WO2003075874A1 - Composition de dentifrice contenant du carbonate de calcium resistant a l'acide et procede de fabrication associe - Google Patents

Composition de dentifrice contenant du carbonate de calcium resistant a l'acide et procede de fabrication associe Download PDF

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Publication number
WO2003075874A1
WO2003075874A1 PCT/IB2003/001322 IB0301322W WO03075874A1 WO 2003075874 A1 WO2003075874 A1 WO 2003075874A1 IB 0301322 W IB0301322 W IB 0301322W WO 03075874 A1 WO03075874 A1 WO 03075874A1
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WO
WIPO (PCT)
Prior art keywords
silicate
calcium carbonate
toothpaste composition
toothpaste
composition according
Prior art date
Application number
PCT/IB2003/001322
Other languages
English (en)
Inventor
Gustavo P. N. De Andrade
Anthony H. Asbridge
Original Assignee
Quimica Industrial Barra Do Pirai Ltda.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Quimica Industrial Barra Do Pirai Ltda. filed Critical Quimica Industrial Barra Do Pirai Ltda.
Priority to BR0308295-4A priority Critical patent/BR0308295A/pt
Priority to AU2003216598A priority patent/AU2003216598A1/en
Publication of WO2003075874A1 publication Critical patent/WO2003075874A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses

