KR19990042912A - Process for preparing dispersible water soluble or water swellable polymer and toothpaste containing same - Google Patents

Abstract

The present invention provides compositions comprising at least partially aggregated granulated water soluble or water swellable polymers by treatment with one or more polyols present at a concentration of greater than about 10 weight percent based on the total weight of the composition. Granulation water soluble or water swellable polymers at least partially aggregated by treatment with polyols hydrate faster than untreated water soluble or water swellable polymers without forming a polymer mass in a solvent containing water. The present invention further provides an improved process for preparing a dentifrice composition comprising at least one anhydrous, water soluble or water swellable polymer, wherein the improved process is at least partially aggregated granulated water soluble or water swellable by treatment with a polyol. Replacing polymers with anhydrous, water soluble or water swellable polymers.

Description

Process for preparing dispersible water soluble or water swellable polymer and toothpaste containing same

The present invention relates to compositions comprising water soluble or water swellable polymers agglomerated by treatment with polyols, and to the use of such compositions in the manufacture of toothpastes.

Toothpaste formulations generally contain a dentally acceptable abrasive, moisturizer, water, and water soluble polymer that acts as a thickener and binder for the components. Various other ingredients, such as fragrances, sweeteners, preservatives and fluorides, may also be used in low concentrations. Glycerol and sorbitol (generally as aqueous solutions) are the most commonly used moisturizers for toothpastes, depending on the characteristics required for the product and polyethylene glycol or propylene glycol may be incorporated. The two types of toothpastes are broadly 1) cream or opaque gels; And 2) as a transparent or translucent gel.

The most commonly used thickeners or binders for toothpastes are carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), silica and magnesium aluminum silicate. Carrageenan, xanthan and polyacrylates may be used but are less extensive.

In the manufacturing process of toothpaste, incorporation of the anhydrous water soluble binder polymer into the composition often presents difficulties because of the tendency to agglomerate when the anhydrous polymer is added and dispersed into the aqueous system. This increases the time required to uniformly hydrate or disperse the binder polymer. As a result, there is a need in the industry for methods of incorporating water-free binder polymers that lead to lump-free products, rapid viscosity improvement and reduced batch production time and allow for normal handling of the binder.

Japanese Patent Application No. 7306167 B is (1) (a) coated with glycerol or alcohol, or (b) coated with starch paste, shellac, gelatin and agar followed by (a) treatment, or (c) ( carboxymethyl cellulose, alginic acid, polyacrylic acid or salts thereof coated with a mixture of the substrate in a) and the substrate in (b); (2) alkali salts of alkali carbonates, bicarbonates, phosphates, polyphosphates or EDTA, optionally treated with the methods of (a), (b) and (c); And optionally (3) a composition comprising glucose, sugar, fructose, maltose, mannitol and common salts. When water is added to the composition, it is rapidly wetted and dispersed, and it is possible to obtain alginic acid, polyacrylic acid or carboxymethyl cellulose solution quickly.

Japanese Patent Application No. 72044335 B teaches to improve its water solubility by coating the water soluble polymer with molten polyhydric alcohol, sugar or emulsifying aid. Water soluble polymers include methyl cellulose, CMC, polyvinyl alcohol, alginic acid salts, polyacrylic acid or salts thereof, and polyacrylamides. Polyhydric alcohols include sorbitol, mannitol and inositol, and sugars include glucose, sucrose and lactose. The coating substrate is used in an amount of 0.5 to 10% by weight, preferably 3 to 5% by weight relative to the polymer.

U.S. Patent No. 3,850,838 to Guckenberger et al. Describes a process for preparing alcohol-insoluble hydrocolloid ions in the form of aggregates that can be readily dispersed and dissolved, and carbohydrate binders that are soluble in both water and aqueous alcohol solvents for alcohols and carbohydrates. A process is disclosed that includes intimately combining hydrocolloids, granulating the resulting mixture, and then drying the aggregated granules.

None of the above patents teach the use of polyol-aggregated water soluble or water swellable polymers in toothpaste compositions.

It is therefore an object of the present invention to provide a polymer composition which can be rapidly dispersed in a solvent without forming a polymer mass by treating with a polyol and a process for preparing the same.

The present invention is directed to compositions comprising at least partially aggregated granulated water soluble or water swellable polymers by treatment with one or more polyols present at a concentration of greater than about 10% by weight based on the total weight of the composition. The composition can be dispersed substantially rapidly in a solvent compared to the corresponding untreated water soluble or water swellable polymer without forming agglomerates of the polymer.

