, sage oil, rosemary oil, cinnamon oil, pimento oil, cinnamon leaf oil, perilla oil, winter green oil, clove oil or eucalyptus oil alone Or they can be combined. The blending amount of the fragrance component is preferably 0.5 to 1.5% of the entire composition.

[0043] Further, at least one sweetener such as saccharin sodium, stepioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl hydrochalcone, perlartin, glycyrrhizin, thaumatin, and asparatylphenol-lanalanine methyl ester may be added. The blending amount of the sweetener is preferably 0.05 to 1% of the entire composition.

[0044] Further, the present invention includes phenolic compounds such as triclosan, hinokitiol, thymol, and piozole, and quaternary ammonium salts such as cetylpyridinum chloride, benzethonium chloride, and benzalkonium chloride. , Enzymes such as dextranase, mutanase, lysozyme, amylase, protease, lytic enzyme, superoxide dimustase (SOD), alkali metal monofluorophosphates such as sodium monofluorophosphate and potassium monofluorophosphate, sodium fluoride, fluoride Fluorides such as stannous, tranexamic acid, epsilon aminocaproic acid, allantoin, dihydrocholesterol, glycyrrhizic acids, glycyrrhetinic acid, glycephosphate, chlorophyll, sodium chloride, xylitol, zinc chloride, water-soluble Rinsani 匕合 product can Oubataekisu, chlorhexidine to chloro, vitamin A, vitamin B group, vitamin C, etc. vitamins and derivatives thereof such as vitamin E, be formulated at least one known active ingredient. The active ingredient can be blended in an effective amount within a range that does not interfere with the effects of the present invention.

[0045] As the colorant, at least one of Blue No. 1, Yellow No. 4, Green No. 3, titanium dioxide, alumina oxide and the like can be blended.

[0046] The dentifrice composition of the present invention is manufactured by a manufacturing apparatus capable of mixing under reduced pressure, and can be used by being filled into a tube laminated with aluminum foil, a plastic multilayer tube, a pump dispenser, a bottle container, or the like. . Example

Hereinafter, the present invention will be specifically described with reference to experimental examples, examples, and comparative examples, but the present invention is not limited to the following examples. In the following examples, the compounding amounts all indicate mass percentages.

[0048] [Experiment 1]

Dentifrices containing the ingredients shown in Table 1 were prepared, and the effects of granule formulation were evaluated on the polishing power and feeling of use (toothpaste dispersibility, brushing feeling, foreign body feeling) by the following methods. The results are shown in Table 1.

[0049] Abrasive power measurement method (RDA method);

In this experiment, polishing power was measured by the RDA method (1's place 0 to 4 were rounded down to 0, and 5 and above were rounded down to 5).

The RDA (Radioactive Dentin Abrasion) method is a method that uses a polishing tester to measure the radioactivity of a small amount of wear components by radiating neutrons to a person's extracted teeth, thereby improving the polishing performance. Is a measurement method for evaluating In ADA (American Dental Association), the dentin polishing value (RDA value) is 100 when calcium pyrophosphate is used as the standard substance. In ADA, the upper limit of RDA value by RDA method is 250 or less. In this experiment, an appropriate RDA value was set to 80-130 in consideration of further safety and sufficient cleaning power.

[0050] Feeling of use (dentifrice dispersibility at the start of brushing, feeling of brushing during dentifrice);

Regarding the feeling of use (dentistry dispersibility, brushing feeling), a sensory test by 10 expert panelists was conducted based on the following evaluation criteria in a relative evaluation with Comparative Example 1, and an average point power evaluation of 10 people was performed. It was.

5-level evaluation

5 points: considerably better than Comparative Example 1

4 points: better than Comparative Example 1

3 points: Same as Comparative Example 1

2 points: worse than Comparative Example 1

1 point: considerably worse than Comparative Example 1

Evaluation results : 4. Over 5 points and under 5 points

0: over 3.5 points, up to 4.5 points

△: Over 3 points, 3.5 points or less

X: 3 points or less

[0051] Feeling of use (foreign substance feeling during dentifrice behavior);

The sensory test by 10 expert panelists was performed by absolute evaluation based on the following evaluation criteria, and the average score of 10 people was evaluated for the foreign body sensation during dentifrice behavior.

