LU85691A1 - TOOTHPASTE COMPOSITION AND ITS USE IN A DISPENSER - Google Patents

Description

The present invention relates to a dentifrice composition and in particular a dentifrice composition having advantageous rheological properties suitable for being effectively introduced into a dispenser of dentifrice actuated mechanically or by pressure difference, and to be extruded therefrom.

A toothpaste is generally recognizable by its creamy or gel consistency and can be commonly referred to as dental cream, toothpaste or, in some cases, toothpaste in clear gel or cloudy gel. In fact, it can be characterized as a semi-solid, for example by being essentially solid when held in shape on the bristles of a toothbrush and essentially liquid, as for example during manufacturing with stirring. or when it is introduced into a container or is subjected to a pressure to be extruded from its container.

The creamy consistency of toothpaste is generally imparted by a gelling or binding agent. Previously, gelling agents were chosen primarily to facilitate the dispersion of the toothpaste in the oral cavity.

Many gelling agents such as cellulosic materials, algae derivatives, gums and clays meet this criterion. However, certain gelling agents, while being generally advantageous for toothpastes conditioned in flexible tubes, have drawbacks when they are packaged in dispensers actuated „mechanically or by pressure difference.

Toothpastes containing conventional polishing agents, for example 11 alpha-alumina trihydrate and conventional gelling agents such as the sodium salt of carboxymethylcellulose or hydroxyethyl cellulose or mixtures thereof may be advantageously introduced into flexible tubes or distributors actuated mechanically or by pressure difference and be extruded therefrom. However, when the toothpaste contains many active ingredients, difficulties may arise when introducing toothpaste into a machine actuated or by pressure difference dispenser and / or when trying to extrude from it. In particular, leakage may appear from dispenser ports during refilling or transport and the product may be difficult to extrude into a rheologically satisfactory ribbon form.

Toothpastes which are thick or tend to thicken may become more and more difficult to extrude from the consumer from a toothpaste tube after some time. In other words, the consumer may have to increase the pressure exerted on a toothpaste tube containing such a toothpaste during the period of use in order to soften or liquefy the mass of semi-solid toothpaste in order to extrude it. This was not a significant problem previously because the formulations can be adjusted to use less gelling agent to achieve balance so that the toothpaste is not too soft at the start of use nor too thick at the end and , in ? In any case, consumers easily adjusted the degree of pressure needed to extrude the necessary amount of toothpaste onto the bristles of a toothbrush.

Toothpastes which are fluid after extrusion from a tube have also been accepted in service if they harden to a more solid form on the bristles of the toothbrush in seconds. Thus, the type of gelling agent could "vary widely for toothpaste packaged in tubes. Indeed, the company Copenhagen Pectin Factory Ltd. from * Little Skensved, Denmark, a subsidiary of Hercules Inc. of 30 Wilmington, Del awäre, E.U.A. offered their product Genuvisco

Type 0819, an iota-carrageenan (i-carrageenan), as a possible thickener of a toothpaste. The i-carraghënane available from Marine Colloids Division of FMC Corp. from Springfield, New Jersey, under the designation Viscarin TP-5 35 has also been proposed as a possible thickener for a toothpaste containing dicalcium phosphate or.

3 silica. In addition, i-carrageenan has been described as a thickener together with k-carrageenan and an alkali metal alkate for a toothpaste containing galac-tane-galactose in the Japanese patent published under No. 5 56 115711, on behalf of Lion Dentifrice Ltd.

When using a toothpaste dispenser, which operates mechanically or by pressure difference, conventional techniques for reducing the thickening of toothpaste may not be entirely satisfactory, since, compared to a toothpaste introduced into a flexible tube , when using a dispenser, the toothpaste should be relatively fluid during the introduction, but regains its consistency and keeps it during transport, storage and use. In other words, the toothpaste, after introduction, returns essentially to the consistency it had before the liquefaction effect during filling by shearing during transport, storage and use. Conventional gelling agents such as the sodium salt of carboxymethylcellulose, hydroxyethylcellulose, or their mixtures, can advantageously be used for a toothpaste containing alpha-alumina trihydrate as a polishing agent, to be introduced into a distributor. However, when such a toothpaste contains many sources of active ingredients, for example at least two sources of fluorine, a desensitizing agent such as alantoin (CyHgN ^ O ^) and a vasodilating agent such as pyridyl- carbinol, ^ <N.