In another aspect, the present invention relates to an improved process for preparing a dentifrice composition comprising at least one anhydrous, water soluble or water swellable polymer, wherein the improvement is at least partially aggregated granular water soluble or water by treatment with a polyol. Swellable polymers, replacing anhydrous water soluble or water swellable polymers. The granulated water soluble or water swellable polymers aggregated by treatment with a polyol hydrate substantially faster than the corresponding untreated water soluble or water swellable polymers without forming a polymer mass in water or a solvent containing water.

The compositions of the present invention comprise at least partially aggregated granulated water soluble or water swellable polymers by treatment with one or more polyols present at a concentration of greater than about 10% by weight based on the total weight of the composition. Coagulation herein is defined as the increase in particle size of the granulation material by the aggregation of individual particles.

Any water soluble or water swellable natural or synthetic polymer can be used to prepare the compositions of the present invention. Preferred water soluble or water swellable polymers are polysaccharides. Useful polysaccharides include cellulose ethers, guar, guar derivatives, locust bean rubber, silium, gum arabic, gatti rubber, karaya rubber, tragacanth rubber, carrageenan, agar, algin, xanthan, scleroglucan, dextran , Pectin, starch, chitin and chitosan, but are not limited thereto.

Preferred polysaccharides are cellulose ethers, carrageenan, guar, guar derivatives and pectin.

Cellulose ethers for use in the present invention include hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), water soluble ethyl hydroxyethyl cellulose (EHEC), carboxymethyl cellulose (CMC), carboxymethyl hydroxyethyl cellulose ( CMHEC), hydroxypropylhydroxyethyl cellulose (HPHEC), methyl cellulose (MC), methylhydroxypropyl cellulose (MHPC), methylhydroxyethyl cellulose (MHEC), carboxymethylmethyl cellulose (CMMC), hydrophobically modified Carboxymethyl cellulose (HMCMC), hydrophobically modified hydroxyethyl cellulose (HMHEC), hydrophobically modified hydroxypropyl cellulose (HMHPC), hydrophobically modified ethylhydroxyethyl cellulose (HMEHEC), hydrophobically modified carboxymethyl Hydroxyethyl cellulose (HMCMHEC), hydrophobically modified hydroxypropyl hydroxyethyl cellulose (HMHPHEC), hydrophobic Hydroly modified methyl cellulose (HMMC), hydrophobically modified methylhydroxypropyl cellulose (HMMHPC), hydrophobically modified methylhydroxyethyl cellulose (HMMHEC), hydrophobically modified carboxymethylmethyl cellulose (HMCMMC), cationic hydride Hydroxyethyl cellulose (cationic HEC) and hydrophobically modified cationic hydroxyethyl cellulose (cationic HMHEC). Preferred cellulose ethers are carboxymethyl cellulose and hydroxyethyl cellulose.

Guar derivatives for use in the present invention include carboxymethyl guar (CM guar), hydroxyethyl guar (HE guar), hydroxypropyl guar (HP guar), carboxymethylhydroxypropyl guar (CMHP guar), cationic guar Hydrophobically modified guar (HM guar), hydrophobically modified carboxymethyl guar (HMCM guar), hydrophobically modified hydroxyethyl guar (HMHE guar), hydrophobically modified hydroxypropyl guar (HMHP guar), hydrophobic Cationic hydroxypropyl guar (cationic HMHP guar), hydrophobically modified carboxymethylhydroxypropyl guar (HMCMHP guar) and hydrophobically modified cationic guar (HM cationic guar).

More preferred polysaccharides for use in preparing the compositions of the present invention are carboxymethyl cellulose, carrageenan and pectin or mixtures thereof. Most preferred is carboxymethyl cellulose.

Polyols used to aggregate the water soluble or water swellable polymers include, but are not limited to, sugars, sugar alcohols, glycerol, polyethylene glycols, propylene glycols, and mixtures thereof.

Examples of sugars are sucrose, glucose, lactose, fructose and xylose or mixtures thereof. Examples of sugar alcohols are sorbitol, inositol, mannitol, galactidol, arabitol, ribitol, xylitol and mixtures thereof.

Preferred polyols for use in the present invention are sorbitol and polyethylene glycol, or mixtures thereof. The molecular weight of polyethylene glycol for use in the present invention is not limited. Preferably, the polyethylene glycol has a molecular weight of about 200 to about 5,000,000, preferably about 600 to about 25,000, most preferably about 1,000 to about 10,000.

In the compositions of the present invention, the polyols used for aggregation are present at concentrations greater than about 10% by weight based on the total weight of the composition. The maximum concentration of the polyol is preferably about 90% by weight, more preferably about 50% by weight and most preferably about 30% by weight.

Aggregated compositions can be prepared by spraying the polyol in liquid form onto the granulation polymer. The polyols may be molten or in solution, with aqueous solutions being preferred. In a preferred method, the molten polyol or polyol solution is sprayed onto the water-soluble or water-swellable particles in a fluidized bed and the particles are dried at the same time if the polyol is a solution. Commercially available fluidized bed spray units can be used for the operation.