3-level evaluation

3 points: I don't feel

2 points: feel a little

1 ^ ；: feel

Evaluation results

0: 2. Over 5 points, 3 points or less

△: 1. Over 5 points, 2.5 or less points

: 1 point or more and 1.5 points or less

[0052] Overall evaluation;

From the above evaluation results of polishing power and usability, comprehensive evaluation was performed according to the following criteria. Comprehensive evaluation

A: The polishing power is in the range of 80 to 130, the evaluation of the feeling of foreign matter is “◯”, and in the evaluation of the feeling of use (toothpaste dispersibility 'brushing feeling) If the rating is “◎”

○: Within the range of polishing power of 80 to 130, the evaluation of the feeling of foreign matter is “◯”, and in the evaluation of the feeling of use (toothpaste dispersibility 'brushing feeling) When the rating is “◯” or “○” and “◎”

: Polishing power is in the range of 80 to 130, and feeling of use (toothpaste dispersibility · brushing feeling · foreign matter feeling

) And there is at least one “△” rating

X: When polishing polish exceeds 30, or when there is at least one evaluation of “X” in the evaluation of the feeling of use (toothpaste dispersibility 'brushing feeling · foreign object feeling), or the property immediately after toothpaste manufacture Condition

In the case of “water separation”

[0053] As a method for evaluating the water separation phenomenon in the properties immediately after the manufacture of the toothpaste, the toothpaste immediately after manufacture filled in a tube laminated with aluminum foil, a plastic multi-layer tube, a pump dispenser, a bottle container, etc. is made with straw half paper (Oji Extruded about 15 cm above the paper (manufactured by Shinko Co., Ltd.), and after 1 minute, a method of confirming the liquid oozing from the back of the straw half paper was used.

Those with oozing were evaluated as “water separation phenomenon”.

[0054] The granules used in each example are as follows. As a method for producing granules, a production method (i) a method of pulverizing water-insoluble inorganic coagulum, a production method (ii) a method of adding water to a water-insoluble inorganic powder to form a slurry, and applying pressure to granulate and dry, a production method (iii) Other methods shall be used. Granule A: Caustic anhydride granule (INEOS BFG-10 production method (i))

(Disintegration strength 20gZ, average particle size 100 / ζπι, difference between 90% particle size and average particle size 50 μm)

Granule B: Caustic anhydride granule (INEOS BFG-10 production method (i))

(Disintegration strength 15gZ, average particle size 140 / ζπι, difference between 90% particle size and average particle size 30 μm)

Granules. ： Zeolite.Keic anhydride.Aluminum oxide mixed granule (COSMO RTK-142 production method (ii), zeolite 'Keic anhydride' acid-aluminum mixture ratio (mass ratio) = 16: 3: 1)

(Disintegration strength 150gZ, average particle size 80 / ζπι, difference between 90% particle size and average particle size 80 μm)

Granule D: Keic anhydride granule (Rhodia Micropearl production method (iii))

(Disintegration strength 5gZ, average particle size 70; ζΐη, difference between 90% particle size and average particle size 30 μΏΐ)

Granule Ε: Zeolite granule (COSITE COLITE-G production method (iii))

(Disintegration strength 250gZ, average particle size 90 / ζπι, difference between 90% particle size and average particle size 50 μm) Granule F: Caustic anhydride granule (INEOS BFG-10 production method (i))

(Disintegration strength 20gZ, average particle size 20; ζΐη, 30% difference between 90% particle size and average particle size)

Granule G: Caustic anhydride granules (INEOS BFG-50 production method (i))

(Disintegration strength 20gZ, average particle size 200 / ζπι, difference between 90% particle size and average particle size 50 μm)

Granule H: Caustic anhydride granule (INEOS BFG-50 production method (i))

(Disintegration strength 20gZ, average particle size 100 / ζπι, difference between 90% particle size and average particle size 150 / zm)

[0055] The disintegration strength, average particle size, and 90% particle size were measured as follows.

Method for measuring decay strength;

Immerse the granules in water, and after 60 seconds, remove them from the water, measure the load when the granules disintegrate when one granule is compressed under the conditions of a plunger diameter of 10 mm and a compression speed of lOmmZ. The measurements in 30 were averaged.

[0056] Average particle size and 90% particle size measurement method;

The average particle size and 90% particle size should be MICROTRACK particle size distribution analyzer (Model 7995-10, Type SRA, manufactured by Nikkiso Co., Ltd.) !, and the sample strength (dV value) force ^). 5 Measured after adjusting to (rounded down).

