SE409545B - TRANSPARENT 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

7201254-5 2 Clear toothpastes that have a transparent or translucent gel base are also known. Such products can be prepared with or without solid ingredients, especially selected polishing material, depending on the preparation which is desired to be achieved, but these ingredients make the toothpaste base opaque.

It has now been found that a transparent toothpaste of the kind initially indicated with an agglomerated material of tooth polish can be produced with such a grain size of the agglomerate that the individual grains or particles become visible to the naked eye. The transparent toothpaste according to the invention is 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 less than 177 μm and are held together in agglomerated form by means of bees. * the agent for forming particles with a particle size of 520-2380 μm, preferably Ä20-8ÄD μm, which agglomerated particles are perceptible and substantially insoluble in the 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. Because the agglomerates or grains are visible to the naked eye, they have a marked effect on the aesthetic appearance of a transparent toothpaste and the agglomerates do not cause the toothpaste to become opaque.

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, trimagnesium orthophosphate and tricalcium phosphate, tricalcalcium. Other polishing agents include calcium carbonate, magnesium carbonate, hydrated alumina, silica, zirconium silicate, aluminum silicate, including calcined aluminum silicate and polymethyl methacrylate. Combinations of polishes can also be used. The preferred polishing agents 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 in question and the insoluble sodium metaphosphate has, as pointed out 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 (hth ed.), Pp. 510-Sll. 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 Å Z 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 agents. These materials exhibit binding and / or lubricating properties or the like so that they form agglomerates which exhibit the desired properties in the clear 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, carboxyethylvinylvinylhydroxyl, , magnesium-aluminum silicate gel and the like. Examples of further 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 ïk fl ë fl dß in the manufacture of tablets and other compressed or agglomerated materials.

Mixtures of agglomerated agents can also be used. When the polishing agents are released from the binding action of these agents upon application of low 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 aggiomerate and imparts a translucent effect to the transparent toothpaste. Typically, the polish consists of about 75.58% by weight of the finished agglomerate. The binder is present in a sufficient amount to facilitate agglomeration, i.e. about 2-25% by 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 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 polish particles and any binder is compressed in a tablet press. In typical cases, essentially all polishing particles have an individual particle size of less than 250 m. The large tablet prepared in this way typically has dimensions of about 6 x 25 mm, but even larger tablets can be produced. The tablet is then crushed into visible granules glomerular with particle sizes suitably up to about 2380 .muM. Typically visible particles are up to BHD rm »such as about ÄZD-8 fi0 Pm. The crushing can be carried out, for example, in a mill, granulator or in a crusher.

When the dry process is used, the mixture intended for agglomeration suitably contains a lubricant such as talc, magnesium stearate, calcium stearate, stearic acid and the like. The lubricant facilitates agglomeration and is available in a quantity 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 smaller than 1 micron, and binder continuously in a "Bravo" tray, 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 pzm. The agglomerates are then dried, for example, in air or in an oven. The agglomerates can then be broken down into desired clearly visible sizes such as between 420 and 840 μm 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 agglomerates formed can be easily inserted into the oral cavity with a visually clear toothpaste and without inconvenience retained in the oral cavity until Visible particles, and generally those having a size greater than about 2380 microns, can therefore be conveniently separated from the agglomerates. It is also convenient to separate small parts having a much smaller particle size than about 420 microns, 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 paints and the like. The dye material is usually used in concentrations of about 1-10%.

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 impact such as when brushing the teeth, gums or other parts of the nun cavity with a toothbrush, tongue a finger or the like. . The agglomerated material according to the invention is mixed in a visually clear toothpaste, i.e. a transparent or transparent gel paste of the gel type, without its clarity being significantly affected in a negative direction. These agglomerated particles are homogeneously dispersed and are present both on the surface and inside the toothpaste. Because the toothpaste is transparent or translucent, all agglomerated particles are visible to the naked eye.

Transparent and transparent toothpastes contain a dental carrier which forms a gel mass of a consistency which can suitably be pressed out of a compressible tube of, for example, aluminum or lead. The carrier contains liquids and solid substances. 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% by weight of the toothpaste. In transparent and translucent toothpastes, the liquid content can be about 20 - 89.5% by weight.

The solid portion of the carrier contains a gelling agent such as natural and synthetic gum materials and gum-releasing materials, for example carrageenan moss, dr-agent, alkali metal carbozocymethylcellulose and hydroxymethylcarbo-ethylcellulose, polyvinylpyrrolidone, starch, 'Carbopol' 934 and 940. Such a solid component in 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 an amount sufficient to achieve distinct particles with an attractive appearance and desired polishing effects.