The agglomerated compositions of the present invention hydrate or dissolve substantially rapidly compared to the corresponding untreated water soluble or water swellable polymers without forming a polymer mass in water or a solvent containing water. This rate of hydration or dissolution is measured using a Haake Visco Tester 501, which is the torque (force) required to maintain rotation of the sensor in solution at a set rate (400 rpm) when the polymer is hydrated and thickened. Measure the amount of. Hydration time is considered the time (in minutes) it takes to achieve a final viscosity of 95%, where final viscosity is the average of the last 20 minutes of viscosity over a two hour test.

In this operation, hydration in water was measured at 55 ° C. For example, under the above conditions, the untreated carboxymethyl cellulose massed immediately and then required about 15 minutes to reach 95% viscosity. While the carboxymethyl cellulose agglomerated by treatment with 20% by weight of sorbitol or 20% by weight of polyethylene glycol immediately massed to some extent, but quickly dispersed and dissolved within 1 minute.

A further advantage of the composition is that the agglomeration phenomenon acts to reduce the amount of dust that occurs when handling untreated polymers.

The toothpaste of the present invention contains an adhesive, a humectant, and a water soluble polymer. Moisturizers are used to retain moisture in toothpastes, particularly at the nozzle end of the tube where the toothpaste can persist in contact with air. Water soluble polymers act as thickeners and binders for the components. Various other ingredients may also be used at low concentrations, such as perfumes, sweeteners, preservatives, detergents, tartar suppressors, plaque inhibitors and fluorides.

Dental abrasives for use in the toothpaste of the present invention typically include silica and insoluble inorganic salts. Preferred inorganic salts include calcium carbonate, dibasic calcium phosphate, tribasic calcium phosphate, calcium sulfate, insoluble sodium metaphosphate, hydrated aluminum oxide, and magnesium carbonate and phosphate. Silica and silica xerogels are particularly useful for translucent or transparent toothpastes.

Typical moisturizers for use in the toothpaste of the present invention are glycerol, sorbitol, propylene glycol or mixtures thereof, which are mixed with suitable moisturizer excipients such as water.

In the toothpaste of the invention, the aggregated water soluble or water swellable polymer may contain a polyol at a concentration of about 0.5 to about 90 weight percent based on the total weight of the aggregated water soluble or water swellable polymer. Preferred concentrations are about 2 to about 50 weight percent, more preferably about 10 to about 30 weight percent.

In the preparation of the toothpaste of the invention, in order to obtain a complete toothpaste formulation, agglomerated water-soluble or water-swellable polymers are treated with a polyol to a) a moisturizer or mixture of moisturizers, b) a moisturizer excipient, most typically water; c) salts, fragrances, colorants, surfactants, and d) abrasives. In a preferred manufacturing method, the aggregated water soluble polymer is added directly to the mixture of the humectant and humectant excipients and stirred until the polymer particles are completely dissolved and swelled. Any salts are then added, followed by the abrasive. The abrasive is added after the salt is completely dissolved. The mixture is stirred until the particles of abrasive are wet, then the fragrance is added followed by the surfactant.

The invention is illustrated by the following examples, which are for illustrative purposes only and are not intended to be limiting. All percentages, parts, etc. are by weight unless otherwise indicated.

Examples 1-14 show the preparation and testing of aggregated carboxymethyl cellulose and carrageenan by treatment with polyethylene glycol or sorbitol. As carrageenan GENU ^R carrageenan (Hercules Incorporated, Wilmington, Delaware) was used. As carboxymethyl cellulose, CMC 7MF or CMC 7MXF (Hercules Incorporated, Wilmington, Delaware) was used.

The polymer was immersed in an aqueous solution of polyethylene glycol, PEG 4600 and 1450 (Union Carbide, Carbowax ^R 4600 and 1450) in a Glat Fluid Bed Processor (model GPCG-5) top spray unit. 33 and 50%) to give a final polyol concentration of about 20% by weight. In addition, by adding a 70% aqueous solution of sorbitol, they were treated with sorbitol at concentrations of 10% and 20%.

In operation, all polyol aqueous solutions were heated to 50 ° C. and measured with a calibrated pump and balance. In all experiments, the glat fluid bed treating apparatus was preheated. The Schlick 945 nozzle was used for a 30 minute / 3 second filter shake cycle and reduced to 2 minutes / 3 second after the particle size increased. Spray air pressure was set to 2 bar. All products were dried to about 6-8% humidity and cooled to 30-34 ° C. The batch size was 3 kg.