[0057] Furthermore, commercially available components can be used as the components used in the experimental examples. As heavy calcium carbonate and water-soluble polymer substances, the following were used (hereinafter the same)

) o

Heavy calcium carbonate:

Classification product (average particle size 25 μm) obtained by classifying RTT-21 made by Bihoku Powder Co., Ltd. using Turbo Classifier TC-15N made by Nissin Engineering Co., Ltd. (Classification conditions: Classification rotor FI NE, AUTO mode, True specific gravity of raw material ρ = 30.0 m, wind

(Quantity Q = 3.0M ³ Zm, rotation speed N = 1100rpm)

Chinese RTT—69 (average particle size 12 m)

RTT—21 made by Bihoku Powder Co., Ltd., Turboclassifier TC made by Nissin Engineering Co., Ltd. — Classification using 15N (average particle size 2 μm) (Classification conditions: Classification rotor FIN E, AUTO mode, true specific gravity of raw material p = 2.8 gZcm ³ , classification point D = 1.5 m, air volume Q

P P

(= 1. LM ³ Zm, rotation speed N = 8390 rpm)

Water-soluble polymer (Carboxymethylcellulose sodium):

CMC Daicel manufactured by Daicel Chemical Industries, Ltd. 1260 Viscosity (2% '25 ° C'BH type Νο. 2-20rp m) 920mPa's, Aethery degree 0.91

[table 1]

Comparison example

Components (¾)

1 2 3 4 5 6 7 8 9 10 1 1 Heavy carbonate or Renum

40

(Average particle size 25 μ πι)

Heavy carbonate or resum

Abrasive 40 40 40 40 40 40 40 40 40 (Average particle size 12 μ πι)

Heavy carbonate or resum

40

(Average particle size 2 μm)

Request 3

Granule B 3

Granule C 3

Yoritori D 3

Granule

Granule E 3

Granule F 3

Reliable G 3 Granule H 3 Water soluble

Calfo "xymethylcellulose

Polymer 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 Sodium

Substance

Base Increased viscosity anhydrous carboxylic acid 3 3 3 3 3 3 3 3 3 3 3 Lopyrenk 'Recall 3 3 3 3 3 3 3 3 3 3 3 Thickener

70% sorbic solution 25 25 25 25 25 25 25 25 25 25 25 Foaming agent Sodium lauryl sulfate 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Sweetener sodium saccharin 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Preservative "Chilling" 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 Fragrance 1 1 1 1 1 1 1 1 1 1 1 Water Residual Residual Residual Residual Residual Residual Residual Residual Residual Residual Total 100 100 100 100 100 100 100 100 100 100 100 Abrasive power RDA 120 160 80 125 120 130 120 130 120 125 125 Toothpaste dispersibility Δ X Δ Δ Δ Δ Δ X Δ Δ Feeling of use Brushing feeling ○ X Δ Δ Δ XXXXX Foreign matter feeling ○ X ○ ○ ○ ○ ○ ○ Δ Δ XX Total s ¥ XXX Δ △ Δ XXXXX From the results in Table 1, compared with Comparative Example 1 in which the average particle size of heavy calcium carbonate was set to 12 μm so as to achieve an appropriate polishing force In Comparative Example 2 in which the average particle size was increased, the polishing power In Comparative Example 3 where the average particle size was reduced, the feeling of toothpaste use (dispersibility, feeling of brushing) was remarkably deteriorated, and the basic functions of the dentifrice composition It was terrible that the cleaning power that was not sufficient. By adding the granules to Comparative Example 1, an attempt was made to improve the feeling of use, but it was not possible to obtain a satisfactory feeling of use with any of the granules. Among them, compared with Comparative Example 1, Comparative Examples 4 to 6 showed good results with a feeling of brushing out of the feeling of use. In Comparative Example 7, the disintegration strength was too weak, so that sufficient toothpaste dispersibility and a feeling of brushing were not obtained. In Comparative Example 8, since the breaking strength was too strong, there was a tendency for the polishing force to increase, and the feeling of use was too strong in the feeling of use, and a foreign object feeling was felt, making it unsuitable for comprehensive evaluation. . In Comparative Example 9, since the average particle diameter was too small, sufficient toothpaste dispersibility and a feeling of brushing were not obtained, which was inappropriate in the overall evaluation. In Comparative Example 10, since the average particle size was too large, the sense of use was too strong in the feeling of use, and a foreign object sensation was felt, which was inappropriate in the overall evaluation. In Comparative Example 11, the sense of use was too strong and a foreign object was felt, making it unsuitable for comprehensive evaluation.

[Experiment 2]

Next, by using the dentifrice composition of Comparative Example 4 having an appropriate polishing power, good brushing feeling and no foreign material feeling, a water-soluble polymer substance was examined, and the feeling of use (especially toothbrushing) Attempted to improve dispersibility.