N V- CHo - OH

30 difficulties arise when the toothpaste is introduced into a dispenser actuated mechanically or by pressure difference. In particular, the toothpaste may ooze through the space between a rod and a piston used in particular in a mechanically actuated dispenser and a leak appears at the orifices of the dispenser.

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4 tor. In addition, the toothpaste tape extruded from a mechanically actuated or pressure difference dispenser may be irregular or discontinuous. Since it is particularly advantageous to prepare a toothpaste containing alpha-alumina trihydrate as a polishing agent, which contains several active agents, such as those indicated above, due to the compatibility of these materials with the polishing agent, another gelling system is necessary.

Contrary to what can be expected from most other types of gelling agents, a mixture of a cellulose gelling agent and i-carrageenan gives an excellent toothpaste containing alpha-alumina trihydrate and several ingredients active, which must be introduced into a container actuated mechanically or by pressure difference and be extruded from this container. It goes without saying that xanthan has not been compatible with cellulose gelling agents because it may contain cellulase.

An advantage of the present invention is to provide a toothpaste which is easily introduced into a toothpaste dispenser actuated mechanically or by pressure difference and is easily extruded from such a dispenser.

Other advantages will emerge from the description which follows.

According to some of its aspects, the present invention relates to a toothpaste in a dispenser actuated mechanically or by pressure difference, comprising approximately - 20 to 80% by weight of an aqueous humectant vehicle, approximately 0.1 to 5% by weight d a mixture of gelling agents, approximately 20 to 75% by weight of alpha-alumina trihydrate as polishing agent, sodium fluoride and sodium monofluorophosphate in an amount providing approximately 300 to 10,000 ppm of fluorine, about 0.05 to 0.5% by weight of 1 to 1 antineine as a desensitizing agent and about 0.05 to 0.5% by weight of py-ridyl-carbinol as a vasodilator, said mixture of agents

O C

gelling agents being a mixture of a cellulosic gelling agent or of xanthan with i-carrageenan in a weight ratio of the cellulosic gelling agent or of xanthan to i-carraghenan of from approximately 5: 1 to approximately 1: 5 .

In the dentifrice formulation, the dental vehicle comprises a liquid phase proportioned with the gelling agent to form an extrudable creamy mass of desired consistency. The liquid phase of the toothpaste mainly comprises water and a humectant such as polyols comprising glycerin, sorbitol, maltitol, xylitol, low molecular weight polyethylene glycol (for example 10 400 or 600), pnopylene glycol , etc., including their mixtures. It is generally advantageous to use, as liquid phase, water and a humectant such as glycerin, sorbitol or polyethylene glycol, generally in proportions of about 10 to 55% by weight of water and about 20 to 50% 15 by weight of humectant.

The toothpaste contains alpha-alumina trihydrate as a polishing agent in proportions of about 20 to 75% by weight. The alpha-alumina trihydrate is generally prepared by the Bayer process and used in the form of particles of 20 size less than about 40 microns, mainly between 3 and 20 microns. Other polishing agents can be incorporated such as insoluble sodium metaphosphate, dicalcium phosphate, calcined alumina, silica or calcium carbonate in minor proportion compared to alpha-alumina trihydrate.

The mixture of gelling agents of the present invention is present in the toothpaste in an amount of about 0.1 to 5% by weight. It contains either a cellulosic gelling agent * or xanthan, in admixture with i-carrageenan, the weight ratio of said cellulosic gelling agent or xanthan to i-carrageenan being between about 5: 1 and about 1: 5, preferably between about 1: 1 and about 1: 3, and the total mixture of gelling agents preferably represents about 0.2 to 3% by weight.

