JPS5938201B2 - toothpaste - Google Patents

Abstract

1413026 Particulate materials COLGATEPALMOLIVE CO 24 Aug 1973 [28 Aug 1972 3 Aug 1973] 40274/73 Heading A5B A finely divided particulate material for use in dentifrices comprises particles of a matrix of a meltable pharmaceutically acceptable binding material and between 5 and 10% by weight of an anti-irritant compound selected from allantoin, aluminium dihydroxy allantoinate and aluminium chlorohydroxyallantoinate and mixtures thereof, the meltable binding material having a melting or softening point lower than the decomposition or melting point of the anti-irritant compound, the particles having a size of 100 to 1000 microns. The binding material may be a C 12 -C 22 saturated fatty acid di- or tri-ester of glycerol or ethylene glycol, e.g. glyceryl tristearate, or a resin, gum, gel, wax or polymer. The dentifrices may also contain conventional additives and antibacterial agents, a number of which are specified.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a toothpaste containing novel particles.

In addition to toothpastes containing fine particles, non-uniformly colored toothpastes are also known, but toothpastes containing fine particles are particularly aesthetically appealing.

In addition to microparticles that do not have a specific effect, also microparticles that have a specific effect, in particular microparticles consisting of tooth abrasives, are known.

This invention aims to provide unique and novel fine particles that are surprisingly suitable for formulation in toothpastes and toothpastes such as toothpastes.

These fine particles have desirable properties and have a specific action, and are effective in promoting the healing of inflamed and bleeding gums, or periodontal ligament tissue.

Inflammation of the gums, or periodontal ligament tissue, is common to many people.

When inflamed, the gums become more sensitive and bleed easily.

For people with such periodontal ligament conditions, it is often difficult to maintain good hygiene of the teeth and gums due to the great pain experienced when brushing the teeth and gums with a toothbrush and toothpaste composition. .

Allantoin (C4H6N403) and aluminum dihydroxyallantoate [At(OH)2C4)I5N
403° or less is called ALDA.

] is disclosed for use in tooth brushing vehicles because of its ability to act on sensitive periodontal ligament tissue and promote its healing.

Aluminum chlorohydroxyterantoate (A4
(0H)4CtC4H5Nρ3. (referred to as Iwang CA)
have similar properties.

Recently, visibly fine particles have been produced that can be incorporated into toothpastes to provide desirable aesthetic and visual effects.

Some of these fine particles contain components with specific effects, such as abrasives, so that the user can better recognize the hygienic effects provided by the specific components.

It has a specific action to relieve pain and sensitivity of the periodontal ligament.

The provision of fine particles for toothpaste formulations is highly desirable.

People with periodontal ligament pain or sensitive conditions can use toothpastes containing these microscopic particles to actually see, and perhaps even feel, the therapeutic ingredients. When using toothpaste containing such therapeutic ingredients, it is natural to take appropriate hygiene precautions.

It is one advantage of the present invention to provide microscopic particles with specific effects, including components that reduce periodontal ligament sensitivity and bleeding.

Anti-irritant compounds such as allantoin have the unique effect of reducing periodontal ligament sensitivity and reducing bleeding.

That is, allantoin and the like have the ability to act on the periodontal ligament tissue and promote its healing.

In this regard, Chemical Abstracts Vol. 7
5 (1971) 18443e, it was reported that the use of a fungal brush containing allantoin significantly improved periodontal ligament inflammation in patients within 14 days.

Other advantages of the invention will become apparent from the description below.

This invention comprises a meltable or soft bonding material and about 5 to 10 compounds selected from the group consisting of allantoin, aluminum dihydroxyallantoate, and aluminum chlorohydroxyallantoate dispersed in the bonding material. a dentifrice containing fine particles consisting of a melting or softening binder material having a melting point or softening point lower than the decomposition point or melting point of the compound; Provides a dentifrice with a macroscopic size of ~1000 microns.

Allantoin is slightly soluble in water (0.5% at 25°C)
, has the empirical formula C4HaN40 s.

The pH of the Satsumasa aqueous solution is about 4-6.

Allantoin is effective in cleaning, healing, and relieving spongy or bleeding gums, or periodontal ligament tissue, without irritating or increasing the sensitivity of the gums.

