CN105828781B

CN105828781B - Dentifrice

Info

Publication number: CN105828781B
Application number: CN201380081774.5A
Authority: CN
Inventors: 吉田秀德; 松元树; 辻优希; 小野田惠一
Original assignee: Kao Corp
Current assignee: Kao Corp
Priority date: 2013-12-18
Filing date: 2013-12-18
Publication date: 2019-06-14
Anticipated expiration: 2033-12-18
Also published as: RU2681077C1; JPWO2015092885A1; RU2016128828A; CN105828781A; JP6324412B2; WO2015092885A1

Abstract

The present invention relates to one kind to be combined with dentifrice made of particle, wherein, the good granular sensation for being disintegrated and having no foreign body sensation occurs when loaded load in the oral cavity, 150 μm of width fine recess portions below as perikymata, nearly middle labial surface ditch, central median ridge and remote middle labial surface ditch portion of tooth etc. can be entered to, higher tartar removal ability or soil removal capabilities are played.The dentifrice is dentifrice made of being combined with the particle containing water-insoluble dusty material (A) and inorganic bond (B), in the particle after being present in the cooperation in the dentifrice, the area (S on the perspective plane of the particle_A) and with the maximum gauge (D in the perspective plane_L) as diameter circumscribed circle area (S_S) ratio (S_A/S_S) average value be 0.5 or more and 0.9 hereinafter, and the intensity of disintegration of particle after cooperating is 1gf/ or more and 20gf/ or less.

Description

Dentifrice

Technical field

The present invention relates to a kind of dentifrices.

Background technique

In recent years, it is known to cooperate just like can by become saprodontia or periodontosis the reason of tartar efficiently remove, and And easily discover the dentifrice of the particle of its effect.In order not to dental surface enamel or gum etc. cause to damage, these Grain is substantially made into spherical flocculated particle, has the particle containing functional materials such as medicament, enzyme agent, grinding agents or seeks it The particle of visual effect.

Adhesive as these particles, it is known to the water-soluble binders such as methylcellulose, carboxymethyl cellulose or wax Equal water-insolubles organic adhesive.In addition, it is also known that have addition using water-insolubles inorganic bonds such as colloidal silicon dioxides Make the dentifrice (referring to patent document 1) of the water-insolubles dusty material such as zeolite bonding and the particle of acquisition.

In addition, it is also known that have added with being manufactured by specific process using silicic acid anhydride using damp process (gel method) Spherical shape and the high silica dioxide granule of deformation rate dentifrice (referring to patent document 2).

Existing technical literature

Patent document

Patent document 1: Japanese Unexamined Patent Publication 1-299211 bulletin

Patent document 2: Japanese Unexamined Patent Publication 2010-275260 bulletin

Summary of the invention

The present invention relates to a kind of dentifrice, the dentifrice is cooperation containing water-insoluble dusty material (A) and inorganic Made of the particle of adhesive (B),

About the particle after the cooperation being present in the dentifrice, the area (S on the perspective plane of the particle_A) and with the throwing Maximum gauge (D in shadow face_L) be diameter circumscribed circle area (S_S) ratio (S_A/S_S) average value be 0.5 or more and 0.9 Hereinafter, and cooperate after particle intensity of disintegration be 1gf/ or more and 20gf/ or less.

Moreover, it relates to a kind of dentifrice, the dentifrice be cooperation containing water-insoluble dusty material (A) and Made of the particle of inorganic bond (B),

About the particle after the cooperation being present in the dentifrice, obtained by laser diffraction/scattering formula particle size distribution measuring In particle (a)~(d) below in size distribution obtained, the volume ratio (b/c) of the amount of the amount and particle (c) of particle (b) is 0.7 or more and 1.2 hereinafter, the volume ratio (d/c) of particle (d) and particle (c) be 0.2 or more and 1 hereinafter, the amount of particle (b) with The volume ratio (b/d) of the amount of particle (d) is greater than 1 and be 5 hereinafter, the amount of particle (c) in particle after cooperating is 15 volume % Above and 55 volume % hereinafter, and the particle after cooperating intensity of disintegration be 1gf/ or more and 20gf/ it is a hereinafter,

(a) partial size is 50 μm of particles more than and less than 100 μm；

(b) partial size is 100 μm of particles more than and less than 150 μm；

(c) partial size is 150 μm of particles more than and less than 200 μm；

(d) partial size is 200 μm of particles more than and less than 250 μm.

With the variation of dietetic life in recent years and living habit etc., the factor of the deterioration of internal environment of oral cavity is not caused also not It is disconnected to increase, therefore, it is easy to attach in diversified dirt, remain in dispersion there are perikymata (perikymata), The situation on the surface of the concave-convex tooth of all sizes such as labial surface ditch, central median ridge and remote middle labial surface ditch portion in close.Above-mentioned patent text There is the granule strength of the appropriateness for being easy disintegration although offering 1 particle, for dental surface is attached to that there are various For the dirt of the concave-convex dental surface of size sufficiently removes, still there is room for improvement.In addition, above patent document 2 Although particle deformation rate is higher, granular sensation is also excellent, for using in view of mitigating the soft tooth to the load of gum Also the dirt for the recess portion for being attached to all size of dental surface sufficiently removed under lesser load in the case where brush and Speech, there is room for improvement.Therefore, seek to be easily accessible to the dentifrice particle of the recess portion of such dental surface, as long as Cooperate dentifrice made of the particle, even if can then expect using in view of mitigating the soft tooth to the load of gum Also the removal ability of tartar or dirt can be improved under lesser load in the case where brush.

Therefore, the present inventors have carried out various researchs, as a result, it has been found that, as long as cooperation has special shape or spy Dentifrice made of different size distribution and particle with specific intensity of disintegration, then these particles interact one on one side While be easily accessible to the fine recess portion of tooth, even if thus under lesser load using soft toothbrush Higher tartar removal ability or soil removal capabilities can also be played.

Dentifrice according to the present invention, due to being combined with special shape or special size distribution and having Specific intensity of disintegration, the specific particle being disintegrated if loaded load form, therefore, good with no foreign body sensation Granular sensation, and particle enters to as perikymata, nearly middle labial surface ditch, central median ridge and remote middle labial surface ditch portion of tooth etc. 150 μm of fine recess portions below, so, can effectively transmit the load from toothbrush, and can by tartar or The dirts such as color dirt fully remove.It therefore, can also be with even if using the toothbrush of soft bristle (bristle) Load is effectively transmitted to fine recess portion, plays higher soil removal capabilities.

Detailed description of the invention

Fig. 1 has been expressed as obtaining the particle after the cooperation in the presence of the dentifrice of embodiment 2 and before the cooperation that uses Particle B's by laser diffraction/scattering formula particle size distribution measuring after cooperation in the presence of particle B' and the dentifrice of embodiment 2 The curve graph of the size distribution of acquisition.

Fig. 2 is the SEM photograph of particle B after cooperation in the presence of the dentifrice of embodiment 2.

Fig. 3 be after cooperation in the presence of the dentifrice for indicating comparative example 1 particle F by laser diffraction/scattering formula partial size The curve graph for the size distribution that measure of spread obtains.

The explanation of symbol:

X: the size distribution of particle B' before cooperating

Y: the size distribution of particle B after cooperation

Specific embodiment

Hereinafter, the present invention is described in detail.

Dentifrice cooperation of the invention with special shape or special size distribution and has specific intensity of disintegration Particle form.Particle after being present in the cooperation in the dentifrice is to contain water-insoluble dusty material (A) and inorganic viscous The particle of mixture (B), hereinafter also referred to " particle after cooperation ".On the other hand, in order to make in dentifrice, there are particles after the cooperation And it is matched with the particle in dentifrice hereinafter also referred to " particle before cooperating ".

It is preferably commonly used in the grinding agent of tooth as the water-insoluble dusty material (A), specifically, Preferably inorganic material.Here, " water-insoluble " refers to that (20 DEG C) of meltage relative to 100g water are 1g or less.It is specific and Speech, such as can enumerate selected from precipitated calcium carbonate, powdered whiting, zeolite, silica, calcium monohydrogen phosphate, calcium phosphate, insoluble It is one kind or two or more in property sodium metaphosphate, aluminium hydroxide, magnesium phosphate, calcium pyrophosphate and magnesium carbonate etc..These can be independent Using a kind, two or more use can also be combined.

In these water-insoluble dusty materials (A), following spies is assigned to particle after being present in the cooperation in dentifrice Different shape or special size distribution, even if load uses in the case where soft toothbrush lower load like that can also be with Higher soil removal capabilities are played, the dirts such as tartar or colored soil can sufficiently be removed, and tooth can be improved From the perspective of the smooth sense of touch and decontamination sense on surface, be preferably selected from precipitated calcium carbonate, powdered whiting, zeolite and It is one kind or two or more in silica, a kind further preferably in precipitated calcium carbonate and powdered whiting or 2 kinds, More preferably powdered whiting.Here, smooth sense of touch, which refers to, will not obtain when touching facing with tongue such as tartar or dirt The dirty sense of touch adhered to such sense of touch and tongue can be made to slide smoothly in dental surface, decontamination sense refers to can be certainly Feel that dental surface becomes smooth and dirt disappearance sense of touch.

About the average grain diameter of water-insoluble dusty material (A), from the viewpoint of tartar or dirt removal after intragranular disintegration It sets out, preferably 0.1 μm or more, further preferably 0.5 μm or more, more preferably 0.8 μm or more, more preferably 1 μm More than.In addition, from the viewpoint of reducing foreign body sensation, preferably 20 μm hereinafter, further preferably 15 μm hereinafter, more excellent 10 μm are selected as hereinafter, more preferably 5 μm or less.In addition, the average grain diameter of water-insoluble dusty material (A) is preferably 0.1 ~20 μm, further preferably 0.5~15 μm, more preferably 0.8~10 μm, more preferably 1~5 μm.

In addition, average grain diameter can be measured by the method recorded in embodiment.

About the content of water-insoluble dusty material (A), ground from the viewpoint and raising for realizing the behavior being slowly disintegrated It is after engagement in the dry state preferably 60 mass % or more, further preferably 70 matter in particle from the perspective of grinding power Measure % or more, more preferably 80 mass % or more, more preferably 82 mass % or more.About water-insoluble dusty material (A) content is preferably 98 matter in particle from the viewpoint of inhibiting to the damage of tooth in the dry state after engagement % is measured hereinafter, further preferably 96 mass % are hereinafter, more preferably 90 mass % or less.In addition, water-insoluble powder material The content for expecting (A) is preferably 60~98 amount % in particle in the dry state after engagement, and further preferably 70~96 Measure %, more preferably 80~96 mass %, more preferably 82~90 mass %.

After inorganic bond contained in particle (B) is due to making cooperation after cooperation in the presence of dentifrice of the invention There is gap in particle and combined with water-insoluble dusty material (A), therefore tartar can sufficiently be removed, and bring and mention The smooth sense of touch of high dental surface and the effect of decontamination sense.As inorganic bond (B), can enumerate selected from water-soluble nothing It is one kind or two or more in machine adhesive and water-insoluble inorganic bond.As water-soluble inorganic adhesive, specifically, 1 kind in sodium metasilicate, polyacrylic acid, modified cellulose class, polyvinylpyrrolidone and silicone etc. or 2 kinds can be enumerated More than, preferably sodium metasilicate.As water-insoluble inorganic bond, specifically, can enumerate selected from colloidal silicon dioxide, It is one kind or two or more in magnesium aluminometasilicate, synthetic aluminium silicate, calcium silicates and alumina sol etc., preferably colloid dioxy SiClx.Wherein, from the viewpoint of playing effect of the invention well, water-soluble inorganic adhesive is preferably comprised, into one Step preferably comprises sodium metasilicate.By being used as inorganic bond containing a kind or 2 kinds in sodium metasilicate and colloidal silicon dioxide (B), can further make the sense of touch of alveolar substance, foaming characteristic and particle become the smooth sense of touch for well improving dental surface and Decontamination sense.

As the sodium metasilicate, can enumerate selected from sodium metasilicate (Na₂SiO₃), sodium orthosilicate (Na₄SiO₄), sodium disilicate (Na₂Si₂O₅), tetrasilicic acid sodium (Na₂Si₄O₉) and their hydrate in it is one kind or two or more.

Sodium metasilicate is usually with Na₂O.nSiO₂.mH₂The molecular formula of O indicates.Coefficient n (SiO₂Relative to Na₂The molecular proportion of O) Referred to as molar ratio can be indicated with following formula (I).

Molar ratio=mass ratio (SiO₂Quality %/Na₂O mass %) × (Na₂Molecular weight/SiO of O₂Molecular weight) (I)

As sodium metasilicate, usually also can be used other than sodium metasilicate No. 1, No. 2, No. 3 documented by the JIS K1408 The waterglass of various molar ratios, wherein be more preferably sodium metasilicate 3.

The physical property of sodium metasilicate according to above-mentioned molar ratio (coefficient n) and it is different, but from alignment pharmaceutical raw material standard adaptation Property, play the viewpoint of effect of the invention well, and the viewpoint for making the pH value of particle after cooperation obtained become alkalinity It sets out, and above-mentioned molar ratio (coefficient n) is preferably 2.0 or more, and further preferably 2.4 or more, more preferably 2.8 or more, more Add preferably 3.0 or more, and preferably 4.0 hereinafter, further preferably 3.5 hereinafter, more preferably 3.4 hereinafter, more Preferably 3.3 or less.Moreover, above-mentioned molar ratio (coefficient n) is preferably 2.0~4.0, and further preferably 2.4~3.5, more Preferably 2.8~3.4, more preferably 3.0~3.3.

