CZ399298A3 - Method of simultaneous joint forcing-out physically separated tooth cleansing preparations in constant proportion - Google Patents

Abstract

A method of coextruding at least two dental components a cleaning agent in controlled proportions, these being folders are stored and physically separated in a multi-space a container body (10) provided with a partition (18) which is disposed divides the inner volume of the container into two separate spaces, wherein said partition (18) is movable in response to pressure the difference that affects it when applying compressive force to the side walls (12), and the individual components of the dental cleanser The compositions contain additives which react together upon mixing. The container side walls (12) are made of a resilient plastic a mass which is compressed under the action of a deflection force of 4.45 N or greater and the dentifrice ingredients formulated to be equally displaceable at basically equal compressive forces. Pressing the side walls (12) the unshaped multilayer stream is displaced multilayer components containing reactive components in advance determined ratios, to achieve optimal levels for the interaction between the reactive ingredients upon extrusion components and their mixing in the oral cavity.

Description

Method of co-extruding physically separated, dentifrices in a constant ratio at the same time

Technical field

The invention relates to a method for co-extruding reactive ingredients in controlled equal proportions, or a packaging system, for storing and simultaneously releasing physically separate components of a multi-component dentifrice at predetermined proportions of components in a multilayer unmixed ratio.

BACKGROUND OF THE INVENTION

Multi-component dentifrice compositions are known in the art, wherein the individual components containing the reactive substances are physically separated during storage and released simultaneously as a viscous paste or as a fluid which interacts when mixed, e.g. whereupon the components are then released in a predetermined proportion of the individual ingredients for optimum efficiency and performance.

For example, it has long been known to add fluoride ion-releasing compounds to dentifrices as caries agents, and have been found to be effective in reducing caries. The efficacy of released fluoride ions is dependent on the amount of fluoride ions available for placement in the dental tissue being treated. Accordingly, it is desirable to formulate compositions of dentifrices in which maximum availability of fluoride ions in the resulting brush brushing solutions in which a dentifrice is used is ensured.

One effective way of storing fluoride ions on teeth is to use a two-component dentifrice composition comprising a calcium component and a second component containing a fluoride ion to thereby precipitate calcium fluoride on the teeth.

For example, U.S. Patent No. 5,045,305 discloses a two-component dentifrice for fluoridating teeth, wherein one component contains calcium chloride CaCl2 and the other component contains fluoride ions in the form of sodium fluoride NaF, and wherein the separate components are mixed immediately prior to introduction into the mouth so as to cause precipitation of calcium fluoride CaF2V US patent no. 5,145,668 describes a process for the fluoridation of teeth, in which during toothbrushing mixing the first component containing a soluble calcium salt such as _CaCl2 and a second component which it contains a hydrolysable complex fluorine compound, such as sodium fluorosilicate (Na 2 SiF 6), where the mixing of the components results in the hydrolysis of the complex fluoride compound and precipitation of the calcium fluoride and its deposition on the tooth surface.

U.S. Patent No. 5,476,647 describes a two-component fluoride storage system, the first component of which comprises a soluble calcium source and a soluble complexing calcium anion, such as diamine tetraacetic acid, wherein calcium is partially bound to the Ca-complexing agent. The second component comprises a fluoride salt, such as sodium fluoride or stannous fluoride. After these components are combined with the precipitation of calcium fluoride (CaF ₂ ), the free Ca is removed from solution and a further portion of free Ca is released from the calcium complexing agent, again causing further CaF ₂ precipitation _<

Co-pending U.S. patent application filed 1996, discloses a dentifrice for tooth fluoridation using an isolated two physically separated semisolid components of a dentifrice composition comprising a fluoride salt and an abrasive component containing calcium ion, which upon mixing upon application to the teeth react, the first component being an aqueous semisolid dentifrice composition containing a salt that releases a fluoride ion, for example an alkali metal salt such as sodium fluoride, in a vehicle whose components do not react with the fluoride salt, and the second component is a vehicle containing an abrasive that contains calcium ions, such as hydrated dibasic calcium phosphate, wherein the individual components of the dentifrice are substantially rheologically equivalent and are simultaneously displaced from stock with two departments. If the ingredients in the released ingredients are in the correct proportions of reactants, the maximum availability of fluoride as precipitated calcium fluoride is achieved after mixing the dentifrice components during application to the teeth, for example brushing.

The most convenient and inexpensive way of releasing physically separated components of the multi-component dentifrice is by releasing it from a compressible plastic tube in which the individual compartments are arranged. Two-compartment compressible tubes for co-extruding two physically separate dental cleanser components are known in the art, and by squeezing the tube, for example by squeezing, one strip of a multilayer product in the form of a strip is released. The body of such a two-compartment tube is usually welded at one end, and is made of a plastic film. The two-compartment tube structure further includes a septum in the tube body which forms separate spaces therein, and a relatively hard portion of the neck formed at the non-closed end of the tube having a through opening orifice whose outer circumferential surface is threaded or otherwise designed to it could be screwed on, or otherwise fixed, a cap to close the tube. As an example of such two-compartment tubing designs for releasing a multi-component dental cleaning composition, see U.S. Patents

Nos. 4,481,757 and 4,687,663.

