SE409544B - OPAK TOOTH CREAM CONTAINING HOMOGENICLY DISPERGED PARTICLES OF AN AGGLOMERATED MATERIAL - Google Patents

Abstract

1284546 Clear toothpastes COLGATEPALMOLIVE CO 4 Aug 1969 [5 Aug 1968 (2)] 10835/72 Divided out of 1284544 Heading A5B A clear toothpaste comprises a clear toothpaste base having dispersed therein particles of agglomerated solid toothpaste ingredient comprising a water-insoluble dental polishing agent e.g. dicalciumphosphate, sodium metaphosphate, calcium carbonate, hydrated alumina, zirconium silicate, or various other phosphates, MgCO 3 , SiO 2 aluminium silicate or polymethyl methacrylate; which agglomerated particles are visible to the naked eye (preferably of size less than 2380 microns) and palpable and substantially retain their identity in the toothpaste and in the presence of saliva but are easily reducible by toothbrushing to fine, impalpable individual particles of the ingredient each of which is invisible to the naked eye (e.g. of size less than 177 microns). The polishing agent is blended with a binding agent e.g. polyethylene glycol, gum acacia or polyvinyl pyrrolidone, and this blend or a blend of polishing and tabletting agents may be compressed into tablets which are then broken down into the agglomerated particles. The agglomerates may be coloured by a dye or pigment and are incorporated into the toothpaste base which may be a gelled dental vehicle typically comprising 20-89.5% liquid and 0.05-5% gelling agent or gum, by weight of the toothpaste. The liquid portion comprises e.g. water, glycerine, sorbitol solution, propylene glycol or polyethylene glycol. Conventional additives may also be present in the toothpaste.

Description

The toothpaste according to the invention is characterized in that the agglomerated material consists of sub-portions of said water-insoluble tooth polish and a water-soluble binder and optionally a dye or pigment, which sub-particles have a particle size of less than I77 μm and are cohesive. in agglomerated form by means of the binder to form particles with a particle size of 420 - 2380 μm, preferably 420 - 8ü0 μm, which agglomerated particles are perceptible and substantially insoluble in the toothpaste, but easily decomposable by toothbrushing by mechanical action to individuals 'small' polish particles, of which the agglomerated particles are composed and which are imperceptible during toothbrushing. Because the agglomerates or grains are visible to the naked eye, they have a marked effect on the aesthetic appearance of an opaque toothpaste and can improve the cleansing effect of the tahd cream.

The water-insoluble tooth polishes which can be agglomerated to obtain said agglomerated materials include insoluble phosphates, such as insoluble sodium metaphosphate, insoluble potassium metaphosphate, calcium pyrophosphate, magnesium orthophosphate, similar to trimagnesium orthophosphate, tricyclic orthophosphate, tricyclic orthophosphate. Other polishing agents include calcium carbonate, magnesium carbonate, hydrated alumina, silica, zirconium silicate, aluminum silicate, among others. a. calcined aluminum silicate and polymethyl methacrylate. Combinations of polishes can also be used. The preferred polishes are dicalcium phosphate and insoluble sodium metaphosphate.

The insoluble alkali metal metaphosphates are preferably insoluble sodium and potassium salts of polymetaphosphoric acid. These materials are well known in the art and the insoluble sodium metaphosphate has, as noted above, been previously suggested as a polishing agent. Such materials can be prepared in any suitable manner, for example, as described in Thorpe's Dictionary of Applied Chemistry, Vol. 9 (üth ed.), Pp. 5l0 - 5ll.

As further examples of suitable materials can be mentioned the forms of insoluble sodium metaphosphate which go under the names Madrell's salt and Kurrol's salt. These metaphosphates have only very low solubility in water and are therefore usually referred to as insoluble metaphosphates. There is a small amount of soluble phosphate material as impurities, usually a few percent, up to about Å% of the weight of the material. The amount of soluble phosphate material, which in insoluble sodium metaphosphate is assumed to be a soluble sodium trimetaphosphate, can be reduced, if desired, by washing the material with water. In accordance with the present invention, these particles are formed into agglomerates by using a material that facilitates agglomeration, i.e. agglomerating agent. These materials exhibit binding and / or lubricating properties or the like so that they form agglomerates which exhibit the desired properties in the opaque toothpaste.

Binders which can be used to facilitate the transfer of the polishing agent to agglomerated particles include water-soluble materials such as gum arabic, gelatin, starch, alkali metal carboxymethylcellulose, polyethylene glycol, glucose, sucrose, methylcellulose, carboxyethylvinylethanol hydroxyl, magnesium aluminum silicate gel and the like. Examples of additional agglomerating agents are talc, magnesium stearate, calcium stearate, stearic acid and the like, which materials are water-insoluble and are also known as lubricants. These various agglomerating agents are typical examples of gums, gels, waxes, polymers, etc. which are known as binders or the like in the manufacture of tablets and other compressed or agglomerated materials.

