SE409413B - AGGLOMERATED MATERIAL FOR USE AS AN INGREDIENT OF A TOOTH CREAM - 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

6910709-2 It has now been found that a material containing agglomerated of water-insoluble polishing agent with a suitable polishing action can be produced in such a grain size that the individual grains become visible to the naked eye. The agglomerates are mainly water-insoluble and the tooth cleaner that contains these grains does not give a feeling of grayness at the same time as the desired grinding effect is achieved. The grains can be easily decomposed by mild mechanical action, for example the mechanical action which occurs when brushing the teeth with the tooth cleaning agent, whereby the grains are divided into the particles of which the agglomerate is built. Then it is easy to rinse the polish out of the oral cavity. Because the grains are visible to the naked eye, they have a marked effect on the appearance of toothpaste.

The agglomerated material according to the invention is characterized in that it 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 Pm and are held together in agglomerated form by means of the binder for to form particles with a particle size of 420 - 2380 Pm, preferably 420 - 840 Pm, which agglomerated particles are perceptible and substantially insoluble in a toothpaste, but easily decomposable by toothbrushing by mechanical action to individual, small polishing particles , of which the agglomerated particles are composed and which are imperceptible during toothbrushing.

Known water-insoluble tooth polishes can be agglomerated according to the invention. The polishes thus include insoluble phosphates, such as insoluble sodium metaphosphate, insoluble potassium metaphosphate, calcium pyrophosphate, magnesium orthophosphate, trimagnesium orthophosphate, tricalcium phosphate, dicalcium phosphate dihydrate, anhydrous dicalcium phosphate and the like. Other polishing agents include calcium carbonate, magnesium carbonate, hydrated alumina, silica, zirconium silicate, aluminum silicate, among others. calcined aluminosilicate and polyethyl methacrylate. Combinations of polishes can also be used. The preferred polishes are dicalcium phosphate and insoluble sodium etaphosphate. '“* L. .so: Ää -w 4.3 ... 6910709-2 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, in the manner described in Thorpe's Dictionary of Applied Chemistry, Vol. 9 (4th ed.), Pp. 510-5ll. As further examples of suitable materials may 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 commonly referred to as insoluble metaphosphates. There is a small amount of soluble phosphate material as impurities, usually a few percent, up to about 4% of the weight of the material. The amount of soluble phosphate material, which in insoluble sodium metaphosphate is assumed to be a soluble sodium phosphate, can be reduced, if desired, by washing the material with water.

The said binder is used to carry out the agglomeration of the polish particles. Examples of binders which may be mentioned are gum arabic, gelatin, starch, alkali metal carboxymethylcellulose, polyethylene glycol, glucose, sucrose, methylcellulose, carboxyethylhydroxymethylcellulose, sodium alginate, polyvinylpyrrolidone, polyvinylgalane, polyvinyl gelalkyl. Mixtures of binders can also be used. When the polishes are freed from these binders, which occurs during the mild mechanical impact that is typically exerted during brushing, the binders are easily dissolved in the saliva.

The polish constitutes about 75 - 98% by weight of the finished agglomerate, the constituent binder constituting about 25 - 2% of the total weight of the finished agglomerate.

The binder is mixed into the polish in the form of a dry powder or a solution in water or alcohol. The material can be 691o709 ~ 2 transferred to agglomerates by a dry or wet process. In the former case, the mixture of polish particles and binder is pressed in a tablet press. In typical cases, one of the polishing particles has a diameter of less than 250 Pm. The large tablet produced in this way typically has the dimensions of approximately 6 x 25 mm, but even larger tablets can be produced. The tablet is then crushed into a granulate, in which the individual grains are visible to the naked eye. Each grain preferably has a diameter up to about 2380 of about 420 - 840 Fm. The crushing is carried out in typical cases, but preferably the particles have a diameter in a mill, in a granulator or in a crusher.

When transferring the material to agglomerates by dry means, it may suitably also contain a lubricant, such as talc, magnesium tearate, calcium stearate, stearic acid and the like. The lubricant facilitates agglomeration.