[0061] The water-soluble polymer substances shown in Table 2 were uniformly dissolved in a 3% aqueous solution of propylene glycol under appropriate conditions in each water-soluble polymer substance to prepare a 1% solution. evaluated. Water-soluble polymer substances that were viscous solutions were classified as viscous polymer substances, and gelled water-soluble polymer substances were classified as gelling polymer substances. As the grouping, from the result of Experimental Example 3 described later, the viscous polymer substance and xanthan gum were classified as group (a), and the gelling polymer substance excluding xanthan gum was classified as group (b).

[0062] As the water-soluble polymer substance, the following commercially available ones were used.

(The same applies hereinafter).

Sodium carboxymethyl cellulose: CMC Daicel 1260 Viscosity (2% · 25 ° C · BH type · Νο. 2 '20rpm) 920mPa's, ethereal degree 0.91 Made by Daicel Chemical Industries Sodium alginate: Kimi Algin Viscosity (2% '25 ° C'BL type · Νο.3-12rpm) 330 OmPa-s

λ—Carrageenan: GENUVISCOtypeCSM-2 Viscosity (2% '25 ° C'BH type · Νο.3 · 20rpm) 2600mPa. s CP Kelco

Xanthan Gum: Monato Gum DA Viscosity (Pharmaceutical Additives Standard) 1388mPa's CP Kelco

Cross-linked sodium polyacrylate: Rheological 250H viscosity (0.5% '25 ° C'BH type · Νο. 5-20rpm) 8220mPa-s made by Nippon Pure Chemical Co., Ltd.

Gelatin: Nintendo gelatin Jelly strength (JIS K-6503) 235g

[0063] [Table 2]

[0064] [Experiment 3]

A dentifrice containing the ingredients shown in Tables 3 and 4 was prepared, and the effect of blending water-soluble polymer substances alone and in combination was determined from polishing power and feeling of use (toothpaste dispersibility, brushing feeling, foreign body feeling). evaluated. The results are shown in Tables 3 and 4. The evaluation method was in accordance with Experimental Example 1.

The mass ratio of group (b) to group (a) [the amount of water-soluble polymer substance in (b) group (%) / (a) group of water-soluble polymer substance (%)] This is also shown in Tables 3 and 4.

[0065] [Table 3] Comparison example

Component (%)

12 13 14 15 16 17 18 19 20 21 22 23 Heavy carbonate or Resium

Abrasive (average particle size 12 40 40 40 40 40 40 40 40 40 40 40 40 m)

Granule condyle ¾A 3 3 3 3 3 3 3 3 3 3 3 3 3

(a) 0.6 0.6 0.6

Sunatricum

Water soluble

Sodium alkoxide 1.2 0.6 0.6 0.6 Polymer

E-Carrageenan 1.2 0.6 0.6 0.6 Substance

Xanthan power 1.2 0.6 0.6 0.6

(b) Group of sodium polyacrylate

1.2 0.6 Water-soluble (cross-linked type)

High molecular

Seratin 1.2 0.6 Substance

Mass ratio of water-soluble polymer

(b) Group amount / (a) Group amount

Base Increased viscosity anhydrous carboxylic acid 3 3 3 3 3 3 3 3 3 3 3 3 Degree of high-end liquid recall 3 3 3 3 3 3 3 3 3 3 3 3

70% sorby's solution 25 25 25 25 25 25 25 25 25 25 25 25 Effervescent agent Sodium lauryl sulfate 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Sweetener Sodium saccharin 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Preservatives Fluorocarbon 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 Fragrance 1 1 1 1 1 1 1 1 1 1 1 1 Water Residual Residual Residual Residual Residual Residual Residual Residual Residual Total 100 100 100 100 100 100 100 100 100 100 100 100 Abrasive power RDA 125 125 125 125 125 125 125 125 125 Toothpaste dispersibility Δ Δ Δ Water separation Δ Δ Δ Δ Δ Δ Water separation Usage feeling Δ Δ Δ Phenomenon Phenomenon Δ Δ Δ Δ Δ Δ Phenomenon Sense ○ ○ ○ ○ ○ ○ ○ ○ ○ Total S Parity Δ Δ Δ XX Δ Δ Δ Δ Δ Δ X Table 4] Example Composition (%)

1 2 3 4 5 6 7 8 9 10 Heavy carbonate

Abrasive 40 40 40 40 40 40 40 40 40 40 (Average particle size 12 / im)

Granule A 3 3 3 3 3 3 3 3

Granule Granule B 3

Granules. 3 Calfo 'xymethyl cellulose

(a) Group 0.6 0.6 0.6 0.6 Sodium

Water soluble

Sodium alkoxide 0.6 0.6

High molecular

λ-Power Raki 'One Nan 0.6 0.6

Substance

Xanthan force 0.6 0.6

(b) Group of sodium polyacrylate

0.6 0.6 0.6 0.6 0.6 0.6 Water-soluble (cross-linked type)

