EP2026748A1 - Verfahren zur herstellung von fliessfähigem kaliumnitrat für die mundpflege - Google Patents

Verfahren zur herstellung von fliessfähigem kaliumnitrat für die mundpflege

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Publication number
EP2026748A1
EP2026748A1 EP06760319A EP06760319A EP2026748A1 EP 2026748 A1 EP2026748 A1 EP 2026748A1 EP 06760319 A EP06760319 A EP 06760319A EP 06760319 A EP06760319 A EP 06760319A EP 2026748 A1 EP2026748 A1 EP 2026748A1
Authority
EP
European Patent Office
Prior art keywords
oral care
admixture
agent
composition
dipotassium hydrogen
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP06760319A
Other languages
English (en)
French (fr)
Inventor
Michael Fooken
Andreas Klingenberg
Romano Ruscelli
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Honeywell International Inc
Original Assignee
Honeywell International Inc
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 Honeywell International Inc filed Critical Honeywell International Inc
Publication of EP2026748A1 publication Critical patent/EP2026748A1/de
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • 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
    • A61K8/24—Phosphorous; Compounds thereof

Definitions

  • the invention relates to free flowing potassium nitrate compositions including anti-caking amounts of dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
  • the composition finds use in oral care compositions such as toothpastes.
  • SU585144, JP50104796 and UD5286272 teach potassium phosphates as anti caking materials in fertilizers containing potassium nitrate.
  • potassium nitrate can be maintained in a free flowing condition when it is admixed with an anti-caking amount of dipotassium hydrogen phosphate and potassium dihydrogen phosphate. It has also been found that an oral care composition, such as toothpaste, has a more uniform distribution of potassium nitrate when the potassium nitrate is preformed with an anti-caking amount of dipotassium hydrogen phosphate and potassium dihydrogen phosphate according to the invention. The resulting composition meets the requirements of the European Pharmacopoeia.
  • the invention provides a composition which comprises an admixture of potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
  • the invention also provides an oral care composition which comprises an orally acceptable vehicle and an admixture of potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
  • the invention further provides a method of preparing an oral care composition which comprises combining a pre-formed composition which comprises an admixture of potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate, with an orally acceptable vehicle.
  • the invention still further provides a method of preparing an oral care composition which comprises combining a pre-formed composition which comprises an admixture of potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate, with an orally acceptable vehicle.
  • a free flowing, anti-caking potassium nitrate composition comprises an admixture of potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
  • the composition may be formed by admixing dry potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
  • the potassium nitrate component is present in the composition in an amount of from about ' 99 wt.% or more.
  • the dipotassium hydrogen phosphate component is usually present in the composition in an amount of from about 0.13 wt.% to about 0.25 wt.%.
  • the potassium dihydrogen phosphate 5 component is usually present in the composition in an amount of from about 0.1 wt.% to about 0.19 wt.%.
  • Both dipotassium hydrogen phosphate and potassium dihydrogen phosphate must be present with the potassium nitrate in order to achieve a neutral pH.
  • Any balance comprises water.
  • the admixture has a water content of from about 0.0 wt.% to about 0.5 wt.%.
  • the mixture 0 always has a neutral pH value since the potassium dihydrogen phosphate and the dipotassium hydrogen phosphate form a buffer keeping the hydrogen cation concentration ate the same level even if some acid or base is added.
  • An oral care composition according to the invention comprises a combination 5 of an orally acceptable vehicle, and the admixture of potassium nitrate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate described above.
  • Orally acceptable vehicles usually comprises water and/or ethanol and may comprise one or more of an anti-caries agent, a flavor, a sweetening agent, an anti-microbial agent, a surfactant, a gel, ethanol, an o abrasive,' colorants, an anti-tartar agent, an anti-plaque agent, anti-calculus agents, a gum, a wax, a gelling, agent, a humectant, a polishing agent, a . stabilizer, a preservative, a source of fluoride ions among others known in the art.
  • the anti-caking potassium nitrate composition may be employed in an oral care composition in an amount of from about 0.25% to about 10% by weight of the oral care composition, preferably from about 2% to about 10% and more preferably from about 3 to about 7% by weight of the oral care composition.
  • the water and/or ethanol content of the oral care composition may be from about 3 to. about 80% by weight and more usually from about 3 to about 30 wt.% for a creamy, or visually transparent or translucent toothpaste in gel form.