U.S. Pat. No. 4,487,757 discloses a two compartment compressible tube divided into two compartments by a septum that extends toward the mouth to release the formulation and which physically isolates the two-component toothpaste when released from the tube, the toothpaste contains reactive ingredients where one component contains an alkali metal bicarbonate (eg sodium bicarbonate NaHCO3) and the other contains an acid or an acid salt (eg citric acid) which reacts with the bicarbonate salt to produce a sparkling effect (carbon dioxide) upon release of unmixed layers of both components and after their intimate mixing when brushing teeth.

U.S. Pat. No. 4,687,663 discloses a two compartment tube that releases a two-component dentifrice consisting of a gel containing hydrogen peroxide and a component containing sodium bicarbonate. This tube is divided into two compartments by a partition extending up to the release mouth.

Disadvantages of the prior art two-compartment systems are disclosed in the above-described patents, which consist in the desire to use such systems with semi-solid displaceable oral dentifrices such as toothpastes and toothpastes. gels containing reactive ingredients that require constant predetermined ratios of ingredients to maximize efficacy result in unequal release of the dentifrice components from the plastic tubing with compartments, so that the optimal interaction of the reactants when mixing the two components while brushing the teeth is not achieved. For example, U.S. Pat. No. 5,137,178 states (paragraphs 1, lines 29-39) that a common problem with known methods for releasing two-component reactive products is the inability to control the relative flow rate of each of its components from its respective compartment from the two Particular problems are the extrusion of equal volumes of both components. U.S. Patent No. 5,020,694 (para. 1, line 64, through paragraph 3, line 3) discloses that prior art two-compartment tubes represented by the aforementioned U.S. Patent Nos. 4 487,757 and 4,687,663 have the disadvantage that they tend to release a two-component dentifrice in uncontrolled variable ratios, although the rheology of the components is similar.

The unequal release of the components of the multi-component dentifrice causes changes in the layers of the individual components of the released multilayered dose of dentifrice, so that although the components that are subsequently released are released simultaneously, the ingredients in the released components do not agree with the correct ratio of reactants for optimal interaction. In the case of multi-component dentifrices of the type described in S.N. used for fluoridation of teeth, the maximum availability of fluoride in the form of precipitated calcium fluoride after the unequally dispensed components have been mixed during tooth cleaning is not achieved

U.S. Pat. Nos. 5,020,694 and 5,038,963 disclose rigid, multi-compartment piston cartridges for co-extruding two or more components of a dentifrice in predetermined amounts. These rigid containers have the advantage of controlling the coextrusion process. However, a considerable amount of plastics is used in their construction. For reasons of environmental protection and high costs, packaging with less plastic is desirable. Therefore, there is a need in the art to provide a non-rigid plastic container or tube with compartments for storing and simultaneously releasing physically separate components of a dentifrice containing reactive ingredients in a fixed, predetermined ratio of ingredients to provide optimal interaction of reactive ingredients, at the same time, such a package would require a considerably smaller proportion of plastic for its manufacture.

7 Summary of the Invention

The present invention relates to a composition for the constant co-release of a dentifrice in predetermined proportions of physically separated components, the composition comprising various reactive ingredients, from a non-rigid container with collapsible side walls, the container comprising:

(1) a compressible part of a body made of plastic that is deformed by a compressive force of about 4.45 N or more applied thereto; and (2) a movable partition in the container body which forms separate spaces, the partition is a diaphragm having a smaller thickness than the side walls of the body and deformed by a compression force of less than 2.23 N, moving in response to the pressure differential exerted thereon when the side walls of the container are squeezed, and deflecting the diaphragm substantially abolishes the pressure difference and equalizes the compressive forces exerted on the dentifrice components stored in the compartments of the cartridge, thereby achieving a substantially constant co-release of the components in predetermined proportions when the components are formulated such that the compressive forces required to displace the individual dentifrice components are essentially equivalent.

Dental cleaning ingredients

By substantially equivalent compressive force as used herein, the individual components of the multi-component dentifrice of the present invention are formulated such that the force required to induce flow and expulsion of the individually deposited dentifrice components from the mouth of the container, did not differ by more than 20% from the strength of any other individually deposited component, so that a properly balanced interaction between the different reactive components of the components is achieved when the components are later mixed.

It has been found that the individual components of the dentifrice, when containing different reactants, have different surface tensions relative to the plastic walls of the collapsible non-rigid container in which they are disposed when extruded from the container compartments and thereby simultaneously coextruding the individual The components used in the preparation of the individual components of the dentifrice must be adjusted to the various surface tensions that occur when the components of the dentifrice are displaced so that the compressive forces required for the controlled extrusion were essentially equivalent.

Further, it has been found that a substantially constant coextrusion of dental cleaning ingredients containing various reactive ingredients is achievable by the coextrusion system of the present invention when the individual dental cleaning ingredients are formulated to be displaceable by a compressive force ranging from about 2.3 to about 89 N, preferably from about 4.45 to about 44.5 N.