Aggregated samples and untreated controls were evaluated using a Hark VT 501 viscometer with FL 10 detector at 55 ° C. for their dispersibility and hydration / dissolution characteristics in deionized water. The instrument measures the amount of torque (force) required to maintain rotation of the sensor in solution at a set speed (400 rpm) when the polymer is hydrated and thickened. This data is mathematically converted into viscous (cps) using a computer.

The hydration time reported in Table 1 is the time (in minutes) required to reach 95% viscosity with 100% viscosity during the last 20 minutes of two hours of operation. The viscosity of each sample was performed at 2% concentration based on the total solution weight. No correction was made to the amount of polyol or moisture in the sample.

Examples 1-8 and Comparative Example A

This example illustrates the aggregation of carrageenan treated with sorbitol and polyethylene glycol. The data is shown in Table 1. Comparative Example A is provided to show the hydration time of untreated carrageenan.

Agglomeration of Carrageenan Treated with Sorbitol and Polyethylene Glycol Example number Polyol Flocculation process Polyol Concentration (% by weight) Spray rate (g / min) Product temperature (℃) Time to reach 95% viscosity (minutes) One Sorbitol (70% aqueous solution) 20 34 50 3 2 Sorbitol (70% aqueous solution) 10 33 48 2 3 PEG 4600 (50% aqueous solution) 20 35-84 42-44 9 4 ¹ PEG 4600 (33% aqueous solution) 20 165 38 <1 5 PEG 4600 (50% aqueous solution) 20 9-20 38-42 11 6 Sorbitol (70% aqueous solution) 10 12 56-62 30 7 Sorbitol (70% aqueous solution) 20 8 60 22 8 Sorbitol (70% aqueous solution) 20 9 40-42 23 A ² - - - - 22 Carrageenan was preaggregated by spraying a 3 kg batch with 1200 g of water at 170 g / min before spraying with PEG in the examples. Untreated carrageenan

Examples 9-14 and Comparative Examples B and C

This example illustrates the aggregation of carboxymethyl cellulose treated with sorbitol and polyethylene glycol. The data is shown in Table 2. Comparative Examples B and C were provided to show the hydration time for untreated carboxymethyl cellulose.

The hydration time of carboxymethyl cellulose is substantially reduced by coagulation with sorbitol or polyethylene at a concentration of at least 10%.

Aggregation of Carboxymethyl Cellulose with Sorbitol or Polyethylene Glycol Example number Polyol Flocculation process Polyol Concentration (% by weight) Spray rate (g / min) Product temperature (℃) Time to reach 95% viscosity (minutes) 9 ¹ Sorbitol (70% aqueous solution) 20 44 52 <1 10 ¹ Sorbitol (70% aqueous solution) 20 8 41 6 11 ¹ PEG 1450 (50% aqueous solution) 20 150 38 <1 12 ^1,3 PEG 1450 (50% aqueous solution) 20 90-100 38 <1 13 ^2,4 PEG 1450 (50% aqueous solution) 20 165 38 <1 14 ¹ Sorbitol (70% aqueous solution) 10 9 42 15 B ¹ - - - - 15 C ² - - - - 10 Carboxymethyl cellulose is CMC 7MF (Hercules Incorporated). Carboxymethyl cellulose is CMC 7MXF (Hercules Incorporated). Carboxymethyl cellulose was preaggregated by spraying a 3 kg batch with 800 g of water at 120 g / min before spraying with PEG in the examples. Carboxymethyl cellulose was preaggregated by spraying 3 kg batches with 1500 g of water at 70 g / min before spraying with PEG in the examples.

Examples 15 and 16 and Comparative Examples D and E

This example illustrates the formulation of a toothpaste with carboxymethyl cellulose aggregated by treatment with sorbitol or polyethylene glycol. Comparative Examples show the formulation of a control composition in which untreated carboxymethyl cellulose was used.

Examples 15 and 16 illustrate the preparation of toothpaste at room temperature using aggregated carboxymethyl cellulose CMC 7MF by treatment with 9% sorbitol and 16% polyethylene glycol (PEG 1450), respectively. Comparative Examples D and E show similar formulations without CMC 7MF treatment. Ingredients and ingredient concentrations for each formulation are shown in Table 3.