Being selected from the inorganic bond (B) contained in particle after the cooperation in the presence of dentifrice of the invention 1 kind or 2 kinds of content in sodium metasilicate (solid content ingredient) and colloidal silicon dioxide, keeps water insoluble from as inorganic bond Property powder material particles from the perspective of, in ingredient (B) be preferably 60 mass % or more, further preferably 80 matter % or more is measured, more preferably 90 mass % or more are sprayed from operability and with drop, inhibit the viewpoint of big particle And after raising cooperation from the perspective of the wet type intensity of disintegration of particle, preferably 100 mass % or less.In addition, above-mentioned inorganic viscous The amount of sodium metasilicate (solid content ingredient) and colloidal silicon dioxide in mixture (B) is after the cooperation for making to extract from dentifrice The amount for eliminating moisture after grain is dry at 90 DEG C or more.

Sodium metasilicate (solid content ingredient) and glue are selected from about in particle after the cooperation in the presence of dentifrice of the invention The a kind or 2 kinds i.e. content of ingredient (B) in body silica, the disintegration from the appropriateness in the drying regime of particle and water are strong The viewpoint of degree, stability in dentifrice, or from the perspective of realizing the behavior being slowly disintegrated, after engagement in particle Under drying regime be preferably 1 mass % or more, further preferably 2 mass % or more, more preferably 5 mass % or more, More preferably 10 mass % or more.About containing for the sodium metasilicate in particle after the cooperation in the presence of dentifrice of the invention Amount is preferably after engagement 30 mass % in particle hereinafter, further preferably 20 matter from the viewpoint of improving yield % is measured hereinafter, more preferably 18 mass % or less.In addition, after cooperation in the presence of dentifrice of the invention in particle The content of sodium metasilicate is preferably 1~30 mass %, further preferably 2~20 mass %, more preferably 5~18 matter Measure %, more preferably 10~18 mass %.

After cooperation in the presence of dentifrice of the invention in particle, from making water-insoluble powder material particles, at For the viewpoint of the intensity of disintegration of appropriateness, and from the perspective of realizing the behavior that is slowly disintegrated, inorganic bond (B) relative to The mass ratio (inorganic bond (B)/water-insoluble dusty material (A)) of water-insoluble dusty material (A) be preferably 0.02 with On, further preferably 0.05 or more, more preferably 0.08 or more.In addition, becoming appropriate from big particle is reduced and collapsing Solve intensity from the perspective of, the mass ratio be preferably 0.5 hereinafter, further preferably 0.3 hereinafter, more preferably 0.18 with Under.Also, the mass ratio is preferably 0.02~0.5, and further preferably 0.05~0.3, more preferably 0.08~0.18. In addition, the content in the case where in mentioned component (B) including sodium metasilicate is solid content ingredient scaled value.

From the viewpoint for assigning the effect for inhibiting tartar to be formed and strengthen by water-soluble silicate or colloidal silicon dioxide shape At reticular structure come from the perspective of improving the physical property being slowly disintegrated, after the cooperation in the presence of dentifrice of the invention Particle preferably further contains the one kind or two or more bonding agent in calcium silicates, magnesia, titanium oxide and zinc oxide (C), as the ingredient (C), zinc oxide is further preferably included at least, is more preferably helped comprising zinc oxide and other bondings Agent.

About the content of ingredient (C), go out from the viewpoint for the physical property for improving the effect for inhibiting tartar to be formed and being slowly disintegrated Hair, after engagement in particle in the dry state be preferably 0.2 mass % or more, further preferably 0.5 mass % or more, More preferably 0.8 mass % or more.In addition, the content about ingredient (C), the viewpoint become excessively high from inhibition intensity of disintegration, From the perspective of improving the foaming characteristic of dentifrice and the viewpoint of alveolar substance of particle after being combined with cooperation and inhibiting metallic taste, After cooperation in particle in the dry state be preferably 5 mass % hereinafter, further preferably 3 mass % hereinafter, be more preferably 2 mass % or less.In addition, the content of ingredient (C) is preferably 0.2~5 mass % in particle in the dry state after engagement, Further preferably 0.5~3 mass %, more preferably 0.8~2 mass %.

About the mass ratio (C/B) of ingredient (C) and ingredient (B) in particle after cooperation, from the intensity of disintegration for realizing appropriateness Viewpoint, improve deposit the viewpoint of the foaming characteristic and alveolar substance of the dentifrice of particle after engagement, all size of dental surface it is recessed From the perspective of the cleaning performance in portion, preferably 0.02 or more, further preferably 0.05 or more, more preferably 0.08 with On, and preferably 1 hereinafter, further preferably 0.5 hereinafter, more preferably 0.3 hereinafter, more preferably 0.2 or less.Separately Outside, the mass ratio (C/B) of the ingredient after cooperation in particle (C) and ingredient (B) are preferably 0.02~1, and further preferably 0.05 ~0.5, more preferably 0.08~0.3, more preferably 0.08~0.2.

Particle can root within the scope of the effect of the invention after cooperation in the presence of dentifrice of the invention According to needing in addition to the above ingredients containing organic fiber, medicinal ingredient, colorant etc..

Other ingredients other than mentioned component can be used alone, and can also combine two or more use.

Particle has special shape, the face on the perspective plane of the particle after cooperation in the presence of dentifrice of the invention Product (S_A) and with the maximum gauge (D in the perspective plane_L) be diameter circumscribed circle area (S_S) ratio (S_A/S_S) average value It is 0.5 or more and 0.9 or less.The area on the perspective plane of particle refers to using JIS Z8801-1 standard after cooperation in the present invention 150 μm of the sieve dentifrice that will be diluted to 10 mass % using pure water by pure water aqueous cleaning after, will remain 1 day dry under room temperature (25 DEG C), the value measured using particle obtained in the particle on sieve.The throwing of particle after cooperation Shadow face refers to using the obtained face of KEENCE VH-5500 (100 times of multiplying power) photography, uses analysis software (WinROOF (three Paddy business Co., Ltd.)) the obtained digital picture of photographing is found out particle a perspective plane area (S_A) and with the projection Maximum gauge (D in face_L) be diameter circumscribed circle area (S_S) ratio (S_A/S_S), further according to from other directions Perspective plane or using the obtained perspective plane of particle after other cooperations, find out S_A/S_SAverage value.In this way, by with perspective plane In maximum gauge (D_L) be diameter circumscribed circle area (S_S) with the area (S on perspective plane_A) S that finds out_A/S_SAverage value As particle closer to it is spherical be more similar to 1 value, as a result, due to the S_A/S_SAverage value be as described above 0.5 or more and 0.9 hereinafter, therefore, particle is not spherical particle after the cooperation in the presence of dentifrice of the invention, but is deposited on surface In shape, that is, special shape of the deformation of multiple bumps, so-called unsetting particle.Moreover, after cooperation of the invention Grain, which is showed, to be gone out notch by Particle Breakage before cooperate or part and is formed with the appropriate unsetting of protrusion, therefore in mouth In do not feel as foreign body sensation, on the other hand, be rallentando disintegrated due to unsetting shape, at the end of brushing teeth A large amount of intragranular disintegrations can be provided and sense of touch that the behavior of brushing teeth terminates.

It is believed that after cooperation in the presence of dentifrice of the invention particle by with such special shape, Even if load is also concentrated and is applied to protrusion when in oral cavity using loaded loads such as toothbrushes, therefore is easy disintegration, and It is slowly disintegrated using the protrusion as starting point.It is considered that the reason is that after cooperation in the presence of dentifrice of the invention Each grain of grain is that primary particle agglomerates to form intermediate particle, and it is further agglomerated made of being formed, therefore gap is suitable Degree ground is scattered in particle, is gradually disintegrated since the intermediate particle for projecting to surface with loaded load.Then, straight During being finally disintegrated to particle, initial change is intermediate particle, which rallentandos while crushing thinner Disintegration.In addition, particle is matched in dentifrice before particle will preferably cooperate after cooperation in the presence of dentifrice of the invention The particle that stirring when later, by the manufacture of dentifrice obtains.In this way, being obtained after using the stirring deposited during fabrication After the cooperation obtained under the service condition of the dentifrice of the invention of particle, particle will not one action due to the load of toothbrush after cooperation Disintegration, and particle is rallentando disintegrated during brushing teeth, the glaze that these are entered to while colliding facing such as tooth is horizontal The fine recess portion of line and effectively transmit the load from toothbrush, so as to fully play tartar or dirt removal The smooth sense of touch and decontamination sense of dental surface can be improved in ability.

Area (S about the perspective plane of particle after cooperation_A) and with the maximum gauge (D in the perspective plane_L) it is diameter Area (the S of circumscribed circle_S) ratio (S_A/S_S) average value, from the viewpoint of the behavior for ensuring slowly to be disintegrated, be 0.5 with On, preferably 0.6 or more, further preferably 0.65 or more, it is still more preferably 0.7 or more.About particle after cooperation Area (the S on perspective plane_A) and with the maximum gauge (D in the perspective plane_L) be diameter circumscribed circle area (S_S) ratio (S_A/ S_S) average value, from appropriate disintegration is shown, the toothbrush for even having soft bristle can also effectively transmit load From the perspective of lotus, for 0.9 hereinafter, preferably 0.85 hereinafter, further preferably 0.82 or less.The projection of particle after cooperation Area (the S in face_A) and with the maximum gauge (D in the perspective plane_L) be diameter circumscribed circle area (S_S) ratio (S_A/S_S) Average value is 0.5 or more and 0.9 hereinafter, preferably 0.6~0.9, further preferably 0.65~0.85, still more preferably It is 0.75~0.82.In addition, as soft bristle, such as the gradually smaller cone of sectional area at the hair end of bristle can be enumerated Shape bristle.The front end of the tapered bristles is thinner, therefore having is soft sense of touch, and hair end is easily accessible to tooth and tooth The property in the gap of tooth.

About the maximum gauge (D in the perspective plane of particle after cooperation_L) and minimum diameter (D_S) ratio (D_L/D_S) be averaged Value, from becoming unsetting particle and show the viewpoint for the behavior being slowly disintegrated and even have a soft bristle Toothbrush also effectively transmit load from the perspective of, preferably 1.2 or more, further preferably 1.3 or more, more preferably It is 1.4 or more.About the maximum gauge (D in the perspective plane of particle after cooperation_L) and minimum diameter (D_S) ratio (D_L/D_S) Average value, from the viewpoint of showing appropriate disintegration and effectively transmitting the load from toothbrush, preferably 1.8 Hereinafter, further preferably 1.7 hereinafter, more preferably 1.65 or less.In addition, the maximum after cooperation in the perspective plane of particle Diameter (D_L) and minimum diameter (D_S) ratio (D_L/D_S) average value be preferably 1.2~1.8, further preferably 1.3~1.7, More preferably 1.4~1.65.

In addition, particle has special size distribution after cooperation in the presence of dentifrice of the invention, about this Grain, in particle (a)~(d) below in the size distribution obtained by laser diffraction/scattering formula particle size distribution measuring, The volume ratio (b/c) of the amount of the amount and particle (c) of grain (b) is for 0.7 or more and 1.2 hereinafter, the volume of particle (d) and particle (c) Than (d/c) be 0.2 or more and 1 hereinafter, the volume ratio (b/d) of the amount of the amount and particle (d) of particle (b) be greater than 1 and be 5 hereinafter, And the content in particle is 15 volume % or more and 55 volume % or less to particle (c) after engagement.

(a) partial size is 50 μm of particles more than and less than 100 μm；

(b) partial size is 100 μm of particles more than and less than 150 μm；

(c) partial size is 150 μm of particles more than and less than 200 μm；

(d) partial size is 200 μm of particles more than and less than 250 μm.

That is, the volume ratio (b/c) of the amount by making these between particle (a) and particle (b) is above range, make Grain (b) is present in dentifrice relative to particle (c) with the amount of same degree, in contrast, due to above-mentioned volume ratio (d/c) Within the above range and particle (b/d) is greater than 1 and is 5 hereinafter, therefore, particle (b) exists with the amount more than particle (d).Cause This, exist it is a large amount of as (b) that partial size is 100 μm of particles more than and less than 200 μm and (c), and partial size for 200 μm with On particle (d) with appropriateness amount exist, therefore, be easy transmitting from diameter be about 200 μm toothbrush bristle stress Particle (d) moderately exist, and there are it is more be easily accessible to the bristle of toothbrush be difficult to enter such as dental surface The particle (b) and particle (c) of fine recess portion as perikymata.It is believed that thus with the tooth for being applied through scrub The load of brush makes these particles slowly while interacting and is disintegrated, and the glaze entered on one side such as tooth is horizontal Fine recess portion as line effectively transmits the load from toothbrush on one side, so as to fully play tartar or dirt Dirty removal capacity, the sense of touch after improving the smooth and smooth sense of touch of dental surface, dirt removal.

In addition, particle refers to through laser diffraction/scattering formula partial size point after cooperation in the presence of dentifrice of the invention The particle that the partial size that cloth measurement is found out is 50 μm or more.Furthermore it is possible to think, the cooperation in the presence of dentifrice of the invention Particle is unsetting particle as described above afterwards, but is big by the partial size that laser diffraction/scattering formula particle size distribution measuring is found out Cause is similar to above-mentioned maximum gauge (D_L) and minimum diameter (D_S) average value value.