Additionally, allantoin aids in the removal of unwanted necrotic tissue and promotes the growth of new, healthy tissue cells.

Allantoin melts at about 227° to 231°C with decomposition.

AL with the empirical formula ALc OH)2C4H5N40 s
DA has an effect similar to allantoin, but the presence of aluminum adds an astringent action and an action to prevent bacterial growth.

ALDA decomposes at temperatures above about 85°C and below about 100°C, typically below about 95°C.

Empirical formula At2(OH)4CtC4I (public.

ALCA with 03 has characteristics similar to ALDA.

Dissolves in water at 20°C by 1.3%.

The fine particles formed by this invention contain approximately 5-10% by weight of allantoin, ALDA or ALCA (hereinafter referred to as
It is called allantoin etc.

)including.

Although it is essential that allantoin and the like be present in the fine particles, they may optionally be present in the toothpaste base material.

Generally, the total amount of allantoin in toothpaste, allantoin, ALDA, ALCA, or mixtures thereof in toothpaste is about 0.05 to 1% by weight or more
．． It is 1 to 0.5%.

Allantoin, ALDA, an anti-irritant compound.

Alternatively, the binding material used to produce fine particles containing ALCA is a meltable or softenable material that readily disperses and binds the liquefied stimulant compound when cooled.

The binding material must have a melting or softening point below the decomposition point of the anti-irritant compound.

Binding materials are used to disperse the anti-irritant compounds of this invention within visible particles.

the particles liquefy the binding material in the presence of an anti-irritant compound;
Since it is formed by subsequent cooling, it is necessary that the bonding material has a melting or softening point lower than the decomposition or melting point of the anti-irritant compound.

Preferred binding materials for use with allantoin, ALDA, and ALCA are glyceryl di- or triesters of 01□-22 saturated fatty acids.

In addition to chrycerin ester, ethylene glycol diester can also be used.

The melting point of these substances is A
It is low enough to be used in both LDA and ALCA.

For example, each grade of glycerin tristearate has a
It melts at 7 to 65°C, at about 72°C at the most.

Other additive materials with specific functions can also be incorporated into the fine particles.

They may be liquids, in which case they may or may not be dissolved in a binder, or they may be solids in finely divided form.

These liquids and solids may be colored or colorless as desired.

The preferred material is a white powder or a colored comminuted solid, with the colorant having a particle size of less than 2 microns, preferably less than 1 micron.

Suitable solids include insoluble sodium metaphosphate, insoluble potassium metaphosphate, calcium birophosphate, magnesium orthophosphate, trimagnesium orthophosphate, tricalcium phosphate, dicalcium phosphate trihydrate, anhydrous dicalcium phosphate, and the like. There are common water-insoluble abrasives that contain phosphates.

Other abrasives include calcium carbonate, magnesium carbonate, hydrated alumina, silica, zirconium silicate, and aluminum silicates, including calcined aluminum silicate.

A combination of abrasives can also be used.

Water-insoluble coloring materials (e.g. pigments), preservatives, whitening agents, ammoniacal substances (e.g. urea, ammonium phosphate), antibacterial agents, flavoring agents, fluorine compounds with beneficial effects on oral hygiene [e.g. Sodium, potassium fluoride, stannous fluoride, stannous chlorofluoride, sodium hexanourostannate, stannous fluoride/potassium fluoride (SnF2-KF'), sodium fluorozirconate, and monofluorophosphoric acid Sodium], surfactants, etc. can also be used.

Generally the glycerin ester matrix makes up the majority of the speckle, for example on about 50 to 95 layers of fine particles, but allantoin, ALDA.

When additives other than ALCA with specific effects are present, speckles can be as small as about one layer.

To obtain the desired speckle effect, the fine particles are of macroscopic (i.e. visible) size, generally in the range of about 100 to 1,000 microns, preferably 20 microns.
0-600 microns, most preferably about 250-500
It needs to be in microns.

Unique physical and chemical properties of the glycerin ester used in this invention, namely softening point and/or melting point,
Due to hardness compatibility, etc., the maximum size of fine particles in toothpaste is not as strict as the maximum size of fine particles that have been proposed for use for this purpose.

The amount of fine particles in the oral composition of this invention is 0.01
-50% by weight, preferably in the range of 0.02 to 20%, more preferably in the range of 0.05 to 10%.