  • Suitable anti-caries agents non-exclusively include a wide variety of fluoride ion-yielding materials as sources of soluble fluoride. Examples of suitable fluoride ion-yielding materials are found in U.S. patents 3,535,421 and 3,678,154.
  • Preferred fluoride ion sources for use herein include sodium fluoride, stannous fluoride, potassium fluoride, potassium stannous fluoride, indium fluoride, zinc fluoride, ammonium fluoride, sodium monofluorophosphate and stannous chlorofluoride as well as mixtures thereof.
  • Stannous fluoride and sodium fluoride are particularly preferred.
  • the oral care compositions have from about 50 ppm to 10,000 ppm, more preferably from about 100 to 3000 ppm, of fluoride ions in the oral care composition.
  • Suitable flavoring agents include oil of wintergreen, oil of peppermint, oil of spearmint, oil of sassafras, sage, eucalyptus, marjoram, cinnamon, lemon, orange, and oil of clove.
  • the amount of flavoring agent in the oral care composition is from about 0.3 wt.% to about 1.2 wt.%.
  • Sweetening agents which can be used in the oral care composition include sucrose, saccharin, dextrose, lactose, maltose, levulose, aspartame, D- tryptopnan, dihydrochalcones, acesulfame and sodium cyclamate. Flavoring agents are generally used in the oral care composition at amounts of from about 0.01 wt.% to 2 wt.% and sweetening agents at amounts of from about 0.05 wt.% to about 2 wt.% by weight of the oral care composition.
  • Typical surfactants include anionic, nonionic, cationic, zwitterionic and amphoteric surfactants of the types described more fully in U.S. patents 3,959,458 and 3,937,807.
  • Anionic surfactants include the water-soluble salts of alkyl sulfates having from 10 to 18 carbon atoms in the alkyl radical and the water-soluble salts of sulfonated morioglycerides of fatty acids having from 10 to 18 carbon atoms.
  • Sodium lauryl sulfate, and sodium coconut monoglyceride 5 sulfonates are examples of anionic surfactants of this type. Mixture of anionic surfactants can also be employed.
  • nonionic surfactants which can be used in the present invention can be produced by the condensation of alkylene oxide groups with an organic hydrophobic compound which may be aliphatic or alklaromatic in nature.
  • suitable nonionic surfactants include the 0 Pluronics, polyethylene oxide condensates of alkyl phenols, products derived from the condensation of ethylene oxide with the reaction product of propylene oxide and ethylene diamine, ethylene oxide condensates of aliphatic alcohols, long chain tertiary amine oxides, long chain tertiary phosphine oxides, long chain dialkyl sulfoxides and mixtures of such materials.
  • the 5 zwitterionic surfactants useful in the oral care compositions of the present invention can be derivatives of aliphatic quaternary ammonium, phosphonium, arid sulfonium compounds, in which the aliphatic radicals can be straight chain or branched, and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms and one contains as anionic water-so ⁇ ubilizing group, o e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate.
  • surfactants useful in the oral care compositions of the present invention can be quaternary ammonium compounds having one long alkyl chain containing from about 8 to about 18 carbon atoms such as lauryl trimethylammonium chloride; cetyl pyridinium chloride; cetyl trimethylammonium bromide; di- 5 isob.utylphenoxyethoxyethyl-dimethylbenzylammonium chloride; coconutalkyltrimethylammonium nitrite; cetyl pyridinium fluoride; etc.
  • Useful quarternary ammonium fluorides are described in U.S. patent 3,535,421.
  • Amphoteric surfactants useful in the present invention can be derivatives of aliphatic secondary and tertiary amines in which the aliphatic radical can be Straight chain or branched and wherejn one of the aliphatic substituents contains from about 8 to about 18 carbon atoms and one contains an anionic water-solubilizing group, e.g., carbox'ylate, sulfonate, sulfate, phosphate, or phosphonate.
  • the surfactant agent can be present in the oral care compositions of this invention in an amount from O.i% to 6% by weight of the total oral care composition.
  • Agglomerating agents which can be used in the practice of this invention include waxes and gelling agents.
  • Suitable waxes are those which are non- toxic and have a hardness value of from about 0 to. about 65 (ASTM Test D 1321-65) and preferably from about 0 to 5.
  • suitable waxes include carnauba wax, candelilla wax, purified montan wax, castor wax, paraffin, ceresin wax and bayberry wax.
  • Preferred waxes have a melting point above 70 0 F.
  • Waxes having these properties which can be used herein are disclosed in Soap & Chem. Specialties, Vol. 33, page 141 (1957). See also Industrial Waxes, Vol. I and II, H. Bennett, Chemical Publishing Co., Inc., New York, 1963, for a discussion of waxes and their properties.
  • Gelling agents for toothpaste vehicles are well ' known in the art. These are often high polymers (e.g., gums or other thickening agents) which are soluble or swellable in water or aqueous medium. Suitable gelling agents, or thickening agents, are those that form stable, firm gels which are non-toxic; hard enough to withstand conventional shear stresses when admixed in a dentifrice or extruded from the toothpaste tube; frangible enough to disintegrate into smaller particles at time of use to give no adverse mouth impression; light colored; innocuous in flavor and odor; and compatible with toothpaste ingredients.