Definitions

  • TOOTHPASTE COMPOSITION INCLUDING ACID RESISTANT CALCIUM CARBONATE AND A METHOD OF MAKING THE SAME
  • the present invention relates to a toothpaste composition having an abrasive system including an acid-resistant calcium carbonate. More particularly, the present invention relates to a toothpaste composition that can provide cost savings through the use of an acid-resistant calcium carbonate abrasive. The present invention further relates to the production of the toothpaste composition according to the present invention.
  • fluoride became a standard active ingredient in toothpastes for the prevention of tooth decay.
  • Silica became the abrasive of choice in toothpaste formulations because silica proved to be compatible with most fluoride sources. While the beneficial impact of the use of fluoride-containing toothpaste on oral hygiene and dental health is well documented, such compositions are relatively expensive for many consumers, and therefore are not widely affordable in many developing countries.
  • Calcium carbonate is significantly cheaper than silica, and would be suitable for use as a lower cost dental abrasive, but for the fact that calcium carbonate is not compatible with most fluoride sources.
  • the present invention provides a lower cost alternative for neutral fluoride containing toothpaste.
  • the present invention replaces expensive silica abrasive with a calcium carbonate that is treated with silicate to render it stable in a neutral environment.
  • the silicate-treated calcium carbonate abrasive of the invention due to its increased acid-resistance, is more stable at the pH range commonly used in toothpaste compositions.
  • the increased acid resistance reduces the acid-induced decomposition of the calcium carbonate, which would otherwise liberate carbon dioxide to eventually cause tube swelling and/or rupture over time.
  • the present invention relates to a neutral toothpaste composition including a toothpaste base and an abrasive system comprising an acid-resistant calcium carbonate abrasive.
  • the acid resistance results from a treatment of the calcium carbonate with at least one silicate.
  • the present invention further relates to a method of making a toothpaste composition including combining a silicate with a calcium carbonate slurry, neutralizing the slurry, drying the calcium carbonate to obtain particles of calcium carbonate that are silicate-treated, and combining the silicate-treated particles with a toothpaste base.
  • Figure 1 illustrates a system for evaluating the acid resistance of silicate-treated calcium carbonate.
  • Figure 2 is a graphical representation of pH versus volume of acid used.
  • Figure 3 is a graphical representation of pH versus volume of acid used.
  • One aspect of the present invention is a toothpaste composition
  • a toothpaste composition comprising a toothpaste base and at least one silicate-treated calcium carbonate.
  • Another aspect of the present invention is a method of making a toothpaste, comprising combining at least one silicate with a calcium carbonate slurry; neutralizing the slurry; drying the calcium carbonate slurry to obtain silicate-treated particles of precipitated calcium carbonate; combining said silicate-treated particles of precipitated calcium carbonate with a toothpaste base.
  • neutral toothpaste composition means a toothpaste composition having a pH ranging from about 6.0 to about 8.0, for example from about 6.8 to about 7.2.
  • the present invention relates to a toothpaste composition which includes an abrasive system comprising an acid-resistant calcium carbonate such as, for example, an acid-resistant precipitated calcium carbonate (PCC).
  • an acid-resistant calcium carbonate such as, for example, an acid-resistant precipitated calcium carbonate (PCC).
  • PCC acid-resistant precipitated calcium carbonate
  • Other calcium carbonates such as ground calcium carbonate, can also be used according to the present invention.
  • the calcium carbonate may be rendered acid-resistant using any art recognized method.
  • the acid-resistant calcium carbonate is rendered acid-resistant by treating the particle with at least one silicate compound. According, to one embodiment, this treatment results in a coated, or "jacketed," particle.
  • Non-limiting examples of silicates suitable for treating the calcium carbonate include alkali metal silicates such as sodium, lithium, and potassium silicate; aluminosilicate; polysilicates (e.g., sodium, lithium, and potassium polysilicates); organic base silicates (e.g., water-soluble quaternary ammonium silicates); mixed organic base/alkali metal silicates (e.g., double silicates of quaternary ammonium with sodium, lithium, or potassium silicates); complex metal ion silicates; and peroxy silicates.
  • alkali metal silicates such as sodium, lithium, and potassium silicate
  • aluminosilicate such as sodium, lithium, and potassium silicate
  • polysilicates e.g., sodium, lithium, and potassium polysilicates
  • organic base silicates e.g., water-soluble quaternary ammonium silicates
  • mixed organic base/alkali metal silicates e.g., double
  • silicate-treated particles are prepared by introducing a silicate, such as sodium silicate, to a calcium carbonate suspension.
  • the calcium carbonate suspension can have a solids content ranging, for example, from about 1 to about 50 % solids, for example about 10 to about 40% solids, and further, for example, from about 15 to about 25 % solids.
  • the sodium silicate may be alkaline, semi-alkaline or neutral, and may be added in an amount ranging from, for example, about 1 to about 20 %, by weight, for example from about 1 to about 10 % by weight, and further, for example, from about 2 to about 6 % by weight.
  • the sodium silicate is considered to be alkaline when the ratio Si0 2 /Na 2 0 ranges from 2.0 to 2.5, and semi-alkaline when the ratio is greater than 3.0.
  • the suspension is neutralized by injection of carbon dioxide.
  • the carbon dioxide is introduced at a flow rate ranging from, for example, about 10 to about 100 m 3 /h, for example from about 40 to about 100 m 3 /h and further, for example, from about 60 to about 80 m 3 /h and at a preferred pressure, for example, from about 1 to about 5 kg/cm 3 , more preferably from about 1 to about 4 kg/cm 3 , and most preferably from about 1.5 to about 3.5 kg/cm 3 .