Toothpaste Formulations (wt%) Ingredient Example 15 Example 16 Comparative Example D Comparative Example E CMC 7MF Aggregated by 9% Sorbitol 1.10 CMC 7MF Aggregated by 16% PEG 1450 1.10 CMC 7MF 1.10 1.10 Glycerol 13.00 Sorbitol (70% aqueous solution) 35.43 35.43 16.88 35.43 Distilled water 8.79 8.79 14.36 8.79 Dicalcium Dihydrate Phosphate 45.0 45.0 45.0 45.0 Tetrasodium pyrophosphate 0.42 0.42 0.42 0.42 Sodium saccharin 0.20 0.20 0.20 0.20 Sodium monofluorophosphate 0.76 0.76 0.76 0.76 Sodium benzoate 0.50 0.50 0.50 0.50 Distilled water 6.25 6.25 6.25 6.25 air freshener 0.55 0.55 0.55 0.55 Sodium Lauryl Sulfate 1.00 1.00 1.00 1.00

For formulations without glycerol (Examples 15, 16 and Comparative Example E), the following procedure was used:

1.Tetrasodium pyrophosphate (0.42 parts), sodium saccharin (0.20 parts), sodium monofluorophosphate (0.76 parts) and sodium benzoate (0.50 parts) are added to 6.25 parts of water under stirring and dissolved by heating at about 60 ° C. I was.

2. Carboxymethyl cellulose (1.10 parts) was added to a sorbitol solution (35.43 parts) in a beaker and stirred for 15 minutes or until properly dispersed. 8.79 parts of water was then added and the resulting mixture was stirred for 15-30 minutes to allow the polymer to fully hydrate (no gel). The warm salt solution from step 1 was then added under stirring and stirring continued for 15 minutes or until homogenized (no lumps or gels). The mixture was transferred to a Ross double planetary mixer.

3. Dihydrate dicalcium phosphate (DCP) (45.00 parts) was placed in a mixer and mixed continuously for 10 minutes to fully wet the DCP. Then the mixer was opened and the side of the stirrer and vessel was scraped off. The mixer was closed again, vacuumed and continuously mixed at high speed for 20 minutes or until mixing became soft.

4. Sodium lauryl sulfate (1.00 parts) was added, the vacuum was removed and mixing continued at low speed for 5 minutes. Then perfume (0.55 parts) was added and then mixed for 2 minutes at low speed. The mixer was opened and the sides of the stirrer and vessel were scraped off. The mixer was closed again, vacuumed and continuously mixed at medium speed for 15 minutes. The mixer was shut down, the vacuum removed and the toothpaste filled.

In Comparative Example D in which glycerol was used, the procedure was essentially the same as above except dispersing the carboxymethyl cellulose in glycerol under agitation in step 2. Stirring is continued for 5 minutes or until the carboxymethyl cellulose is properly dispersed. Sorbitol solution was then added and stirring continued for an additional 10 minutes. Water (14.36 parts) was added and stirring continued for 15-30 minutes to allow the polymer to fully hydrate (no gel). Warm salt solution was added and stirring continued for 15 minutes or until homogenized (no lumps or gels). The mixture was then transferred to a Ross mixer for the remaining steps.

In Examples 15 and 16, it was observed that the aggregated carboxymethyl cellulose was very easily dispersed in aqueous sorbitol solution. Hydration of the polymer started within about 3-4 minutes and progressed slowly until water and salt solution was added. Agglomeration of carboxymethyl cellulose was not observed at all.

In Comparative Example D, the untreated carboxymethyl cellulose was easily dispersed in anhydrous glycerol without forming a lump. In Comparative Example E, however, the untreated carboxymethyl cellulose was dispersed in the sorbitol solution only under very high speed agitation. Hydration of the polymer started within 1 to 2 minutes. Some lumps of carboxymethyl cellulose were observed in the sorbitol / salt solution.

Examples 17 and 18 and Comparative Examples F and G

This example illustrates the formulation of a toothpaste with carboxymethyl cellulose aggregated by treatment with sorbitol or polyethylene glycol at 55 ° C. The comparative example shows the formulation of the control composition when using untreated carboxymethyl cellulose.

Examples 17 and 18 illustrate the preparation of toothpastes at room temperature using carboxymethyl cellulose CMC 7MF aggregated by treatment with 9% sorbitol and 16% polyethylene glycol (PEG 1450). Comparative Examples F and G show similar formulations when CMC 7MF is not treated. Ingredients and ingredient concentrations for each formulation are shown in Table 4.

Toothpaste Formulations (wt%) Ingredient Example 17 Example 18 Comparative Example F Comparative Example G CMC 7MF Aggregated by 9% Sorbitol 1.00 CMC 7MF Aggregated by 16% PEG 1450 1.00 CMC 7MF 1.00 1.00 Glycerol 13.00 Sorbitol (70% aqueous solution) 35.43 35.43 16.86 35.43 Distilled water 8.89 8.89 14.46 8.89 Dicalcium Dihydrate Phosphate 45.00 45.00 45.00 45.00 Tetrasodium pyrophosphate 0.42 0.42 0.42 0.42 Sodium saccharin 0.20 0.20 0.20 0.20 Sodium monofluorophosphate 0.76 0.76 0.76 0.76 Sodium benzoate 0.50 0.50 0.50 0.50 Distilled water 6.25 6.25 6.25 6.25 air freshener 0.55 0.55 0.55 0.55 Sodium Lauryl Sulfate 1.00 1.00 1.00 1.00

For formulations without glycerol (Examples 17, 18 and Comparative Example G), the following procedure was used:

1.Tetrasodium pyrophosphate (0.42 parts), sodium saccharin (0.20 parts), sodium monofluorophosphate (0.76 parts) and sodium benzoate (0.50 parts) are added to 6.25 parts of water under stirring and dissolved by heating at about 60 ° C. I was.