  • high polymers e.g., gums or other thickening agents
  • Suitable gelling agents, or thickening agents are those that form stable, firm gels which are non-toxic; hard enough to withstand conventional shear stresses when admixed in a dentifrice or extruded from the toothpaste tube; frangible enough to disintegrate into smaller particles at time of use to give no adverse mouth impression;
  • Gelling agents which can be used to form agglomerates of pigment particles include sodium carboxymethylcellulose, gum tragacanth, gum arabic, gum karaya, sodium alginate, hydroxyethyl cellulose, methyl Cellulose, ethyl cellulose, carrageen a,nd other polysaccharides, polyvinyl pyrollidones agar-agar, cassava starch, microcrystalline cellulose, complex magnesium aluminum silicate and high molecular weight carboxyvinyl polymers.
  • the amount of thickening agent used in the practice of this invention is preferably sufficient to impart to the mixture the pasty consistency, body and the non-tacky nature which is characteristic of conventional dental creams or toothpastes.
  • dental creams are extrudable from ordinary collapsible toothpaste tubes to form a ribbon of substantial thickness (e.g., about 3/8 inch) which if left undisturbed, substantially retains its original thickness over a period of, say, one minute or more (and does not penetrate substantially into the bristles of a toothbrush when resting on the.ends of such bristles for a similar period); but which preferably offers no substantial resistance to brushing or to deformation when, for instance, one touches it lightly with a finger; and which has little tack, in that it does not tend to form a string when the finger is pulled away from the ribbon.
  • the proportion of the thickening agent is often within the range of about 0;5 to 2%, such as about 0.8 to 1.5%, of the oral care composition.
  • Useful stabilizers for oral care composition include dicalcium phosphate dihydrate 1 and calcium pyrophosphate.
  • a description of the method of preparation of dicalcium phosphate dihydrate and of its stabilization is found in U.S.. patent 3,169,096. See also "Cosmetic Science” Vol. 1 pub. 1972 (Wiley Interscience) edited by Balsam and Sagarin pages 477-479.
  • a useful preservative for the oral care composition may be sodium benzoate, methyl paraben, propyl paraben, phenyl mercuric nitrate, sodium bisulfite, disodium calcium EDTA, chlorobutanol, and mixtures thereof in amounts of from about 0.5 to about 15 percent by weight, based on the total weight of the oral care composition
  • Suitable anti-microbial agents include alcohols, formaldehyde preparations and compounds which liberate formaldehydes, hypochloride substances, iodine preparations, mercury preparations and phenolic compounds such as halogenated diphenyl ethers, halogenated salicylanilides, benzoic esters, halogenated carbanilides, phenol and its homologs, mono- and poly-alkyl and aralkyl halophenols, resorcinol and its derivatives, bisphenolic compounds; N 1 -(4-chlorobenzyl)-N 5 -(2,4-dich
  • the oral care composition may contain a colorant such as a food grade pigment or dye.
  • Pigment particles must be essentially color-fast, i.e., must. not leach a significant amount of color in the presence of water.
  • water- soluble dyes per se are not preferred in the practice of this invention.
  • Water- soluble dyes can be used to prepare pigment particles which will not leach - color.
  • Other pigment particles which can be used to prepare colored oral care compositions include, for example,.
  • non-toxic water-insoluble, inorganic pigments such as chromium oxide greens, carbon blacks, ultramarine blues and pinks, and ferric oxides; dyed cellulose particles such as dyed cotton linters and dyed wood pulp; and water- insoluble dye lakes prepared by extending calcium or aluminum salts, of FD&C water-soluble dyes on alumina, such as FD&C Green #1 lake, FD&C Blue #2 lake and FD&C Yellow #5 lake.
  • the mean particle size of the pigment particle can range from about 5 to about 490 microns, and preferably from 10 to about 200 microns. Larger particles tend to feel gritty in the mouth and stick between the teeth.
  • the particle sizes referred to herein can be determined for example by microscopic measurements using a calibrated eyepiece.
  • the pigment particles can comprise from, about 10% to about 50% by Weight of the total oral care composition.
  • the pigment is used at a concentration in the range from about 30% to about 50% by weight of the total oral care composition.
  • Typical abrasives, or polishing agents, contemplated for use in the present invention can be any material which does not excessively abrade teeth. These may be water soluble, such as sodium bicarbonate, or water insoluble materials provided (hey do not remove tooth material but rather to removal of deposits on dental enamel from and polishing the teeth.