  • the suspension is neutralized for a period of time ranging from about 25 minutes to about 50 minutes.
  • the suspension is then subjected to a drying process that may be performed with, for example, any art recognized dryer.
  • Suitable dryers for use in accordance with the present invention include drum dryers.
  • the suspension is dried at a temperature ranging from, for example, about 100° to about 150°C, for example ranging from about 110° to about 140°C, and further, for example, at a temperature ranging from about 115° to about 125°C.
  • the drying time depends on the quantity of product to be dried and the product humidity to be achieved. Appropriate drying times would be readily apparent to the skilled artisan.
  • the suspension is dried to yield a silicate-treated precipitated calcium carbonate.
  • the acid resistance of the resulting silicate-treated precipitated calcium carbonate ranges from, for example, about 100 to about 1000 ml of 0.1 N H 2 S0 4 per 100 g of calcium carbonate, or from about 200 to about 400 ml of 0.1 N H 2 S0 4 per 100 g of calcium carbonate.
  • the acid resistance is at least about 100 ml of 0.1 N H 2 S0 4 per 100 g of calcium carbonate.
  • the acid resistance is at least about 200 ml of 0.1 N H 2 S0 4 per 100 g of calcium carbonate, for example at least about 400 ml of 0.1 N H 2 S0 4 per 100 g of calcium carbonate.
  • silicate-treated calcium carbonate such as silicate-treated ground calcium carbonate
  • Ground calcium carbonate is commonly prepared by the grinding of a chalk, marble, or limestone source material to the required degree of fineness. The grinding can be accomplished in dry or aqueous process conditions, and using varying types of proprietary or commercially available grinding equipment, as known to those of ordinary skill in the art. The ground calcium carbonate is then subjected to the silicate treatment process according to the present invention to yield an acid-resistant silicate-treated ground calcium carbonate.
  • the ground calcium carbonate is mixed with water to give a suspension with a solids content ranging from about 15 to about 25% solids, relative to the total weight of the suspension.
  • the silicate compound such as sodium silicate, may be added in an amount ranging from about 2 to about 6% by weight, relative to the total weight of the suspension.
  • the suspension is neutralized by injection of carbon dioxide or by any other suitable means of pH neutralization, including but not limited to the addition of at least one acid, for example at least one acid chosen from mineral acids and organic acids.
  • At least one additional abrasive may be used with the acid- resistant calcium carbonate in the abrasive system of the present invention.
  • the at least one additional abrasive material may be chosen from any fluoride compatible abrasive material. Suitable non-limiting examples of abrasive materials that may be used in accordance with the present invention may be chosen from, for example, silica, alumina, aluminosilicate, dicalcium phosphate, sodium bicarbonate, sodium metaphosphate, potassium metaphosphate, tricalcium phosphate, calcium pyrophosphate, calcium carbonate, and bentonite.
  • the abrasive system of the present invention including the silicate-treated calcium carbonate, may be present in the toothpaste base according to the present invention in an amount ranging from, for example, about 1 % to about 40 %, by weight, relative to the total weight of the composition, for example from about 5 % to about 40 % by weight. According to another aspect of the invention, the abrasive system of the present invention may be present in an amount ranging from about 4 % to about 25 % by weight, relative to the total weight of the composition.
  • the abrasive system is combined with a toothpaste base.
  • the toothpaste base includes at least one ingredient chosen from thickening agents, gelling agents, humectants, foaming agents (detergents), and polishing agents.
  • the toothpaste base may also contain at least one additional ingredient chosen from, for example, water, preservative agents, flavorants, sweeteners, and fluoride containing compounds. It will be readily apparent to the skilled artisan that the components and their relative amounts in the toothpaste base may be modified to achieve the desired toothpaste product.
  • the toothpaste base according to the present invention may contain at least one thickener, which may also be referred to as a gelling agent. Any art recognized gelling or thickening agent may be used. Thickening or gelling agents for use in the present invention may be selected from natural, synthetic and gum-like materials, including, but not limited to, carboxyl methyl cellulose, carrageenin, xantham gum, and bentonite. The at least one thickening or gelling agent may be present in the toothpaste base according to the present invention in an amount ranging from, for example, about 0.1 % to about 5 % by weight, for example from about 0.1 % to about 3 % by weight. According to another aspect of the invention, the at least one thickening or gelling agent is present in the toothpaste base in an amount ranging, for example, from about 0.5 % to about 1.5 % by weight.
  • the toothpaste base according to the present invention may also contain at least one ingredient chosen from detergents and surfactants.
  • suitable non-limiting examples of appropriate detergents for use in the toothpaste of the present invention include anionic surfactants, such as sodium alkylsulfates, sodium laurylsulfate, sodium myristylsulfate and sulfosuccinic acid surfactants; dialkyl sodium sulfosuccinate; non-anionic surfactants; and amphoteric surfactants.
  • the at least one ingredient chosen from detergents and surfactants may be present in the toothpaste base according to the present invention in an amount ranging from, for example, about 0.1 % to about 10 % by weight, for example from about 0.1 % to about 5 % by weight, and further, for example, from about 0.5 % to about 3 % by weight.