When the binder in the form of a dry powder is mixed with the polish and the agglomeration is carried out wet, solvents such as water or ethanol or a solution of an additional amount of binder are mixed into the mixture in an amount sufficient to wet the pulp. Conversion of the pulp to a wet granulate can be accomplished by wetting a powder mixture of water-insoluble toothpaste in the form of a particulate mass in which the individual particles typically have a diameter of less than 74 .mu.m, and binder continuously. in a "Dravo" trough, in a "Hobart" mixer or other suitable powder mixer, so as to obtain a wet mass. The wetting can be accomplished by bringing the polish into contact with a solid binder and then wetting the mixture with a solvent for the binder. The wet mass thus obtained is then pressed through a sieve with uniform openings so that agglomerates with a diameter of 420 - 2380 Pm are formed. The agglomerates are then typically dried in air or in an oven. The agglomerates can then be divided into fractions with suitable sieve analyzes, for example 420 - 840 Fm by sieving. If the wet pulp is produced in a "Dravo" tray, pressing through a sieve may be superfluous. The agglomerates formed should be easily inserted into the oral cavity by means of a toothpaste. For this purpose, grains with a diameter of over about 2380 Pm should be removed; removed from the granulate. In order to make the appearance of the granulate as aesthetic as possible when it is mixed with toothpaste, it is convenient to separate grains with a diameter below about 420 Fm. However, all 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 also contain non-abrasive diluents or fillers, such as lactose, starch. mannitol and the like in amounts corresponding to between about 1 and about 5% of the total weight of the agglomerate. This improves the polishing effect of the agglomerate. In addition, the mixture may contain bicomponents, for example a dye or a pigment. Typical dyes and pigments include water-insoluble dyes and substrate pigments (F, D & C) and the like. Paint materials are usually used in concentrations of about 1-10%.

Due to the fact that the main amount in the polishing agent units consists of water-insoluble polishing agent, the agglomerates are mainly water-insoluble. In the oral cavity, the grains of the agglomerate are rapidly degraded and change from grains visible to the naked eye, which can be felt in the mouth, to particles which are invisible to the naked eye, which cannot be felt in the mouth. This is due to the mild mechanical stress to which the agglomerates are subjected. of the teeth, gums or other parts of the oral cavity with a toothbrush. Degradation can also occur by rubbing the tooth cleaner against the teeth, gums or other parts of the oral cavity, with the tongue, a finger or the like.

The agglomerated material according to the invention can be mixed with a transparent or transparent gel toothpaste, but it can of course also be mixed into an opaque toothpaste. Grains of the agglomerated polishing particles are present both on the surface of the dentifrice and inside it. When the tooth cleaner is a transparent or translucent toothpaste, all the grains are visible to the naked eye. On the other hand, when the toothpaste is opaque, only the grains on the surface are visible.

Transparent, transparent and opaque toothpastes contain a carrier which forms a gel or a creamy mass, the consistency of which is such that the cream can be squeezed out of a tube, for example of aluminum or lead. The carrier contains liquids and solids. In general, the liquid portion contains water, glycerol, sorbitol, propylene glycol, polyethylene glycol 400 or the like including suitable mixtures of these materials. It is usually advantageous to use a mixture of both water and a humectant, such as glycerol, sorbitol, propylene glycol and the like. The total liquid content is generally between about 20 and about 89.5% of the total weight of the toothpaste. In transparent or translucent toothpaste, the liquid content can be between about 20 and about 89.5%, while opaque toothpaste usually contains a total of about 20 - sd% liquid.

The solid portion of the carrier is a gelling agent, for example, natural or synthetic materials such as carrageenan, tragacanth, alkali metal carboxymethylcellulose and hydroxymethylcarboxyethylcellulose, polyvinylpyrrolidone, starch, water-soluble hydrophilic colloidal carboxyvinyl polymers, such as the materials which are Carbopol "934 and 940. The solids in the carrier typically comprise about 10, preferably about 0.5 - 5% of the total weight of the toothpaste.