The term compressive force measured in Newtons (Ν) as used in the specification and the appended claims means the force required to force 1-2 grams of the dentifrice component stored in a stainless steel container up to 5 millimeters through an orifice with a diameter

3.8 millimeters at 23 ° C at 150 millimeters / minute. To measure this compressive force, the dentifrice component is placed in a stainless steel container with an internal diameter of 2.0 centimeters. The bottom of the stainless steel tank is equipped with a 20 mm nozzle and an inner diameter of 0.38 centimeters. A non-friction teflon piston having an outer diameter equal to the inner diameter of the stainless steel container is placed on top of the dentifrice. To measure the force required to move the Teflon piston down by 5 millimeters at a speed

150 mm / min, an Instron® pressure gauge is used. The compressive force required for extrusion is determined from the inflection point on the force versus distance curve, when the force applied to the piston induces a linearly increasing flow of the dentifrice component until the inclination indicating the start of displacement of the dentifrice component is changed. In order to achieve the same release of separately deposited components of the dentifrice, it is critical for the practice of the present invention that the compressive forces measured at the inflection point of each component lie within ± 20% of each other.

The compressive force required to induce the extrusion of the dentifrice ingredients of the present invention can be adjusted by selecting and concentrating the vehicle ingredients of the dentifrice in which the reactive substances are incorporated.

The dentifrice vehicle used in the practice of the present invention is adapted to impart to the dentifrice component the paste-like consistency, density, and tack that are typical of conventional toothpastes or gels. The vehicle is non-reactive to the dentifrice reactive ingredients and includes water, a suitable humectant such as glycerin, sorbitol, propylene glycol, polyethylene glycol, or any suitable mixture thereof, and a thickening agent.

The humectant typically comprises about 10 to 70% by weight of the dentifrice component, preferably about 20 to about 50% by weight. The water may be present in the vehicle at a concentration of from about 6% to about 70% by weight of the component, and is preferably about 15 to 40% by weight.

Thickeners included in the dentifrice component include natural and synthetic gums and colloids, such as iota carrageenan, kappa carrageenan, lambda carrageenan and mixtures thereof, xanthan gum, carboxymethylcellulose, sodium carboxymethylcellulose, starch. , polyvinylpyrrolidone, hydroxyethylpropylcellulose, hydroxybutylmethylcellulose, hydroxypropylmethylcellulose, hydroxyethylcellulose, laponites and magnesium aluminum silicates. Preferred thickeners are those which impart an elastic structure to the dentifrice component, thereby preventing gradual different thickening of the dentifrice component during storage. When such thickeners are used in the preparation of the dentifrice component used in the practice of the present invention, the compressive force required to extrude the dentifrice component does not change substantially during storage. Examples of thickeners that impart an elastic structure include carrageenans of various types, laponites,

- 11 magnesium aluminum silicates, commercially available under the name Veegum, and polyoxyethylene and polyoxypropylene block copolymers available under the name Pluronic.

The thickener which imparts the desired elastic structure to the dentifrice components most preferred in the practice of the present invention is a cellulose gel formed from spray-dried cellulose and cellulose gum, or spray-dried, or bulk drying, a co-treated mixture of microcrystalline cellulose and cellulose gum. , such as carboxymethylcellulose, xanthan gum, or sodium alginate. Examples of such cellulose gels are those sold by FMC Corporation under the trade name Avicel, which generally contain about 80% to about 90% by weight of microcrystalline cellulose and about 10 to about 20% by weight of cellulose gum. The gel particle size range ranges from submicroscopic particle size, i.e. from less than 0.2 µm to about 100 µm, and preferably from about 0.2 to about 20 µm. A particularly preferred gel for practicing the present invention is Avicel RC-591-F, which is a spray-dried cellulose gel having the following composition and properties:

% microcrystalline cellulose% colloidal (0.2 µm)% carboxymethylcellulose Initial viscosity * «»

Viscosity after solidification

- 175 at 1,2% (0,039 - 0,175 Pa.s) 1250 cps at 1,2% (1,250 Pa.s) * Initial viscosity: determined after 120 seconds with a Brookfield RVT viscosimeter with spindle # 1 at 20 rpm, * · * Viscosity after solidification: determined after 24 hours using a Brookfield RVT viscometer with spindle # 1 at 20 rpm.

Thickeners, such as Avicel RC-591-F, can be added to the dentifrice ingredients at concentrations of from about 0.05 to about 2% by weight, and preferably from about 0.1 to about 1.5% by weight.

In the preparation of the dentifrice ingredients of the present invention, surfactants are used to aid in the perfect dispersion of the dentifrice ingredients throughout the oral cavity when applied to the mouth as well as to improve the cosmetic acceptance and wetting and foaming properties of the constituents. The surfactant is included in the vehicle of the individual dentifrice components of the present invention at a concentration of from about 0.5 to about 3.0% by weight, and preferably from about 1.0 to about 2.0% by weight.