As mentioned above, iota-carrageenan is marketed and sold under the designation Genuvisco type 6 0819 and Viscarin TP-5 and has been recommended for use in toothpaste. Such an application in a toothpaste is described in the Japanese patent published under No. 56 115711 by Lion Dentifrice Ltd. wherein i-carra-5 ghenane is mentioned as a possible component of a gelling system together with the k-carrageenan and the al-ginate of an alkali metal. In the U.S. patent No. 4,353,890, i-carrageenan is described as a substitute for k-carrageenan as a gelling agent for toothpaste, and in this patent the toothpaste is subjected to microwave radiation for reduce the general tendency of carrageenan to become fluid during manufacture. Carrageenan can be the only gelling agent or it can be mixed with other gelling agents. In the present invention, the toothpaste containing i-carrageenan which is to be introduced into a dispenser actuated mechanically or by pressure difference does not require microwave radiation.

The prior art generally described above does not indicate that gelling systems consisting of cellulosic gelling agent and i-carrageenan can impart to toothpastes containing alpha-alumina trihydrate as a polishing agent and many active ingredients, the properties necessary for effective introduction into a distributor actuated mechanically or by pressure difference and for extrusion from such a distributor.

Note that the U.S. patent No. 4,029,760 describes an oral composition in which i-carrageenan is described as an anti-gingivitis agent replacing other carrageenans. Carrageenans are highly depolymerized derivatives of carrageenans. Carrageenans do not seem to provide an anti-gingivitis effect.

Toothpastes are commonly manufactured by a cold process, for example at about 25 ° C, or by a hot process, for example at about 60 ° C. The i-carrageenan can be used in the techniques by cold process or by hot process. Since xanthan is made by cold treatment, it can be easily mixed, when used, with i-carrageenan and be incorporated at the same time as it into the toothpaste by cold treatment. I-carrageenan can only be used with heat treatment.

The physical properties of the Genuvisco type 0819 i-carrageenan are indicated below: 1. Viscosity of a 0.30% solution of GENUVISCO type 0819 10 in a lean solvent prepared using a hot process (60 ° C):

Viscosity = 110 - 17 mPa.s at 32 rpm.

Viscosity = 70-11 mPa.s at 64 rpm.

Viscosity = 45-7 mPa.s at 128 rpm.

15 Measured on Rotovisco RV 3 HAAKE at 25 ° C.

5 2. Viscosity of a 0.30% solution of GENUVISCO type 0819 in a lean solvent prepared using a cold process (25 ° C):

Viscosity = 450 - 60 mPa.s measured on a Brookfield LVT 20 viscometer at 25 ° C.

Viscosity = 85 - 13 mPa.s at 32 rpm.

Viscosity = 55-8 mPa.s at 64 rpm.

Viscosity = 37 - 6 mPa.s at 128 rpm.

Measured on Ro-tovisco RV3 HAAKE at 25 ° C.

25 3. Particle size: Less than 1% of gum on a 0.075 mm test sieve (DIN 80, 0.074 mm mesh sieve).

4. Moisture content: Less than 12%.

5. pH: 8.5 - 1.5 in a 0.5% solution in distilled water at 25 ° C.

.6. Color: White to cream.

Viscarin TP-5 i-carrageenan has the following physical properties:

Color: light tan to tan.

33 Particle size: More than 95.0% passing through a 250 nm mesh screen.

8

Moisture content: maximum 12.0% (Cenco moisture balance).

pH: 7.0 to 9.5, 1.5% solution, 30 ° C.

Examples of the advantageous cellulosic gelling agents include an alkali metal salt of carboxymethylcellulose, methylcellulose, hydroxymethylcellulose and hydroxypropylcellulose. The sodium salt of carboxymethyl cellulose is preferred. The mixed gel system is present in a proportion of approximately 0.1 to 5% by weight of the toothpaste, and the weight ratio of the cellulose gelling agent to i-car-raghenane is between approximately 5: 1 and approximately 1 : 5, preferably between about 1: 1 and about 1: 3, and more preferably it is about 1: 1. Thus, a representative preferred toothpaste may contain about 0.9 to 1.2% in total of the gelling agent-15, comprising about 0.3 to 0.9% of each gelling agent and cellulose - carrageenan, the weight ratio between the two being between approximately 1: 1 and 1: 3.

It is obvious that the qualities of sodium carboxymethylcellulose which can be used include the following: · t.