After cooperation in the presence of dentifrice of the invention in particle, from the behavior for showing slowly to be disintegrated, and The recess portion further preferably effectively entered to fine recess portion to width for 150 μm of sizes below is effectively entered, is mentioned Height brush teeth after the smooth sense of touch of dental surface from the perspective of, the grain that is obtained by laser diffraction/scattering formula particle size distribution measuring The volume ratio (b/c) of the amount of the amount and particle (c) of particle (b) in degree distribution is 0.7 or more, preferably 0.75 or more, into One step is preferably 0.8 or more.After cooperation in the presence of dentifrice of the invention in particle, from particle (b) one side and particle (c) interaction on one side be slowly disintegrated and exist with particle of various shapes from the perspective of, by laser diffraction/scattering Formula particle size distribution measuring obtain size distribution in particle (b) amount and particle (c) amount volume ratio (b/c) be 1.2 with Under, preferably 1.1 hereinafter, further preferably 1.0 hereinafter, more preferably 0.95 or less.In addition, cleaning the teeth in of the invention After cooperation in the presence of agent in particle, by the particle in laser diffraction/scattering formula particle size distribution measuring acquisition size distribution (b) volume ratio (b/c) of amount and the amount of particle (c) be 0.7 or more and 1.2 hereinafter, preferably 0.75 or more and 1.1 hereinafter, Further preferably 0.8 or more and 1.0 hereinafter, be still more preferably 0.8 or more and 0.95 or less.

It is negative from the stress of the bristle of easy transmitting toothbrush after cooperation in the presence of dentifrice of the invention in particle The particle (d) of lotus is slowlyed while with particle (b) and particle (c) interaction to be disintegrated and exists with of various shapes From the perspective of particle, the amount of the particle (d) in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring with The volume ratio (d/c) of the amount of particle (c) is 0.2 or more, preferably 0.25 or more, further preferably 0.3 or more.In this hair After cooperation in the presence of bright dentifrice in particle, make particle (b) and particle (c) also effectively from by particle (d) It enters to from the perspective of fine recess portion, in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring Grain (d) amount and particle (c) amount volume ratio (d/c) be 1 hereinafter, preferably 0.9 hereinafter, further preferably 0.85 with Under, more preferably 0.8 or less.In addition, after cooperation in the presence of dentifrice of the invention in particle, by laser diffraction/ Scattering formula particle size distribution measuring obtain size distribution in the amount of particle (d) be with the volume ratio (d/c) of the amount of particle (c) 0.2 or more and 1 hereinafter, preferably 0.25 or more and 0.9 hereinafter, further preferably 0.25 or more and 0.85 hereinafter, more excellent It is selected as 0.3 or more and 0.8 or less.

After cooperation in the presence of dentifrice of the invention in particle, the size distribution of particle is after cooperation with particle (c) centered on content, and containing being difficult to reach than particle (d) being easily accessible to the bristle of the toothbrush of dental surface mostly Fine recess portion particle (b), improve the viewpoint of the dirt removal capacity of the fine recess portion of dental surface, and improve and deposit After engagement from the perspective of the foaming characteristic or alveolar substance of the dentifrice of particle, obtained by laser diffraction/scattering formula particle size distribution measuring The volume ratio (b/d) of the amount of the amount and particle (d) of the particle (b) in size distribution obtained is greater than 1, preferably 1.1 or more, into One step is preferably 1.2 or more.About particle after cooperation of the invention, from particle (d) by the bristle of toothbrush load and one side With particle (c) and particle (b) interaction on one side be slowly disintegrated and exist with particle of various shapes from the perspective of, The body of the amount of the amount and particle (d) of the particle (b) in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring Product is than (b/d) for 5 hereinafter, preferably 4 hereinafter, further preferably 2.8 or less.In addition, the institute in dentifrice of the invention After existing cooperation in particle, by the particle (b) in laser diffraction/scattering formula particle size distribution measuring acquisition size distribution The volume ratio (b/d) of amount and the amount of particle (d) is greater than 1 and is 5 hereinafter, preferably 1.1~4, further preferably 1.2~ 2.8。

In addition, after cooperation in the presence of dentifrice of the invention before particle and following cooperations particle size distribution It is to be obtained by laser diffraction/scattering formula particle size distribution measuring, to be present in particle after the cooperation in dentifrice the case where Under, the aqueous solution that dentifrice is diluted to 10 mass % is measured using by ion exchange water；It is being clean for being matched with Before cooperation in tooth agent in the case where particle, it is measured using the aqueous solution for being diluted to 5 mass % by ion exchange water. More specifically, to by ion exchange water will be present cooperation after particle dentifrice be diluted to 10 mass % aqueous solution (or Particle is diluted to the aqueous solution of 5 mass % before being cooperated by ion exchange water), pass through mixing machine (ROTARY MIXER NPC-20, NISSIN company manufacture) disperse particle under conditions of 75 revs/min, horizontal direction rotation, 2 hours.Then, The dentifrice after the dispersion of particle after engagement is deposited into dilution and obtain aqueous solution (or be dispersed with cooperate before particle it is water-soluble Liquid) it is saved 1 day under room temperature (25 DEG C).Make the aqueous dispersion after the preservation after ten minutes again by above-mentioned mixing machine, makes Laser diffraction/scattering formula particle size distribution device (Partica LA-950V2, HORIBA corporation is utilized with the aqueous solution Make) in refractive index: 1.58, circulation rate (scale: 5), mixing speed (scale: 5) under conditions of be measured.

After cooperation in the presence of dentifrice of the invention in particle, by laser diffraction/scattering formula particle size distribution measuring The amount of particle (c) in the size distribution of acquisition is 15 volume % or more and 55 volume % or less in particle after engagement.About The amount of particle (c), from the width of dental surface be 150 μm of sizes below recess portion dirt removal capacity viewpoint and When being scrubbed using toothbrush with the fine recess portion of size of the width less than 200 μm of other Interaction between particles and dental surface Removal capacity from the perspective of, after engagement in particle be 15 volume % or more, preferably 20 volume % or more, further Preferably 23 volume % or more, and be 55 volume % hereinafter, preferably 50 volume % are hereinafter, further preferably 45 volume % Hereinafter, more preferably 40 volume % or less.In addition, the amount of particle (c) is 15 volume % or more and 55 in particle after engagement Volume % is hereinafter, preferably 20~50 volume %, further preferably 23~45 volume %, more preferably 23~40 bodies Product %.

For particle after the cooperation in the presence of dentifrice of the invention, by make particle (c) particle (a)~(d) it In the more amount presence that exists with most volume or make particle (c) and particle (b) with roughly the same degree, to make dentifrice It is middle that there are the particles of the recess portion of more size of the unapproachable width of the bristle that can enter to toothbrush less than 200 μm.About The total amount of particle (b) and particle (c), from the higher dirt removal of the unapproachable fine recess portion of the bristle of toothbrush From the perspective of energy, after engagement in particle be preferably 30 volume % or more, further preferably 35 volume % or more, more Preferably 40 volume % or more are still more preferably 50 volume % or more.About the total amount of particle (b) and particle (c), It is also fully transferred to particle (a)~(c) from by the stress generated by the bristle of toothbrush, even if using the brush for having softness In the case where the toothbrush of hair, the not only recess portion of size of the width less than 200 μm, and also until width is 100 μm below big Small fine recess portion, from the perspective of can also effectively playing higher dirt removal capacity, after engagement in particle Preferably 85 volume % hereinafter, further preferably 80 volume % hereinafter, more preferably 75 volume % or less.In addition, particle (b) with the total amount of particle (c) preferably 30~85 volume %, further preferably 35~80 volumes in particle after engagement %, more preferably 40~80 volume %, more preferably 50~75 volume %.

After cooperation in the presence of dentifrice of the invention in particle, from the toothbrush for even having soft bristle, Also by the scrub stress transfer generated by toothbrush to lesser 200 μm of particles below, and make cooperation after particle effectively into Enter the viewpoint of the recess portion to the dental surface that width is 200 μm of sizes below, and improves the dentifrice for depositing particle after engagement Foaming characteristic or alveolar substance from the perspective of, in size distribution that obtained by laser diffraction/scattering formula particle size distribution measuring The volume ratio ((a+b)/(c+d)) of the total amount of the total amount and particle (c) and particle (d) of grain (a) and particle (b) is preferably 0.5 or more, further preferably 0.6 or more, more preferably 0.65 or more, and preferably 1 hereinafter, further preferably 0.9 Hereinafter, more preferably 0.85 or less.In addition, the conjunction of the total amount of particle (a) and particle (b) and particle (c) and particle (d) The volume ratio ((a+b)/(c+d)) of metering is preferably 0.5~1, further preferably 0.6~0.9, more preferably 0.65~ 0.85。

Particle can also further exist and be obtained by laser diffraction/scattering formula particle size distribution measuring after cooperation of the invention Size distribution in partial size be 250 μm of particles (e) more than and less than 350 μm.About the particle in particle after the cooperation (a) and the volume ratio ((a+b)/e) of the amount of the total amount of particle (b) and particle (e) it, is generated from improving by particle (a)~(d) Cleaning performance from the perspective of, preferably greater than 1, further preferably 1.1 or more, more preferably 1.2 or more, more into one Step is preferably 1.3 or more, and preferably 20 hereinafter, further preferably 18 or less.In addition, the conjunction of particle (a) and particle (b) The volume ratio ((a+b)/e) of metering and the amount of particle (e) is preferably greater than 1 and for 20 hereinafter, further preferably 1.1~20, more Add preferably 1.2~18, is still more preferably 1.3~18.

After cooperation in the presence of dentifrice of the invention in particle, from by being greater than particle (a) between partial size Intergranular is so that it is guaranteed that particle largely enters to the fine recess portion of dental surface after the viewpoint of the behavior being slowly disintegrated, cooperation From the perspective of improving tartar removal capacity, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution The amount of particle (a) preferably 3 volume % or more, further preferably 5 volume % or more in particle after engagement, steep from improving From the perspective of matter and foaming characteristic, more preferably 7 volume % or more promote from interacting with particle (b) or particle (c) From the perspective of entering into particle to fine recess portion, preferably 15 volume % hereinafter, further preferably 12 volume % with Under, more preferably 10 volume % or less.In addition, being spread out in particle by laser after cooperation in the presence of dentifrice of the invention The amount of the particle (a) in the size distribution of formula particle size distribution measuring acquisition is penetrated/scattered after engagement preferably 3~15 in particle Volume %, further preferably 5~12 volume %, more preferably 7~10 volume %.

After cooperation in the presence of dentifrice of the invention in particle, about by laser diffraction/scattering formula particle diameter distribution Measure obtain size distribution in particle (b) amount, interact well from one side with particle (a), on one side by between Partial size is greater than between the particle of particle (b) and from the perspective of the behavior for ensuring slowly to be disintegrated, and is preferably in particle after engagement 12 volume % or more, further preferably 15 volume % or more, more preferably 20 volume % or more, and preferably 50 bodies % is accumulated hereinafter, further preferably 40 volume % are hereinafter, more preferably 35 volume % or less.

After cooperation in the presence of dentifrice of the invention in particle, about by laser diffraction/scattering formula particle diameter distribution The amount for measuring the particle (d) in the size distribution obtained, from one side is passed through by the stress transfer of the bristle of toothbrush to particle (a) ~particle (c) is interacted well with these particles so that it is guaranteed that from the perspective of the behavior being slowly disintegrated on one side, is being matched After conjunction in particle be preferably 5 volume % or more, further preferably 10 volume % or more, more preferably 12 volume % or more, And preferably 25 volume % hereinafter, further preferably 22 volume % hereinafter, more preferably 20 volume % or less.

In addition, after cooperation in the presence of dentifrice of the invention in particle, about by laser diffraction/scattering formula grain The amount for the particle (e) in size distribution that diameter measure of spread obtains, from improving by particle (a)~(d) cleaning performance generated Viewpoint is set out, and is preferably greater than 0 volume %, further preferably 1 volume % or more, more preferably 2 bodies in particle after engagement Product % or more, and preferably 25 volume % hereinafter, further preferably 20 volume % hereinafter, more preferably 18 volume % with Under.

After cooperation in the presence of dentifrice of the invention in particle, by laser diffraction/scattering formula particle size distribution measuring The amount for the particle that partial size in the size distribution of acquisition is 350 μm or more after engagement in particle preferably 0 volume % or Greater than 0 volume % and be 35 volume % hereinafter, further preferably 15 volume % hereinafter, more preferably 10 volume % hereinafter, It is still more preferably 5 volume % or less.Particle matches after cooperation in the presence of for obtaining dentifrice of the invention Before closing in particle, the amount for the particle that partial size is 350 μm or more is preferably 10 volume % or more in particle before cooperation, further Preferably 15 volume % or more, more preferably 20 volume % or more, and preferably 35 volume % or less.It is believed that this hair Particle cooperates in the mixed processes after particle preferably in dentifrice by making particle after cooperation in the presence of bright dentifrice A part shortcoming or make Particle Breakage and size distribution made to change, clean the teeth as long as being present in after the mixed processes Particle after the cooperation in agent, then when using dentifrice, on one side to bringing the touching that can perceive particle well in oral cavity Sense, is disintegrated, to become easy the fine recess portion for entering to dental surface on one side by using the scrub of toothbrush.