Mixtures of agglomerating agents can also be used. When the polishing agents are released from the binding action of these agents upon application of a small pressure, which occurs during toothbrushing, these agents dissolve or disperse easily in the saliva so that the particles of the polishing material are allowed to exert the desired polishing or cleaning effect at the same time as the rest of the toothpaste.

The polish is present in the agglomerate and gives the opaque toothpaste a polishing effect. In typical cases, the polish consists of about 75 - 98% by weight of the finished agglomerate. The binder is present in a sufficient amount to facilitate agglomeration, ie. about 2 - 25% by weight of the finished agglomerate.

Binder is mixed into the polish in the form of a dry powder or a solution in water or alcohol. The agglomerate can be formed by a dry process known as a slugging process or by a wet granulation process. In the dry process, the mixture of polishing particles and any binder is compressed in a tablet press. Typically, substantially all polishing particles have individual particle size of less than 250 .mu.m The large tablet thus prepared typically has dimensions of about 6 x 25 mm, but even larger tablets can be made. The tablet is then crushed into visible granule agglomerates with particle sizes suitably up to about 2580 / ¿(m. Typical visible particles are up to 840 / ¿¿m, such as about 420 - 840 / ¿4m. The crushing can for example be carried out in a mill, granulator or in a crusher.

When the dry process is used, the agglomeration mixture suitably contains a lubricant such as talc, magnesium stearate, calcium stearate, stearic acid and the like. The lubricant facilitates agglomeration and is present in an amount suitably suited for this purpose.

When dry powdered binder is mixed with the polish in the wet granulation process, the mixture is contacted with a solvent such as water or ethanol or a solution of additional binder, the amount of solvent being sufficient to wet the pulp.

The wet granulation process can be carried out by wetting a powder mixture of water-insoluble toothpaste particles having, for example, a particle size of less than 74 .mu.m, and binder continuously in a "Dravo" trough, in a "Hobart" mixer or other suitable powder mixer, so that you get a wet mass. The wetting can be accomplished by contacting the polish with a solid binder and then wetting the mixture with a solvent for the binder.

The wet mass formed by the polish and the binder is then pressed through a sieve with uniform openings so that agglomerates are formed, each having a size of between 420 - 2380 / Am. The agglomerates are then dried, for example, in air or in an oven. The agglomerates can then be disintegrated into desired clearly visible sizes such as between 420 and 840 .mu.m by passing them through sieves or meshes of suitable sizes. If the wet mass is produced in a "Dravo" trough, the pressing through a sieve or a mesh may be superfluous.

It is desirable that the formed agglomerates can be easily inserted into the oral cavity with a toothpaste and without inconvenience retained in the oral cavity until they are reduced - in size during toothbrushing. Visible particles and generally those having a size greater than about 2380 .mu.m can therefore be conveniently separated from the agglomerates. In order to achieve the best possible aesthetic appearance of the agglomerates when incorporated in a toothpaste, it is also suitable to separate small parts, which have a much smaller particle size than about 420, LLm.

However, any agglomerates containing the components of the invention which are visible to the naked eye fall within the scope of the invention.

If desired, the dry or wet agglomeration mixture may optionally contain non-abrasive diluents or fillers, such as lactose, starch, mannitol and the like in amounts up to about 1 to 5% by weight of the agglomerate to improve the polishing effect of the agglomerate. In addition, the mixture may contain minor constituents such as a dye or pigment. Typical dyes and pigments include water-insoluble F, D and C dyes and lacquers and the like.

The dye materials are usually used in concentrations of about 1-1o%.

Depending on the nature of the water-insoluble polish, which comprises the bulk of the agglomerate, the agglomerate is characterized as substantially water-insoluble. In the oral cavity, the agglomerate grains are reduced from visible and perceptible grains to individual, invisible, small and imperceptible grains, when the agglomerate is subjected to a mild mechanical action such as when brushing the teeth, gums or other parts of the oral cavity with a toothbrush, tongue, finger or similar.

The agglomerated material according to the invention is mixed in an opaque toothpaste. These agglomerated particles are homogeneously dispersed and are present both on the surface and inside the toothpaste. In the opaque toothpaste, the agglomerated particles present on the surface are visible to the naked eye.