Surfactants useful in the practice of the present invention include salts of higher alkyl sulfates, such as sodium lauryl sulfate, or other suitable alkyl sulfates containing from about 8 to about 18 carbon atoms in the alkyl group; sodium lauryl sulfoacetate, salts of sulfonated higher fatty acid monoglycerides, such as sodium coconut monoglyceride sulfonate, or other suitable sulfonated fatty acid monoglycerides containing 10 to 18 carbon atoms; salts of higher fatty acid amides, for example C 12 -C 16 acids, with lower aliphatic amino acids such as sodium N-methyl-N-palmitoyltauride, sodium N-lauroyl sarcosinate, sodium N-myristoyl sarcosinate and sodium N-palmitoyl sarcosinate; salts of esters of these fatty acids with isotonic acid or with glycerol monosulfate, such as monosulfated monoglyceride sodium of hydrogenated coconut oil; olefin sulfonate salts such as alkene sulfonates or alkene sulfonates or mixtures thereof with 12 to 16 carbon atoms in the carbon chain of the molecule; and higher fatty acid soaps having 12 to 18 carbon atoms, for example, coconut fatty acids. The salt cation may be sodium, potassium or a monoethanolamine, diethanolamine or triethanolamine cation.

The present invention is applied so that the components of the dentifrice must usually be physically separated from each other, since each individually contains ingredients that interact with each other. For example, peroxide compounds are very reactive ingredients and must be separated from most ingredients of the dentifrice such as fragrance and pastry ingredients, vitamins (A, C, Ε), antibacterial agents such as triclosan, and polyphosphates such as sodium tripolyphosphate. Cationic compounds such as stannous ion, chlorhexidine di-gluconate and cetylpyridinium chloride must also be separated from the anionic components of the dentifrice such as anti-tartar (sodium tripolyphosphate), calcium and silica abrasives and the like.

In a particular case where tooth fluoridation by calcium fluoride precipitation is desired, the first component of the two-component dentifrice composition comprises a water-soluble salt releasing fluoride such as an alkali metal fluoride such as sodium fluoride NaF, potassium fluoride KF, sodium monofluorophosphate or stannous fluoride SnF 2 - The preferred fluoride for the purposes of this invention is sodium fluoride NaF. The fluoride is added to the first component of the dentifrice composition of the invention at a concentration of from about 0.1 to about 1% by weight, and preferably from about 0.25 to about 0.5% by weight. At these preferred concentrations, about 750 ppm to about 1500 ppm of fluoride ion will be present on the tooth surface after the first and second components of the dentifrice composition are combined after application of the composition to the teeth.

Other specific examples of reactive ingredients that may be added to the first dentifrice component include peroxidic compounds such as hydrogen peroxide, calcium peroxide, or organic acidic ingredients such as citric acid or salts thereof which may be included in the first a dentifrice component in a concentration of from about 0.5 to about 5% by weight of the dentifrice composition.

The second component of the composition of the dentifrice composition of the present invention comprises reactive polishing or abrasive additives such as dicalcium phosphate or an alkali metal bicarbonate. If the second component of the dentifrice composition contains as the abrasive hydrated sodium hydrogen phosphate or calcium orthophosphate dihydrate, the abrasive is added to the second component of the dentifrice composition at a concentration of from about 1 to about 60% by weight and preferably from about 20 to about 50% by weight of the second component, when the abrasive is an alkali bicarbonate salt such as sodium bicarbonate, the bicarbonate salt is added to the second component at a concentration of from about 5 to about 25% by weight.

Other specific examples of the two components of the dentifrice composition that can be used in the practice of the present invention include dentifrice ingredients that interact normally and are not compatible with one another, such as a calcium-containing abrasive and polycarboxylated polymers (e.g. Gantrez), or potassium nitrate.

The reactive abrasive is contained in a vehicle formulated in such a way as to obtain a vehicle-like composition of the first component of the dentifrice so that both components will have similar physical characteristics, allowing it to be easily formulated for coextrusion at substantially the same compressive forces. For example, to do so. the compression force was substantially the same to displace both components at a precisely predetermined ratio, and to achieve optimal precipitation of calcium fluoride, the vehicle composition of the second component, especially the humectant content, was adjusted to accommodate the difference in component additive characteristics. Thus, for example, in the case of a two-component dentifrice in which one component contains fluoride and the other a calcium abrasive, the humectant content of the other component is adjusted to accommodate the addition of the abrasive middle calcium phosphate. The abrasive is included in the second component of the dentifrice at a concentration of from about 10% to about 30% by weight, and preferably at a concentration of from about 15% to about 25% by weight. At these abrasive levels, the humectant concentration ranges from about 15% to about 70% by weight, and preferably from about 20% to about 40% by weight.

Similar adjustment of the sodium bicarbonate concentration in the second component of the multi-component dentifrice used according to the present invention can be carried out so that the compressive forces required to extrude both components are substantially equivalent to release components at a predetermined ratio to achieve optimal reaction and foaming between the bicarbonate additive in the second component and the organic acid or peroxide additive contained in the first component.

The striped dentifrice is obtained in the practice of the present invention by incorporating into each of the dentifrice ingredients used in the present invention contrasting dyes which are pharmacologically and physiologically non-toxic when used in the recommended amounts. Colorants used in the practice of the present invention include both pigments and dyes.

Pigments used in the practice of the present invention include non-toxic, water-insoluble inorganic pigments such as titanium dioxide and green chromium oxides, ultramarine blue and roses and ferric oxides, as well as water-insoluble paints prepared by coating with calcium or alumina FD&C dye salts such as FD&C Green # 1, FD&C Blue # 2, FD&C R&D # 30 and FD&C Yellow # 15. These pigments have a particle size in the range of 5 to 1000 gm, preferably in the range of 250 to 500 gm, and are present in a concentration of from 0.5% to 3% by weight.