High molecular

Ce 7th 0.6 0.6 0.6 0.6

Substance

Mass ratio of water-soluble polymer

1 1 1 1 1 1 1 1 1 1

(b) Group amount / ω group amount

Base Thickening anhydrous anhydrous 3 3 3 3 3 3 3 3 3 3 Render Recall 3 3 3 3 3 3 3 3 3 3 Thickener

70% Calebit solution 25 25 25 25 25 25 25 25 25 25 Foaming agent Sodium lauryl sulfate 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Sweetener Sodium saccharin 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Antiseptic agent 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 Fragrance 1 1 1 1 1 1 1 1 1 1 Water Residual Residual Residual Residual Residual Residual Residual Residual Total 100 100 100 100 100 100 100 100 100 100 Abrasive power RDA 125 125 125 125 125 125 125 125 125 125 Toothpaste dispersibility ◎ ◎ ◎ ◎ 〇〇〇 ◎ Feeling of use and impression ◎ ◎ 〇〇〇 ◎ Foreign body sensation 〇〇〇〇〇 Overall evaluation ◎ © ◎ © 〇〇〇〇〇 From the results in Tables 3 and 4, it was found that in any case when water-soluble polymer substance was used alone, the overall evaluation could not exceed Comparative Example 4. Depending on the use of the same viscous polymer as in Comparative Example 4 (Comparative Examples 12-14), the feeling of use (dentist dispersibility) cannot be improved. The overall evaluation was stronger than Comparative Example 4. The use of gelling polymer materials different from those in Comparative Example 4 (Comparative Examples 15 and 16) caused water separation, and the overall evaluation was stronger than Comparative Example 4. In addition, xanthan gum, which is a gelling polymer material, had a tendency similar to that of a viscous polymer material with a water separation phenomenon.

When water-soluble polymer substances were used in combination at a ratio of 1: 1, the tendency was as follows. In the case of viscous polymer materials (Comparative Examples 17, 18, 20) and gelling polymer materials (Comparative Example 23), the results were the same as in the case of single use.

When xanthan gum is used as a gelling polymer substance and combined with a viscous polymer substance (Comparative Examples 19, 21, and 22), the feeling of use (dentist dispersibility) is not improved, and the overall evaluation is The force was not able to exceed Comparative Example 4. Based on the results of single use and combination use, xanthan gum was classified into group (a) for viscous polymer substances and xanthan gum and group (b) for gelling polymer substances excluding xanthan gum.

[0068] On the other hand, when a water-soluble polymer substance of group (a) and a crosslinked sodium polyacrylate as a gelling polymer substance are used (Examples 1 to 4), the feeling of use ( (Toothpaste dispersibility) was improved, and the overall evaluation was significantly higher than that of Comparative Example 4. The notable result here is that there is a synergistic effect that the brushing feeling is improved if the dentifrice dispersibility is significantly improved. When gelatin was used as the gelling polymer substance, the feeling of use (toothpaste dispersibility) was improved, and the overall evaluation exceeded that of Comparative Example 4.

[Experiment 4]

Next, the mass ratio between the water-soluble polymer substance in group (a) and the water-soluble polymer substance in group (b) and the appropriate range of the total amount of combination were examined.

[0070] A dentifrice composition containing the components shown in Tables 5 and 6 was prepared, and the mass ratio of the water-soluble high-molecular substances in the groups (a) and (b) [the water-soluble polymer substance in the (b) group] The amount (%) / (a) group of water-soluble polymer substance blending amount (%)] was evaluated from polishing power and feeling of use (dentist dispersibility, brushing feeling, foreign body feeling). The evaluation method was in accordance with Experimental Example 1.

[0071] [Table 5] Example Comparison Example Composition (%)

11 12 24 25 Heavy carbonate

Abrasive 40 40 40 40

(Average particle size 12 μm)

Granule Granule A 3 3 3 3

(a) High water solubility of group

Carboxy "xymethylol cellulose sodium 0.95 0.3 1 0.25 molecular substance

(b) Group water-soluble

Ho. Sodium acrylate (cross-linked) 0.25 0.9 0.2 0.95 Molecular substance

Mass ratio of water-soluble polymer

0.26 3 0.2 3.8 (b) Sho amount / (a) Group amount

Base Thickener Anhydrous carboxylic acid 3 3 3 3

70% sorbite solution 25 25 25 25 Foaming agent Sodium lauryl sulfate 1.5 1.5 1.5 1.5 Sweetening agent Sodium saccharin 0.2 0.2 0.2 0.2 Preservatives To chilling V 0.01 0.01 0.01 0.01 Fragrance 1 1 1 1 Water residue Residual residue Total 100 100 100 100 Abrasive power RDA 125 125 125 125 Dentifrice dispersibility 〇 © Δ