The opaque toothpastes contain a dental carrier which forms a gel or cream-like mass of a consistency which can be conveniently pressed out of a compressible tube of, for example, aluminum or lead. The carrier contains liquids and solids. In general, the liquid portion consists of water, glycerol, sorbitol, propylene glycol, polyethylene glycol 400 or similar or suitable mixtures of these substances. It is usually advantageous to use a mixture of both water and a humectant, such as glycerol, sorbitol, propylene glycol or the like. The total content of liquid generally amounts to about 20 - 89.5, usually about 20 - 50% by weight of the toothpaste.

The solid portion of the carrier contains a gelling agent such as natural and synthetic gum materials and gum-like materials, for example, carrageenan moss, tragacanth, alkali metal carboxymethylcellulose and hydroxymethylcarboxyethylcellulose, polyvinylpyrrolidone, starch, water-soluble hydrophilic colloidal carboxyls and 940. Such a solid component of the carrier is typically present in an amount up to about 10% by weight of the toothpaste and preferably between about 0.5 and 5% by weight.

The agglomerated particles, which form a substantially insoluble polishing material, are mixed into the base material of the toothpaste in a sufficient amount to achieve different particles with an attractive appearance and desired polishing effects. They may typically be included in any suitable amount up to about 75, e.g. up to 50% by weight depending on the desired appearance, polishing effects and type of preparation that the manufacturer wishes to produce. The agglomerated particles can also generally be present in an amount of 5 ~ 75% by weight of the toothpaste, which gives a substantial amount of polishing material. The toothpaste may contain the usual water-insoluble polish previously used and having a particle size of less than about 74 microns. This previously used polishing material is not visible in the base material of the toothpaste and increases the polishing effect further beyond that obtained by the agglomerates. The total amount of polishing material, e.g. essentially about 5 - 75%, is in this case divided into the agglomerates and the base material of the clear toothpaste as desired.

The tooth cleaner may also contain a surfactant. It is preferred that the total amount of surfactant, including that which may be included in the agglomerates, be about 0.05-5, preferably about 1-5% of the total weight of the dentifrice. Suitable surfactants include water-soluble sulphates of compounds with long-chain alkyl radicals (for example, alkyl particles with a chain length or 10 to 18 clays). A preferred material is a long chain fatty acid monoglyceride sulphate, for example sodium salt of hydrogenated coconut fatty acid monoglyceride sulphate alone or in combination with sodium lauryl sulphate. Other suitable materials are the fatty acid amides of amino acids, such as sodium N-lauryl sarcosinate. The detergent content is usually between 1 and 10%.

Other types of material can be mixed into the oral preparation according to the invention.

Examples of such materials are colorants or whiteners, preservatives, silicones, chlorophyll compounds, ammonia derivatives such as carbide, diammonium phosphate and mixtures thereof, etc. Each of these additives may typically be incorporated into the present toothpaste in amounts up to about 5%. When dyes are used, the agglomerates may be colored with a suitable contrasting color. The toothpaste may also contain antibacterial agents in concentrations up to eirke o, o1 - 5%. Blend typical examples of the other active agents are guanidines, biguanides and amines such as: N1- (4-chlorobenzyl) -N5-2,4-dichlorobenzyl) -biguanide; 4-chlorobenzhydrylguanylurea; Nq3-lauroxypropyl-N5-n-chlorobenzyl biguanide; 1,6-di-p-chlorophenylbiguanido-hexane; 1- (lanryl-dimethylammonium) -8- (p-chlorobenzyldimethylammonium) -octane dichloride; 5,6-dichloro-2-guanidinobenzimidazole; N1-p-chlorophenyl-Naural uryl biguanide; 5-amino-1,5-bis (2-ethylhexyl) -5-methylhexahydropyrimidine; and the non-toxic acid additive salts of these compounds.

Oils, for example from garden mint, peppermint, evergreens, sassafras, clover, sage, -Y- in eucalyptus, marjoram, cinnamon, lemon and orange as well as sodium methyl salicylate can be used as suitable aroma and sweetening sialagogues. Suitable sweeteners are sucrose, lactose, maltose, sorbitol, sodium cyclamate and saccharin. Suitable flavors and sweeteners may be included in the toothpaste in a total content of between about 0.01 and 5% or more based on the total weight of the compositions of the invention. .

The compositions of the present invention may suitably also contain a suitably selected fluorine-containing compound having a beneficial effect, for example reducing the solubility of tooth enamel in acid and protecting the teeth from destruction. Examples of such fluorine-containing compounds are sodium fluoride, tin (fluoride, potassium fluoride, potassium tin, fluorine) (sodium KF), sodium hexafluoro stannate, stannous chlorofluoride, sodium fluorofurzirconate and sodium monofluorophosphate, as well as aqueous monofluorophosphate. preferably at effective but non-toxic levels, usually between about 0.01 and 1% by weight of the water-soluble fluorine content contained therein.