About the average grain diameter r (μm) of particle after the cooperation in the presence of dentifrice of the invention, adequately ground from having From the perspective of grinding power, preferably 75 μm or more, further preferably 100 μm or more, more preferably 125 μm or more, from suppression From the perspective of foreign body sensation in donsole chamber, preferably 250 μm hereinafter, further preferably 220 μm hereinafter, be more preferably 210 μm hereinafter, be still more preferably 180 μm or less.Also, particle after the cooperation in the presence of dentifrice of the invention Average grain diameter r (μm) is preferably 75~250 μm, further preferably 100~220 μm, more preferably 125~210 μm, more Further preferably 125~180 μm.

In addition, the average grain diameter r of particle is volume average particle size after cooperation, and for by laser diffraction/scattering formula partial size Median particle diameter in the size distribution for the particle that the partial size that measure of spread obtains is 50 μm or more.

After the above-mentioned cooperation with special shape or special size distribution in the presence of dentifrice of the invention The intensity of disintegration of grain is 1gf/ or more and 20gf/ or less.By the way that toothbrush etc. can be being utilized with above-mentioned intensity of disintegration It is rallentando disintegrated when loaded load by unsetting shape, and will not feel foreign body sensation, Er Qieke in mouth So that particle enters to fine recess portion and fully removes the dirts such as tartar or colored soil.About particle after cooperation Intensity of disintegration, from show the behavior being slowly disintegrated and improve dirt removal capacity viewpoint, by with particle after cooperation The interaction of special shape or special size distribution can also make to match to the toothbrush for even having soft bristle Particle is entered to while the stress for passing through toothbrush is slowly disintegrated from the perspective of fine recess portion after conjunction, is 1gf/ More than, preferably 2gf/ or more, further preferably 3gf/ or more.About the intensity of disintegration of particle after above-mentioned cooperation, From even by the viewpoint and drop for using the load of lower load whens soft toothbrush etc. also to assign appropriate disintegration From the perspective of low foreign body sensation, for 20gf/ hereinafter, preferably 15gf/ hereinafter, deposit the clean of particle after engagement from improving From the perspective of the foaming characteristic or alveolar substance of tooth agent, further preferably 10gf/ hereinafter, more preferably 8gf/ or less.Separately Outside, the intensity of disintegration of above-mentioned particle is 1gf/ or more and 20gf/ hereinafter, preferably 2~15gf/ is a, further preferably It is 3~10gf/, more preferably 3~8gf/.

In addition, the intensity of disintegration of particle is value when measuring under moisture state after cooperation used in the present invention, and And be that particle after 10~20 cooperations is extracted from dentifrice, using compression test (Shimadzu Seisakusho Ltd., MCTM-500), When the measurement of each particle was compressed and was disintegrated to the particle of partial size (180~200 μm) with loading velocity 1.51gf/ seconds Load, the average value found out.In addition, the intensity of disintegration about particle after cooperation used in the present invention, under moisture state It is identical value with the intensity of disintegration under drying regime.

Particle can according to need the inorganic bond of ingredient (B) after cooperation in the presence of dentifrice of the invention Aqueous solution (hereinafter referred to as " inorganic bond aqueous solution ") is made, is mixed with the water-insoluble dusty material of ingredient (A), preferably Use the particle formed in the middle addition inorganic bond aqueous solution of ingredient (A) particle as before cooperating, is matched with and is cleaned the teeth In agent.When these are mixed, can also further adding ingredient (C) bonding agent.

In the case where containing sodium metasilicate as ingredient (B), as the sodium metasilicate, sodium silicate aqueous solution can be used, close The content of sodium metasilicate (solid content ingredient) in sodium silicate aqueous solution, from the sight of the disintegration properties, the manufacturing of particle of particle Point set out, in sodium silicate aqueous solution be preferably 20 mass % or more, further preferably 30 mass % or more, further it is excellent 35 mass % or more are selected as, from the viewpoint of inhibiting big particle, preferably 65 mass % are hereinafter, further preferably 60 Quality %.In addition, the sodium metasilicate (solid content ingredient) in sodium silicate aqueous solution can be asked by method documented in embodiment Out.In addition, comprising sodium metasilicate as ingredient (B), if with the matter of ingredient (A) and inorganic bond aqueous solution Measure be than (A/ inorganic bond aqueous solution) substantially 10~1, preferably 8~5 coverage modulation, then can particle well Change, therefore, inorganic bond aqueous solution can use the inorganic viscous of 3 times of amounts sodium metasilicate of the water dilution comprising ingredient (B) below Mixture is modulated.Further, water can not also be utilized to be diluted and mixed with the water-insoluble dusty material of ingredient (A) It closes, addition inorganic bond aqueous solution forms particle before cooperation preferably in ingredient (A).Gap one is effectively formed from one side Side is agglomerated and is formed from the perspective of particle, which is preferably added to ingredient (A) with the speed of mitigation Water-insoluble dusty material in.

Specifically, for example, the water-insoluble of the adding speed of inorganic bond aqueous solution relative to 100 mass parts Powder body material (A), preferably 35 mass parts/minute hereinafter, further preferably 20 mass parts/minute hereinafter, be more preferably 10 mass parts/minute hereinafter, and preferably 0.5 mass parts/more than minute, further preferably 0.8 mass parts/more than minute, More preferably 1 mass parts/it is more than minute.Recorded in using JIS K1408 sodium metasilicate No. 1, No. 2 or 3 of above range In the case where number preferably.Also, the adding speed of the inorganic bond aqueous solution, the water-insoluble relative to 100 mass parts Powder body material (A), preferably 0.5~35 mass parts/minute, further preferably 0.8~20 mass %, more preferably 1~ 10 mass %.

In addition, the adding speed about sodium metasilicate (solid content ingredient), from the viewpoint of same as described above, relative to The water-insoluble powder body material (A) of 100 mass parts, preferably 19 mass parts/minute is hereinafter, further preferably 11 mass Part/minute hereinafter, more preferably 5.5 mass parts/minute hereinafter, and preferably 0.1 mass parts/more than minute, it is further excellent It is selected as 0.2 mass parts/more than minute, more preferably 0.3 mass parts/it is more than minute.Also, about the sodium metasilicate (Gu Shape object ingredient) adding speed, relative to the water-insoluble powder body material of 100 mass parts, preferably 0.1~19 mass parts/point Clock, further preferably 0.2~11 mass %, more preferably 0.3~5.5 mass %.

As described above, the aqueous solution (inorganic bond aqueous solution) of adding ingredient (B), as needed in ingredient (A) Ingredient (C) formation before the cooperation of particle after being cooperated by rolling comminution granulation for when particle, preferably being manufactured.Pass through Particle is matched in dentifrice before with being manufactured from rolling comminution granulation, and can obtain has spy used in the present invention The particle of the particle of different shape and the not all the time general spherical shape obtained by spray granulation, furthermore it is possible to Size distribution particle before the wide cooperation of wide scope is obtained, it is possible thereby to which obtaining used in the present invention has specifically Size distribution particle, furthermore it is possible to be present in the dispersion of more gaps in particle, it is hereby achieved that having above-mentioned Characteristic and show particle after the cooperation of the behavior being slowly disintegrated.

In addition, when through particle before rolling comminution granulation manufacture as described above for the cooperation of particle after being cooperated, It is preferable to use container rotating type pelletizers.As the container rotating type pelletizer, rotary drum granulator can be enumerated and disc type is made Grain machine.It is just not particularly limited as rotary drum granulator as long as the cylinder of drum type rotates come what is handled.In addition to Other than horizontal or slightly angled rotary drum granulator, cone drum pelletizer also can be used, multistage bore rouses pelletizer etc..These Device can be batch-type, continuous any.

Further, as described above, inorganic bond aqueous solution is added to the water of ingredient (A) not with the speed of mitigation , it is preferable to use multi fluid nozzle when in water-soluble pulverulent material.In addition, multi fluid nozzle is to keep liquid and micronized gas (empty Gas, nitrogen etc.) by independent flow path be circulated to spray nozzle front end portion nearby mixed, the nozzle of micronized, it is specific and Speech, can enumerate: second fluid nozzle, three fluid tips, four fluid tips etc..

About use multi fluid nozzle supply inorganic bond aqueous solution when inorganic bond aqueous solution temperature, from From the perspective of stability when addition, preferably 5 DEG C or more, further preferably 10 DEG C or more, and preferably 50 DEG C with Under, further preferably 30 DEG C or less.Also, inorganic bond when using multi fluid nozzle supply inorganic bond aqueous solution The temperature of agent aqueous solution is preferably 5~50 DEG C, and further preferably 10~30 DEG C.

In addition, preferably cooperating the ingredient (C) together with ingredient (A) using the bonding agent of ingredient (C). Specifically, the manufacturing process of particle is preferably provided with using container rotating type before cooperation in the case where obtaining gradation composition (C) The process that pelletizer mixes the water-insoluble dusty material of ingredient (A) with the bonding agent of ingredient (C), more preferably further Have use multi fluid nozzle to ingredient (A) and ingredient (C) (the preferably mixture of ingredient (A) and ingredient (C)) supply as The process of the inorganic bond aqueous solution of ingredient (B).

After ensure to cooperate the stability of particle, the cooperation obtained for particle after being cooperated Preceding particle is preferably further dried.As the drying, specifically, can enumerate: canopy is dry, fluidized bed is dry, decompression Drying, microwave drying etc..Wherein, from the viewpoint of in equipment, preferably canopy is dry, fluidized bed is dry.

From the viewpoint of thermic load, drying temperature is preferably 60 DEG C or more, and further preferably 70 DEG C or more, more Preferably 80 DEG C or more.Additionally, it is preferred that be 200 DEG C hereinafter, further preferably 150 DEG C hereinafter, more preferably 110 DEG C, more Add preferably 90 DEG C or less.Also, drying temperature is preferably 60~200 DEG C, and further preferably 70~150 DEG C, more preferably It is 80~110 DEG C, more preferably 80~90 DEG C.

Drying time is preferably 10 minutes or more, further preferably 20 minutes or more, more preferably 30 minutes with On, and preferably 24 hours hereinafter, further preferably 20 hours hereinafter, more preferably 5 hours or less.Also, when drying Between preferably 10 minutes~24 hours, further preferably 20 minutes~20 hours, more preferably 30 minutes~5 hours.

About particle before the cooperation for obtaining the particle after the cooperation in the presence of dentifrice of the invention, by swashing In particle below (b')~(e-1') in size distribution that optical diffraction/scattering formula particle size distribution measuring obtains, particle (b') Amount and particle (c') amount volume ratio (b'/c') be preferably 0.6 or more and 1.25 hereinafter, particle (d') amount and particle (c') volume ratio (d'/c') of amount is preferably 0.7 or more and 1.2 hereinafter, the amount of particle (e-1') and the amount of particle (c') Volume ratio (e-1'/c') is preferably 0.4 or more and 1.1 or less.That is, before cooperating in particle partial size be 100 μm more than and less than The particle of 300 μm of range have with wide peak existing for the amount of roughly the same degree, by being cooperated, can make as Particle is present in dentifrice after the upper cooperation with special shape or special size distribution.

(b') partial size is 100 μm of particles more than and less than 150 μm；

(c') partial size is 150 μm of particles more than and less than 200 μm；

(d') partial size is 200 μm of particles more than and less than 250 μm；

(e-1') partial size is 250 μm of particles more than and less than 300 μm；

In addition, particle refers to the cooperation for obtaining particle after the cooperation in the presence of dentifrice of the invention before cooperating Particle before dentifrice, and be the partial size that is found out by laser diffraction/scattering formula particle size distribution measuring be 50 μm or more Particle.Furthermore it is possible to which it is above-mentioned to be substantially similar to think the partial size found out by laser diffraction/scattering formula particle size distribution measuring Maximum gauge (D_L') and minimum diameter (D_S') average value value.

Before cooperation in particle, from the volume ratio (b/ of the amount for the amount and particle (c) for making the particle (b) after cooperation in particle C) from the perspective of becoming desired value, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution The volume ratio (b'/c') of the amount of the amount and particle (c') of grain (b') is preferably 0.6 or more, and further preferably 0.75 or more, more Add preferably 0.8 or more.Before cooperation in particle, particle effectively assigns the sight for the behavior being slowly disintegrated after to cooperation Point sets out, the amount and particle of the particle (b') in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring (c') volume ratio (b'/c') of amount be preferably 1.25 hereinafter, further preferably 1.15 hereinafter, more preferably 1.05 with Under.In addition, before cooperation in particle, by the particle in laser diffraction/scattering formula particle size distribution measuring acquisition size distribution (b') volume ratio (b'/c') of the amount of amount and particle (c') is preferably 0.6 or more and 1.25 hereinafter, further preferably 0.75~1.15, more preferably 0.8~1.05.

Before cooperation in particle, from the volume ratio (d/ of the amount for the amount and particle (c) for making the particle (d) after cooperation in particle C) from the perspective of becoming desired value, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution The volume ratio (d'/c') of the amount of the amount and particle (c') of grain (d') is preferably 0.7 or more, and further preferably 0.8 or more, more Add preferably 0.85 or more.Before cooperation in particle, particle effectively assigns the sight for the behavior being slowly disintegrated after to cooperation Point sets out, the amount and particle of the particle (d') in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring (c') volume ratio (d'/c') of amount be preferably 1.2 hereinafter, further preferably 1.15 hereinafter, more preferably 1.05 with Under.In addition, before cooperation in particle, by the particle in laser diffraction/scattering formula particle size distribution measuring acquisition size distribution (d') volume ratio (d'/c') of the amount of amount and particle (c') is preferably 0.7 or more and 1.2 hereinafter, further preferably 0.8 ~1.15, more preferably 0.85~1.05.