The particle size of the solids incorporated into and/or with the glycerin ester should be small enough to avoid creating a "janky" feel in the mouth, generally less than about 200 microns.

Abrasives, as commonly used, have a particle size of about 100 microns or less, generally 75 microns or less.

The other solids, especially the pigments, should have a particle size of about 2 microns or less, and the glycerin ester used in this invention has a suitable melting point of about 40-80°C, preferably 55-72°C. Generally characterized as a soft fatty substance.

Mixtures of esters are of course equally suitable, provided they meet the specifications.

The elongated particles of this invention are most conveniently prepared by liquefying the ester and then incorporating the desired additives.

The resulting mixture is then spray cooled to produce particles of varying particle size.

The particle size depends on spray pattern characteristics, spray pressure, cooling conditions (eg, cooling gas temperature, gas velocity), and the like.

Examples of suitable conditions include cooling gas at room temperature, air pressure of 2 to 10 atmospheres, and the like.

The mixture of ester and additives was passed through a chilled mill roll (Ch
It can also be cooled on a milled mill roll and recovered in pulverized form in a conventional manner.

Spray cooling is preferred because it provides a homogeneous, uniformly sized product with a desired particle size that is relatively easily controlled.

Colorants suitable for use in the fine particles, including white, can be selected from water-insoluble dyes, or pigments, which are stable in the fine particles and do not run into the bulk of the toothpaste.

When the colorant is a finely ground solid, it is imperative that the average particle size is less than 2 microns, preferably less than 1 micron, and that the maximum particle size does not exceed 5 microns.

It is truly surprising that such a small particle size prevents the colored material from leaching into the main body of the toothpaste, and one possible explanation for this unique behavior is that the particles are subdivided and highly It is in a fine condition,
Since it is very homogeneously dispersed in the ester matrix, a small concentration of filler, i.e. as low as 0.1-2%, preferably 0.2-1%, produces acceptable color density in fine particles. It lies in the fact that you can give.

Examples of coloring materials that can be used include titanium dioxide, calcium carbonate, magnesium carbonate, aluminum hydroxide, azulene, color index number: 12490,751
20°75130.75810,69800,7749
2゜75470.75300,77510.77007
and 74260 colorants, and mixtures thereof.

Other bonding materials known in the art as bonding materials may also be used provided they meet the above requirements.

For example, resins, gums, gels, waxes, polymers, etc. can also be used.

A group of fine particles that are attractive to this invention are natural and synthetic materials classified as thermoplastics (ie, materials that soften and can be molded when heated).

Typical examples of thermoplastics that can be used are ethylenically unsaturated polymers such as polyethylene, polyvinyl chloride,
Polyvinyl acetate, copolymers of polyvinyl chloride and vinyl alcohol, copolymers of vinyl acetate and vinylidene chloride, polystyrene, polymethylstyrene; synthetic rubbers, such as styrene-butadiene copolymers, α-methylstyrene and vinyl Copolymers with toluene; polymethacrylates, such as polymethyl methacrylate, polyethyl methacrylate, polyisopropyl methacrylate, polyisobutyl methacrylate; polyacrylates; polyamides, such as nylon; cellulose acetate, cellulose butyrate, etc. Substances whose main component is cellulose; polycarbonate; bisphenol-A
and epichlorohydrin; polymers that are composed of monopolymers containing at least two polymerizable groups and that initially become plastic when heated and harden with continued heating, such as polymethacrylic acid; Allyl, polymer of methacrylic acid diester and ethylene glycol; coumaron-indene resin, polyethylene/y-IJ
ml -le, and natural waxes such as carnauba wax, paraffin wax; and mixtures of the above materials.

IJ), which is a temporary aspect of this invention, is about 500 to about 20
．． Advantageous results can be obtained by utilizing thermoplastics having a molecular weight of 0.000, preferably at least about 1,000 as the binder.

Hardness of preferred materials for this class (100g 15s 25
It is expressed in degrees Celsius (ASTMDI 321) in units of 1'omm.

) is typically about 1 to 15, although even harder grades can be used if their presence in the final toothpaste is acceptable.

The following table lists the properties of thermoplastic bonding materials representative of this preferred class.