The dyes used in the practice of the present invention are uniformly dispersed throughout the dentifrice component, including the dyes generally used as additives to food products approved under the Food Drug & Cosmetic Act for use in foods and ingested medicines, including colorants such as for example, FD&C Red # 3 (tetrajodofluorescein sodium), FD&C Yellow # 5 (4-p-sulfophenylazo-5-hydroxypyrazole-3-carboxylic acid sodium), FD&C Yellow # 6 (p-sulf sodium phenylazo). -naphthol-6-monosulfonate), FD & 3- (4 - {[4- (N-ethyl-p-sulfobenzylamino) -phenyl] (4-hydroxy-2-sulfoniumphenyl) methylene} disodium salt - [1- (N-ethyl-N-psulfobenzyl) - AE-3,5-cyclohexadienimine], FD&C blue # 1 (dibenzyldiethyldiaminotrifenylcarbinoltrisulfonic anhydride sodium salt), FD&C blue # 2 (indigotine disulfonic acid sodium) and mixtures thereof in different proportions. of the present invention ranges from about 0.0005% to about 2% by weight of the dentifrice composition.

It is preferred that the colorant contained in one of the dentifrice components is a pigment such as titanium dioxide TiC > 2, and that the colourant is dispersed throughout the mass of the other dentifrice component and has a colourant. a color other than the pigment contained in the first component of the dentifrice.

Any flavoring or sweetening agent (sweetener) may also be used, for example, curly mint oil, peppermint oil, oil of wintergreen, safflower oil, clove oil, sage oil, eucalyptus oil, marjoram oil, cinnamon oil, lemon oil, orange oil and methyl salicylate. Suitable sweeteners include sucrose, lactose, maltose, sorbitol, sodium cyclamate, perillartin and saccharin sodium. Flavoring agents and sweeteners may be present together in an amount of from 0.01% to 5% or more of the composition,

Various other ingredients may be added to the dentifrice ingredients of the present invention. Examples include, but are not limited to, preservatives, silicones and chlorophyll compounds, antibacterial agents such as chlorohexidene, halogenated diphenyl ethers such as triclosan, desensitizing agents such as potassium nitrate and potassium citrate, and mixtures thereof . These ingredients are added to the dentifrice ingredients in amounts that do not substantially adversely affect the desired properties and characteristics, which ingredients are selected and used in appropriate amounts depending upon the type of dentifrice ingredients contemplated.

To prepare the individual components of the dentifrice, humectants such as glycerin, polyethylene glycol and a sweetener are dispersed in a conventional mixer until the mixture forms a homogeneous gel phase. To this gel phase is added a fluoride salt or dibasic calcium phosphate as an abrasive. These ingredients are mixed until a homogeneous phase is formed. The thickener, flavorant and surfactant are then added as ingredients, and the ingredients are blended at high speed under a vacuum of about 20 to 50 psi. The resulting product is a homogeneous, semi-solid, extrudable pasty product.

Release tray

The mass from which the side walls of the multi-chamber container body used in the practice of the present invention are made is a flexible, durable plastic material that flexes when a force is applied to the central membrane. In the practical application of the present invention, it has been found that a plastics material that flexes when applying a force of up to about 4.4 is particularly suitable for co-releasing the dentifrice components in fixed, predetermined proportions from squeezable tubular compartments. up to about 13.2 N.

The aforementioned deformation force as used in this specification and the following claims means the maximum force, expressed in Newton, required to deform the bar bent into an inverted U-shape by a form adapter mounted on a compression member of the apparatus, for example Instron® Tensile. Strenght Testing Machine, where this force is applied axially downward to the arc section of the U-shaped bulkhead at a speed of 305 millimeters / minute.

n

This adapter, installed on the Instron, is

140 millimeters high and consists of a stainless steel block of 6.35 millimeters in thickness and an area of 6.45 cm @ 2 with a stainless steel wire of 3.2 millimeters in diameter, which is curved downward into an open rectangular section of 127 millimeters wide and 63.5 in height millimeter. The adapter is mounted on the π jaw of the Instron and moves downward to contact and deform the test membrane surface.

The plastic barrier to be tested is held in a sample holder consisting of a stainless steel base with a thickness of 3.2 millimeters with a slot of 25.4 millimeters wide, 102 millimeters long and 51 millimeters high. The base projection of this base, 25.4 millimeters long, attaches it to the worktop of the Instron®. The sample support is mounted in the base to hold the plastic membrane in the base, comprising a channel of 102 millimeters long, 24.8 millimeters wide and 51 millimeters high, and a wall thickness of 15.9 millimeters. The specimen support holds the diaphragm in the inverted U-shaped base.

Six plastic film samples cut in the machine direction and six plastic film samples cut across the machine direction, each measuring 101.6 x 101.6 millimeters, are measured to measure the deformation force. Each test sample is placed in the sample holder and held in place by an abutment so that it has the shape of an inverted U. No sample is reused. The specimen holder with the specimen is placed in an Instron and the adapter is lowered just above the specimen and then reduced at a rate of 305 millimeters per minute to cause the specimen to deflect by 8.9 millimeters. The force in Newtons required to deflect (deform) the film in this manner is recorded as the deformation force.