They may typically be present in any suitable amount up to about 50% by weight of a transparent or translucent toothpaste depending on the desired appearance, polishing effects and type of preparation which 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 polishing material is selected so that it becomes invisible in the base material of the clear toothpaste and increases the effect further in addition to that obtained by the agglomerates. The total amount of polishing material, e.g. mainly about 5 - 75%, is in this case divided into the agglomerates and the clear toothpaste base material as desired.

The tooth cleaner may also contain a surfactant. It is preferred that the total amount of surfactant be about 0.05 - 5, preferably about 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 with a chain length of 10 to 18 carbon atoms). A preferred material is a long chain fatty acid monoglyceride sulfate, for example sodium salt of hydrogenated coconut fatty acid monoglyceride sulfate alone or in combination with sodium lauryl sulfate. Other suitable materials are the fatty acid amides of amino acids, such as sodium N-1auryl sarcosinate. The detergent content is usually between about 1 and about 10%.

Other types of material can be mixed into the oral preparation according to the invention. Examples of such materials are colorants or whitening agents, preservatives, silicones, chlorophyll fillings, 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 at levels up to about 0.01 - 5 X. Typical examples of such antibacterial agents include guanidines, biguanides and amines such as: N1- (4-chlorobenzyl) -N5-2,4-dichlorobenzene. syl) -biguanide; p-chlorophenyl biguanide; 4-chlorobenzhydryl biguanide; 4-chlorobenzhydryl-guanylurea; N-3-1auroxypropyl-N5-n-chlorobenzyl biguanide; 1,6-di-p-chlorophenyl-biguanido-hexane; 1- (1auryl-dimethylammonium) -8- (p-chlorobenzyldimethylammonium) -octane dichloride; 5,6-dichloro-2-guanidinobenzimidazole; N1-p-chlorophenyl-N5-lauryl biguanide; 5-amino-1,3-bis (2-ethylhexyl) -5-methylhexahydropyrimidine; and the non-toxic acid addition salts of these compounds.

Oils, for example from garden mint, peppermint, evergreens, sassafras, clover, sage, 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 flavoring and sweetening agents may be included in the toothpaste at a total level of between about 0.01 and 5 X 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, renal fluorine, xalium fluoride, xalum: (11) fluoride (acid-tr), sodium mexafluoroanstannate, tin (II) chlorofluoride, sodium fluorosirconate and sodium monofluorofluorose. Soluble materials which dissociate and give off fluorine-containing ions in water 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 visually clear toothpaste of 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 sodium carboxymethylcellulose or Carbopol 934, and a preservative, such as 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 l sorbitol solution, can then be mixed into the dispersion, which is then heated at about 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. A suitable flavoring agent can be added afterwards, after which the toothpaste is deaerated again.

The agglomerates are then dispersed in the visually clear 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 illustrated, but it is of course not limited to the embodiments described in the examples. Parts and percentages refer to parts by weight and percentages by weight, respectively, unless otherwise expressly stated. Example 220 220 parts of average calcium particle size dihydrate of about 2.4 microns were moistened with 91 parts of a 10 X aqueous aqueous solution of acacia rubber in a "Hobart" mixer to a uniformly wet mixture. The wet mass was pressed through a sieve with uniform openings of 2380 μm and oven dried for 1 hour at 65 ° C. The dried agglomerates were then sieved through a sieve with uniform openings of 420 μm. 132 parts of the agglomerated dicalcium phosphate dihydrate were retained on the sieve with uniform openings of 840 μm and 37 parts passed through the sieve with uniform openings of 420 μm.

Similar agglomerates of water-insoluble tooth polish were prepared by mixing 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 microns; anhydrous dicalcium phosphate: I. form of particles, substantially all of which were less than about 7.4 microns; and insoluble sodium metaphosphate having an average particle size of about 4.8 μm.

These polishes were mixed with a 10 X aqueous solution of acacia gum.

Example 2 20 parts of the agglomerate particles of Example 1, which passed through a sieve with uniform openings of 840 μm and which were retained on a sieve with uniform openings of 420 μm, are mixed with 80 parts of a transparent toothpaste according to the following recipe: water in 81.00 X methyl parahydroxybenzoate 0.15 X propyl parahydroxbenzoate 0.15 74 sodium saccharin 0.20 Z glycerol 10.00 K "Carbopol" 940 2.00 in sodium lauryl sulfate 1.50 X sodium hydroxide solution (10 X) 5.00 X Similar tooth cleaners can be prepared using aggregates obtained by mixing with a 10 μg acacia gum solution; hydrated aluminum with a particle size of less than about 2.5 rooms; calcium carbonate in the form of a particulate mass, in which substantially all particles have a size less than about 7 .4 μm; and insoluble sodium naphosphate in the form of a particulate mass having an average particle size of about 4.8 microns. 7201254-5 m The toothpastes described in this example are transparent and 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, as a light pressure is applied with the toothbrush; 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 grams of acacia gum powder and 50 parts of tragacanth gum. The mixture was then moistened with a 10 X aqueous solution of acacia gum. The agglomerates were prepared and then sieved in the manner set forth in Example 1.