Soft (A) Hardness Specific gravity Average viscosity CP tree
Fat Average Molecular Weight (Kake.

A (A) Polyethylene' 2.00
0 105°G 3.5 0.92 200(1
40°C) II 2,20
0 107°G 3.0 0.92 220(1
4-0°C) II 3,5
00 116°C1,00,93350(140°C)
/l 5,000 109°
C2,50,924000 (140°C)/l
1.500 1.02℃ 7.5
0.91 145 (140℃)/l
2,000 96°C9,50,91
230 (140°C) oxidized polyethylene”
1,800 104°C4,00,94320('
125°C)/l 3,00
0 106°C3,00,941200(125°C)
Polyamide 3 6,000-9,000”11
00C4, 0,982200 (150°C)/l
6,000-9,000 95°CI5
0.98 1100 (1500C)tt
6,000-9,000 110°C30,983
800 (150°C) α-methylstyrene and vinyltoluene 1.000 100
°C--3500 (140 °C) Copolymer 1, Allied Chemical Company
Chemica ICompan Trademark name A-
C polyethylene, grade 6.6A, 7,7A, 8,8
A, 615°617.617A, G-201,400.

2. Eastman Chemical Products (Eastm
a Chemical Products) (Kin
gsport.

It is available under the trade name EPOLENE from John Tenn.

These materials can be emulsified and have acid and saponification numbers of 9-10.

Allied Chemical Company (Alli)
Trade name A-C polyethylene, grade 656, 629, 65 from edChemical Company
Available as 5°680.

3. Manufactured from ethylenediamine according to the invention of US Pat. No. 2,379,413.

General Mills Corporation
Department of Chemistry (Kankakee)
, II l, ) from the trade name elsamide (V
ersamid), grade 930°940.950
It is available as .

4. Biff Range Company (Picco Re
sinCompany) (Clairton, Pa.)
Trade name Piccotex 10
Available as 0.

Considering the melting or softening points of bonding materials of the above type, allantoin is suitable for inclusion in these materials.

However, ALDA decomposes at temperatures below the melting or softening point of the binder.

ALCA is also not suitable. The materials are non-toxic, tasteless, and do not attack the materials from which the toothpaste packaging tube is constructed (eg, aluminum or lead lined).

As previously pointed out, the toothpaste may be a powder, but a paste is preferred, and the paste may be opaque, translucent or transparent.

The paste is a toothpaste vehicle that forms a gel-like or cream-like mass with a consistency that can be squeezed out of hand-dispense tubes such as aluminum, lead, or plastic tubes. containing particles dispersed within it.

This vehicle includes liquids and solids.

Generally, the liquid portion of the vehicle is water, glycerin, sorbitol, propylene glycol, polyethylene glycol 400. It is composed of other similar materials and mixtures thereof.

It is usually advantageous to use a mixture of water and humectants such as glycerin, sorbitol, propylene glycol, silica, and the like.

The total amount of liquid in a toothpaste is generally about 20-89.5% by weight.

For transparent or translucent toothpastes, the amount of liquid in the toothpaste may be about 20-89.5% by weight, while for opaque toothpastes it is usually about 20-50% by weight.

The solid portion of the vehicle includes gelling agents such as natural and synthetic gums, gummy substances such as iris moss, tragacanth, alkali metal carboxymethyl cellulose, and hydroxymethyl carboxyethyl cellulose;
Polyvinylhydridone, starch, water-soluble hydrocolloidal carboxyvinyl polymers (such as those sold under the trade name Carbopol 1934.940), trade name Laponite (trade name
) clay, and silica aerogel.

The solid portion of the vehicle is typically about 10% of toothpaste.
It is present in an amount up to % by weight, preferably about 0.5-5% by weight.

It is noted that a reaction readily occurs between aluminum compounds such as ALDA, ALCA and alkali metal (eg, sodium) carboxymethyl cellulose to form a precipitate of aluminum carboxymethyl cellulose.

For this reason, 1. ALDA. Or, when using ALCA, especially when it is included in a toothpaste base material, it is preferable to use a gelling agent other than sodium carboxymethylcellulose as the gelling agent, since the amount of gelling agent in the toothpaste is reduced. .

When ALDA or ALCA is present in the toothpaste base material, the gelling agent is preferably iris moss or hydroxyethyl cellulose.

