WO2000003949A1 - Composition administree par voie orale - Google Patents
Composition administree par voie orale Download PDFInfo
- Publication number
- WO2000003949A1 WO2000003949A1 PCT/EP1999/004920 EP9904920W WO0003949A1 WO 2000003949 A1 WO2000003949 A1 WO 2000003949A1 EP 9904920 W EP9904920 W EP 9904920W WO 0003949 A1 WO0003949 A1 WO 0003949A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- calcium carbonate
- calcitic
- producing
- spheroidal
- chelating agent
- Prior art date
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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/51—Chelating agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Definitions
- the present invention relates to a process for the preparation of calcium carbonate especially in the calcitic form with a spheroidal morphology and a synergistic dentifrice composition comprising spheroidal calcite to impart superior sensory properties.
- Calcium carbonate or chalk exists in three crystal forms: calcite, aragonite and vaterite.
- the natural morphology of calcite is rhombohedral or cuboidal, acicular or dendritic for aragonite and spheroidal for vaterite.
- calcium carbonate or chalk known as precipitated calcium carbonate is produced by carbonation method in which carbon dioxide gas is bubbled through an aqueous suspension of calcium hydroxide. In this process the crystal type of calcium carbonate is calcite or a mixture of calcite and aragonite .
- Precipitated calcite having a spherical morphology and with a particle size ⁇ 10 ⁇ have a wide application in paper, rubber, polymer and paint industry to impart specific advantages .
- a wide variety of particulate abrasive agents are employed in the manufacture of personal and home care products.
- the most frequently used material for imparting abrasive properties are precipitated silicas.
- Chalk or calcium carbonate is a cost-effective alternative to silica as an abrasive.
- One of the important applications of chalk is in dental care products.
- Spheroidal calcite will be superior in its use as an abrasive in dental care products as it will have improved sensory properties over normal rhombohedric calcite without compromising on cleaning properties.
- Morphology and particle size of calcium carbonate are significantly influenced by the addition of various additives during the carbonation process.
- additives such as polyphosphates, chelating agents, amino acids, polysaccharides and polybasic organic acids and others have been used at various concentrations and at different stages of the carbonation process.
- US 4,714,603 discloses a process of preparation of spheroidal calcite and its specific application to produce a coated paper having a combination of dull finish and good printability, wherein carbon dioxide is introduced into an aqueous slurry of calcium hydroxide containing dissolved polyphosphate.
- Amino acids have been used as additives during carbonation at significantly high levels (Calcium hydroxide to amino acid 1:1 to 1:5) (J. Ceram. Soc. Japan, 1986, vol.104, pp.1081-1084) .
- the crystal form of calcium carbonate obtained is vaterite.
- JP 88010923 discloses the production of spheroidal calcite by heating vaterite at 400-800° C under 1-10 atmos. pressure and its use in dentifrices.
- the object of the present invention is to provide a process for preparing calcitic calcium carbonate essentially with a spheroidal morphology.
- Another object of the present invention is to provide a process for preparing calcitic calcium carbonate essentially with a spheroidal morphology with an average particle size less than 20um such that 80% of the particles lie within 4um of the average particle size.
- Yet another object of the present invention is to provide a synergistic dentifrice composition comprising spheroidal calcite to impart superior sensory properties.
- a process for the preparation of calcitic calcium carbonate essentially with a spheroidal morphology and with an average particle size less than 20 ⁇ m, such that 80% of the particles lie within 4 ⁇ m of the average particle size which comprises the introduction of carbon dioxide into an aqueous slurry of 1-30% calcium hydroxide and a soluble organic chelating agent in the weight ratio of between 1000:1 to 10:1 at a temperature range of 10-50°C.
- the process of the present invention comprises a process for the preparation of calcitic calcium carbonate essentially with a spheroidal morphology and with an average particle size less than lOum, such that 80% of the particles lie within 2 ⁇ m of the average particle size which comprises the introduction of carbon dioxide into an aqueous slurry of 1-30% calcium hydroxide and a soluble organic chelating agent in the weight ratio of between 1000:1 to 10:1 at a temperature range of 10-50°C under stirring at a speed of 100-1000 rpm.
- carbon dioxide is introduced into a slurry of 1-30% calcium hydroxide and a soluble organic chelating agent.
- the said calcium hydroxide may also be obtained by the addition of water to calcium oxide but making sure that the temperature of this mixture is not higher than 50 deg. C at the time of introduction of carbon dioxide.
- the preferred strength of calcium hydroxide is 10-20%.
- the soluble organic chelating agent can be chosen from mono, di or poly carboxylic acids such as citric acid, oxalic acid, maleic acid ; amino acids, certain di or tri peptides, ethylene diamine tetra acetic acid or their alkali metal salts and any other chelating agent known in the art.