Example 4 20 parts of the agglomerate particles described in Example 3 are mixed with 80 parts of a transparent toothpaste according to the following composition: p glycerol 10.00 1 sodium carboxymethylcellulose 2.00 X sodium benzoate 0.50 in sodium saccharin 0.20 2 sodium uryl sulfate 2.50 X dye 0.10% ethanol (95 Z) 10.00 X flavor 1.30 2 sorbitol solution (70 L) 73.40 X Example 5 Agglomerates of the type described in Example 3 can be prepared when the mixture is moistened with ( A) a 20 Z aqueous solution of acacia glue or rubber, (B) a 10 Z solution of polyvinylpyrrolidone, (C) water, (D) ethanol or (E) glucose solution. Example 6 Toothpastes similar to that of Example 4 can be prepared using aggregates. The toothpastes described in this example are transparent and 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.

Example 7 Powder 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 420 μm, respectively, to obtain particle sizes greater than 840 μm, particle sizes between 420 and 840 μm, and agglomerated finer than 420 fu-m; 23.23; Polishing agent (A) (ß) (C) (D) (E) (F) (G) (H) W (I) (J) Dical cium phosphate dihydrate 890 91 0 Calcium carbonate 440 86 5 Insoluble sodium metaphosphate 450 865 865 * 900 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 Example 8 20 parts of each of the agglomerate particles according to Example 7 described above mixed with 80 parts of a transparent toothpaste having the following composition: '7201254-5 12 glycerol 10,00 74 sorbi wlias (70 x) 75,10 x sodium benzoate V 0,50 75 7 sodium carboxymethylcellulose 2,00 74 sodium lauryl sulphate 1,50 in flavoring 80 Z ethanol (95 74) 1o, oo 74 dye 0.10 71 These toothpastes are transparent and have an aesthetically pleasing appearance. Visible particles of the agglomerated polishes are dispersed in the toothpastes. During toothbrushing, the agglomerated particles are first perceptible, but are then easily reduced to individual small size polish particles, as a light pressure is applied with the toothbrush.

Example 9 99 parts of unmalted dicalcium phosphate dihydrate with an average particle size of about 118 in 33 parts 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 by sieves with uniformly spaced openings of 840 and 420 ppm, respectively.

Example 10 20 parts of the agglomerate particles of Example 9, which passed through the sieve with apertures of 840 μm, and which were retained on the sieve with openings of 420 μm, were mixed with 80 parts of a transparent toothpaste having the following composition: glycerol 10,000 X sorbitol 74.075% sodium carboxymethylcellulose 2,000 X sodium benzoate 0.500% sodium saccharin 0.200 X dye 0.100 2 sodium lauryl sulfate. 1,500 7š ethanol (95 75) 10,000 Z flavor _ 1,625 X 720125lr-5 13 'The toothpaste described in this example is transparent and 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 disintegrated into individual small size polish particles when a light pressure is applied with the toothbrush.

Example 11 200 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 μm, and 1 part of substrate pigment (D&C Lake Red No. 30) were moistened with 40 parts of a 10% -a aqueous solution of acacia rubber in a "Hobart" mixer for 10 minutes. The colored wet mass thus obtained was pressed through a sieve with uniform openings amounting to 2380 μm and oven dried for 1 hour at 65 ° C. The dried agglomerates were then sieved through a sieve with uniform openings amounting to 840 μm and a sieve with uniform openings. amounting to 420 | Lm.

When the agglomerated particles are incorporated in a toothpaste, they are first perceptible during toothbrushing and are then easily reduced to individual small-size polishing particles, when a light pressure is applied with toothpaste.

Claims (2)

7201254-sl lll P a t e n t k r a v 1.; Transparent toothpaste comprising a gel or cream-like matrix normally contained in a transparent or translucent 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 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 μm and are held together in agglomerated form by the binder to form particles with a particle size of 420 - 2380 μm, preferably 420 - 840 μm, which agglomerated particles are perceptible and substantially insoluble in the toothpaste, but easily decomposable by toothbrushing by mechanical action to individual, small polishing particles, of which the agglomerated particles are composed and which are impermeable during toothbrushing. Toothpaste 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 Å _ US 1,082,681 (424-49), 2,196,150 (424-57)