In addition to the above, the toothpaste substrate includes a water-insoluble, non-visible abrasive having typical particle sizes used in the prior art, such as particle sizes of about 74 microns or less.

Typical dentally acceptable water-insoluble abrasives include insoluble sodium metaphosphate, trimagnesium phosphate, tricalcium phosphate, trimacnesium phosphate, alumina trihydrate, anhydrous alumina, zirconium silicate, synthetic Examples include amorphous sodium aluminosilicate, crystalline silica, and colloidal anhydrous silica.

The total amount of abrasive in the toothpaste is about 10 to 75 parts, preferably about 15 to 50 parts.

Allantoin, ALDA, or ALCA may also be present in the toothpaste base.

The total amount of allantoin, ALDA, ALCA, or mixtures thereof present in the speckles, or speckles and toothpaste base, is generally about 0.0 as previously stated.
1-51-5% by weight or about 0.05-1% by weight.

In addition to agents such as those that can be present in the speckles, the toothpaste substrate can also include surfactants.

The total amount of surfactant, together with the amount of agent that can be present in the speckles, is about 0.05 to 100% of toothpaste.
5% by weight, preferably about 1-3% by weight.

Various other materials can be incorporated into the oral preparations of this invention.

Examples are colorants or whitening agents, preservatives, silicones, chlorophyll compounds, ammoniacal substances such as urea, diammonium phosphates, and mixtures thereof, and other ingredients.

These adjuvants can typically be included in the toothpastes of this invention in amounts of up to about 5 parts each.

Engagement with a colorant should color the speckles with a suitable contrasting color.

Whitening materials that can be used include titanium dioxide in an amount of about 0.01 to 10%.

The toothpaste of this invention may also contain an antimicrobial agent in an amount of about 0.01-5%.

Typical examples of antimicrobial agents that can be used are gutnisin, biguanidine, and amines such as N1-(4-chlorobenzyl).
-N5-2.4-dichlorobenzyl biguanide; p-chlorphenyl biguanide; 4-chlorobenzhydryl biguanide; 4-chlorobenzhydryl guanylurea; N
-3-lauroxypropyl-mer p-chlorobenzylbiguanide; 1,6-di(p-chlorphenylbiguanide)hexane; 1゜6-bis(2-ethylhexylbiguanide)hexane7; 1-(lauryldimethyl ammonium)-8-(p-rebenzyldimethylammonium)octane dichloride; 5,6-dichloro-2-guanidinobenzimidazole; N'-p-chlorophenyl-N5-lauryl biguanide; 5-amino-1,3 -bis(2-ethylhexyl)-5-methylhexahydropyrimidine; and non-toxic acid addition salts of the above substances.

Suitable flavoring agents and sweet saliva stimulants can be used in the flavor formulation of the compositions of this invention.

Examples of suitable numbered ingredients include, in addition to methyl salicylate, fragrant oils such as spearmint oil, peppermint oil, wintergreen oil, satsafras oil, clove oil, sage oil, eucalyptus oil, marjora oil, cinnamon oil, lemon oil,
and orange oil.

Suitable sweeteners include sucrose, lactose, maltose, sorbitol, sodium cyclamate, and saccharin.

Flavoring and sweetening agents together make up about 0.0 of the composition of this invention.
Suitably, it accounts for 1 to 5% or more.

Suitably, the compositions of the invention also contain fluorine compounds that have beneficial effects on oral care and hygiene, such as reducing the acid dissolution of enamel and preventing tooth decay. .

Examples of fluorine compounds that can be used are sodium fluoride,
These include stannous fluoride, potassium fluoride, sodium hexafluorostannate, stannous chlorofluoride, sodium fluorozirconate, and sodium monofluorophosphate.

These dissociate or liberate fluorine-containing ions in the water, so that an effective and non-toxic amount, usually about 0.0
Suitably it is present in a water-soluble fluorine content in the range 1 to 1% by weight.

The most preferred fine particles of this invention are prepared using glyceryl tristearate, which contains about 5 to 10 molecules of allantoin, ALDA, or ALCA.

and contains about 0.05-10% by weight of coloring material.

Allantoin is a preferred anti-irritant. ALDA is also highly desirable.