  • silica gel colloidal silica, complex amorphous alkali metal aluminosilicates and mixtures thereof, and resinous abrasive materials such as particulate condensation products of urea and formaldehyde, and other such as disclosed in U.S. patent 3,070,510.
  • resinous abrasive materials such as particulate condensation products of urea and formaldehyde, and other such as disclosed in U.S. patent 3,070,510.
  • Still other suitable polishing materials include the particulate thermosetting resins described in U.S. patent. 4,070,510, such as melamine-, phenolic-, and urea-formaldehydes, and crosslinked polyepoxides and polyesters.
  • abrasives may also be iisecL Silica dental abrasives, of various types, can provide the unique benefits of exceptional dental cleaning and polishing performance without unduly abrading tooth enamel.
  • the abrasive polishing materials useful herein generally have an average particle size ranging between about 0.1 to 30 5 microns, preferably 5 and 15 microns.
  • the silica abrasive can be precipitated silica or silica gels such as the silica xerogels as described in U.S. patents 3,538,230; 3,862,307 and 4,340,583.
  • the abrasive in the compositions described herein is present in an amount of from about 6% to about 35%, preferably from about 15% to about 25% by weight of the oral care o composition.
  • Suitable anti-tartar agents non-exclusively include an alkali metal polyphosphate or a phosphono anti-tartar agent.
  • the polyphosphates may be ' any of various water soluble polyphosphates, including alkali metal 5 pyrophosphates, such as tetrapotassium pyrophosphate, trisodium pyrophospate, dipotassium pyrophosphate, tetrasodium pyrophosphate and disodium pyrophosphate, with the sodium salts being preferred.
  • the tripolyphosphates and other polyphosphates such as the hexametaphosphates, may be substituted, at least in part.
  • the pyrophosphates o are considered to be superior as anti-tartar agents that help to desensitize the teeth.
  • a most preferred pyrophosphate is tetrasodium pyrophosphate, but the corresponding tetrapotassium pyrophosphate or tri, -di and mono sodium and potassium pyrophosphates may also be used, at least in part.
  • the anti-tartar agent may be a phosphono compound such as azacyloalkane-2,2- diphosphosphonic acid, preferably azacycloheptane-2,2-diphosphonic acid, phosphonopropane tricarboxylic acid, phosphono butane- 1,2,4-tricarboxylic acid and ethanedihydroxy diphosphonic acid and water soluble salts thereof.
  • the anti-tartar agent is employed in an effective anti-tartar amount which is generally about 0.1 to 10% by weight of the oral care composition, preferably about 0.8 to 7%.
  • Suitable anti-calculus agents may be known phosphorus-containing anti- calculus agents such as disodium ethane- 1 -hydroxy- 1, 1-diphosphonate which are described in U.S. patent 3,488,419.
  • Suitable anti-plaque agents include bis-biguanide compounds such as cholorhexidine (l,6-bis[N 5 -p-chlorophenyl- N 1 -biguanido]hexane), the soluble and insoluble salts thereof and related materials such as l,2-bis-(N 5 -p-tri-fluoromethylphenyl-N 1 -biguanido)ethane as described in U.S: patents 3,934,002 and 3,937,807.
  • a humectant component of the oral care composition serves to keep the toothpaste compositions, from hardening upon exposure to air.
  • Suitable humectants for use in this invention include edible polyhydric alcohols such as glycerine,' sorbitol, xylitol, glycerol, polyethylene glycol, propylene glycol and polypropylene glycols.
  • a normal range of molecular weights for the polyethylene glycol humectants is 200 to 1,000, preferably 400 to 600 or 800, e.g., about 600.
  • the humectant content is usually from about 10% to about 80%, preferably from about 20% to about 70%, ' and more preferably from about 30% to 65%, by weight of the oral care compositions herein.
  • the oral care composition such as a toothpaste, has a more uniform distribution of potassium nitrate when the potassium nitrate is preformed with an anti-caking amount of dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
  • the oral care compositions of the invention when in the form of toothpaste compositions, are used in conventional manner.
  • the toothpaste compositions or slurries thereof are brushed, onto dental surfaces and subsequently rinsed away.
  • pastes or slurries generally contact dental surfaces for at least about 30 seconds. More
  • 7000 1 water are then evaporated from the solution by using vacuum and maintaining the temperature at 50 °C. Residual water is evaporated to reach a temperature of below 25°C. A centrifuge is then used to reduce the water content further. The final moisture content is reached by drying the material in a tumble dryer under vacuum while maintaining a temperature of 60-70°C. 0.13% K 2 HPO 4 and 0.1% KH 2 PO 4 by weight are added. Then a tumble dryer is used to homogenize the material by operating it for another three hours. The free flowing material is filled into bags via a 5 mm mesh sieve.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)
EP06760319A 2006-05-23 2006-05-23 Verfahren zur herstellung von fliessfähigem kaliumnitrat für die mundpflege Withdrawn EP2026748A1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2006/019993 WO2007136381A1 (en) 2006-05-23 2006-05-23 Process to prepare free flowing potassiium nitrate for oral care