Before cooperation in particle, after be easy to get with the cooperation of behavior being slowly disintegrated particle, The amount of the particle (e-1') in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring and the amount of particle (c') Volume ratio (e-1'/c') be preferably 0.4 or more, further preferably 0.5 or more, more preferably 0.6 or more, more into one Step preferably 0.7 or more.Before cooperation in particle, particle effectively assigns the sight for the behavior being slowly disintegrated after to cooperation Point sets out, the amount and particle of the particle (e-1') in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring (c') volume ratio (e-1'/c') of amount is preferably 1.1 hereinafter, further preferably 1 or less.In addition, the particle before cooperation In, the amount and particle (c') of the particle (e-1') in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring The volume ratio (e-1'/c') of amount is preferably 0.4 or more and 1.1 hereinafter, further preferably 0.5~1.1, and more preferably 0.6 ~1, more preferably 0.7~1.

In addition, before cooperation in particle, the viewpoint of particle after being easy to get the cooperation with the behavior being slowly disintegrated Set out, (a') partial size in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring be 50 μm more than and less than The volume ratio (a'/c') of the amount of the amount and particle (c') of 100 μm of particle (particle (a')) is preferably 0.2 or more, further excellent It is selected as 0.3 or more.Before cooperation in particle, from obtaining with the behavior that is slowly disintegrated and can also effectively enter to micro- After the cooperation of thin recess portion from the perspective of particle, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution (a') partial size be 50 μm of particles (particle (a')) more than and less than 100 μm amount and particle (c') amount volume ratio It (a'/c') is preferably 1.2 hereinafter, further preferably 1 or less.In addition, before cooperation in particle, by laser diffraction/scattering formula (a') partial size in size distribution that particle size distribution measuring obtains is 50 μm of particles (particle (a')) more than and less than 150 μm Amount and the volume ratio (a'/b') of amount of particle (b') be preferably 0.2~1.2, further preferably 0.3~1.

Before cooperation in particle, particle (a) or particle (b) after making cooperation in particle interact well and From the perspective of the behavior for ensuring slowly to be disintegrated, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution The amount of particle (a') be preferably 3~20 volume % in particle before cooperation, further preferably 5~18 volume % are more excellent It is selected as 7~15 volume %.

Before cooperation in particle, from making particle (c) be present in desired amount the viewpoint after cooperation in particle and make Particle (a) or particle (b) interact well and from the perspective of the behaviors that ensure slowly to be disintegrated, by laser diffraction/ The amount for the particle (c') in size distribution that scattering formula particle size distribution measuring obtains is preferably 5~30 bodies in particle before cooperation Product %, further preferably 8~25 volume %, more preferably 10~20 volume %.

Further, before cooperation in particle, the sight of particle after being easy to get the cooperation with the behavior being slowly disintegrated Point sets out, and (e-2') partial size in size distribution obtained by laser diffraction/scattering formula particle size distribution measuring is 300 μm or more And the volume ratio (e-2'/b') of the amount of the amount of the particle (particle (e-2')) less than 550 μm and particle (b') be preferably 0.3 with On, further preferably 0.4 or more.Before cooperation in particle, from obtaining with the behavior that is slowly disintegrated and can also be effective Ground enters to after the cooperation of fine recess portion from the perspective of particle, is obtained by laser diffraction/scattering formula particle size distribution measuring The volume ratio (e-2'/b') of the amount of the amount and particle (b') of particle (e-2') in size distribution is preferably 1 hereinafter, further Preferably 0.95 or less.In addition, being divided before cooperation in particle by the granularity that laser diffraction/scattering formula particle size distribution measuring obtains The volume ratio (e-2'/b') of the amount of the amount and particle (b') of particle (e-2') in cloth is preferably 0.3~1, further preferably 0.4~0.95.

Before cooperation in particle, interact well from the particle (a) or particle (b) made after cooperation in particle, it is ensured that From the perspective of the behavior being slowly disintegrated, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution Grain (e-2') amount before cooperation in particle be preferably 2~15 volume %, further preferably 5~12 volume %, more preferably For 7~12 volume %.

In addition, before cooperation in particle, by laser diffraction/scattering formula particle size distribution measuring acquisition size distribution Partial size be 350 μm or more particle amount before cooperation in particle be preferably 5~50 volume %, further preferably 10~45 Volume %, more preferably 15~42 volume %.

R'(μm of the average grain diameter about particle before cooperating), from the viewpoint of with sufficient abrasive power, preferably 50 μm or more, further preferably 75 μm or more, more preferably 100 μm or more go out from the viewpoint of the foreign body sensation in inhibition oral cavity Hair, preferably 500 μm hereinafter, further preferably 450 μm hereinafter, more preferably 400 μm or less.Also, particle before cooperating R'(μm of average grain diameter) be preferably 50~500 μm, further preferably 75~450 μm, more preferably 100~400 μm.

In addition, the average grain diameter r' of particle is volume average particle size before cooperating, and for by laser diffraction/scattering formula grain The median particle diameter of the size distribution for the particle that the partial size that diameter measure of spread obtains is 50 μm or more.

About cooperate before particle intensity of disintegration, from after cooperation in the presence of dentifrice of the invention in particle really It protects from the perspective of the behavior being slowly disintegrated and higher dirt removal capacity, preferably 1gf/ or more, further preferably It is 2gf/ or more, more preferably 3gf/ or more.About the intensity of disintegration of particle before above-mentioned cooperation, from even by making The load of lower load whens with soft toothbrush etc. also assigns particle after the cooperation in the presence of dentifrice of the invention From the perspective of giving the viewpoint of appropriate disintegration and reducing foreign body sensation, preferably 20gf/ hereinafter, further preferably 15gf/ hereinafter, more preferably 10gf/ is a hereinafter, more preferably 8gf/ or less.In addition, the disintegration of above-mentioned particle is strong Degree preferably 1gf/ or more and 20gf/ a hereinafter, preferably 2~15gf/ is a, and further preferably 3~10gf/ is a, more Preferably 3~8gf/.

In addition, the intensity of disintegration of particle is value when measuring under moisture state before cooperation used in the present invention, it can To be found out and method same as the intensity of disintegration of particle after cooperation.In addition, about particle before cooperating, under moisture state Intensity of disintegration and drying regime under intensity of disintegration be identical value.

Area (S about the perspective plane of particle before cooperating_A') and with the maximum gauge (D in the perspective plane_L') it is diameter Circumscribed circle area (S_S') ratio (S_A'/S_S') average value, assigned from particle after the cooperation obtained to particle before with From the perspective of the behavior being slowly disintegrated, preferably 0.5 or more, further preferably 0.6 or more, more preferably 0.65 More than.Area (S about the perspective plane of particle before cooperating_A') and with the maximum gauge (D in the perspective plane_L') it is the outer of diameter Meet round area (S_S') ratio (S_A'/S_S') average value, particle is shown after the cooperation that particle obtains before making with The disintegration of appropriateness and from the perspective of effectively transmitting the load from toothbrush, preferably 0.9 hereinafter, further preferably It is 0.85 or less.In addition, cooperating the area (S on the perspective plane of preceding particle_A'), maximum gauge (D_L'), using it as the external of diameter Round area (S_S') and than (S_A'/S_S') average value be to be found out and method same as particle after above-mentioned cooperation Value.

About the maximum gauge (D in the perspective plane of particle before cooperating_L') and minimum diameter (D_S') ratio (D_L'/D_S') Average value, particle is obtained as unsetting and show the sight of particle after the cooperation of the behavior being slowly disintegrated before with Point sets out, and preferably 1.2 or more, further preferably 1.3 or more, more preferably 1.5 or more.About particle before cooperating Maximum gauge (D in perspective plane_L') and minimum diameter (D_S') ratio (D_L'/D_S') average value, particle obtains before with From the perspective of particle shows appropriate disintegration and effectively transmits the load from toothbrush after the cooperation obtained, preferably For 2 hereinafter, further preferably 1.8 hereinafter, more preferably 1.75 or less.In addition, before cooperating in the perspective plane of particle most Major diameter (D_L') and minimum diameter (D_S') ratio (D_L'/D_S') average value be preferably 1.2~2, further preferably 1.3~ 1.8, more preferably 1.5~1.75.

About particle after the cooperation in the presence of the dentifrice of the invention obtained by using particle before above-mentioned cooperation Amount, improve tartar or dirt removal effect from the disintegration behavior for fully playing the particle and improve use feeling Viewpoint is set out, in dentifrice of the invention be preferably 1 mass % or more, further preferably 3 mass % or more, it is more excellent It is selected as 5 mass % or more.About the amount of particle after the cooperation in the presence of dentifrice of the invention, foreign body sensation is never felt And not the enamel of damage tooth and from the perspective of playing tartar or dirt removal effect, in dentifrice of the invention Preferably 50 mass % hereinafter, further preferably 30 mass % hereinafter, more preferably 25 mass % hereinafter, further Preferably 20 mass % or less.In addition, the amount of particle cleans the teeth in of the invention after cooperation in the presence of dentifrice of the invention It is preferably 1~50 mass %, further preferably 3~30 mass %, more preferably 5~25 mass %, more into one in agent Step is preferably 5~20 mass %.

There is special shape or special granularity point as described above in the presence of dentifrice of the invention in order to obtain Particle after the cooperation of cloth, after following binders is preferably cooperated in dentifrice, particle is matched with dentifrice before cooperating In.Further, in the process after binder is cooperated in dentifrice, after particle before above-mentioned cooperation is added in dentifrice, Agitating device or mixing time are also depended on to the mixing speed that the dentifrice is stirred, but preferably with 10rpm with enterprising Row stirring, is further preferably stirred with mixing speed 20rpm or more, and preferably carried out with mixing speed 250rpm or less Stirring, additionally, it is preferred that being stirred with mixing speed 10rpm or more and 250rpm or less, further preferably with mixing speed 20rpm or more and 250pm or less is stirred.When stirring dentifrice with above-mentioned mixing speed, such as can use omnipotent mixed Close blender (manufacture of 5XDMV-10-r, Dalton company), paddle mixer (TK Paddle Mixer 2SL-10, special machine Device Co., Ltd.) etc. well known to blender be stirred, in the case where stating omnipotent mixing and blending machine in use, preferably incite somebody to action from The mixing speed turned is set as 40~230rpm, is more preferably set as 90~200rpm, preferably sets the mixing speed of revolution It is set to 20~110pm, is more preferably set as 35~75rpm.In the case where stating paddle mixer in use, the stirring of paddle Speed is preferably 10~70rpm, and the mixing speed of turbine is preferably 20~90rpm.In addition, in the stirring of dentifrice, as long as The particle in dentifrice can be made decentralized, in the case that low whipping speed is low speed, as long as mixing time is set as Long-time, in the case that low whipping speed is high speed, as long as mixing time is set as the short time.From above-mentioned sight Point sets out, and mixing time is preferably 5 minutes~90 minutes, and further preferably 10 minutes~60 minutes.

In the manufacturing method of dentifrice of the invention, it is preferably provided with before addition cooperates after particle, to the dentifrice The process being stirred.By having the process, so that particle includes more partial size before the cooperation with wide size distribution For 100~200 μm of particle, and the granularity of the partial size with the peak for being less than size distribution comprising more partial size can be obtained Particle after the cooperation of distribution.

Dentifrice of the invention is that cooperation contains mentioned component (A) and ingredient (B), ingredient as needed (C) or ingredient (D) made of particle, due to be present in the particle (particle after cooperation) after the cooperation in dentifrice have special shape or Special size distribution, and show the behavior being slowly disintegrated, therefore, from the synergy by foaming characteristic ensure compared with From the perspective of high cleaning effect, preferably further matching surface activating agent.Thus, it is possible to good foaming characteristic is brought, And continue foaming characteristic, it can fully bring the removal of tartar or dirt effect until as the gap of tooth and tooth Narrow region, smooth sense of touch can be assigned to facing in using the oral cavity after dentifrice of the invention, also improve make With sense.

As surfactant, anionic surfactant, nonionic surfactant, amphoteric ion table can be used Face activating agent.It as the anionic surfactant, such as can enumerate: the alkane such as NaLS, myristyl sulfate Base sulfate；The N- acyl sarcosinates such as N- sodium N-lauroyl sarcosinate, N- myristoy sarcosine sodium；N- palmityl The N- such as sodium glutamate acyl glutamate, N- methyl-N acyl methyltaurin sodium, N- methyl-N- acylalaninies sodium, alpha-olefin Sodium sulfonate, dioctyl sodium sulphosuccinate etc..As the anionic surfactant, from bringing good foaminess or use From the perspective of sense, preferably anionic surfactant, the more preferably alkyl sulfates such as NaLS.

About the use level of surfactant, from good foaming characteristic is ensured, improves and clean effect or use feeling and bring It is preferably 0.2 mass % or more, further preferably 0.3 matter in dentifrice of the invention from the perspective of good fragrance Measure % or more, more preferably 0.5 mass % or more.In addition, the use level about surfactant, damages fragrance from inhibition From the perspective of, in dentifrice of the invention be preferably 2.0 mass % hereinafter, further preferably 1.7 mass % hereinafter, More preferably 1.5 mass % or less.Further, the use level of surfactant is preferably 0.2 in dentifrice of the invention ~2.0 mass %, further preferably 0.3~1.7 mass %, more preferably 0.5~1.5 mass %.Of the invention cleans the teeth After above-mentioned cooperation in agent the mass ratio (particle/surfactant after cooperation) of particle and surfactant be preferably 0.5~ 250, more preferably 2~100, more preferably 4~40.