Other thick and car-heavy speckles have an average molecular weight of about 1.50.
0, a softening point of 102°C, a hardness of 7.5, a specific gravity of 0.91, and an average viscosity of $145 cps.
Contains 10% by weight of colored material.

Precipitated calcium carbonate on the order of 5-10 times is also desirably included in the fine particle preparation.

Suitable usage ranges for some of the additives with specific functions that can be used in the fine particles of this invention include: 1 to 80% by weight of abrasive, preferably 5 to 50%; 0.01% of fluorine compound; ~50% by weight, preferably 0.01-20
%; preservatives 0.01-50% by weight; and fragrance 0.
01 to 50% by weight.

The following examples are intended to illustrate, but not limit, the invention.

Amounts, proportions, and parts listed in the examples are by weight unless otherwise specified.

Example 1 90 parts of glyceryl tristearate are added to 72 parts of glyceryl tristearate in a suitable container.
Melt at ~75°C, add 10 parts allantoin and mix homogeneously.

The mixture was then poured into a pilot 3-roll mill with Mazzoni type rolls in which water circulated to cool it.

The resulting allantoin bound solidified ester was scraped from the mill, then placed in a granulator and then vibrated through a vibrating sieve to produce a product having a size of 290-420 microns.

Example 2 Example 1 was repeated using ALDA instead of allantoin.

Example 3 Example 1 was repeated using ALCA instead of allantoin.

Example 4 Examples 1-3 were repeated.

However, the produced particles were sieved to obtain a product having a size of 420 to 840 microns.

Example 5 Instead of glyceryl tristearate (3) Glycerin nistearate (B) Glycerin tripalmitate (C) Glycerin trilaurate (D) Glycerin tritocosylate (E) Glycol nistearate Examples 1 to 4 were repeated using

Example 6 The following coloring materials were added to the ester before it was melted,
Examples 1-5 were repeated.

(Al Pigment Red 5 0.5% (B) Pigment Red 5 1.0% (C) Pigment Red 52.0% (D) Azulene 1.0% (E)
Azulene 2.5% (F) C,1,
75210-0,3% (G) C, 1,758101
,0% ()])C,1,754700,1% (I) C,1,775100,4% (J) C,1,751300,5% [)C,1,698000,3% (L) C, 1,770071,0% (To) 2.0%〃 (N) Pigment Green 70.4% (Color Index 74260) All pigments used in this example had an average particle size of 2 microns or more/JX size. .

Example 7 Examples 1-6 were repeated adding the following ingredients to the ester.

(3) Titanium dioxide 2.0% (B)
Calcium carbonate 5.0% (C)
Titanium dioxide 20.0%) Calcium carbonate 50.0% (9 Sodium fluoride 5.0% (F) Sodium monofluorophosphate 5.0% (Gl) Dicalcium phosphate with an average particle size of 4.2 microns. Dihydrate 6060
%■ Sodium benzoate 5.0% (I)
Zirconium silicate 25.0% (J)
Hydrated alumina 35.0% ■ Dicalcium phosphate dihydrate 60.0% azulene
1.5% (L) Hydrated alumina
50.0% Pigment Red 5
0.8% Zirconium Silicate 40.0
% Pigment C, 1,751,300,5% Example 8 A clear formulation was made with the following ingredients.

Ingredients Glycerin 2480 Sodium carboxymethylcellulose 1.00 Um Saccharin 0.11 Sodium benzoate 0.50 Sorbitol (70% aqueous solution) 44.90 Deionized water
3.60 Syloid
oid) 244 (Silica 5.00 thickening agent) Sodium aluminum silicate p-16,00820 (
Abrasive) Sodium lauryl sulfate 2.00 Fragrance
0.90 The following fine particles were separately incorporated into the above formulation in the indicated amounts.

■ Example 7 (K) - Glyceryl tristearate (25
0-420 microns) 5% (B) Example 7 (K) - Glyceryl tristearate (420-84
0 microns) 5% (C) Example 7 (Low glyceryl tristearate (250-420 microns) 5% (DJ) Example 7 (L) - Glyceryl tristearate (420-840 microns)
5% (E) Example 7 (L) - Glyceryl tristearate (250-420 microns) 5
% (F) Example 7 (M) - Glyceryl tristearate (250-420 microns) 3% Example 9 An opaque toothpaste with the following composition was prepared.