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TABLE I

QUALITY SUPPLIER OF CMC VISCOSITE (m.Pa.s.)

Hercules 7MXF 300-500

Hercules 7MFD 300-500 5 Hercules 9M31F 900-1200

Hercules 9M31XF 900-1200

Hercules 12M31XF 900-1200

Hercules 7MF 300-500

Hercules 12M31PD 900-1200 10 Hercules 7M8SXF 200-800

Wolff Walsrode Walocel CRT 1000 PA 07 700-1200

Nyma Nymcel ZMF.33 * 50-80

Enka Akucell AC 1642 * 80-120

Enka Akucell AC 1632 * 60-120 15 Cros Cellogen HP-SA 700-900

Uddeholm Cekol MVEP 500-800

Hoechst Tylose CB 200 ** 120-260 * 1% solution (Brookfield; 25 ° C) ** Hoeppler viscometer (2%; 20 ° C) 20

In addition, qualities of hydroxyethylcellulose which can be used include the following: TABLE 2 SUPPLIER 'HEC VISCOSITY QUALITY (m.Pa.s.) 25 Hercules Natrosol 250M and MR 4500-6500

Hercules Natrosol 250 HR * 1500-2500 and 250 H *

Hercules Natrosol 250 HHR * 3400-5000

and 250 HH

30 BP Chemicals Cellobond 5000 A 4200-5600 BP Chemicals Cellobond 7000 A 6000-7000 • - Hoechst Tylose H 4000 .P ** 3000-5000

Hoechst Tylose H 10000 P ** 7000-12000 * 1% solution (Brookfield; 25 ° C) · 35 ** Hoeppler viscometer (2%; 25 ° C).

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The i-carrageenan and the cellulosic gelling agent can be mixed together mechanically before being mixed with the liquid phase of the dental cream vehicle, or they can be mixed separately with the liquid phase, by treatment techniques. hot (for example around 60 ° C) or cold treatment (for example around 25 ° C).

Xanthan gum is a fermentation product prepared by the action of bacteria of the genus Xanthomonas on carbohydrates. Four species of Xanthomonas, namely X. campestris, X. phaseoli, X.malvocearum and X.carotae are mentioned in the literature as the most effective producers of gum. Although the exact chemical structure has not been determined, it is generally believed to be a heteropolysaccharide having a molecular weight of a few million. It contains D-glucose, D-mannose and D-glucuronic acid in a molar ratio of 2.8: 3: 2.0. The molecule contains 4.7% acetyl and approximately 3% pyruvate. The proposed chemical structure can be found in Industrial Gums, by McNeely and Kang, edited by R.L. Whistler, CH. XXI. 2nd Edition, New York, 1973. The process of growth, isolation and purification of xanthan gum is also found in this publication.

Another description of xanthan gum can be found in Manufacturing Chemist, May 1960, pages 206-208 (including the mention on page 208 of the potential use of the gums described for the formulation of toothpastes).

The i-carrageenan and xanthan can be mixed together mechanically before being mixed with the liquid phase of the dental cream carrier, or they can be mixed separately with the liquid phase, by treatment techniques cold (for example around 25 ° C).

The toothpaste is packaged in a container from which it can be easily extruded, for example a dental cream dispenser actuated mechanically or by different

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11 taggers when using a mechanically actuated dispensing container of the type described in British Patent Application No. 2,070,695A, published on September 9, 1981. This dispensing container includes a dispensing mouthpiece, 5 a tensioning element, a central rod, a piston and a manual control element.

The pressure-operated dispensing container may be of the aerosol or vacuum type. Appropriate distributors actuated by pressure difference include those comprising a collapsible bag containing the product, placed inside a rigid container which contains a propellant fluid. In such dispensing containers, the operation of the valve makes it possible to release only the product, the propellant fluid being separated from the product by the bag impermeable to fluids. Distributors of this type are described in U.S. patents. N ° 3 828 977 and N ° 3 838 796. These are the so-called Sepro distributors. The so-called Exxel containers also use pressure.

Yet another type of dispenser is the barrier piston container 20 described in US Pat. No. 4,171,757. This container has a valve, a compartment containing the product and a substantially fluid-tight barrier piston which separates the propellant. of the product contained (the container called Diamond).