The agglomerated particles are usually mixed into the toothpaste in an amount corresponding to about 5 - 75, preferably 10 - 75% of the total weight of the toothpaste. In transparent or transparent toothpastes, the agglomerates are typically included in amounts corresponding to up to about 50% of the total weight of the toothpaste. 6910709-2 In addition to carriers and agglomerates, the tooth cleaner may contain water-insoluble polishes with such a particle size that the individual particles are invisible to the naked eye, ie. such polishes hitherto used in toothpastes and having a particle diameter of less than about 74 .mu.m. This is the case if one wishes to increase the polishing effect beyond that which can be achieved with the aid of the agglomerates.

The tooth cleaner may also contain surfactants. It is preferred that the total amount of surfactant be about 0.05 - 5%, preferably 1 - 3% of the total weight of the dentifrice.

Suitable surfactants include water-soluble sulphates of compounds with long-chain alkyl radicals (for example alkyl radicals having a chain length of 10 to 18 carbon atoms). 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.

Other materials can be mixed into the oral preparation according to the invention. Examples are colorants or optical brighteners, preservatives, silicones, chlorophyll compounds, ammonia derivatives such as urea, diammonium phosphate and mixtures thereof, etc. Each of these agents can typically be incorporated into the dentifrices of the invention in amounts corresponding to up to cikra 5%. When dyes are used, the agglomerates may be colored with a suitable contrasting color.

The dentifrice may also contain antibacterial agents in levels up to about 0.01 - 5%. Typical examples of such antibacterial agents include guanidines, biguanides and amines, such as: N1- (4-chlorobenzyl) -N5-2,4-dichlorobenzyl) biguanide; p-chlorophenyl biguanide; 4-chlorobenzhydryl biguanide; 4-chlorobenzhydrylguanylurea; N-3-lauroxypropyl-N5-p-chlorobenzyl biguanide; 1,6-di-p-chlorophenylbiguanidohexane; 1- (lauryl dimethylammonium) -8- (p-chlorobenzyldimethylammonium) octane dichloride; 5,6-dichloro-2-guanidinobenzimidazole; N1-p-chlorophenyl-N5-lauryl biguanide and 5-amino-1,3-bis (2-ethylhexyl) -5-methylhexahydropyrimidine, and non-toxic acid addition salts thereof.

Oils can be used as suitable flavoring and sweetening agents, for example from garden mint, peppermint, evergreens, sassafras, clover, sage, eucalyptus pus, marjoram, cinnamon, lemon and orange as well as sodium methyl salicylate. Suitable sweeteners are sucrose, lactose, maltose, sorbitol, sodium cyclamate and saccharin. Suitable flavoring and sweetening agents may be included in the dentifrice in a total content of between about 0.01 and 5% based on the total weight of the mixture.

The mixtures according to the invention may suitably also contain a fluorine-containing compound with a beneficial effect, for example reduction of the solubility of the tooth enamel in acid and protection of the teeth against destruction. Examples of such fluorine-containing compounds are sodium fluoride, üHm (II) fluoride, potassium fluoride, potassium stannous fluoride (SnF2.KF), sodium hexafluoro stannate, stannous chlorofluoride, sodium fluorofurcirconate and sodium monofluorophosphate. These materials, which dissociate in water and give off fluorine-containing ions, are suitably present in effective but non-toxic contents, 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 prepares the agglomerates in the manner indicated above. Thus dispersed together with a wetting agent, for example glycerol, a gelling agent, for example sodium carboxymethylcellulose or "Carbopol" 934, and a preservative, for example sodium benzoate, if used. 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 about 40-65 ° C to form a paste, a gel or a cream. If a surfactant, for example sodium lauryl sulphate, is used, it is then dispersed in the mixture, which is finally deaerated and cooled. the desired aroma can be added afterwards, after which the cream must be 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.

The following examples further illustrate the invention, but it is of course not limited to the embodiments described in the examples. Parts and percentages refer to parts by weight and percentage by weight, respectively, unless otherwise stated in detail.

Example 1: 220 parts of average particle size dicalcium phosphate dihydrate about 2.4 Pm were moistened with 91 parts of a 10% aqueous solution of acacia paste in a "Hobart" mixer to a uniformly wet mixture. This was pressed through a sieve with uniform openings 2380 Fm and oven dried for 1 hour at 65 ° C. The dried agglomerates were then sieved through a sieve with uniform openings 420 Pm. 132 parts of agglomerated dicalcium phosphate dihydrate were retained on the sieve with uniform openings 840 Pm and 37 parts passed through the sieve with uniform openings 420 Pm.