Water separation Feeling of actual use ◎ ◎ Δ

Phenomenon Feeling of foreign objects 〇〇〇 Overall parity 〇 ◎ Δ X Table 6]

Example Comparison Example Composition (%)

13 14 15 16 26 27 28 29 Heavy carbonate

Abrasive 40 40 40 40 40 40 40 40

(Average particle size 12 μm)

Granule Granule A 3 3 3 3 3 3 3 3

( _a ) Group water-soluble

Carboxy "xymethylcellulose sodium 0.8 0.25 1.1 0.35 0.36 0.12 1.26 0.4 Molecular substances

(b) Group water solubility

Sodium polyacrylate (cross-linked) 0.2 0.75 0.3 1.05 0.09 0.35 0.34 1.2 Polymer

Total amount of water-soluble polymer substance

1 1 1.4 1.4 0.45 0.47 1.6 1.6 ω Sho amount + (b) Sho S3 amount

Mass ratio of water-soluble polymer

0.25 3 0.27 3 0.25 2.92 0.27 3 (b) Group amount / (a) Group amount

Base Thickener Anhydrite 3 3 3 3 3 3 3 3 Propylene Daricol 3 3 3 3 3 3 3 3 Thickener

70% Calebit solution 25 25 25 25 25 25 25 25 Foaming agent Sodium lauryl sulfate 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Sweetening agent Sodium saccharin 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Antiseptic preservative 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 Fragrance 1 1 1 1 1 1 1 1 Water residue Residue Residue Residue Residual residue Total 100 100 100 100 100 100 100 100 Abrasive power RDA 125 125 125 125 125 125 Dentifrice dispersibility ○ ◎ ○ Δ Feeling of use Cleaning feeling ○ ◎ ○ ◎ Phenomenon Phenomenon Δ Δ Foreign object sensation ○ ○ ○ ○ ○ ○ Total evaluation ○ ◎ ○ ◎ XX Δ Δ Regarding the mass ratio of the water-soluble polymer substances in groups (b) and (b), those in which (a) group: (b) group = 1: 0.25 to 1: 3 were good. If there is too much water-soluble polymer in group (a), the dentifrice dispersibility will be poor and overall evaluation will be poor, and if there is too much water-soluble polymer in group (b), water separation will occur. The overall evaluation deteriorated.

In addition, regarding the total amount of the water-soluble polymer substances in the groups (a) and (b), 0.5 to 1.5% was satisfactory. If the total amount is too large, the dentifrice dispersibility will deteriorate and comprehensive evaluation will occur. In addition, when the total blending amount was too small, water separation phenomenon was caused and the overall evaluation deteriorated.

[Experiment 5]

The types of water-soluble polymer substances other than those shown in Table 2 were examined in the same manner as in Experimental Example 2.

[0075] The water-soluble polymer substances shown in Table 7 are classified into viscous polymer substances and gelling polymer substances in the same manner as in Experimental Example 2, and the viscous polymer substances are classified into group (a). The gelling polymer material was classified as (b) group.

[0076] As the water-soluble polymer substance, the following commercially available ones were used (the same applies hereinafter).

Methylcellulose: Metrows SM viscosity (2% '20 ° C'BH type · Νο.2-20rpm) 2400m Pa-s Shin-Etsu Chemical Co., Ltd.

Hydroxyethyl cellulose: HEC Daicel viscosity (1% '25 ° C'BH type Νο.3-30rp m) 2790mPa's, methoxykyl group 29.0% Made by Daicel Chemical Industries

Linear sodium polyacrylate: Alonbis S viscosity (2% '25 ° C'BH type · Νο.2-20rp m) 973mPa-s made by Nippon Pure Chemical Co., Ltd.