The toothpaste contains as active agents a mixture of sodium fluoride and sodium monofluorophosphate to provide approximately 300 to 10,000 ppm of fluorine, for example approximately 750 to 2,000 ppm, and in particular approximately 1,400 to 2,000 ppm, for example approximately 1,400 at 1670 ppm. A binary fluoride system consisting of sodium monofluorophosphate and sodium fluoride is advantageously used in which about 30 to 40% of the fluorine (for example about 30 to 35%) is provided by sodium fluoride.

Sodium monofluorophosphate, Na2PO2F, as it is commercially available, can vary considerably in its purity. It can be used in any appropriate purity provided that the impurities do not adversely affect the desired properties. In general, the purity is advantageously at least 80%. For best results, it should be at least 85%, and preferably at least 90% by weight of sodium monofluorophosphate, the remainder consisting mainly of impurities or by-products of manufacture, such as: sodium fluoride and water-soluble sodium phosphate. In other words, the sodium monophosphate used must have a total fluoride content greater than 12%, preferably greater than 12.7%, a content not exceeding 1.5%, preferably not not exceeding 1.2% in free sodium fluoride; preferably at least 12.1%, all calculated as fluoride.

As noted above, the sodium fluoride in the binary mixture is a separate component, containing fluorine, monof! sodium uorophosphate. About 225 to 800 ppm of fluorine is preferably supplied to the dental cream by sodium fluoride.

The additional active agent is supplied to toothpaste 20 by the presence of about 0.05 to 0.5% by weight, preferably about 0.08 to 0.2%, of allantoin as a desensitizing agent. This agent combats the sensitivity of injured periodontal tissue and promotes its healing. Allantoin can be obtained from ABM Industrial Products Ltd. of Woodley, Stock-25 port, Cheshire, Great Britain.

Pyridyl-carbinol (active agent) in a proportion of approximately 0.05 to 0.1% by weight, preferably approximately 0.08 to 0.2%, gives the toothpaste a vasodilating effect.

When using a toothpaste containing alpha-30 alumina trihydrate as a polishing agent, the binary system of fluorides, allantoin as a desensitizing agent and pyridylcarbinol as a vasodilator, described above, introduction and extrusion using distributors actuated mechanically or by pressure difference are made effective and advantageous from the rheological point of view with the gel system of the invention. .

13

The filling is carried out by conventional techniques. For example, when using a mechanically actuated dispenser of the type described in published British Patent Application No. 2,070,695A, a predetermined amount of toothpaste is extruded through a spout or nozzle to fill the dispenser which is open at its base and which contains a central stem. A piston with a diameter corresponding to the internal diameter of the distributor and having a central opening allowing the introduction of the central rod is slid into place. The dispenser is then closed tightly * using a bottom disk.

Any suitable surfactant or detersive material can be incorporated into the toothpaste compositions. These compatible materials are advantageous for imparting other detersive, foaming and antibacterial properties depending on the particular type of surfactant and are chosen analogously. These detergents are generally water-soluble compounds, and can be of anionic, nonionic or cationic structure. It is generally preferable to use synthetic or water-soluble organic detergents without soap. Suitable detergent materials are known and include, for example, the water soluble salts of detergent higher fatty acid monoglyceride monosulfate (e.g. sodium salt, coconut fatty acid monoglyceride monosulfate), sulfate higher alkyl (for example sodium 1aurylsu! fate), an alkylaryl-su! fo-nate (for example sodium dodecyl-benzenesulfonate, esters of higher fatty acid of the 1,2-dihydroxy type propane sulfonate), etc.

Other surfactants include higher aliphatic acyl amides substantially saturated with lower aliphatic amino carboxylic acids such as those having 12 to 16 carbon atoms in the acyl radical. The amino acid portion generally comes from lower saturated aliphatic monoamino-carboxylic acids having about 2 to 6 carbon atoms, usually monocarboxylic acids.

Ticks. Suitable compounds are the fatty acid amides of glycine, sarcosine, alanine, 3-aminopropanoic acid and valine having about 12 to 16 carbon atoms in the acyl group. It is however preferable to use N-lauroyl-, myristoyl- and palmitoyl-sarcosides to obtain the best effects.