About the use level of anionic surfactant, from the good degree, cleaning effect or use feeling for improving foaming characteristic It is preferably 0.2 mass % or more in dentifrice of the invention, further preferably and from the perspective of bringing good fragrance For 0.3 mass % or more, more preferably 0.5 mass % or more.In addition, the use level about anionic surfactant, from It is preferably 2.5 mass % hereinafter, further preferably in dentifrice of the invention from the perspective of inhibiting damage fragrance 2.0 mass % are hereinafter, more preferably 1.7 mass %.Further, the use level of anionic surfactant is of the invention It is preferably 0.2~2.5 mass %, further preferably 0.3~2.0 mass %, more preferably 0.5~1.7 matter in dentifrice Measure %.About the use level of alkyl sulfate, from the good degree, cleaning effect or the use feeling that improve foaming characteristic and bring good It is preferably 0.2 mass % or more, further preferably 0.3 matter in dentifrice of the invention from the perspective of good fragrance Measure % or more, more preferably 0.5 mass % or more.In addition, the use level about alkyl sulfate, damages fragrance from inhibition From the perspective of, in dentifrice of the invention be preferably 2.5 mass % hereinafter, further preferably 2.0 mass % hereinafter, More preferably 1.7 mass % or less.Further, the use level of alkyl sulfate is preferably in dentifrice of the invention 0.2~2.5 mass %, further preferably 0.3~2.0 mass %, more preferably 0.5~1.7 mass %.

Dentifrice of the invention preferably further cooperates binder.As binder, can enumerate: carboxymethyl cellulose Sodium, Sodium Polyacrylate, hydroxyethyl cellulose, montmorillonite, xanthan gum, carragheen, sodium alginate, guar gum, pectin etc., can also To use a kind or 2 kinds or more in these, dentifrice is preferably toothpaste, and more preferably cooperation is selected from carboxymethyl cellulose It is one kind or two or more in sodium, xanthan gum and carragheen.About the use level of the binder in dentifrice of the invention, from Make mentioned component exist while dissolving, dispersing in oral cavity effectively to spread, effectively play and match using what is be slowly disintegrated The tartar of particle or dirt removal effect after conjunction, so as to improve the smooth sense of touch and decontamination sense of dental surface, by with The synergy of surfactant brings the viewpoint of good foaming characteristic, and the synergy by particle and surfactant Maintain brush teeth during good foaming characteristic from the perspective of, in dentifrice of the invention be preferably 0.1 mass % with On, further preferably 0.5 mass % or more, more preferably 0.7 mass % or more, and preferably 3 mass % hereinafter, into One step is preferably 2 mass % hereinafter, more preferably 1.8 mass % or less.In addition, the binder in dentifrice of the invention Use level in dentifrice of the invention be preferably 0.1~3 mass %, further preferably 0.5~2 mass %, more Preferably 0.7~1.8 mass %.(match about the mass ratio of particle and binder after the above-mentioned cooperation in dentifrice of the invention Particle/binder after conjunction), it effectively spreads, effectively plays from making mentioned component exist in oral cavity while dissolving, dispersing Out using the tartar or dirt removal effect of particle after the cooperation being slowly disintegrated, so as to improve the smooth of dental surface Sense of touch and decontamination sense, from the perspective of bringing good foaming characteristic, preferably 0.2~500, more preferably 1~60, more Add preferably 2.5~30.

From the viewpoint of improving storage stability or intraoral sense of touch, dentifrice of the invention is preferably in addition to above-mentioned Further cooperate thickening silica other than binder.Thickening silica refers to that oil absorption is 200~400mL/100g Silica, from oil absorption be the abrasive silica of 50~150mL/100g it is different.Here, oil absorption is to indicate two The oil mass that silica can support, measuring method are the methods by being based on JISK5101-13-2 (formulating for 2004), according to The amount of the boiled linseed oil absorbed carries out specific.The use level of thickening silica in dentifrice of the invention is at this In the dentifrice of invention be preferably 1 mass % or more, further preferably 2 mass % or more, more preferably 3 mass % with On, and preferably 15 mass % are hereinafter, further preferably 10 mass % or less.In addition, the increasing in dentifrice of the invention The use level of consistence silica is preferably 1~15 mass %, further preferably 2~10 mass %, more preferably 3~ 10 mass %.

Dentifrice of the invention can also further cooperate wetting agent.As wetting agent, can enumerate selected from sorbose It is alcohol, glycerol, propylene glycol, 1,3 butylene glycol, ethylene glycol, polyethylene glycol, polypropylene glycol, xylitol, maltitol, lactitol, red It is one kind or two or more in moss sugar alcohol etc..About the use level of the wetting agent in dentifrice of the invention, from making mentioned component one Side dissolution, dispersion are effectively spread in oral cavity on one side, are effectively played and are utilized particle after the cooperation being slowly disintegrated Tartar or dirt removal effect, with surfactant interact and from the perspective of bringing good foaming characteristic, in the present invention Dentifrice in preferably 5 mass % or more, further preferably 10 mass % or more, more preferably 15 mass % or more, And preferably 60 mass % hereinafter, further preferably 50 mass % hereinafter, more preferably 40 mass % or less.In addition, The use level of wetting agent in dentifrice of the invention is preferably 5~60 mass % in dentifrice of the invention, further excellent It is selected as 10~50 mass %, more preferably 15~40 mass %.

Dentifrice of the invention can also further hydrous water.About the amount of moisture in dentifrice of the invention, from making It states ingredient and exists while dissolving, dispersing and effectively spread in oral cavity, effectively play and utilize the particle being slowly disintegrated Tartar or dirt removal effect can also be played higher even with the lower load of the loads such as soft toothbrush Soil removal capabilities, in addition, from the perspective of bringing good foaming characteristic with surfactant interaction, of the invention It is preferably 3 mass % or more, further preferably 5 mass % or more, more preferably 7 mass % or more in dentifrice, and excellent 50 mass % are selected as hereinafter, further preferably 45 mass % are hereinafter, more preferably 40 mass % or less.In addition, about this Amount of moisture in the dentifrice of invention, from the sight for bringing good dissolubility or dispersibility and tartar or soil removal capabilities Point set out, in dentifrice of the invention be preferably 3~50 mass %, further preferably 5~45 mass %, more preferably For 7~40 mass %.In addition, the amount of moisture is by the amount of moisture in amount of moisture and other ingredients joined together joined together All add up obtained amount, these can also be calculated by each use level using calculating, such as can use karl Fischer water Meter is divided to be measured.As karl Fischer moisture meter, (the flat natural pond industry strain formula meeting of determination of trace water device can be used for example Society).For the device, dentifrice 5g can be taken, is allowed to be suspended in anhydrous methanol 25g, divides and suspension 0.02g is taken to carry out Measured amount of moisture, is set as the use level of water by measurement.About particle after the above-mentioned cooperation in dentifrice of the invention and The ratio (pellets/water component after cooperation) of amount of moisture, from bringing good dissolubility or dispersibility and tartar or dirt to remove From the perspective of ability, preferably 0.02~15, more preferably 0.1~6, more preferably 0.2~3.

Dentifrice of the invention preferably cooperates pH adjusting agent.As the pH adjusting agent, the wind of the invention from improvement Taste from the perspective of preventing harmfulness, can be enumerated: phosphoric acid and its salt (sodium phosphates such as disodium hydrogen phosphate, sodium dihydrogen phosphate Deng), citric acid and its salt, malic acid and its salt, gluconic acid and its salt, maleic acid and its salt, aspartic acid and its salt, Portugal Grape saccharic acid and its salt, succinic acid and its salt, glucuronic acid and its salt, fumaric acid and its salt, glutamic acid and its salt, adipic acid and Its salt, hydrochloric acid, sodium hydroxide, potassium hydroxide etc. can be used a kind in these or it is preferable to use two or more.This hair Bright dentifrice preferably comprises phosphoric acid in disodium hydrogen phosphate, sodium dihydrogen phosphate and its salt as pH adjusting agent.PH value As long as the use level of regulator becomes desired pH value, it is not particularly limited, in dentifrice of the invention preferably 0.01~5 mass %, further preferably 0.1~3 mass %.In addition, the pH value of dentifrice of the invention is preferably greater than 7, into One step is preferably 7.5 or more, and more preferably 7.8 or more, and preferably 11 hereinafter, further preferably 10 hereinafter, more excellent It is selected as 9.5 or less.Here, the pH value of dentifrice of the invention refer to when being diluted with water to 10 mass % using pH electrode benefit The value measured at 25 DEG C.

Dentifrice of the invention can cooperate other ingredients other than the above, such as grinding agent, excipient, sweetener, anti- Rotten agent, fragrance, medicinal ingredient, colorant, other commonly used ingredients.

Above-mentioned other ingredients can be used alone, and can also combine two or more use.

About above-mentioned embodiments of the present invention, dentifrice particle and dentifrice below are further disclosed.

[1] a kind of dentifrice, wherein the dentifrice is cooperation containing water-insoluble dusty material (A) and inorganic viscous Made of the particle of mixture (B),

[2] such as the dentifrice of above-mentioned [1], wherein about being present in the particle after the cooperation in dentifrice, the particle Maximum gauge (D in perspective plane_L) and minimum diameter (D_S) ratio (D_L/D_S) average value be preferably 1.8 hereinafter, further it is excellent Be selected as 1.7 hereinafter, more preferably 1.65 hereinafter, and preferably 1.2 or more, further preferably 1.3 or more, more preferably It is 1.4 or more.

[3] such as the dentifrice of above-mentioned [1] or [2], wherein the area (S on the perspective plane of the particle after cooperation_A) and with this Maximum gauge (D in perspective plane_L) be diameter circumscribed circle area (S_S) ratio (S_A/S_S) average value be preferably 0.6 with On, further preferably 0.65 or more, be still more preferably 0.7 or more, and preferably 0.85 hereinafter, further preferably 0.82 or less.

[4] a kind of dentifrice, wherein the dentifrice is cooperation containing water-insoluble dusty material (A) and inorganic viscous Made of the particle of mixture (B),

(a) partial size is 50 μm of particles more than and less than 100 μm；

(b) partial size is 100 μm of particles more than and less than 150 μm；

(c) partial size is 150 μm of particles more than and less than 200 μm；

(d) partial size is 200 μm of particles more than and less than 250 μm.

[5] such as the dentifrice of above-mentioned [4], wherein in particle after engagement, by laser diffraction/scattering formula particle diameter distribution The volume ratio (b/c) for measuring the amount of the particle (b) in the size distribution obtained and the amount of particle (c) is preferably 0.75 or more, into One step is preferably 0.8 or more, and preferably 1.1 hereinafter, further preferably 1.0 hereinafter, more preferably 0.95 or less.

[6] such as the dentifrice of above-mentioned [4] or [5], wherein in particle after engagement, by laser diffraction/scattering formula grain The volume ratio (d/c) of the amount of the amount and particle (c) for the particle (d) in size distribution that diameter measure of spread obtains is preferably 0.25 More than, further preferably 0.3 or more, and preferably 0.9 hereinafter, further preferably 0.85 hereinafter, more preferably 0.8 Below.

[7] as above-mentioned [4] to any one of [6] dentifrice, wherein in particle after engagement, by laser diffraction/ The volume ratio (b/d) of the amount and the amount of particle (d) of the particle (b) in size distribution that scattering formula particle size distribution measuring obtains is excellent 1.1 or more, further preferably 1.2 or more, and preferably 4 are selected as hereinafter, further preferably 2.8 or less.

[8] as above-mentioned [4] to any one of [7] dentifrice, wherein in particle after engagement, by laser diffraction/ The amount for the particle (c) in size distribution that scattering formula particle size distribution measuring obtains is preferably 20 volume % or more, further preferably For 23 volume % or more, and preferably 50 volume % hereinafter, further preferably 45 volume % hereinafter, more preferably 40 bodies Product % or less.

[9] as above-mentioned [4] to any one of [8] dentifrice, wherein in particle after engagement, particle (b) with The total amount of grain (c) is preferably 30 volume % or more, further preferably 35 volume % or more, more preferably 40 volume % More than, be still more preferably 50 volume % or more, and preferably 85 volume % hereinafter, further preferably 80 volume % with Under, more preferably 75 volume % or less.

[10] as above-mentioned [4] to any one of [9] dentifrice, wherein in particle after engagement, by laser diffraction/ The total amount and particle (c) and particle for the particle (a) and particle (b) in size distribution that scattering formula particle size distribution measuring obtains (d) volume ratio ((a+b)/(c+d)) of total amount is preferably 0.5 or more, and further preferably 0.6 or more, more preferably 0.65 or more, and preferably 1 hereinafter, further preferably 0.9 hereinafter, more preferably 0.85 or less.

[11] such as the dentifrice of above-mentioned [4] to any one of [10], wherein in particle after engagement, spread out by laser Penetrate/scatter the total amount of the particle (a) and particle (b) in the size distribution of formula particle size distribution measuring acquisition and the amount of particle (e) Volume ratio ((a+b)/e) be preferably greater than 1, further preferably 1.1 or more, more preferably 1.2 or more, further it is excellent 1.3 or more, and preferably 20 are selected as hereinafter, further preferably 18 or less.