- the preferred chelating agents are citric acid, amino acids such as glycine, serine, alanine, phenyl alanine, aspartic acid and glutamic acid and ethylene diamine tetra acetic acid or their alkali metal salts.
- the ratio of calcium hydroxide to the chelating agent is in the range of 1000:1 to 10:1 and preferably 200:1 to 50:1.
- the carbonation reaction is preferably carried out till the pH of the medium is in the range 6.5-9 and more preferably below 8.
- the reaction is carried out at a temperature range of 10-50 deg. C and preferably in the range 20-40° C under stirring at a speed of 100-1000 rpm and preferably at 200-600 rpm.
- the invention provides for a synergistic dentifrice composition
- a synergistic dentifrice composition comprising atleast 10% calcitic spheroidal calcium carbonate prepared according to the present invention and other conventional ingredients.
- the invention provides for a synergistic dentifrice composition
- a synergistic dentifrice composition comprising 25-45% calcitic spheroidal calcium carbonate prepared according to the present invention and other conventional ingredients.
- the spheroidal chalk prepared according to the present invention can be incorporated into any dentifrice formulation to partially or fully replace the abrasives in the formulation.
- the additional abrasives can be abrasive silicas, chalks, hydrated aluminas, calcium phosphate, calcium pyrophosphates, hydroxy apatites, insoluble metaphosphates; etc.
- the dentifrice compositions of the invention may contain one or more additional components, as will be described below.
- Dentifrice compositions of the invention preferably comprise one or more surfactants, preferably selected from anionic, nonionic, amphoteric and zwitterionic surfactants and mixtures thereof.
- the preferred anionic surfactants may include sodium lauryl sulphate, sodium dodecylbenzene sulphonate, sodium lauroyl sarcosinate and sodium coconut monoglyceride sulphonate.
- Nonionic surfactants which may be suitable for use in compositions of the invention include sorbitan and polyglycerol esters of fatty acids, as well as ethylene oxide/propylene oxide block copolymers.
- Amphoteric surfactants which may be suitable include betaines such as cocamidopropyl betaine, and sulphobetaines .
- the surfactant may be present in the oral composition of the invention in a total amount from 0.1 to 3% by weight.
- Water is another preferred component of the oral compositions of the invention and may be present in an amount of from about 1 to 90% by weight, preferably from about 10 to about 60%, more preferably from about 15 to about 50%.
- Toothpastes and creams of this invention may also contain humectants, for example polyols such as glycerol, sorbitol, polethylene glycol, xylitol and hydrogenated corn syrup.
- humectants for example polyols such as glycerol, sorbitol, polethylene glycol, xylitol and hydrogenated corn syrup.
- the total amount of the humectant, if present, may be in the range of 10 to 85% by weight of the composition.
- thickening agents and/or suspending agents are included.
- thickening agents which may be used are thickening silicas, polyacrylic acid copolymers and cross-linked polymers of acrylic acid, esters of ethylene glycol, esters of polyethylene glycol, heteropolysaccharide gums, cellulose derivatives such as sodium carboxymethyl cellulose and others known in the art.
- the thickening agents may be used singly or as mixtures of two or more such materials and may be present in an amount from 0.1 to about 50% by weight and preferably from 5 to 15% for silica thickening agents; preferably from 0.1 to about 5% for polymer suspending agents.
- composition of the invention may contain other conventional ingredients such as flavouring substances, peroxy substances, opacifiers, pigments and colouring agents, preservatives, moisturising agents, flouride containing compounds and other benefit agents.
- compositions in accordance with the present invention may be made by conventional methods of preparing oral compositons .
- 1.5 Kg of calcium oxide was taken in a stainless steel jacketed reactor and 15L water was added. 15g of sodium citrate was added to the slurry and mixed well using a mechanical stirrer at a speed of 300 rpm. The pH of the system was 13 and the temperature of the system was brought down to 30 °C by circulating cold water. The carbonation was started by bubbling carbon dioxide through the slurry. The slurry temperature was maintained at 30°C throughout the reaction. The reaction was monitored by measuring the pH of the system continuously. Carbon dioxide bubling was stopped when the pH of the system reached between 7.0 and 8.0. After the carbonation, the slurry was filtered immediately and dried in an oven at a temperature of 110-120 °C. The dried material was then pulverised to get the final powder.
- Example 1 a The reaction was carried as in Example 1 a except that an amino acid such as serine or glycine was added in place of sodium citrate.