Jelang gum: G—100 Jelly strength (JIS K—6503) 635 g Kibun Food Chemifa Agar: Inagel Jelly strength CFISK— 6503) 603 g Ina Foods

κ—Carrageenan: GENUGELtypeWR Viscosity (2% '25 ° C'BH type · Νο.7.20rpm) 13560mPa-s CP Kelco

I—Carrageenan: GENUVISCO RBK-19 Viscosity (1% '25 ° C'BH type · Νο.1-6 Orpm) 32mPa-s CP Kelco

Pectin: GENUpectinLM—85AS Gel Strength (Copenhagen Pectin Cotrol Method 0339—01) 21% SAG CP Kerco

[0077] [Table 7] Water-soluble polymer substance 1% solution state Classification Group Cellulose Methyl cellulose Viscous solution Viscous polymer substance (a) Human "Loxocheil cellulose Viscous solution Viscous polymer substance (a) Group Sodium Liacrylate (Linear) Viscous solution Viscous polymer material (a) Group “Elan force crumbly brittle gel” (b) Agar Crab brittle gel Polymeric substances (b) group

K ichiraki rakininan sukui gel kelp polymerizing polymer (b) group

1-Karaki "Inan" Viscous gel chelating high molecular weight material (bW to cutin Viscous gel chelating high molecular weight material (b) group

[0078] A dentifrice containing the components shown in Table 8 was prepared, and the water-soluble polymer substance (b) Group Z content Z

(a) The effect of the combination blending ratio of 1: 1 in the group was evaluated from the polishing power and the feeling of use (toothpaste dispersibility, brushed feeling, foreign body feeling). The results are shown in Table 8. The evaluation method was the same as in Experimental Example 1.

[0079] [Table 8]

Example

Component (%)

17 18 19 20 21 22 23 24 Heavy carbonate

Abrasive 40 40 40 40 40 40 40 40

(Average particle size 12 μ ηι)

Granule mm 3 3 3 3 3 3 3 3

Calfo 'xymethyl cellulose

0.6 0.6 0.6 0.6 0.6

(a) Sodium in group

Water-soluble methylcellulose 0.6

High molecular weight human "Lochetyl cellulose 0.6

Substance Sodium sodium acrylate

0.6

(Linear type)

Sodium sodium acrylate

0.6 0.6 0.6

(Bridge type)

(b) group

Shiran force 0.6

Water soluble

Agar 0.6

High molecular

Kappa Raki 'Ichinan 0.6

Substance

Ichiraki Raki "Ichinan 0.6 Kuching 0.6 Water-soluble ftfe High molecular weight ratio

1 1 1 1 1 1 1 1

(b) Group amount / (a) Group amount

Base Increased viscosity anhydrous key acid 3 3 3 3 3 3 3 3

Propylene Daricol 3 3 3 3 3 3 3 3 Thickener

70% Calebit solution 25 25 25 25 25 25 25 25 Foaming agent Sodium lauryl sulfate 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Sweetening agent Sodium saccharin 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Antiseptic preservative 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01

Perfume 1 1 1 1 1 1 1 1 Water residue Residue residue Residual residue Residual residue 100 100 100 100 100 100 100 100 Abrasive power RDA 125 125 125 125 125 125 125 125

Dentifrice dispersibility ◎ ◎ ◎ ◎ 〇 ◎ 〇 Usability Feeling of cleaning ◎ ◎ ◎ ◎ ○ ◎ 〇〇

Foreign body sensation 〇〇〇〇〇〇〇

Overall evaluation ◎ ◎ ◎ ◎ 〇 ◎ 〇〇 Based on the results in Table 8, when water-soluble polymer substances shown in Table 7 are used, they are also shown in Table 2. The same effect as in the case of using a water-soluble polymer substance was confirmed.

[Example]

A dentifrice composition having the composition shown in Table 9 was prepared and evaluated in the same manner as in the above experimental example. As a result, it was confirmed that both had excellent polishing power and feeling of use.

[0082] As the heavy calcium carbonate, the following were used.

Classified product (average particle diameter 7 μm) obtained by classifying RTT-21 made by Bihoku Powder Co., Ltd. using Turbo Classifier TC-15N made by Nisshin Engineering Co., Ltd. (Classification conditions: Classification rotor FIN E, AUTO mode, True specific gravity of raw material p = 2.8gZcm ³ , classification point D = 9.0 m, air volume Q

P P

= 2.4M ³ Zm, rotation speed N = 3050rpm)

Chinese RTT—69 (average particle size 10 m)

Classification product of Chinese RTT-69 using Nisshin Engineering Co., Ltd. turbo classifier TC-15N (average particle size 13 μm) (Classification conditions: Classification rotor FINE, AUT O mode, true specific gravity of raw materials p = 2.8gZcm ³ , classification point D = 15.0 m, air volume Q = 3.0

P P

(M ³ Zm, rotation speed N = 2140 rpm)

[0083] Further, as the water-insoluble inorganic granule, the same granule A as described above and the following granules I to K were used: Granule I: Caustic anhydride granule (BFG-10 production method (i) manufactured by INEOS)