[12] such as the dentifrice of above-mentioned [4] to any one of [11], wherein in particle after engagement, spread out by laser The amount for the particle (a) penetrated/scatter in the size distribution of formula particle size distribution measuring acquisition is preferably 3 volume % or more, further excellent 5 volume % or more, more preferably 7 volume % or more are selected as, and preferably 15 volume % are hereinafter, further preferably 12 bodies % is hereinafter, more preferably 10 volume % or less for product.

[13] such as the dentifrice of above-mentioned [4] to any one of [12], wherein in particle after engagement, spread out by laser The amount for the particle (b) penetrated/scatter in the size distribution of formula particle size distribution measuring acquisition is preferably 12 volume % or more, further Preferably 15 volume % or more, more preferably 20 volume % or more, and preferably 50 volume % are hereinafter, further preferably 40 volume % are hereinafter, more preferably 35 volume % or less.

[14] such as the dentifrice of above-mentioned [4] to any one of [13], wherein in particle after engagement, spread out by laser The amount for the particle (d) penetrated/scatter in the size distribution of formula particle size distribution measuring acquisition is preferably 5 volume % or more, further excellent 10 volume % or more, more preferably 12 volume % or more are selected as, and preferably 25 volume % are hereinafter, further preferably 22 Volume % is hereinafter, more preferably 20 volume % or less.

[15] such as the dentifrice of above-mentioned [4] to any one of [14], wherein containing by laser in particle after engagement Partial size is 250 μm of particles (e) more than and less than 350 μm in the size distribution that diffraction/scattering formula particle size distribution measuring obtains, And the amount of particle (e) is preferably greater than 0 volume %, further preferably 1 volume % or more, more preferably 2 volume % or more, And preferably 25 volume % hereinafter, further preferably 20 volume % hereinafter, more preferably 18 volume % or less.

[16] such as the dentifrice of above-mentioned [1] to any one of [15], wherein the intensity of disintegration of the particle after cooperation is preferred It is 2gf/ or more, further preferably 3gf/ or more, and preferably 15gf/ is a hereinafter, further preferably 10gf/ Hereinafter, more preferably 8gf/ or less.

[17] such as the dentifrice of above-mentioned [1] to any one of [16], wherein the water-insoluble powder in the particle after cooperation The content of powder material (A) in the dry state be preferably 60 mass % or more, further preferably 70 mass % or more, more Preferably 80 mass % or more, more preferably 82 mass % or more, and preferably 98 mass % are hereinafter, further preferably 96 mass % are hereinafter, more preferably 90 mass % or less.

[18] such as the dentifrice of above-mentioned [1] to any one of [17], wherein water-insoluble dusty material (A) preferably selects From one kind or two or more in powdered whiting, precipitated calcium carbonate, zeolite and silica, further preferably heavy carbonic acid Calcium.

[19] such as the dentifrice of above-mentioned [1] to any one of [18], wherein inorganic bond (B) includes to be selected from sodium metasilicate And a kind in colloidal silicon dioxide or 2 kinds, and sodium metasilicate is selected from inorganic bond (B) contained in the particle after cooperating 1 kind or 2 kinds of content in (solid content ingredient) and colloidal silicon dioxide is preferably 60 mass % or more, further preferably 80 mass % or more, more preferably 90 mass % or more, and preferably 100 mass % or less.

[20] such as the dentifrice of above-mentioned [1] to any one of [19], wherein as selected from sodium metasilicate (solid content ingredient) And the content of a kind or 2 kinds of ingredient (B) in colloidal silicon dioxide is preferably 1 matter in particle in the dry state after engagement Measure % or more, further preferably 2 mass % or more, more preferably 5 mass % or more, more preferably 10 mass % with On, and preferably 30 mass % hereinafter, further preferably 20 mass % hereinafter, more preferably 18 mass % or less.

[21] such as the dentifrice of above-mentioned [1] to any one of [20], wherein the particle after cooperation is preferably comprised selected from silicon One kind or two or more bonding agent (C) in sour calcium, magnesia, titanium oxide and zinc oxide, further, the content of ingredient (C) It is in the dry state preferably 0.2 mass % or more, further preferably 0.5 mass % or more, more preferably 0.8 matter Measure % or more, and preferably 5 mass % hereinafter, further preferably 3 mass % hereinafter, more preferably 2 mass % hereinafter, It is still more preferably 1.2 mass % or less.

[22] such as the dentifrice of above-mentioned [1] to any one of [21], wherein the amount of the particle after cooperation is preferably 1 matter Measure % or more, further preferably 3 mass % or more, more preferably 5 mass % or more, and preferably 50 mass % hereinafter, Further preferably 30 mass % are hereinafter, more preferably 20 mass % or less.

[23] such as the dentifrice of above-mentioned [1] to any one of [22], wherein the particle after cooperation is preferably by rolling Comminution granulation and obtain, additionally, it is preferred that for addition cooperation before particle after with mixing speed 10rpm or more and 250rpm or less It stirs dentifrice and obtains.

[24] such as the dentifrice of [1] to any one of [23], wherein preferably comprise binder, further preferably select From the one kind or two or more binder in sodium carboxymethylcellulose, xanthan gum and carragheen.

[25] such as the dentifrice of above-mentioned [1] to any one of [24], wherein about for the particle after being cooperated Particle before cooperation, the particle below (b') in the size distribution obtained by laser diffraction/scattering formula particle size distribution measuring In~(e-1'), the volume ratio (b'/c') of the amount of the amount and particle (c') of particle (b') be preferably 0.6 or more and 1.25 hereinafter, The volume ratio (d'/c') of the amount of the amount and particle (c') of particle (d') is preferably 0.7 or more and 1.2 hereinafter, particle (e-1') The volume ratio (e-1'/c') of amount and the amount of particle (c') be preferably 0.4 or more and 1.1 hereinafter,

(b') partial size is 100 μm of particles more than and less than 150 μm；

(c') partial size is 150 μm of particles more than and less than 200 μm；

(d') partial size is 200 μm of particles more than and less than 250 μm；

(e-1') partial size is 250 μm of particles more than and less than 300 μm.

[26] such as the dentifrice of above-mentioned [25], wherein the intensity of disintegration of the particle before cooperation is preferably 1gf/ or more, Further preferably 2gf/ or more, more preferably 3gf/ or more, and preferably 20gf/ is a hereinafter, further preferably 15gf/ hereinafter, more preferably 10gf/ or less.

[27] a kind of manufacturing method of dentifrice, wherein be the dentifrice for manufacturing above-mentioned [1] to any one of [26] Method has: after cooperation binder, the process of adding particle；And it is stirred with mixing speed 10rpm or more and 250rpm or less The process for mixing the dentifrice added with particle.

Embodiment

Hereinafter, being specifically explained based on embodiment to the present invention.In addition, as long as no particularly showing in table, then respectively The use level of ingredient indicates the total amount (quality %) of each ingredient in the presence of dentifrice.In addition, the measurement of each physics value passes through The following method carries out.

" 1: the measuring method of the average grain diameter of water-insoluble powder "

The average grain diameter of water-insoluble powder using laser diffraction/scattering formula particle size distribution device (LA-920, HORIBA company manufacture), in solvent: ion exchange water, refractive index: 1.2, circulation rate (scale: 4), mixing speed (scale: 3) it is measured under conditions of.

" 2: the solid content ingredient of sodium metasilicate "

Using dropper by 2.5g sample in such a way that 1 drop becomes the drop of 5~10mm of diameter or so (so that drop is each other Mode as nonoverlapping as possible) be added dropwise be disseminated to aluminum diameter be 11.5cm container on, thereafter, use infrared moisture Meter (manufacture of Co., Ltd., KETT Science Institute, FD240), with moisture benchmark moisture mode determination in 105 DEG C of temperature, Auto Condition (be considered as final tested volume when becoming the variable quantity of measured value within 0.05% in 30 seconds and terminate to measure) Under be measured, remove measured volatilization free moisture, thus calculate.

" 3: the size distribution of particle and the measuring method of average grain diameter before cooperating "

It is measured using the aqueous solution that particle before being cooperated by ion exchange water is diluted to 5 mass %.For passing through Particle is diluted to the aqueous solution of 5 mass % before ion exchange water will cooperate, by mixing machine (ROTARY MIXER NPC-20, The manufacture of NISSIN company), disperse particle under conditions of 75 revs/min, horizontal direction rotation, 2 hours.Then, will disperse There is the aqueous solution of particle to save 1 day under room temperature (25 DEG C).Make the aqueous solution after the preservation point again by above-mentioned mixing machine It dissipates 10 minutes, then, using the aqueous solution, utilizes laser diffraction/scattering formula particle size distribution device (Partica LA- The manufacture of 950V2, HORIBA company), in refractive index: 1.58, circulation rate (scale: 5), mixing speed (scale: condition 5) Under be measured.In addition, using ion exchange water as solvent.

" 4: the area (S on the perspective plane of particle after cooperation_A), maximum gauge (D_L), with D_LFor the area of the circumscribed circle of diameter (S_S) and minimum diameter (D_S)》

(i) area on the perspective plane of particle will by pure water using 150 μm of sieve of JISZ8801-1 standard after cooperating After being cleaned using the aqueous solution that pure water is diluted to the dentifrice of 10 mass %, by the particle remained on sieve in room temperature (25 DEG C) under dry 1 day, be measured using particle obtained.

(ii) area (S on perspective plane_A), maximum gauge (D_L) and minimum diameter (D_S) measurement be using KEENCE VH- 5500 (100 times of multiplying powers) are photographed, using analysis software (WinROOF (three paddy business Co., Ltd.)) as obtained by photographing Digital picture obtain each particle a perspective plane area (S_A), maximum gauge (D_L), minimum diameter (D_S).It will pass through The data of 5~10 particles of measurement and acquisition are average, the area (S on a perspective plane as each particle_A), maximum gauge (D_L), minimum diameter (D_S).Based on these data, the area (S on a perspective plane of particle is further found out_A) and with maximum straight Diameter (D_L) be diameter circumscribed circle area (S_S) ratio (S_A/S_S), maximum gauge (D_L) and minimum diameter (Ds) ratio (D_L/ Ds)。

" 5: being present in the size distribution, average grain diameter of particle and the measuring method of amount after the cooperation in dentifrice "

(i) dentifrice the decentralized processing of the particle in the aqueous solution of measurement: is diluted to 10 to by ion exchange water Aqueous solution obtained from quality %, by mixing machine (manufacture of ROTARY MIXER NPC-20, NISSIN company) at 75 revs/min Clock, horizontal direction rotation dispersed particle under conditions of 2 hours.Then, it is obtained being diluted to the dentifrice after dispersion The aqueous solution obtained saves 1 day under room temperature (25 DEG C).Make the aqueous dispersion 10 after the preservation again by above-mentioned mixing machine After minute, handled with laser diffraction/scattering formula particle diameter distribution device.

Particle is extracted according to method identical with (i) of " 4 ".

(ii) measurement of size distribution, average grain diameter and amount: laser diffraction/scattering formula particle size distribution analyzer is used (manufacture of Partica LA-950V2, HORIBA company), in refractive index: 1.58, circulation rate (scale: 5), mixing speed (carve Degree: 5) particle after powder obtained and cooperation is measured under conditions of.Use ion exchange water as solvent.

In addition, in the present invention, according to the granularity measured by laser diffraction/scattering formula distribution of particles measurement device point Cloth calculates the amount (volume %) of particle (a)~(e) ((a')~(e')) of each particle size range.Specifically, for laser is passed through The range of each partial size of diffraction, by the content of the range of each partial size calculated multiplied by the ratio of particle size range particle (a)~ (e) amount.For example, the partial size obtained using laser diffraction be 45 μm of particles more than and less than 51 μm be 0.2 volume %, In the case that 51 μm of particles more than and less than 101 μm are 7.5 volume %, the content of particle (a) is 0.2 volume % × 1/ (51-45)+7.5 volume % × (100-51)/(101-51), calculated result are 7.4 volume %.

[Production Example 1: the manufacture of particle A'~E' before cooperating]

By powdered whiting (CALFINE CO., LTD. manufacture, quotient in a manner of becoming the particle of content shown in table 1 The name of an article: ACE-25, about 3 μm of average grain diameter) it puts into the mixture of various bonding agents (C) to the 75L rotary drum with partition PelletizerIn, on one side at 12.6 ° of 0.2/ drum angular of rotary drum revolving speed 30r.p.m/ Froude number Under the conditions of mix and add sodium metasilicate by spraying using 1 external mix type second fluid nozzle (manufacture of Atomax Co., Ltd.) on one side (Fuji Chemical Industry Co., Ltd's manufacture, trade name: No. 3 sodium metasilicate: Na₂·3SiO₂Solution, solid content ingredient 38.5%, benefit With 3 times of amount water below dilutions, 25 DEG C) it is granulated.In addition, batch size is 8kg.The addition speed of sodium silicate aqueous solution Degree is 3.3ml/ minutes.

After spraying sodium silicate aqueous solution, continuess to mix 1 minute, then, be discharged from rotary drum granulator, use electric canopy After drying machine is 90 minutes dry at 80 DEG C, particle A'~E' before cooperating is obtained.

The size distribution of particle A'~F' before each cooperation is shown in Table 2, and the size distribution of preceding particle B' will be cooperated Curve graph it is shown in Figure 1.

[table 1]

[table 2]

[Examples 1 to 10, comparative example 1]

It is formulated according to shown in table 3, adds particle A'~F' and each ingredient before cooperation obtained, filled using omnipotent mixing (manufacture of 5XDMVV10-r, Dalton company) is set to stir at the mixing speed 75rpm of revolution, the mixing speed 200rpm of rotation 10 minutes, obtain the dentifrice of particle A~F after the cooperation that particle A'~F' is obtained before being respectively present with.