The plastic film from which the sidewalls of the body are made can be made of any suitable plastic, such as polyethylene (low and high density), polypropylene, ethylene-propylene copolymers, and polyethylene terephthalate. The plastics film mass may have a laminated structure in which a gas barrier material such as ethylene vinyl alcohol, nylon, or polyvinylidene chloride is sandwiched between layers of polyethylene, polypropylene, or copolymers thereof. The gas barrier material prevents the loss of some of the ingredients in the dentifrice components that pass into the gas phase and penetrate the plastic mass of the non-gas leakage barrier structures.

The multi-compartment container of the present invention has a collapsible outer sidewall and a movable partition dividing the container into a plurality of compartments, the outer side walls of the compartment being compressed thereby expelling the dentifrice components from each compartment when applying compressive force to the outer walls. wherein the movable partition compensates for the deformation of the outer walls of the tube, so that the compressive forces acting on the individual components of the dentifrice to displace them from the cartridge are compensated.

Description of attached pictures

The invention is illustrated in more detail with the aid of the accompanying drawings in which like and like parts are denoted by the same reference numerals in all different views.

Figure 1 is a front elevational view of one embodiment of a multi-chamber container, a collapsible tube used in the application of the present invention; Figure 2 shows a vertical cross-section of the multi-chamber tube according to line 2-2 of Figure 1; 2, and FIG. 4 is a cross-sectional view of the tube shown in FIG. 3 in a depressed state.

Figure 1 shows a multi-chamber tube suitable for storing and physically separating dental cleaning ingredients containing reactive ingredients. This tube, illustrated in Figures 2 to 4, is formed by an elongated body 10, which in the illustrated embodiment has a circular cross-section but may have a different shape, for example oval. The tube has a body 10 which is of an easily compressible, compressible or deformable type and is formed by a side wall 12 formed of a durable plastic material which can deflect by a deformation force of about 4.4 N to about 13.5 N, as mentioned above. . One end 20 of the body 10 is sealed while the other end 22 is open and has a neck 22a. by which the components of the multi-component dentifrice are forced through the openings 23 and 23a. The neck 22a is provided with fixation means for fastening the closing cap (not shown).

The thickness of the side wall 12 typically ranges from about 0.25 to about 1.20 millimeters. In a preferred embodiment of the invention, the side wall thickness is from about 0.25 to about 0.35 millimeters.

In the embodiment shown, the interior of the body 10 is longitudinally divided into two compartments 14 and 15 (or spaces) by means of a partitioning membrane or partition 18. The partition 18 is soft and laterally movable. Depending on the design of the body 10, this partition 18 can be integrally formed together with the body 10 as a unitary part of the body 10. In an alternative embodiment

23, the partition 18 may be formed as a separate part, suitably attached to the container body. In particular, when the body 10 and the partition 18 are made of a thermoplastic material such as polyethylene, thermal bonding or adhesive bonding methods may be used to connect the two halves of the body 10 together with the partition 18 attached to the outer edges of the side wall 12. The peripheral edges of the baffle 18 are permanently attached to the inner surface of the side wall 12 by suitable thermal or adhesive bonding.

In Figure 2, the baffle 18 is longitudinally shown in a wavy or pleated configuration so that lateral movement of the baffle 18 is induced when the outer walls of the tube are compressed or deformed.

In Figure 3, the baffle 18 is shown in its original rest position before the side walls of the container 12 are compressed, and in Figure 4, the baffle 18 is laterally deflected to the broken line when the collapsible side walls 12 of the container are compressed to release the components together. a dentifrice from compartments (or spaces) 14 and 16.

The partition 18 is formed of a very flexible and soft film of thermoplastic material, such as low density polyethylene or polypropylene, or may be laminated, wherein the gas barrier is disposed between opposing layers of polyethylene or polypropylene. The partition 18 has a thickness substantially less than the thickness of the plastic from which the sidewalls 12 are made, and generally has a thickness in the range of 0.005 to 0.20 millimeter and preferably in the range of about 0.075 to 0.15 millimeter.

<* t

The bottom 20 of the body 10 may have any suitable arrangement. This bottom of the body 10 is sealed by crimping or squeezing the walls of the body 10, which are joined by means of an adhesive or a heat seal to each other and to the inner partition 18.

The compartments 14 and 16 of the container body 10 are filled in a conventional manner with the dentifrice components before the end 20 of the body 10 is sealed, i.e. the container is provided with a closure cap (not shown), then inverted and filled with the lower end. The dentifrice components containing different reactive components will exhibit different flow characteristics when subjected to a compressive force on the sidewall 12, wherein the dentifrice components, while flowing on the inner surfaces of the sidewall, encounter different, i.e. means greater or lesser resistance to their flow, which is relatively different for each component. To compensate for these differences in flow that occur in response to the applied compressive force, the dentifrice components are formulated taking into account these differences so that the compressive force required to induce the flow of the components is substantially the same, with the necessary compressive force it is usually in the range of about 2.25 N to about 9 N, preferably in the range of about 4.45 N to about 44.5 N. When this compressive force of the above range is applied to the side wall of the container. 10, for example by compressing the side walls of the cartridge, the individual components of the dentifrice are forced to flow simultaneously. The baffle 18 is moved laterally from its fixed position in response to any pressure difference that occurs within the interior of the tube, thereby compensating for differences in compression force. If the difference in compression forces required to push the individual f Γ components out of the tube exceeds 20% and cannot be offset by adjusting the components of the dentifrice, the difference in compression forces required to push the components out of the tube may be adjusted by changing the hole geometry 23, 23a. through which the individual components are extruded.