The toothpaste according to the invention is prepared by preparing a mixture which does not contain agglomerates and separately preparing the agglomerates in a suitable manner. Thus, a gelling agent such as, for example, sodium carboxymethylcellulose or Carbopol 934 and a preservative such as, for example, sodium benzoate and any polishing material used are dispersed together with a wetting agent such as glycerol. Water can also be added. Additional wetting agent and water, for example a 70% sorbitol solution, can then be mixed into the dispersion, which is then heated at a 40-65 ° C, for example 50 ° C to form a gel. if a surfactant such as sodium lauryl sulfate is used, it is then dispersed in the mixture, which is finally deaerated and cooled. Suitable flavoring agent can be added afterwards, after which the toothpaste is deaerated again.

The agglomerates are then dispersed in the toothpaste with the least possible mechanical agitation, i.e. with such gentle stirring that the agglomerate grains are not crushed to any appreciable degree. The toothpaste is then ready and can be packed in tubes after re-venting.

In the following examples the invention is further elucidated, but it is of course not limited to the embodiments described in the examples. Parts and percentages refer to parts by weight resp. % by weight unless otherwise expressly stated.

Example 1,200 parts of anhydrous dicalcium phosphate in the form of a particle mass, in which substantially all the particles had a size below about 7.4 .mu.m, and 1 part of the substrate pigment (D & C Lake Red No. 50) were moistened with 40 dollars of one. zzmzsz-v -ß- 0 10 ß-aqueous solution of acacia rubber in a "Hobart" mixer for 10 minutes. The colored wet mass obtained in this way was pressed through a sieve with uniform openings amounting to 2380 .mu.m and oven-dried for 1 hour at 6500. The dried agglomerates were then sieved through a sieve with uniform openings amounting to 840 .mu.m and a sieve with uniform openings amounting to 420 .mu.m. 10 parts of the dried grains of agglomerated particles, which passed through the sieve with openings of 840 .mu.m and which were retained on, the sieve with openings of 420 .mu.m, were mixed with 90 parts. of an opaque toothpaste having the following composition: - Glycerol (99.3 gg 19-950% Sodium carboxymethylcellulose 0.850% I Sodium saccharin o.2o0% 5 Sodium benzoate 0.500% Tetrasodium pyrophosphate 0.250 1, Water 19-986 75 Trimagnesium cicarbonate Dicacium phosphate anhydrate 46.550% Sodium N-nanrylar sarcosinate (55 na 5.714% Flavor 0.800% The opaque toothpaste of this example has visible particles of the agglomerates which are distributed throughout its surface. During toothbrushing, the agglomerated particles are first perceptible and then easily reduced to individual small size polishing particles when a light pressure is applied with the toothbrush.

Example 2 220 'parts of the average particle size dicalcium phosphate dihydrate about 2.4 .mu.m were moistened with 91 parts of a 10% aqueous solution of acacia gum in a "Hobart" mixer to a uniformly wet mixture. The wet mass was pressed through a sieve with uniform openings of 2380 .mu.m and oven dried for 1 hour at 6500. The dried agglomerates were then sieved through a sieve with uniform openings of 420/4; m. 132 parts of the agglomerated dicalcium phosphate dihydrate were retained on the screen with uniform openings of 840 .mu.m and 57 parts passed through the screen. with uniform openings of 420 / u m.

Similar agglomerates of water-insoluble dentifrices were prepared by mixing hydrated alumina with an average particle size of about 2.5 .mu.m of calcium carbonate consisting of particles, substantially all of which had a particle size of less than about 7.4 .mu.m; anhydrous dicalcium phosphate v- 12o12ss ~ 7 in the form of particles, essentially all of which were less than about 7.4 μm; and insoluble sodium metaphosphate having an average particle size of about 4.8 .mu.m.

These polishes were mixed with a 10% aqueous acacia gum solution. 20 parts of the agglomerate particles according to this example, which passed through a sieve with uniform openings of 840 μm and which were retained on a sieve with uniform openings of 420 μm, can be mixed with 80 parts of a toothpaste according to Example 1.

Similar dentifrices can be prepared using aggregates obtained by mixing with a 10% acacia gum solution; hydrated alumina having a particle size of less than about 2.5, LLm; calcium carbonate in the form of a particulate mass, in which substantially all particles have a size less than about 7.4 / Am; and insoluble sodium metaphosphate in the form of a particle mass with an average particle size of about A fl e / “mf Such toothpastes have an aesthetically pleasing appearance. The toothpastes contain dispersed visible particles of the agglomerate polish. During toothbrushing, the agglomerated particles are first perceptible but are then easily reduced to individual polish particles of small size when a light pressure is applied with the toothbrush.