- Example la&b The structural characterization of the spheroidal calcium carbonate prepared according to the invention as described in Example la&b was done by the X-ray (powder) diffraction technique using an X-Ray (Powder) Diffractometer (Siemens, D5000) .
- the XRD patterns were compared with the JCPDS powder data file and confirmed that the polymorphic phase of calcium carbonate obtained had a calcitic crystal form (Fig.l).
- the Infrared spectral studies were carried out using a FT-IR Spectrometer (BOMEM, MB-102) .
- the infrared absorption bands observed also confirmed that the calcium carbonate obtained according to the invention was calcitic. (Fig.2) .
- the particle size and particle size distribution were measured using a Coulter Counter (Model: Coulter Multisizer II) .
- the particle size distribution pattern is given in Fig. 4 depicting a very narrow distribution with more than 80% of particles lying below 10 urn.
- a dentifrice composition as described in table 1 was prepared using the commercially available precipitated calcium carbonate Pacal-H supplied by Citurgia Biochemicals, Rishikesh, UP (Control) and in the experimental sample the same was replaced with the spheroidal calcium carbonate prepared according to the present invention.
- Table 1 A dentifrice composition as described in table 1 was prepared using the commercially available precipitated calcium carbonate Pacal-H supplied by Citurgia Biochemicals, Rishikesh, UP (Control) and in the experimental sample the same was replaced with the spheroidal calcium carbonate prepared according to the present invention.
- Control and experimental formulations were evaluated by the standard quantitative descriptor analyses (QDA) using an expert panel for their organoleptic properties.
- the panel consisted of 15 members who evaluated the sensory properties on a 0 to 10 scale. Different sensory properties such as squeeze, smothness, spreadability, grittiness, chalkiness, foam, creaminess, flavour, freshness, pungency and cooling were evaluated by the panel.
- the data presented in Table 2 shows that the pastes containing chalk with spheroidal morphology exhibited significant decrease in grittiness without any drying effect in the mouth as compared to the control. However, with respect to other parameters the experimental sample containing spheroidal chalk was not significantly different as compared to the control.
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Organic Chemistry (AREA)
- Epidemiology (AREA)
- Birds (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Cosmetics (AREA)
Abstract
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU49101/99A AU4910199A (en) | 1998-07-14 | 1999-07-09 | Oral composition |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9815289.5 | 1998-07-14 | ||
GBGB9815289.5A GB9815289D0 (en) | 1998-07-14 | 1998-07-14 | Speroidal calcitic calcium carbonate |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2000003949A1 true WO2000003949A1 (fr) | 2000-01-27 |
Family
ID=10835513
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP1999/004920 WO2000003949A1 (fr) | 1998-07-14 | 1999-07-09 | Composition administree par voie orale |
Country Status (3)
Country | Link |
---|---|
AU (1) | AU4910199A (fr) |
GB (1) | GB9815289D0 (fr) |
WO (1) | WO2000003949A1 (fr) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2826950A1 (fr) * | 2001-07-04 | 2003-01-10 | Solvay | Procede pour l'obtention de particules de carbonate de calcium precipite structurees a l'echelle nanometrique |
EP1280735A2 (fr) * | 2000-03-06 | 2003-02-05 | 3P Technologies Ltd. | Aragonite precipitee et procede de production associe |
WO2003020642A2 (fr) * | 2001-09-05 | 2003-03-13 | 3P Technologies Ltd. | Aragonite precipitee et procede de production associe |
US6808700B2 (en) * | 2001-03-14 | 2004-10-26 | Kao Corporation | Dentrifice comprising calcium carbonate granules |
EP2870986A4 (fr) * | 2012-07-05 | 2015-06-24 | Aisin Seiki | Procédé d'extraction de métal alcalin et/ou de métal alcalino-terreux |
EP2870987A4 (fr) * | 2012-07-05 | 2015-07-15 | Aisin Seiki | Procédé d'extraction de métal alcalin et/ou de métal alcalino-terreux |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4157379A (en) * | 1976-04-16 | 1979-06-05 | Toyo Soda Manufacturing Co., Ltd. | Process for producing chain structured corpuscular calcium carbonate |