2. The sorbitol solution (35.43 parts) was heated to 55 ° C. and carboxymethyl cellulose (1.00 parts) was added under stirring and stirring was continued for 15 minutes or until properly dispersed. Water heated to 55 ° C. (8.89 parts) was added and stirring continued for 15-30 minutes to allow the polymer to fully hydrate (no gel). The warm salt solution from step 1 was then added under stirring and continued for 15 minutes or until homogenized (no lumps or gels). The mixture was transferred to a Ross double planetary mixer.

3. Dihydrate dicalcium phosphate (DCP) (45.00 parts) was added to the mixer and mixing was continued for 10 minutes to fully wet the DCP. Then the mixer was opened and the side of the stirrer and vessel was scraped off. The mixer was closed again, vacuumed and continuously mixed at high speed for 20 minutes or until mixing became soft.

4. Sodium lauryl sulfate (1.00 parts) was added, the vacuum was removed and mixing continued at low speed for 5 minutes. Then perfume (0.55 parts) was added and then mixed for 2 minutes at low speed. The mixer was opened and the sides of the stirrer and vessel were scraped off. The mixer was closed again, vacuumed and continuously mixed at medium speed for 15 minutes. The mixer was shut down, the vacuum removed and the toothpaste filled.

The procedure of Comparative Example F differed from the above only in step 2. Carboxymethyl cellulose was dispersed under stirring at 55 ° C. and stirring was continued for 5 minutes or until properly dispersed. Sorbitol solution was then added and stirring continued for an additional 10 minutes. Water at 55 ° C. was added and stirring continued for 15-30 minutes to allow the polymer to fully hydrate (no gel), then add warm salt solution from step 1 and homogenize (lump or gel) for 15 minutes Stirring was continued). The mixture was then transferred to a Ross mixer for the remaining steps.

In Examples 17 and 18 and Comparative Example F, it was observed that the carboxymethyl cellulose material was easily and uniformly dispersed in hot sorbitol without forming agglomerates. Hydration of the polymer started after about 1 to 2 minutes and proceeded rapidly after addition of the water and salt solution. The resulting gel phase was very soft and the resulting paste was a soft cream. In contrast, in Comparative Example G, it was not possible for the untreated carboxymethyl cellulose to disperse gently. Even under high speed agitation, the polymer could not be prevented from severely clumping.

Example 19

This example illustrates the preparation of a toothpaste containing aggregated carrageenan by treatment with 20% sorbitol.

Ingredients:

Glycerol 22 parts

Carrageenan (0.96 parts of 20% sorbitol)

Agglomerated by treatment)

0.50 parts sodium benzoate

Sodium Saccharin 0.2Part

0.25 parts tetrasodium pyrophosphate

Sodium monofluorophosphate 0.76 parts

21.28 parts of deionized water

Dicalcium phosphate 51.75 parts

Sodium Lauryl Sulfate1.50

Peppermint oil 0.80

step:

Anhydrous blends of sodium saccharin, sodium benzoate, aggregated carrageenan, sodium monofluorophosphate, tetrasodium pyrophosphate were mixed with glycerol and stirred for 5 minutes. Then water was added and the resulting mixture was heated at 66-71 ° C. for 15 minutes. The weight was readjusted to the original weight by adding distilled water. The mixture was transferred to a Hobart mixer, dicalcium phosphate was added and the resulting mixture was stirred at mixer speed 1 for 2 minutes. The mixer was stopped, the vessel and the blades were scraped off, and mixed again at speed 2 for 10 minutes.

The paste was transferred to a vacuum degassing paddle, sodium lauryl sulfate and fragrance oil were added under mixing, and the mixture was degassed at 0.98 bar for 5 minutes. The resulting toothpaste was then filled into tubes for storage.

During the preparation, the aggregated carrageenan dispersed rapidly without forming a lump.

The provided examples should not be construed as limiting the invention, which is intended to illustrate some of the specific embodiments of the invention. The present invention may be variously changed and modified without departing from the scope of the appended claims.

According to the present invention, a polymer composition which can be rapidly dispersed in a solvent without forming a polymer mass by treating with a polyol, a process for preparing the same, and a toothpaste prepared thereby are provided.