Example § 6000 parts of anhydrous dicalcium phosphate in the form of a particle mass with the particle sizes given in Example 2 were mixed with 150 grams of acacia rubber powder and 50 parts of tragacanth rubber. The mixture was then moistened with a 10% aqueous acacia gum solution. The agglomerates were prepared and then sieved in the manner set forth in Example 2. 20 parts of the agglomerate particles described above in this example can be mixed with 80 parts of a toothpaste.

Example 4 Agglomerates of the type described in Example 3 can be prepared when the mixture is moistened with (A) a 20% aqueous solution of acacia glue or rubber, (B) a 10% solution of polyvinylpyrrolidone, (C) water, ( D) ethanol or (E) glucose solution.

Toothpastes similar to those of Example 1 can be prepared using the assemblies of this example.

The toothpastes described in this example have an aesthetically pleasing appearance. The toothpastes contain dispersed visible particles of the agglomerate polish. During toothbrushing, the agglomerated particles are first perceptible, but are then easily reduced to individual small size polish particles when a light pressure is applied with the toothbrush. Calcium mixtures of the components listed below were converted into agglomerates by compression on a rotary tablet press to obtain tablets about 6 x 25 mm in size. The tablets were then crushed in an oscillating granulator and the particles thus obtained were sieved with sieves with uniformly spaced openings of 840 and 840, respectively. 420 .mu.m to obtain particle sizes greater than 840 .mu.m, particle sizes between 420 and 840 .mu.m, and agglomerates finer than 420; ¿m: Qålaš Polishing agent (A) (B) (v) (D) (E) (F) ( G) (H) (I) (J) Dicalcium phosphate amine aarate 910 090 440 855 Insoluble sodium metaphosphate Hydrated alumina Binder 450 865 865 900 890 790 ^ 89O 'Polyethylene glycol 6000 Lubricant Magnesium stearate 10 10 10 10 10 10 10 10 Talk - 35 Stearic acid I 5 100 100 100 200 100 100 100 100 100 100 100 parts of each of the agglomerate particles of this example are mixed with 80 parts of a toothpaste. These toothpastes also have an aesthetically pleasing appearance.

Visible particles of the agglomerate polishes are dispersed therein in the toothpastes. During toothbrushing, the agglomerated particles are first noticeable, but are then easily reduced to individual polish particles of small size when a light pressure is applied with the toothbrush.

Example 6 99 parts of unmalted dicalcium phosphate dihydrate with an average particle size of about 118 33 33 / Lm were mixed with 1 part of magnesium stearate as lubricant. The powder mixture was pressed in a rotary tablet press into tablets with a size of 6 x 25 mm. The tablets were then granulated in an oscillating granulator to obtain smaller agglomerate particles. These particles were sieved through sieves with uniformly spaced openings of 040 roßp. 420 / lm. . in 20 parts of the agglomerate particles according to this example, which passed through the sieve with openings of 840 / Am and which were retained on the sieve with openings of 420 [mu] m, were mixed with 80 parts of a toothpaste.

The toothpaste described in this example also has an aesthetically pleasing appearance. Visible particles of the agglomerate polish are dispersed therein in the toothpaste. During toothbrushing, the agglomerated particles are first perceptible, but are then easily reduced or decomposed into individual small size polish particles when a light pressure is applied with the toothbrush.

Claims (2)

7201253-'7 _12. P a t e n t k r a v Opaque toothpaste comprising a gel or cream-like matrix normally incorporated in opaque toothpaste having homogeneously dispersed particles of an agglomerated material therein comprising a water-insoluble toothpaste, characterized in that the agglomerated material consists of sub- particles of said water-insoluble tooth polish and a water-soluble binder and optionally a dye or pigment, which sub-particles have a particle size of less than 177 .mu.m and are held together in agglomerated form by the binder to form particles having a particle size of 420 - 2380 .mu.m , preferably 420 - 840 .mu.m, which agglomerated particles are perceptible and substantially insoluble in the toothpaste, but easily decomposable by toothbrushing by mechanical action into individual, small polishing particles, of which the agglomerated particles are composed and which are imperceptible below toothbrushing. Toothpaste according to claim 1, characterized in that the polishing agent comprises water-insoluble phosphates, silica, hydrated alumina or zirconium silicate. STATED PUBLICATIONS: storbriurann fi en 628 315 us 1 usz 681 (424-49), 2 1% 150 Mza-sv)