JPH02243514A (ja) * | 1989-03-15 | 1990-09-27 | Kyodo Kumiai Tsukumi Fine Ceramics Kenkyu Center | 微細球状バテライト系炭酸カルシウムの製造方法 |
US5007964A (en) * | 1988-03-09 | 1991-04-16 | Shiraishi Central Laboratories Co., Ltd. | Calcium carbonate, calcium carbonate pigment, process for preparing same, coating composition for information recording paper and information recording paper |
DE19643657A1 (de) * | 1995-10-26 | 1997-04-30 | Solvay Barium Strontium Gmbh | Mikronisiertes Erdalkalimetallcarbonat |
GB2309692A (en) * | 1996-02-02 | 1997-08-06 | You Kyu J | Preparing colloidal calcium carbonate particles |
-
1998
- 1998-07-14 GB GBGB9815289.5A patent/GB9815289D0/en not_active Ceased
-
1999
- 1999-07-09 WO PCT/EP1999/004920 patent/WO2000003949A1/fr active Application Filing
- 1999-07-09 AU AU49101/99A patent/AU4910199A/en not_active Abandoned
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4157379A (en) * | 1976-04-16 | 1979-06-05 | Toyo Soda Manufacturing Co., Ltd. | Process for producing chain structured corpuscular calcium carbonate |
US5007964A (en) * | 1988-03-09 | 1991-04-16 | Shiraishi Central Laboratories Co., Ltd. | Calcium carbonate, calcium carbonate pigment, process for preparing same, coating composition for information recording paper and information recording paper |
JPH02243514A (ja) * | 1989-03-15 | 1990-09-27 | Kyodo Kumiai Tsukumi Fine Ceramics Kenkyu Center | 微細球状バテライト系炭酸カルシウムの製造方法 |
DE19643657A1 (de) * | 1995-10-26 | 1997-04-30 | Solvay Barium Strontium Gmbh | Mikronisiertes Erdalkalimetallcarbonat |
GB2309692A (en) * | 1996-02-02 | 1997-08-06 | You Kyu J | Preparing colloidal calcium carbonate particles |
Non-Patent Citations (1)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 014, no. 562 (C - 0788) 13 December 1990 (1990-12-13) * |
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1280735A4 (fr) * | 2000-03-06 | 2003-07-09 | 3P Technologies Ltd | Aragonite precipitee et procede de production associe |
EP1280735A2 (fr) * | 2000-03-06 | 2003-02-05 | 3P Technologies Ltd. | Aragonite precipitee et procede de production associe |
US6808700B2 (en) * | 2001-03-14 | 2004-10-26 | Kao Corporation | Dentrifice comprising calcium carbonate granules |
US7708973B2 (en) | 2001-07-04 | 2010-05-04 | Solvay (Societe Anonyme) | Method for obtaining precipitated calcium carbonate particles of nanometric scale structure |
WO2003004414A1 (fr) * | 2001-07-04 | 2003-01-16 | Solvay (Société Anonyme) | Procede pour l'obtention de particules de carbonate de calcium precipite structurees a l'echelle nanometrique |
US7501107B2 (en) | 2001-07-04 | 2009-03-10 | Solvay (Societe Anonyme) | Method for obtaining precipitated calcium carbonate particles of nanometric scale structure |
FR2826950A1 (fr) * | 2001-07-04 | 2003-01-10 | Solvay | Procede pour l'obtention de particules de carbonate de calcium precipite structurees a l'echelle nanometrique |
WO2003020642A2 (fr) * | 2001-09-05 | 2003-03-13 | 3P Technologies Ltd. | Aragonite precipitee et procede de production associe |
WO2003020642A3 (fr) * | 2001-09-05 | 2003-09-25 | 3P Technologies Ltd | Aragonite precipitee et procede de production associe |
EP2870986A4 (fr) * | 2012-07-05 | 2015-06-24 | Aisin Seiki | Procédé d'extraction de métal alcalin et/ou de métal alcalino-terreux |
EP2870987A4 (fr) * | 2012-07-05 | 2015-07-15 | Aisin Seiki | Procédé d'extraction de métal alcalin et/ou de métal alcalino-terreux |
AU2013285918B2 (en) * | 2012-07-05 | 2015-11-05 | Aisin Seiki Kabushiki Kaisha | Alkali metal and/or alkali earth metal extraction method |
US20150322547A1 (en) * | 2012-07-05 | 2015-11-12 | Aisin Seiki Kabushiki Kaisha | Alkali metal and/or alkali earth metal extraction method |
AU2013285917B2 (en) * | 2012-07-05 | 2015-11-26 | Aisin Seiki Kabushiki Kaisha | Alkali metal and/or alkali earth metal extraction method |
US9631256B2 (en) | 2012-07-05 | 2017-04-25 | Aisin Seiki Kabushiki Kaisha | Alkali metal and/or alkali earth metal extraction method |
US10113214B2 (en) | 2012-07-05 | 2018-10-30 | Aisin Seiki Kabushiki Kaisha | Alkali metal and/or alkali earth metal extraction method |
Also Published As
Publication number | Publication date |
---|---|
AU4910199A (en) | 2000-02-07 |
GB9815289D0 (en) | 1998-09-09 |
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