Claims (37)

A composition comprising a granulated water soluble or water swellable polymer at least partially aggregated by treatment with one or more polyols present at a concentration of greater than about 10 weight percent based on the total weight of the composition. The method of claim 1, A composition that can be dispersed in a solvent substantially faster than an untreated water soluble or water swellable polymer without forming a polymer mass. The method of claim 1, Said treatment comprising spraying one or more polyols in liquid form on the particles of the water-soluble or water-swellable polymer in the fluidized bed, and at the same time drying the particles. The method of claim 1, A composition wherein the water soluble or water swellable polymer is one or more polysaccharides. The method of claim 4, wherein Polysaccharides include cellulose ethers, guar, guar derivatives, locust bean rubber, silium, gum arabic, gati rubber, karaya rubber, tragacanth rubber, carrageenan, agar, algin, xanthan, scleroglucan, dextran, pectin And at least one member selected from the group consisting of starch, chitin and chitosan. The method of claim 4, wherein Polysaccharides include hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), water soluble ethyl hydroxyethyl cellulose (EHEC), carboxymethyl cellulose (CMC), carboxymethyl hydroxyethyl cellulose (CMHEC), hydroxypropyl hydroxy Ethyl cellulose (HPHEC), methyl cellulose (MC), methylhydroxypropyl cellulose (MHPC), methylhydroxyethyl cellulose (MHEC), carboxymethylmethyl cellulose (CMMC), hydrophobically modified carboxymethyl cellulose (HMCMC), hydrophobic Hydrolysed hydroxyethyl cellulose (HMHEC), hydrophobically modified hydroxypropyl cellulose (HMHPC), hydrophobically modified ethylhydroxyethyl cellulose (HMEHEC), hydrophobically modified carboxymethylhydroxyethyl cellulose (HMCMHEC), Hydrophobically modified hydroxypropylhydroxyethyl cellulose (HMHPHEC), hydrophobically modified methyl cellulose (HMMC), small Hydrophobically modified methylhydroxypropyl cellulose (HMMHPC), hydrophobically modified methylhydroxyethyl cellulose (HMMHEC), hydrophobically modified carboxymethylmethyl cellulose (HMCMMC), cationic hydroxyethyl cellulose (cationic HEC) and At least one cellulose ether selected from the group consisting of hydrophobically modified cationic hydroxyethyl cellulose (cationic HMHEC). The method of claim 4, wherein Polysaccharides are carboxymethyl guar (CM guar), hydroxyethyl guar (HE guar), hydroxypropyl guar (HP guar), carboxymethylhydroxypropyl guar (CMHP guar), cationic guar, hydrophobically modified guar (HM) Guar), hydrophobically modified carboxymethyl guar (HMCM guar), hydrophobically modified hydroxyethyl guar (HMHE guar), hydrophobically modified hydroxypropyl guar (HMHP guar), hydrophobically modified cationic hydroxypropyl At least one guar derivative selected from the group consisting of guar (cationic HMHP guar), hydrophobically modified carboxymethylhydroxypropyl guar (HMCMHP guar) and hydrophobically modified cationic guar (HM cationic guar). The method of claim 4, wherein Wherein the polysaccharide is carboxymethyl cellulose. The method of claim 4, wherein The polysaccharide is carrageenan. The method of claim 4, wherein Wherein the polysaccharide is a mixture of carboxymethyl cellulose and carrageenan. The method of claim 1, The polyol is selected from the group consisting of sugars, sugar alcohols, glycerol, polyethylene glycols, propylene glycols and mixtures thereof. The method of claim 1, Polyols from the group consisting of sorbitol, inositol, mannitol, galactidol, arabitol, ribitol, xylitol, sucrose, glucose, lactose, fructose, xylose, glycerol, polyethylene glycol, propylene glycol and mixtures thereof Selected composition. The method according to any one of claims 1 and 8 to 10, The polyol is selected from the group consisting of sorbitol, polyethylene glycol and mixtures thereof. The method of claim 1, Wherein the maximum concentration of the polyol is about 90% by weight based on the total weight of the composition. The method of claim 14, The maximum concentration of the polyol is about 50% by weight based on the total weight of the composition. The method of claim 15, The maximum concentration of the polyol is about 30% by weight based on the total weight of the composition. The method of claim 1, The water soluble or water swellable polymer is at least one member selected from the group consisting of carrageenan, carboxymethyl cellulose and mixtures thereof, and the polyol is at least one member selected from the group consisting of sorbitol, polyethylene glycol and mixtures thereof, wherein the maximum of the polyol Wherein the concentration is about 50% by weight based on the total weight of the composition. In the process of preparing a dentifrice composition comprising the use of at least one anhydrous, water soluble or water swellable polymer, instead of the anhydrous, water soluble or water swellable polymer, at least