After filling the multi-chamber container, the baffle 18, as shown in Figures 2 and 3, is substantially compressed so that it can deflect in both directions due to the pressure difference acting on it. In Figure 4, the baffle 18 is shown tilted longitudinally to the right in response to a compression deflection from the left side of the tube that is greater than a push deflection from the opposite side.

As the components are forced out of the orifice 22a through the openings 23 and 23a. the individual components combine into a single striped stream of matter. A single stream is advantageous and easily directed to a limited surface area so that, in the case of toothpaste, the toothpaste can be applied cleanly and easily to a narrow toothbrush in predetermined proportions to achieve optimal therapeutic delivery of reactive ingredients by mixing the layers of ingredients. brushing teeth or dental tissue in the oral cavity.

In use, the cartridge 10 may be squeezed intermittently to dispense small portions of the two-component dentifrice ingredients stored in sections 14 and 16. If such a cartridge is grasped by different users having individual grip, such squeezing may exert more pressure on one component than the other, if this occurs, then the pressure difference across the baffle 18 deflects the baffle 18 until the pressures are equalized. The baffle 18 is thus a displaceable pressure-sensitive wall that balances the component pressures, thereby achieving a relatively constant ratio of co-released components, since both components of the dentifrice are folded so as to be displaceable by the same compressive force and their proportions displaced by moving partition 18.

The diameter of the discharged individual stream can be regulated according to the packing data by adjusting the diameter of the holes 23 and 23a. The stream is typically in the form of a cylindrical strip having a diameter of about 0.3 to about 2 centimeters. If different coloring ingredients are added to the individual components of the dentifrice, then the multilayer stream of dentifrice components exits from the throat exit opening as an attractive striated toothpaste.

DETAILED DESCRIPTION OF THE INVENTION

The present invention will be explained in more detail by way of the following specific example, which, however, is illustrative only, and is not intended to limit the scope of the invention in any way. Unless otherwise indicated, all percentages are by weight and all temperatures are in ° C.

Example

A series of 40 millimeter tubes with two compartments with a body length of 158 millimeters was manufactured from a laminated film with a PE / EVOH / PE structure, where PE is polyethylene and EVOH is a copolymer of ethylene with vinyl alcohol having a thickness of 0, 3 millimeters. During testing, the deformation force n was required to compress the film

7.1 N as determined by the Instron instrument as described above.

This tube was divided lengthwise into two compartments of approximately equal volume by means of a pleated partition made of 0.12 millimeter polyethylene, which deformed at a applied compressive force of 0.34 N.

The two-compartment tube compartments were filled with dental cleanser components labeled 1 and 2 constituting a multi-component dental cleanser, labeled Dental Cleaner A, containing the ingredients listed in Table I.

The viscosities of the two dentifrice components measured in Brookfield units using a Brookfield RVT viscometer with a spindle E at 5 rpm were substantially the same, with the viscosity of component 2 being 17% lower than that of component 1.

Table I

Dental Cleaner Ingredient Component 1 wt. SiO ₂ content Component 2 wt. content phosphate Sorbitol (70%) 36.36 - Glycerol 10.00 22.0 Polyethylene glycol-600 3.00 - Carrageenan rubber 0.60 0.92 Avicel RC591-F 0.30 - Sodium diphosphate 0.50 0.25 tío ₂ 0.30 · Sodium saccharin 0.25 0.20 sodium fluoride NaF 0.51 - Calcium hydrogen phosphate - 48.76 Abrasive, silica 22.0 - Thickening agent, silica 2.50 - Dye 0.03 - Aromatizing oil 0.95 0.89 Sodium lauryl sulfate 1.20 1.20 Deionized water according to needs. according to needs. Viscosity (Brookfield units) 42 36

The compressive force, determined by the previously described procedure, to induce flow of component 1 and component 2 was substantially the same, with the compressive force required to displace component 1 of the dentifrice A by 2.4% lower than for component 2. The compressive forces required for the extrusion of components 1 and 2 of dentifrice A are shown in Table III.

For comparison, the procedure of the example was repeated except that the comparative multi-component dentifrice, designated component B, was used. The ingredients in components 1 and 2 of the comparative dentifrice B and their viscosities are shown in Table II.

The compressive forces required to extrude the individual components of the dentifrice B were not within ± 20%, in particular component 2 of the dentifrice B required a compressive force which was 45% lower than that of component 1. The compressive forces needed to extrude the dentifrice components of composition B are shown in Table III below.

The viscosity of component 2 of the comparative dentifrice B was substantially the same as component 1, with component 2 having a viscosity 12% lower than component 1.