Publications (1)

Publication Number Publication Date
EP2026748A1 true EP2026748A1 (de) 2009-02-25

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EP06760319A Withdrawn EP2026748A1 (de) 2006-05-23 2006-05-23 Verfahren zur herstellung von fliessfähigem kaliumnitrat für die mundpflege

Country Status (5)

Country Link
EP (1) EP2026748A1 (de)
JP (1) JP2009538297A (de)
CN (1) CN101489521A (de)
AU (1) AU2006344090A1 (de)
WO (1) WO2007136381A1 (de)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2246031B1 (de) 2008-06-10 2017-06-28 The Procter & Gamble Company Zinn-Chlorid-und Silica Zusammensetzungen
US9220667B2 (en) 2009-06-08 2015-12-29 The Procter & Gamble Company Stannous chloride compositions
AU2017240683B2 (en) * 2016-04-01 2020-01-16 The Procter & Gamble Company Oral care compositions containing potassium nitrate and peroxide
EP3435957A1 (de) * 2016-04-01 2019-02-06 The Procter and Gamble Company Mundpflegezusammensetzungen mit gelnetzwerken und kaliumnitrat
AU2017240034B2 (en) 2016-04-01 2020-02-06 The Procter & Gamble Company Oral care compositions containing a gel network phase
BR112018069874A2 (pt) * 2016-04-01 2019-02-05 Procter & Gamble composições para tratamento bucal contendo uma fase de rede de gel e nitrato de potássio

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SU802249A1 (ru) * 1977-07-06 1981-02-07 Предприятие П/Я А-1676 Способ получени сложных удобрений
SU1131859A1 (ru) * 1983-07-08 1984-12-30 Предприятие П/Я Р-6603 Способ устранени слеживаемости аммиачной селитры
SU1721016A1 (ru) * 1989-01-09 1992-03-23 Государственный научно-исследовательский и проектный институт метанола и продуктов органического синтеза Способ получени нитрата кали
CN1180048A (zh) * 1996-08-30 1998-04-29 西宁星火化工厂 一种防止硝酸钾结块的组合物及其用途
CN1189395C (zh) * 2002-07-10 2005-02-16 上海化工研究院 硝酸钾防结块剂

Non-Patent Citations (1)

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Title
See references of WO2007136381A1 *

Also Published As

Publication number Publication date
JP2009538297A (ja) 2009-11-05
CN101489521A (zh) 2009-07-22
WO2007136381A1 (en) 2007-11-29
AU2006344090A1 (en) 2007-11-29

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