(Disintegration strength 30gZ, average particle size 95 / ζ πι, difference between 90% particle size and average particle size 45 μ ηι)

Condylar fistula: anhydrous silicate granules (manufactured by INEOS BFG-50 (i))

(Disintegration strength 45gZ, average particle size 120m, difference between 90% particle size and average particle size 70

： Zeolite / Keic anhydride / Aluminum oxide mixed granule (COSMO production method (ii), Zeolite / Keic anhydride / Acid / aluminum mixing ratio (mass ratio)) = 7: 2

: 1)

(Disintegration strength 35gZ, average particle size 90 m, difference between 90% particle size and average particle size 20 μΏΐ)

[0084] [Table 9] Implementation side

Components (%)

Heavy coal

(Average particle size

Abrasive Heavy coal Rushium

(Average particle size

Heavy coal

(Average particle size

Granule 7 2 Granule

Condyles

Granule

Calfo "xymethyl cellulose sodium

( _a ) Group of water-soluble arun if thorium

Polymeric Materials-Karaki "Nan

Xanthan power

Group (b) water-soluble sodium acrylate (cross-linked)

Polymer material / Isshiki La Ichinan

Total amount of water-soluble polymer substance

Group blend amount Group blend amount

Mass ratio of water-soluble polymer

2. 00

(b) Group amount / ω group amount

Base Viscosity anhydride

Frojlenk Cole

Ho Ethylenek Recall 3

Thickener

Sorbit solution 25

Xylit

Sodium lauryl sulfate

Lau Moutil Sarcosine Sodium

Blowing agent

Polyoxyethylene castor oil

Polyoxyethylene stearyl ether

Sweetener saccharin sodium

Hexa chloride rucoum

Antiseptic benzoin stt thorium

Fucilhahuhen

Sodium monofluorophosphate

Tranexam

£ -aminocapnic acid

Ohha "Quex

Sodium pyrophosphate

Active ingredient

Sodium phosphate

Aluminum lactate

Glassium

Triclosan

Cetylbilici chloride "um

Fragrance

Water Residual Residual Residual Residual Residual Residual Residual Residual Residual Residual Residual Total

Polishing power

Toothbrush dispersibility ® © © © © © © © ® Feeling of use Printing feeling Θ Θ Θ Θ Θ Θ Θ Θ Foreign object feeling 〇〇〇〇〇〇〇〇〇 Overall evaluation Θ Θ Θ Θ

Claims

The scope of the claims

[1] (A) Heavy calcium carbonate with an average particle size of 5 to 15 μm

(B) Water-insoluble inorganic granules having a disintegration strength of 10 to 200 gZ, an average particle size of 50 to 150 111, and a difference between the 90% particle size and the average particle size of 100 μm or less

(C) The following (a) water-soluble high molecular weight material with selected group power and the following (b) water-soluble high molecular weight material with selected group power in mass ratio: (b) group Z (a) group = 0.25--3 Water-soluble polymer substance

Characterized in that 0.5 to 1.5% by mass of the total amount of the water-soluble polymer materials of group (a) and group (b) of component (C) is combined. Toothpaste composition.

[2] The water-insoluble inorganic granule of component (B) is obtained by pulverizing a water-insoluble inorganic coagulum or granulating and drying the water slurry of a water-insoluble inorganic powder under pressure. The dentifrice composition according to claim 1 in the range.

[3] More than 70% by mass of the water-insoluble inorganic granule component of component (B) is anhydrous silicate and zeolite

The dentifrice composition according to claim 1 or 2, wherein the calcium carbonate power is selected.

[4] The blending amount of the heavy calcium carbonate as the component (A) is 5 to 50% by mass of the total composition, (B

The dentifrice composition according to any one of claims 1 to 3, wherein the blending amount of the water-insoluble inorganic granule as a component is 0.1 to 20% by mass of the whole composition.

[5] (C) Component (a) The water-soluble polymer substance selected for group strength is at least one of sodium alginate, sodium carboxymethyl cellulose, and xanthan gum, and the water-soluble polymer substance selected from group (b) is κ It is at least one kind of laginane, cross-linked sodium polyacrylate, and contains a water-soluble polymer substance at a mass ratio of (b) group Z (a) group = 0.3-2, The power of any one of claims 1 to 4, wherein the total amount of the water-soluble polymer substances in groups a) and (b) is 0.9 to 1.4% by mass of the total composition. Dentifrice composition as described / vu / O sz-oissooifcld 686εοο900ΝAV

Vain.