  • the toothpaste base according to the present invention may also contain at least one humectant.
  • humectants for use in the toothpaste of the present invention include those chosen from glycerin, sorbitol, propylene glycols, polyethylene glycols and mixtures thereof.
  • the at least one humectant may be present in the toothpaste base according to the present invention in an amount ranging from, for example, about 10 % to about 90 % by weight, for example from about 20 % to about 80 % by weight.
  • the at least one humectant may be present in an amount ranging from about 30 % to about 70 % by weight.
  • the toothpaste base according to the present invention may contain at least one coloring or whitening agent. Any art recognized coloring or whitening agent may be used. Coloring and whitening agents for use in the present invention may include, for example, titanium dioxide. Coloring or whitening agents may be present in the toothpaste base according to the present invention in an amount ranging from about 0.1 % to about 5 % by weight, for example ranging from about 0.1 % to about 3 % by weight, and further, for example, from about 0.1 % to about 1 % by weight.
  • the toothpaste base according to the present invention may contain at least one preservative. Any art recognized preservative may be used. Preservatives for use in the present invention may be selected from, for example, sodium benzoate and methyl paraben. Preservatives may be present in the toothpaste base according to the present invention in an amount ranging from, for example, about 0.1 % to about 3 %, by weight, for example ranging from about 0.1 % to about 1 % by weight, and further, for example from about 0.1 % to about 0.5 % by weight.
  • the toothpaste composition prepared in accordance with the method of the present invention may further contain at least one additional ingredient chosen from therapeutic ingredients, water-insoluble non-cationic antibacterial agents, for example, triclosan, and cationic antibacterial agents.
  • the toothpaste base according to the present invention may also contain at least one foaming agent. Any art recognized foaming agent may be used in the present invention. Appropriate foaming agents will be readily apparent to the skilled artisan.
  • the toothpaste base according to the present invention may contain at least one flavoring agent. Any art recognized flavoring agent may be used in the present invention. Appropriate flavoring agents will be readily apparent to the skilled artisan. Flavoring agents may be chosen, for example, from oils of spearmint, peppermint, wintergreen, sassafras, clove, sage, eucalyptus, cinnamon, lemon, orange and methyl salicylate.
  • the toothpaste base according to the present invention may contain at least one sweetener. Any art recognized sweetener may be used in the present invention. Appropriate sweeteners will be readily apparent to the skilled artisan. Sweeteners may be chosen, for example, from at least one of sucrose, lactose, maltose, xylitol, sodium cyclamate, perillartine, aspartyl phenyl alanine methyl ester and saccharine.
  • the toothpaste base according to the present invention may contain fluoride.
  • Fluoride for use in the present invention includes any compatible composition that will dissociate and release fluorine-containing ions in water.
  • Fluoride compositions for use in the present invention can be chosen from one or more of sodium fluoride, stannous fluoride, sodium monofluorophosphate, potassium fluoride, potassium stannous fluoride, sodium fluorostannate, stannous chlorofluoride and amine fluoride.
  • Fluorides may be present in the toothpaste base according to the present invention in an amount ranging from about, for example, 0.1 % to about 3 %, by weight, for example from about 0.1 % to about 1 % by weight, and further, for example, from about 0.2 % to about 0.8 % by weight.
  • Silicate-treated precipitated calcium carbonate was prepared by adding 2% semi-alkaline sodium silicate to a calcium carbonate suspension, having a 20 % solids content, obtained from the carbonation of a calcium hydroxide suspension. The suspension was again carbonated with carbon dioxide for 50 minutes at a flow rate of 72 m 3 /h and at a pressure of 2 kg/cm 3 . The neutralized product was then dried in a drum dryer at 130°C. Properties of the silicate-treated precipitated calcium carbonate are provided below under the designation "A.”
  • Apparent volume was determined by placing 40 g of a previously sieved sample into a graduated cylinder. The cylinder was placed in a wood support, closed, and dropped 50 times from a 1 inch height, with 2 seconds for each fall, over a period of 1 minute and 40 seconds. Apparent volume was determined from the final volume in the graduated cylinder. (Quimbarra STM 200/98)
  • Glycerin absorption was determined by placing 20 g of the sample in a dry 250 ml Becker. Twenty milliliters of glycerin was slowly added, and the sample was mixed with circular movements until a paste was formed. Subsequently, 0.5 ml of glycerin (1 :1 W/W) was continuously added with the assistance of a glass stick, until the final absorption was achieved. The Becker was inclined to 45° and, after cleaning half of the bottom of the Becker, it was returned to the vertical position. The final absorption point was determined when the paste covered the Becker's bottom in at least 30 seconds. (Quimbarra STM 206/94)
  • a sedigraph analysis was performed using a Micromeritics Sedigraph 5100. Seven grams of PCC was placed in a Becker, and 5 drops of Polysal was added to make the volume 80 ml. The sample was analyzed in the sedigraph. (Quimbarra STM 235/97)
  • Toothpaste compositions were prepared by combining a toothpaste base, described below, with an abrasive system. Toothpaste formula used: sorbitol - 55.0% glycerin - 15.0% CMC - 0.7% methylparaben - 0.1% water - 12.3% saccharin sodium - 0.2% sodium fluoride/sodium monofluorophosphate - 0.2%/0.8%
  • Toothpaste compositions were prepared by combining a toothpaste base, the same described in page 12, with an abrasive system.
  • the physical characteristics of the toothpaste are set forth in Table 14, below. TABLE 12