partially aggregated granulated water soluble or water swellable polymer is used by treatment with a polyol. This improved process. The method of claim 18, Wherein the aggregated water soluble or water swellable polymer hydrates substantially faster than untreated water soluble or water swellable polymer without forming a polymer mass in water or a solvent containing water. The method of claim 18, Wherein the water soluble or water swellable polymer is a polysaccharide. The method of claim 20, Polysaccharides include cellulose ethers, guar, guar derivatives, locust bean rubber, silium, gum arabic, gati rubber, karaya rubber, tragacanth rubber, carrageenan, agar, algin, xanthan, scleroglucan, dextran, pectin , At least one member selected from the group consisting of starch, chitin and chitosan. The method of claim 20, Polysaccharides include hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), water soluble ethyl hydroxyethyl cellulose (EHEC), carboxymethyl cellulose (CMC), carboxymethyl hydroxyethyl cellulose (CMHEC), hydroxypropyl hydroxy Ethyl cellulose (HPHEC), methyl cellulose (MC), methylhydroxypropyl cellulose (MHPC), methylhydroxyethyl cellulose (MHEC), carboxymethylmethyl cellulose (CMMC), hydrophobically modified carboxymethyl cellulose (HMCMC), hydrophobic Hydrolysed hydroxyethyl cellulose (HMHEC), hydrophobically modified hydroxypropyl cellulose (HMHPC), hydrophobically modified ethylhydroxyethyl cellulose (HMEHEC), hydrophobically modified carboxymethylhydroxyethyl cellulose (HMCMHEC), Hydrophobically modified hydroxypropylhydroxyethyl cellulose (HMHPHEC), hydrophobically modified methyl cellulose (HMMC), small Hydrophobically modified methylhydroxypropyl cellulose (HMMHPC), hydrophobically modified methylhydroxyethyl cellulose (HMMHEC), hydrophobically modified carboxymethylmethyl cellulose (HMCMMC), cationic hydroxyethyl cellulose (cationic HEC) and At least one cellulose ether selected from the group consisting of hydrophobically modified cationic hydroxyethyl cellulose (cationic HMHEC). The method of claim 20, Polysaccharides are carboxymethyl guar (CM guar), hydroxyethyl guar (HE guar), hydroxypropyl guar (HP guar), carboxymethylhydroxypropyl guar (CMHP guar), cationic guar, hydrophobically modified guar (HM) Guar), hydrophobically modified carboxymethyl guar (HMCM guar), hydrophobically modified hydroxyethyl guar (HMHE guar), hydrophobically modified hydroxypropyl guar (HMHP guar), hydrophobically modified cationic hydroxypropyl At least one guar derivative selected from the group consisting of guar (cationic HMHP guar), hydrophobically modified carboxymethylhydroxypropyl guar (HMCMHP guar) and hydrophobically modified cationic guar (HM cationic guar). The method of claim 20, The polysaccharide is selected from the group consisting of carboxymethyl cellulose, carrageenan, pectin and mixtures thereof. The method of claim 20, Wherein the polysaccharide is carboxymethyl cellulose. The method of claim 20, Process in which polysaccharide is carrageenan. The method of claim 20, Wherein the polysaccharide is a mixture of carboxymethyl cellulose and carrageenan. The method of claim 18, The polyol is selected from the group consisting of sugars, sugar alcohols, glycerol, polyethylene glycols, propylene glycols and mixtures thereof. The method of claim 18, Polyols from the group consisting of sorbitol, inositol, mannitol, galactidol, arabitol, ribitol, xylitol, sucrose, glucose, lactose, fructose, xylose, glycerol, polyethylene glycol, propylene glycol and mixtures thereof Selected process. The method according to any one of claims 18 and 25 to 27, The polyol is selected from the group consisting of sorbitol, polyethylene glycol and mixtures thereof. The method of claim 18, A process for producing at least partially aggregated granulated water soluble or water swellable polymer by spraying one or more polyols in liquid form onto the particles of the water soluble or water swellable polymer in a fluidized bed and simultaneously drying the particles. The method of claim 31, wherein The polyol is in the form of an aqueous solution. The method of claim 18, Wherein the polyol in the aggregated water soluble or water swellable polymer is present at a concentration of about 0.5 to about 90 weight percent based on the total weight of the aggregated water soluble or water swellable polymer. The method of claim 33, wherein Wherein the polyol in the aggregated water soluble or water swellable polymer is present at a concentration of about 2 to about 50 weight percent based on the total weight of the aggregated water soluble or water swellable polymer. The method of claim 34, wherein Wherein the polyol in the aggregated water soluble or water swellable polymer is present at a concentration of about 10 to about 30 weight percent based on the total weight of the aggregated water soluble or water swellable polymer. A toothpaste prepared by the process of claim 18 or 31. Toothpaste prepared by the process of claim 30.