Similar agglomerates of water-insoluble tooth polish were prepared by mixing together hydrated alumina having an average particle size of about 2.5 microns; calcium carbonate consisting of particles, substantially all of which had a particle size of less than about 7.4 Pm; anhydrous dicalcium phosphate in the form of particles, substantially all of which are less than about 7.4 Pm; and insoluble sodium metaphosphate with an average particle size of about 4.8 Pm. These polishes were mixed with a 10% aqueous solution of acacia adhesive.

Example 2: 20 parts of agglomerate according to Example 1, which passed through a sieve with uniform openings 840 Pm and retained on a sieve with uniform openings 420 Pm were mixed with 80 parts of a transparent toothpaste with the following composition: Water 81 .00% Methyl parahydroxybenzoate 0.15% Propyl parahydroxybenzoate 0.15% Sodium saccharin 0.20% Glycerol '10.00% "Carbopol" 940 2.00% Sodium lauryl sulphate I 1.50% Sodium hydroxide solution (10%) 5.00% Similar tooth cleaners can prepared using agglomerates prepared by mixing with a 10% acacia adhesive solution of: hydrated alumina having an average particle size less than about 2.5 .mu.m; calcium carbonate in the form of a particulate mass, in which substantially all the particles were smaller than about 7.4 Pm in size; anhydrous dicalcium phosphate in the form of a particulate mass, in which substantially all the particles were less than about 7.4 Pm; and insoluble sodium metaphosphate in the form of a particle mass of average particle size of about 4.8 .mu.m.

The toothpastes described in this example are transparent and have an aesthetically pleasing appearance. In the toothpastes are dispersed grains visible to the naked eye. During toothbrushing, these grains are first noticeable but are easily crushed during brushing. 6910709-2 ll Example 3: 6000 parts of anhydrous dicalcium phosphate in the form of a particle mass with the particle sizes given in Example 1 were mixed with 150 g of acacia paste powder and 50 parts of dragant. The mixture was then moistened with a 10% aqueous solution of acacia adhesive. Agglomerates were then prepared and sieved in the manner set forth in Example 1.

Example 4: 20 parts of the granulate prepared as indicated in Example 3 were mixed with 80 parts of a clear toothpaste having the following composition: Glycerol 10.00% Sodium carboxymethylcellulose 2.00% Sodium benzoate 0.50% Sodium saccharin 0.20% Sodium lauryl sulfate 2.50% Dye 0.10% Ethanol (95%) 10.00% Flavor 1.30% Sorbitol solution (70%) 73.40% Example 5: Agglomerates of the type described in Example 3 can be prepared when the mixture moistened with (A) a 20% aqueous solution of acacia adhesive, (B) a 10% solution of polyvinylpyrrolidone, (C) water, (D) ethanol or (E) glucose solution.

Example 6: Tooth cleaning agents of the type described in Example 4 can be prepared using aggregates according to Example 5.

Toothpastes described in this example are transparent and have an aesthetically pleasing appearance. Grains of agglomerated polish particles visible to the naked eye are dispersed in the toothpastes. During toothbrushing, the grains are first noticeable but are easily crushed into fine particles.

Example 7: The following agglomerates are prepared by mixing polishes, binders and lubricants to form a powder mixture. The powder mixtures listed below were pressed in a rotary tablet press into tablets with approximate dimensions 6 x 25 mm. The tablets were then crushed in an oscillating granulator and the particles thus obtained were then sieved with sieves having uniformly spaced openings with a diameter of 840 and 420 Fm, respectively, to obtain particles with particle sizes above 840, between 420 and 840 sqm and finer than 420 sqm.