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  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
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Abstract

L'invention porte sur une composition de dentifrice contenant un système abrasif comprenant un matériau abrasif de carbonate de calcium résistant à l'acide. Cette invention concerne aussi un procédé de fabrication de la composition de dentifrice.
PCT/IB2003/001322 2002-03-08 2003-03-07 Composition de dentifrice contenant du carbonate de calcium resistant a l'acide et procede de fabrication associe WO2003075874A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
BR0308295-4A BR0308295A (pt) 2002-03-08 2003-03-07 Composição de pasta de dente e método de preparar uma pasta de dente
AU2003216598A AU2003216598A1 (en) 2002-03-08 2003-03-07 Toothpaste composition including acid resistant calcium carbonate and a method of making the same

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US36245102P 2002-03-08 2002-03-08
US60/362,451 2002-03-08
US37363902P 2002-04-19 2002-04-19
US60/373,639 2002-04-19

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WO2003075874A1 true WO2003075874A1 (fr) 2003-09-18

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PCT/IB2003/001322 WO2003075874A1 (fr) 2002-03-08 2003-03-07 Composition de dentifrice contenant du carbonate de calcium resistant a l'acide et procede de fabrication associe

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AU (1) AU2003216598A1 (fr)
BR (1) BR0308295A (fr)
WO (1) WO2003075874A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2069572B1 (fr) 2006-08-17 2015-03-18 Specialty Minerals (Michigan) Inc. Amélioration du rendement du brillant du vernis anti-uv grâce à un nouveau pigment, et procédé de fabrication correspondant
US10780031B2 (en) 2013-12-13 2020-09-22 Omya International Ag Abrasive cleaning composition

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2885366A (en) * 1956-06-28 1959-05-05 Du Pont Product comprising a skin of dense, hydrated amorphous silica bound upon a core of another solid material and process of making same
GB1476063A (en) * 1976-01-26 1977-06-10 Boots Co Ltd Dentifrice
FR2747569A1 (fr) * 1996-04-22 1997-10-24 Rhone Poulenc Chimie Composition dentifrice comprenant un abrasif a base de silice et de carbonate de calcium, compatible avec le fluor
WO2001092422A1 (fr) * 2000-06-01 2001-12-06 J.M. Huber Corporation Pigment composite de carbonate de calcium/compose de silicium precipites

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2885366A (en) * 1956-06-28 1959-05-05 Du Pont Product comprising a skin of dense, hydrated amorphous silica bound upon a core of another solid material and process of making same
GB1476063A (en) * 1976-01-26 1977-06-10 Boots Co Ltd Dentifrice
FR2747569A1 (fr) * 1996-04-22 1997-10-24 Rhone Poulenc Chimie Composition dentifrice comprenant un abrasif a base de silice et de carbonate de calcium, compatible avec le fluor
WO2001092422A1 (fr) * 2000-06-01 2001-12-06 J.M. Huber Corporation Pigment composite de carbonate de calcium/compose de silicium precipites

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2069572B1 (fr) 2006-08-17 2015-03-18 Specialty Minerals (Michigan) Inc. Amélioration du rendement du brillant du vernis anti-uv grâce à un nouveau pigment, et procédé de fabrication correspondant
US10780031B2 (en) 2013-12-13 2020-09-22 Omya International Ag Abrasive cleaning composition

Also Published As

Publication number Publication date
AU2003216598A1 (en) 2003-09-22
BR0308295A (pt) 2005-05-10

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