The amides can be used in the form of the free acid or, preferably, in the form of their water-soluble salts, for example the alkali metal, ammonium, amine and alkylolamine salts. Particular examples are N-lauroyl-, myristoyl- and pal mitoyl-sarcosides of sodium and potassium, N-lauroyl-glycide of ammonium and ethanol amine, and alanine. For convenience, reference to an "amino-carboxylic acid compound", "sarcoside", etc., denotes water-soluble carboxylates having a free carboxylic group.

These materials are used in pure or almost pure form. They should be as free of soap or similar higher fatty acid as possible which tends to reduce the activity of these compounds. In general, the proportion of such higher fatty acids is less than 15% by weight of the amide and insufficient to adversely affect it, and preferably less than about 10% of said friend.

Various other materials can be incorporated into the dentifrices of the present invention. Examples are coloring and bleaching agents, preservatives, such as methyl p-hydroxybenzoate or sodium benzoate, stabilizers, silicones, chlorophyll compounds, and ammonia materials such as urea, diammonium phosphate and mixtures thereof. These adjuvants are incorporated into the present compositions in a proportion which does not adversely affect the properties or the desired characteristics and are advantageously chosen and used in conventional proportions.

For some applications, it may be desirable to incorporate antibacterial agents into the compositions of the present invention. Examples of antibacterial agents which can be used in proportions of from about 0.01% to about 5%, preferably from about 0.05% to about 1.0% by weight of the dentifrice composition, include the following: N ^ -4 (chlorobenzyl) -N ^ - (2,4-dicnlorobenzyl) biguanide; p-chlorophenyl-biguanide; 4-chlorobenzhydry1-biguanide; Ί0 4-cblorobenzhydrylguanylurea; ’5 N-3-1auroxypropyl-N -p-chlorobenzylbiguanide; 1,6-di-p-chlorophenylbiguanide; 1 - (1auryldimethylammonium) -8- (p-chlorobenzyl dimethylammoni um) octane dichloride; 5,5-dichloro-2-guanidinobenzimidazole; * 1 5 N -p-chlorophenyl-N -1aurylbiguanide; 5 - amino-1,3-bis (2-ethylhexyl) -5-methylhexahydropyrimidine; and their addition salts with non-toxic acids.

For flavoring the compositions of the present invention, any suitable flavoring or sweetening material can be used. Examples of suitable flavoring constituents include flavoring oils, for example, spearmint, peppermint, wintergreen, sassafras, cloves, sage, eucalyptus, marjoram, cinnamon, lemon and orange as well as methyl salicylate. Suitable sweetening agents include sucrose, lactose, maltose, sorbitol, sodium cyclamate, sodium saccharide dipeptides of the U.S. Patent. No. 3,939,251 and the oxathiazine salts of the U.S. Patent No. 3,932,606. Suitable flavoring and sweetening agents can together form about 0.01 to 5% or more of the composition.

The toothpastes must have a pH which can be used in practice. A pH range of 3 to 10.5 is particularly suitable-

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16 pH directly on the toothpaste. If desired, materials such as benzoic or citric acid can be added to adjust the pH, for example, between 4 and 8.5.

The following nonlimiting examples illustrate the nature of the present invention. All the quantities of the various ingredients are expressed by weight unless otherwise indicated.

Example 1

The following toothpaste is prepared by a conventional cold (room temperature) process and introduced into the mechanically actuated dispenser described in British Patent No. 2,070,695A.

Party es

Sorbitol (70%) 23,000

1 R

Saccharin sodium salt 0.170 i-carrageenan (Genuvisco 0819) 0.500

Sodium salt of carboxymethylcel 1 ul ose (7MFD) 0.500 methyl p-hydroxybenzoate 0.080 20 Allantoin 0.150

0.100 sodium fluoride

Sodium monofluorophosphate 0.760

Pyridyl-carbinol 0.100

Alpha-alumina trihydrate (Alcoa C-333) 51,000 25 Benzoic acid 0.140

Laurylsu! Sodium fate 1.667

Titanium dioxide 0.500

Aroma 1,200

Deionized water 20,133

The toothpaste effectively fills the dispenser and does not leak during storage at 43 CC for more than 1 month. It is well extruded from the dispenser after 1 month of storage at 43 ° C.