The agglomerates were prepared as above from the following components: Parts Polishing (A) (B) (C) (D) (E) (F) (G) (H) (I) (J) Nicalcium phosphate dihydrate 890 910 Calcium carbonate 440 865 Insoluble sodium metaphosphate 450 ess is seen 900 in Hydrated alumina 890 790 890 Binder Polyethylene glycol 6000 100 100 100 200 100 100 100 130 100 100 Lubricant Magnesium stearate 10 10 10 10 10 10 Talc 35 35 35 Stearic acid 8 '5 Example 8: 20 parts of each of the granules prepared as in Example 7 was mixed with 80 parts of a clear toothpaste having the following composition: Glycerol 10.00% Sorbitol solution (70%) p75, 10% Sodium benzoate 0.50% Sodium carboxymethylcellulose 2, 00% Sodium lauryl sulphate 1.50% Flavor 7 0.80% Ethanol (95%) 10.00% Dye 0.10% The toothpastes described in this example are transparent and aesthetically pleasing. Particles visible to the naked eye 6910709-2 13 are dispersed in the toothpaste. When brushing teeth, the grains are first perceptible in the mouth but are then easily broken down into the individual particles.

Example 9: 99 parts of unmalted dicalcium phosphate dihydrate having an average particle size of about 18 μm 33 Pm were mixed with 1 part of magnesium stearate as lubricant. The powder mixture was pressed in a rotary tablet press into 6 x 25 mm tablets. These were crushed in an oscillating granulator and the product was sieved through sieves with openings at a uniform distance from each other with diameters of 840 and 420 square meters, respectively.

Example 10: 20 parts of the agglomerates prepared as indicated in Example 9, which passed through the sieve with openings 840 Fm and which were retained on the sieve with openings 420 Pm, were mixed with 80 parts of transparent toothpaste with the following composition: Glycerol 10,000% Sorbitol (70%) - 74.075% Sodium carboxymethylcellulose 7 2,000% Sodium benzoate 0.500% Sodium saccharin 0.200% Dye 0.100% Sodium lauryl sulphate 1,500% Ethanol (95%) 10,000% Flavor Ä 1.625% The toothpaste described in this example is transparent and has a transparent appearance. . The toothpaste contains dispersed grains of agglomerated polish particles visible to the naked eye. During toothbrushing, the grains are first noticeable in the mouth but disintegrate easily.

Example 11: 200 parts of anhydrous dicalcium phosphate in the form of a particle mass, in which substantially all the particles had a diameter below about 7.4 Pm, and 1 part of substrate pigment (D&L Lake Red No. 30) was moistened with 40 parts of a 10% aqueous solution of acacia glue in a "Hobart" mixer for 10 minutes. The colored wet pulp obtained in this way was pressed through a sieve with uniform openings 2380 Pm and oven dried for 1 hour at 65 ° C. The dried agglomerates were then sieved through a sieve with uniform openings 840 Pm and a sieve with uniform openings 420 Pm. 10 parts of the dried grains of agglomerated particles which passed through the sieve with openings of 840 Pm and which were retained on the sieve with openings of 420 Pm were mixed with 90 parts of an opaque toothpaste having the following composition: Glycerol (99.3%) 19.950% Sodium carboxymethylcellulose 0.850% Sodium saccharin f 0.200% Sodium benzoate 0.500% Tetrasodium pyrophosphate - 0.250% Water 19.986% Trimagnesium phosphate 0.200% Calcium carbonate 5,000% Dicalcium phosphate dihydrate examples had agglomerate grains visible to the naked eye distributed over the entire surface. During toothbrushing, the grains are first noticeable in the mouth but soon crumble;

Claims (2)

6910 '? 09 "2 15 P a t e n t k r a v Agglomerated material for use as an ingredient in a toothpaste, which agglomerated material comprises a water-insoluble tooth polish, 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, sub-particles have a particle size of less than 177 mn and are held together in agglomerated form by means of the binder to form particles with a particle size of 420 - 2380 mn, preferably 420 - 840 m, which agglomerated particles are perceptible and in substantially insoluble in a toothpaste, but easily decomposed by brushing by mechanical action to individual, small polishing particles, of which the agglomerated particles are composed and which are imperceptible during brushing. Agglomerated material according to claim 1, characterized in that the polishing agent comprises water-insoluble phosphates, silica, hydrated alumina or zirconium silicate. PROMISED PUBLICATIONS: Great Britain 628 315 US 1,082,681 (167-93), 2,196,150 (424-57), 3,431,339 (424-52)