Ingredients % Glycerin (98% cp) 6.12 Carboxymethyl cellulose sodium 1.00 Lium Sodium benzoate 0.50 Saccharin 0.12 Tetrasodium birophosphate 0.30 Sorbitol (70
% aqueous solution) 16.00 deionized water
24.61 Calcium carbonate
8.00 Dicalcium phosphate dihydrate 4
0.0ON-Nauroylsarcosinate 2.0
5 Lium Titanium Dioxide 0.30 Fragrance
Fine particles ranging from 0.80 to 100.00% were separately blended in the indicated amounts.

■ Example 6 (A) - Glyceryl tristearate (24
(0-420 microns) 0.5% (B) Example 6 (D) - Glyceryl tristearate (250-420 microns) 0.5% (C) Example 6 (3) - Glyceryl tristearate (2
50-420 microns) 0.5%) Example 6 (J) - Glyceryl tristearate (42
0-840 microns) 0.5% (E) Example 6 ■) - Glyceryl tristearate (
420-840 microns) 0.5% (F) Example 6 (J) - Glyceryl tristearate (420-840 microns) 0.5% (G Example 6 (N) - Glyceryl tristearate (2
96-420 microns) 0.4% Example 10 A clear gel toothpaste formulation containing the abrasive sodium aluminosilicate and having the following composition was prepared.

Ingredients Sorbitol (70% aqueous solution) 44.68 Laponite (I, aponite) (synthetic hex 2
．． Glycerin 26.10 Deionized water 3.00 Syroid
244 (thickening agent) 5.0ON-sodium lauryl sarcosinate 2,00 soluble saccharin
0.17 Sodium aluminum silicate 16.00 Fragrance 1
．． 00 Speckle from Example 9 was also used in this example.

Example 11 Example 9 was repeated replacing 0.5% water with an equal amount of allantoin.

Example 12 0.5% of the fine particles of Example 6 (N) were dispersed in 99.5% toothpaste having the following composition.

Ingredients Glycerin
18-24 Hydroxyethylcellulose-soluble saccharin 0.1-0.3 Hydrated alumina 48-56 Sodium lauryl sulfate 1-1.5 Pyridyl carbinol 0.05-0.2 Allantoin
Example 13 Example 12 was repeated using ALDA in place of allantoin.

Example 14 Fine particles produced by the method described below were incorporated into the clear gel toothpaste of Example 8.

90 parts of non-emulsifying grade granular polyethylene having the following properties were dry mixed with 10 parts of allantoin in a suitable container.

The container containing the resulting dry mixture was heated in a suitable heating device and stirred during this time.

The binder polyethylene softened, but before it melted, the container was removed from the heating device and allowed to cool.

During this time, stirring continued.

The cooled mass is then crushed into granules, passed through a sieve, and
Particles with a size of 50-420 microns were obtained.

Example 15 Example 14 was repeated including 0.4 parts of Color Index Pigment Green 7 in the mixture.

Example 16 The microparticles of Example 15 were prepared using 5 Miyakonojo polyethylene and containing 5 parts calcium carbonate.

Add 0.5 part of these fine particles to the toothpaste 9 of Example 11.
It was blended in 9.5 parts.

Example 17 90 parts of glyceryl tristearate are added to 7 parts of glyceryl tristearate in a suitable container.
Melt at 2-75°C, add 10 parts of allantoin, mix homogeneously, spray and cool at room temperature.

The particles thus formed are sieved and
A product with a size of 420 microns was obtained.

This method was repeated using ALDA instead of allantoin.

The particles obtained were colored according to the previous example and incorporated into a toothpaste.

The above examples include preferred and typical formulations of the invention, but are not intended to limit the invention in any way.

Claims (1)

[Claims] 1. A finely divided compound consisting of a meltable or softenable bonding material and about 5 to 10% by weight of a compound selected from the group consisting of allantoin, aluminum dihydroxyaladoinate and aluminum chlorohydroxyallantoate dispersed in the bonding material. a dentifrice containing particles of about 100 to 1000 microns, the meltable or softenable binder material having a melting point or softening point lower than the decomposition point or melting point of the compound; Toothpaste that is visible to the naked eye.