Table II

Dental Cleaner Ingredient Component 1 wt. Component 2 wt. NaF - 0.486 Saccharin 0.20 0.20 Sorbit - 38,524 Glycerol 22,00 25,00 Polyethylene glycol 600 - 3.00 Calcium hydrogen phosphate 48.76 - Abrasive, silica - 18.00 Thickening agent, silica - 5.50 Aromatizing agent 0.89 0.89 Sodium lauryl sulfate 1.20 1.20 TiO ₂ - - Carboxymethylcellulose 1.00 - Water 25.75 - Sodium diphosphate 0.25 - Viscosity (Brookfield units) 65 58

Table III

Compressive force required for extrusion (N) Preparation A Preparation B Folder 1 11.3 24.5 Folder 2 11.5 44.5

In this example, it has been found that components 1 and 2 of dental cleanser A are released substantially equally from the multi-chamber tubes in which they are stored, while the components of dental cleanser B do not, although for both dental cleaners the viscosity of the individual basically the same.

Claims (27)

PATENT CLAIMS CLAIMS 1. A method for co-extruding reactive reagents in controlled equal proportions, characterized in that the reagents are contained in at least two components of a dentifrice disposed and physically separated in a multi-compartment container body having compressible side walls, an outlet and separating means. the internal volume of the body on a plurality of separate storage portions, wherein the outlet is provided with an outlet opening connected to the compartments, the partition being made of plastic material less than the side walls of the body, and movable to compensate for differences in extruded component flow rates after compressing the side walls, the process comprising filling the compartments with the individual components of the dentifrice, the components being formulated to be displaceable from the aperture when substantially the same ejection force, the compressive force being the force measured in Newtons to expel 1 to 2 grams of the dental cleaning component stored in a stainless steel container within 5 millimeters through a 3.8 millimeter diameter hole at 23 ° C at a speed of 150 millimeters / minute, the side walls of the body are made of a plastics material which deforms upon application of a deformation force of about 4.45 N or more, the deformation force being the maximum force, expressed in Newton, required to deform the partition bent into a mold an inverted U-shaped adapter mounted on a compression member, wherein this force is applied axially downward to the arc section of the U-shaped baffle at a speed of 305 millimeters / minute, and then squeezing the side walls of the body to eject a single stripe The active ingredients are in proportions predetermined to achieve an optimum level of reacted ingredients after the extruded components are mixed in the oral cavity. Method according to claim 1, characterized in that the compressive forces causing the extrusion of the components of the dentifrice do not deviate by more than ± 20% from each other. The method of claim 1, wherein the dentifrice components are formulated to be displaceable at a compressive force in the range of about 2.2 to about 89 N. The method of claim 1, wherein the dentifrice components are formulated to be displaceable at a compressive force in the range of about 4.45 to about 44.5 N. The method of claim 1, wherein the plastics material from which the side walls of the body are formed is deformed by a deformation force of from about 4.45 N to about 13.4 N. The method of claim 1, wherein the sidewalls have a thickness of from about 0.25 millimeter to about 1.2 millimeter. The method of claim 1, wherein the baffle is deflected by a deformation force of less than 2.25 N. The method of claim 1, wherein the partition has a wall thickness of from about 0.005 millimeter to about 0.20 millimeter. The method of claim 8, wherein the partition is folded and movable in response to a compressive force applied to the sidewalls. 10. The method of claim 1 wherein the dentifrice component comprises a thickener to impart an elastic structure to it. The method of claim 10, wherein the thickener is a cellulose gel. The method of claim 10, wherein the thickener is carrageenan rubber. The method of claim 1, wherein the reactive ingredients that are included in the dentifrice component are a calcium-containing abrasive and a fluoride-releasing salt. The method of claim 13, wherein the fluoride-releasing salt is sodium fluoride NaF. The method of claim 13, wherein the calcium abrasive is calcium phosphate. 16. The method of claim 1 wherein the reactive ingredients included in the dentifrice ingredients are an alkali metal bicarbonate polishing agent and an organic acid. 17. The process of claim 16 wherein the alkali metal bicarbonate is sodium bicarbonate. The method of claim 16, wherein the organic acid is citric acid. 19. The method of claim 1 wherein the reactive ingredients included in the dentifrice ingredients are an alkali metal bicarbonate and a peroxide compound. The method of claim 19, wherein the peroxide compound is hydrogen peroxide or calcium peroxide. 21. The method of claim 1, wherein the reactive ingredients contained in the dentifrice ingredients are an abrasive containing calcium and potassium nitrate. The method of claim 21, wherein the reactive ingredients contained in the dentifrice ingredients are a calcium-containing abrasive and a polycarboxylated polymer. 23. The method of claim 1 wherein the reactive ingredients included in the dentifrice ingredients are a peroxide compound and sodium tripolyphosphate. 24. The method of claim 1 wherein the reactive ingredients contained in the dentifrice ingredients are a peroxide compound and a flavoring agent. 25. The method of claim 1 wherein the reactive ingredients contained in the dentifrice ingredients are a peroxide compound and a vitamin. 26. The method of claim 1 wherein the reactive ingredients included in the dentifrice ingredients are a peroxide compound and an antibacterial agent. 27. The method of claim 1 wherein the reactive ingredients included in the dentifrice ingredients are a cationic compound and an anionic compound.