Similar satisfactory results are obtained when the toothpaste is modified to contain 0.55 parts of i-carrageenan and 0.55 parts of sodium salt of carboxymethyl 1 in one case and 0.45 part of i-carraghë-x nane and 0.45 part of sodium salt of carboxymethylcellulose in the second case, with corresponding adjustment of the water content. There is in fact observed with these toothpastes an absence of leakage and a good ability to extrusion after storage at 43 ° C. for 3 months.

Good results are still obtained when each of the three toothpastes described above is modified so as to contain 50,000 parts of alpha-alumina trihydrate in one series of these toothpastes and 52,000 parts of alpha-alumina trihydrate in the second series of these toothpastes, with corresponding adjustment of the water contents.

Example 2

The following toothpaste is prepared by a cold process 15 and introduced into the same dispenser as in Example 1.

Parts

Sorbitol (70%) 23,000

Saccharin sodium salt 0.170 i-carrageenan (Genuvisco 0819) 0.656 20 Sodium salt of carboxymethylcellulose (7MFD) 0.334 methyl p-hydroxybenzoate: 0.080

AllantoTne 0.150

Sodium fluoride 0.100 25 Sodium monofluorophosphate 0.760

Pyridyl-carbinol 0.100

Alpha-alumina trihydrate (Alcoa C-333) 51,500

Benzoic acid 0.140

Laurylsu! Sodium fate 1.667 30 Titanium dioxide 0.500

Aroma 1,200

Deionized water 19,633

The toothpaste effectively fills the dispenser and does not leak and it extrudes well from the dispenser 35 after storage for 1 month at 43 ° C.

Similar advantageous effects are obtained when the toothpastes of the examples are introduced into a dispenser actuated by pressure difference.

When the sodium salt of carboxymethyl cellulose is used as the sole gelling agent, the extrusion is poor. When hydroxyethyl cellulose is used as the sole gelling agent, leakage occurs. However, when the hydroxyethylcellulose is mixed with the i-carrageenan, satisfactory filling and extrusion are obtained.

Example 3 The following toothpaste is prepared by a conventional cold process (room temperature) and introduced into the mechanically actuated dispenser of British Patent No. 2,070,695A.

Parts 15 Sorbitol (70%) 23,000

Saccharin sodium salt 0.170 i-carrageenan (Genuvisco 0819) 0.500

Xanthane (Keltrol) 0.500 methyl p-hydroxybenzoate 0.080 20 Allantoin 0.150

0.100 sodium fluoride

Sodium monofluorophosphate 0.760

Pyridyl-carbinol 0.100

Alpha-alumina trihydrate (Alcoa C-333) 51,000 25 Benzoic acid 0.140

Sodium lauryl sulfate 1.667

Titanium dioxide 0.500

Aroma 1,200

Deionized water 20,133 30

The toothpaste effectively fills the dispenser and does not leak during storage at 43 CC for more than 1 month. It extrudes well from the dispenser after storage for 1 month at 43 ° C.

Similar satisfactory results are obtained when the toothpaste is modified so that it contains 0.55 part 19 of i-carrageenan and 0.55 part of xanthan in one case and 0.45 part of i-carrageenan and 0, 45 parts of xanthan in a second case, with corresponding adjustment of the water contents. Indeed, the absence of leakage and good aptitude for extrusion after storage at 43 ° C. for 3 months is observed with the toothpaste containing 0.45 part of xanthan and 0.45 part of i-carrageenan.

Satisfactory results are also observed when each of the three toothpastes described above is modified so that it contains 50,000 parts of alpha-alumina trihydrate in a first series of these toothpastes and 52,000 parts of alpha-alumina trihydrate in the second series of these toothpastes, with corresponding adjustment of the water contents.

Phosphoric acid can be used in place of benzoic acid and similar results can be obtained.

Example 4

The following toothpaste is prepared by a cold process and introduced into the same dispenser as in E-20 xample 3.