Then, using each dentifrice, each evaluation is carried out by the following method.

It shows the result in table 3.

In addition, the size distribution of particle A~F is shown in Table 4 after the cooperation that will be present in each dentifrice, by embodiment 1 Dentifrice in the presence of cooperation after particle B size distribution curve graph it is shown in Figure 1, and particle B SEM (electricity Sub- microscope: Hitachi S-4800) photo it is shown in Figure 2.It further, will be after the cooperation in the presence of the dentifrice of comparative example 1 The curve graph of the size distribution of particle F is shown in Figure 3.

[test example 1: the evaluation of tartar removal ability (dirt removal rate)]

Using relief pattern below and dirty model, scrub test is carried out as follows, and is calculated dirt and gone Except rate.It shows the result in table 3.

(relief pattern)

Prepare to be set at intervals and in parallel on long 15mm × wide 15mm × thickness 3mm stainless steel with 620 μm and angled is 90 DEG C of 100 μm of linear width, 100 μm of depth groove relief pattern.

(dirty model)

Above-mentioned concave-convex mold is rubbed into using red wax crayon (Pentel company manufactures, CRAYON RED) as dirty model The entirety of the groove of type is filled, by make the horizontal plane of scraper along relief pattern surface slide and will be in concave-convex mold The surface of type dirty model outstanding or the dirty model removal for being attached to surface.

(scrub test)

Above-mentioned relief pattern is embedded in the 15mm × 15mm for being set to the center of aluminium sheet (30mm × 80mm × 5mm) The recess portion of the square of × 3mm, in each dentifrice 2g, toothbrush (Deep Clean Compact, flower king manufacture), brush swepting slip part: Load 200g, speed 80rpm, amplitude 30mm, 1 minute, brush swept direction: being parallel to the direction in the direction of the groove of relief pattern Under conditions of carry out scrub test.In addition, being arranged on the angle of the recess portion of the square of aluminium sheet in the outside of square Having, which makes relief pattern be easy digging out for taking-up, uses recess portion.

(calculation method of dirt removal rate)

After scrub, relief pattern is taken out from aluminium sheet, after washing, the dentifrice for being attached to the surface of relief pattern passes through On one side by the surface of relief pattern press on paper (PPC paper A4 size, KOKUYO) be allowed on one side slide and remove.

It to the relief pattern before scrub and eliminates the relief pattern of dentifrice using digital camera and photographs, will brush The area in the region coloured in the relief pattern before washing by wax crayon is set as painted areas area (mm²).In addition, will coloring The area in the region scrubbed in region by toothbrush is set as evaluation region area (mm²), by wax in the evaluation region Pen is removed and the area (mm of the part of the bottom surface of recess portion exposing (bleaching)²) it is set as dirt removal area.Then, under It states formula (1) and calculates the dirt removal area relative to evaluation region area entirety as dirt removal rate (%).In addition, coloring Region area is the area that the region of the coloring generated by false fouling material is detected when being photographed using digital camera, The region swept in the region through toothbrush brush is set as evaluation region.

Dirt removal rate (%)=(it is whole that dirt removes area/evaluation region area) × 100 (1)

Even if carrying out the case where brush is swept merely with toothbrush in flat face in addition, being rubbed into the wax crayon of the recess portion of breadboard Under, as long as also applying specific load, wax crayon falls off and exposes the face of breadboard.In addition, in the photography using digital camera In, using flash lamp, polaroid filter is used in order to eliminate surface reflection.

[test example 2: the evaluation of use feeling]

Using various dentifrice 1g obtained in Examples 1 to 10 and comparative example 1, toothbrush (Check is used Standard, flower king manufacture) it scrubs, according to benchmark shown in following to foaming characteristic, alveolar substance (sophistication of foam), brush Bubble duration, the granular sensation at initial stage of brushing teeth during tooth, just brush teeth after smooth feeling, brush teeth during granular sensation hold Continuous property is evaluated, to foaming characteristic, alveolar substance, the granular sensation at initial stage of brushing teeth, just brush teeth after smooth feeling carry out 1~5 5 grades Evaluation.Above-mentioned evaluation is carried out by 5 professional evaluators, its average value is found out according to result obtained.

In addition, in above-mentioned evaluation, for during brushing teeth bubble duration, brush teeth during granular sensation duration, It counts in 5 professional evaluators and answers lasting number.It shows the result in table 2.

" foaming characteristic "

5: particularly well blistering

4: blistering well

3: blistering

2: being difficult to blister

1: not blistering

" alveolar substance (sophistication of foam) "

5: feeling that foam is very fine and smooth

4: feeling that foam is fine and smooth

3: feeling that foam is somewhat fine and smooth

2: feeling that foam is somewhat coarse

1: feeling that foam is coarse

" granular sensation at initial stage of brushing teeth "

5: feel appropriate particle there are senses

4: feel particle there are senses

3: particle that there are senses is small

2: particle that there are senses is minimum

1: totally can not feel the presence of particle

" smooth feeling after just brushing teeth "

Sense of touch in the facing sliding tongue after just brushing teeth (after gargling dentifrice using water).

5: very smooth, the presence of imperceptible dirt

4: it is smooth, hardly feel the presence of dirt

3: it is somewhat smooth, but slightly feel the presence of dirt

2: slightly discovery is concave-convex, slightly feels the presence of dirt

1: feeling that dental surface has the bumps caused by dirt

[table 4]

According to the above results it is found that the dentifrice of Examples 1 to 10 compared with the dentifrice of comparative example 1 have it is excellent Use feeling.

Claims

1. a kind of dentifrice, wherein

The dentifrice is combined with made of particle, and the particle contains water-insoluble dusty material (A) and inorganic bond (B),

Water-insoluble dusty material (A) is a kind or 2 in powdered whiting, precipitated calcium carbonate, zeolite and silica Kind or more,

Inorganic bond (B) is a kind or 2 kinds in sodium metasilicate and colloidal silicon dioxide,

The content of ingredient (B) in particle be in the dry state 1 mass % or more and 30 mass % hereinafter,

About the particle after the cooperation being present in the dentifrice, the area S on the perspective plane of the particle_AWith in the perspective plane Maximum dimension D_LThe area S of circumscribed circle as diameter_SRatio S_A/S_SAverage value be 0.7 or more and 0.9 hereinafter, and cooperating The intensity of disintegration of particle afterwards be 1gf/ or more and 20gf/ it is a hereinafter,

About being present in the particle after the cooperation in dentifrice, the maximum dimension D in the perspective plane of the particle_LWith minimum diameter D_S Ratio D_L/D_SAverage value be 1.2 or more and 1.8 hereinafter,

About the particle after the cooperation being present in the dentifrice, obtained by laser diffraction/scattering formula particle size distribution measuring In particle (a)~(d) below in size distribution, the volume ratio b/c of the amount of the amount and particle (c) of particle (b) is 0.7 or more And 1.2 hereinafter, the volume ratio b/d of the amount of the amount and particle (d) of particle (b) is greater than 1 and for 5 hereinafter, particle (a) and particle (b) Total amount and particle (c) and particle (d) total amount volume ratio (a+b)/(c+d) be 0.5 or more and 1 hereinafter,

(a) partial size is 50 μm of particles more than and less than 100 μm；

(b) partial size is 100 μm of particles more than and less than 150 μm；

(c) partial size is 150 μm of particles more than and less than 200 μm；

(d) partial size is 200 μm of particles more than and less than 250 μm.

2. dentifrice as described in claim 1, wherein

About being present in the particle after the cooperation in dentifrice, the maximum dimension D in the perspective plane of the particle_LWith minimum diameter D_S Ratio D_L/D_SAverage value be 1.4 or more and 1.65 or less.

3. dentifrice as claimed in claim 1 or 2, wherein

About being present in the particle after the cooperation in dentifrice, the area S on the perspective plane of the particle_AWith in the perspective plane most Major diameter D_LThe area S of circumscribed circle as diameter_SRatio S_A/S_SAverage value be 0.7 or more and 0.82 or less.

4. dentifrice as described in claim 1, wherein

The volume ratio d/c of particle (d) and particle (c) is 0.2 or more and 1 hereinafter, the amount of the particle (c) in particle after cooperation is 15 volume % or more and 55 volume % hereinafter, and the particle after cooperating intensity of disintegration be 1gf/ or more and 20gf/ it is a with Under.

5. dentifrice as claimed in claim 4, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The total amount of particle (a) and particle (b) in degree distribution is greater than 1 with volume ratio (a+b)/e of the amount of particle (e) below and is 20 hereinafter,

(e) partial size is 250 μm of particles more than and less than 350 μm.

6. dentifrice as claimed in claim 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains Degree distribution in particle (a) and particle (b) total amount and particle (e) amount volume ratio (a+b)/e for 1.1 or more and 18 with Under.

7. dentifrice as claimed in claim 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains Degree distribution in particle (a) and particle (b) total amount and particle (e) amount volume ratio (a+b)/e for 1.3 or more and 18 with Under.

8. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains Volume ratio (a+b)/(c+ of the total amount of the total amount and particle (c) and particle (d) of particle (a) and particle (b) in degree distribution It d) is 0.65 or more and 0.85 or less.

9. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The volume ratio b/c of the amount of the amount and particle (c) of particle (b) in degree distribution is 0.8 or more and 0.95 or less.

10. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The volume ratio d/c of the amount of the amount and particle (c) of particle (d) in degree distribution is 0.3 or more and 0.8 or less.

11. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The volume ratio b/d of the amount of the amount and particle (d) of particle (b) in degree distribution is 1.2 or more and 2.8 or less.

12. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The amount of particle (a) in degree distribution is 3 volume % or more and 15 volume % or less.

13. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The amount of particle (b) in degree distribution is 12 volume % or more and 50 volume % or less.

14. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The amount of particle (c) in degree distribution is 23 volume % or more and 40 volume % or less.

15. dentifrice as described in claim 4 or 5, wherein

About being present in the particle after the cooperation in dentifrice, the total amount of particle (b) and particle (c) be 40 volume % or more and 75 volume % or less.

16. dentifrice as described in claim 4 or 5, wherein

About the particle after the cooperation in dentifrice is present in, pass through the grain that laser diffraction/scattering formula particle size distribution measuring obtains The amount of particle (d) in degree distribution is 5 volume % or more and 25 volume % or less.

17. dentifrice as described in claim 4 or 5, wherein

Contain the grain obtained by laser diffraction/scattering formula particle size distribution measuring in particle after being present in the cooperation in dentifrice Partial size is 250 μm of particles (e) more than and less than 350 μm in degree distribution, and the amount of particle (e) is greater than 0 volume % and is 20 bodies Product % or less.

18. dentifrice as claimed in claim 1 or 2, wherein

The content of inorganic bond (B) is 2 mass % in the particle being present in after the cooperation in dentifrice in the dry state Above and 30 mass % or less.

19. dentifrice as claimed in claim 1 or 2, wherein

The amount of particle after being present in the cooperation in dentifrice is 1 mass % or more and 50 mass % or less.

20. dentifrice as claimed in claim 1 or 2, wherein

Particle after being present in the cooperation in dentifrice is obtained by rolling comminution granulation.

21. dentifrice as claimed in claim 1 or 2, wherein

Particle after being present in the cooperation in dentifrice contain a kind in calcium silicates, magnesia, titanium oxide and zinc oxide or Bonding agent (C) of more than two kinds.

22. dentifrice as claimed in claim 21, wherein

In particle after being present in the cooperation in dentifrice, bonding agent (C) and the mass ratio C/B of inorganic bond (B) are 0.02 or more and 1 or less.

23. dentifrice as claimed in claim 1 or 2, wherein

About the particle being added to before cooperating used in dentifrice, obtained by laser diffraction/scattering formula particle size distribution measuring Size distribution in particle below (b')~(e-1') in, the volume ratio b' of the amount of the amount and particle (c') of particle (b')/ C' be 0.6 or more and 1.25 hereinafter, the volume ratio d'/c' of the amount of the amount and particle (c') of particle (d') be 0.7 or more and 1.2 with Under, the volume ratio e-1'/c' of the amount of the amount and particle (c') of particle (e-1') is 0.4 or more and 1.1 hereinafter, and before cooperation The intensity of disintegration of particle is 1gf/ or more and 20gf/ hereinafter, the particle before the cooperation is present in dentifrice for obtaining In cooperation after particle,

(b') partial size is 100 μm of particles more than and less than 150 μm；

(c') partial size is 150 μm of particles more than and less than 200 μm；

(d') partial size is 200 μm of particles more than and less than 250 μm；

(e-1') partial size is 250 μm of particles more than and less than 300 μm.

24. dentifrice as claimed in claim 1 or 2, wherein

After particle after being present in the cooperation in dentifrice is the particle before addition cooperation, with mixing speed 10rpm or more and 250rpm or less is stirred dentifrice and obtains.

25. a kind of manufacturing method of dentifrice, wherein

It is the method for dentifrice described in any one of manufacturing claims 1~24, the dentifrice is to be combined with particle to form , the particle contains water-insoluble dusty material (A) and inorganic bond (B),

Have: after cooperating binder, the process of the particle before addition cooperation, the particle before the cooperation makes an addition to dentifrice Middle use；And with the process of mixing speed 10rpm or more and the 250rpm dentifrice stirred below added with particle.