Party es

Sorbitol (70%) 23,000

Saccharin sodium salt 0.170 i-carrageenan (Genuvisco 0819) 0.750 25 Xanthane (Keltrol) 0.250 methyl p-bydroxybenzoate 0.080

Allantoin 0.150

0.100 sodium fluoride

Sodium monofluorophosphate 0.760 30 Pyridyl-carbinol 0.100

Alpha-alumina trihydrate (Alcoa C- 3 3 3) 51, 000

Benzoic acid 0.140

Sodium laurylsulfa 1,667

Titanium dioxide 0.500 35 Aroma 1.200

Eaudionized 20,133.

20

The toothpaste effectively fills the dispenser and does not leak and it extrudes well from the dispenser after storage for 3 months at 43 ° C.

The same advantageous results are obtained with 50,000 5 parts of alpha-alumina trihydrate. Each variant also provides similar results with a gel system containing (a) 0.825 part of i-carrageenan and 0.275 part of xanthan and (b) 0.675 part of i-carrageenan and 0.225 part * of xanthan.

Identical advantageous effects are obtained when the toothpastes of the examples are introduced into a dispenser actuated by pressure difference.

Claims (8)

21 1. Toothpaste in a dispenser actuated mechanically or by pressure difference, characterized in that it comprises approximately 20 to 80% by weight of an aqueous moistening vehicle, approximately 0.1 to 5% by weight of a mixture of gelling agents, approximately 20 to 75 I by weight of trihy-dratated alpha-alumina as polishing agent, sodium fluoride and sodium monofluorophosphate in proportions providing approximately 300 to 10,000 ppm of fluorine, about 0.05 to 0.5%, in. 10 weight of allantoTne as desensitizing agent and approximately 0.05 to 0.5% by weight of pyridyl-carbinol as vasodilator, the mixture of gelling agents being a mixture of a cellulose gelling agent or of xanthan with i-carrageenan in a weight ratio of the cellulosic gelling agent to the i-carrageenan of about 5: 1 to about 1: 5. 2. Toothpaste according to claim 1, characterized in that the weight ratio of the cellulose gelling agent or of xanthan to i-carrageenan is from approximately 3: 1 to approximately 1: 3 and the mixture of gelling agents is present approximately 0.2 to 3% by weight. 3. Toothpaste according to claim 2, characterized in that the cellulose gelling agent is present and is the sodium salt of carboxymethylcellulose. 4. Toothpaste according to claim 2, characterized in that xanthan is present. 5. Toothpaste according to claim 2, characterized in that the weight ratio of the cellulosic gelling agent or of xanthan to i-carrageenan is approximately 1: 1. 6. Toothpaste according to claim 1, characterized in that the sodium fluoride and the sodium monGfluorophosphate are present in proportions providing at least 750 to 2000 ppm of fluorine, and about 30 to 40% of the fluorine are provided by the fluoride. sodium. 7. Toothpaste according to claim 1, characterized in that the toothpaste is contained in a mechanically actuated dispenser. 1 22 8. Process for preparing a dispenser containing a toothpaste comprising approximately 20 to 80% by weight of an aqueous humectant vehicle, approximately 0.1 to 5% by weight of a mixture of gelling agents, approximately 20 to 75% by weight of al-5 phaalumine trihydrate as polishing agent, sodium fluoride and sodium monofluorophosphate in proportions providing about 300 to 1000 ppm of fluorine, about 0.05 to 0.5% by weight of allantoTne as agent desensitizer and 'about 0.05 to 0.5% by weight of pyridyl-carbinol as a vasodilator, said gelling mixture being a mixture of cellulosic gelling agent and i.-carrageenan in a weight ratio of i-carra-ghénane cellulosic gelling agent of approximately 5: 1 to approximately 1: 5, characterized in that a predetermined quantity of said toothpaste is extruded into a mechanically actuated distributor by means of a nozzle for filling a dispenser which is open at its base and which contains a central rod and, co smoother in place around said central rod, a piston having a diameter corresponding to the internal diameter of the distributor and a central opening intended to receive said central rod, then the distributor is closed in leaktight manner by means of a bottom disk. 4.