Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
  • C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
• • 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
  • A61K8/26—Aluminium; Compounds thereof
• • 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
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
  • A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
  • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q19/00—Preparations for care of the skin
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/40—Dyes ; Pigments
  • C11D3/42—Brightening agents ; Blueing agents
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/02—Inorganic compounds
  • C11D7/04—Water-soluble compounds
  • C11D7/10—Salts
  • C11D7/14—Silicates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/22—Organic compounds
• • 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
  • A61K2800/42—Colour properties
  • A61K2800/43—Pigments; Dyes
  • A61K2800/434—Luminescent, Fluorescent; Optical brighteners; Photosensitizers

Definitions

• This invention relates to a bipolar particulate fluorescer for use in laundry detergent compositions, fabric conditioners and personal care compositions and a process for making the same.
• detergents and personal care especially in laundry (wash and fabric conditioning) and in personal care compositions (e.g. skin lightening and sunscreen compositions) for giving a consumer desired optical effect to the substrates.
• Fluorescers are also known as optical brighteners . These molecules generally absorb amongst other invisible light such as ultraviolet light, and emit this energy in another form. For the purpose of detergent products, the light is generally emitted in the visible spectrum, preferably blue or green light. The extra emission in the blue and/or green range of the spectrum makes fabrics or textiles washed with detergent comprising fluorescer molecules look brighter after washing. Fluorescer molecules get adsorbed in or otherwise attached to the fabric and give the desired effect.
• fluorescers are generally fabric specific. Some fluorescers work well on e.g. cotton, but not on polyester and vice versa.
• carrier material for better fluorescer deposition on to fabric is also disclosed in literature.
• US2007/0203052 discloses a particulate fluorescer (brightener) wherein the carrier is urea formaldehyde, in order to deposit particulate brightener on to consumer articles during the wash
• WO00/58431 discloses the use of a brightener pigment comprising a cellulose powder which is dispersible in water and a water soluble fluorescent whitening agent for increasing the whiteness of cleansers or detergents.
• DE 195 38 039 use swellable clay which are not anisotropic in terms of their surface characteristics.
• US 5,449,402 discloses a functionally modified pigment particle is prepared by mixing a flocculated pigment of kaoline clay or calcium carbonate with a modifier having charge sites opposite in sign to the charge sites of the flocculated pigment.
• the flocculated kaoline clay is first binded with a latex binder and then treated with modifier. This particle thus does not show anisotropic behaviour with respect to their surface property and thus not suitable for the present purpose.
• Skin lighteners are known in the art and serve a useful purpose in the repertoire of cosmetics. Skin lightening agents are generally biochemically active molecules which help to modulate the melanin synthesis.
• Sunscreens/sunblocks are generally used for this purpose.
• Sunscreens are generally organic molecules that absorb the UV light and emit the energy in a different form, for instance in the visible range of the spectrum or in the form of heat, thereby protecting the skin against sunburn.
• sunblocks help to protect the skin against possible sunburn.
• These sunblocks generally comprise inorganic particulates (like ZnO, Ti0 2 ) that reflect the incident rays in uv-visible region thus protecting the skin.
• Formulations using these molecules in the form of a cream, a lotion, gel, or spray are known. Many consumers believe that the currently available sunscreens or skin lightening agents in cosmetics may penetrate inside the skin which is not desirable. Another problem associated with currently available sunscreens in cosmetics is that there are usually many other ingredients apart from sunscreens, with which they may interact thereby reducing their stability.
• fluorescer molecules tagged by surface reaction onto naturally occurring asymmetric clay surfaces act as a fluorescer particle with improved retention properties, low fabric specificity, higher stability in
• the present invention provides a bipolar
• topospecific particulate fluorescer which precursor is an asymmetric 1:1 or 2:1:1 clay particle comprising alternating tetrahedral and octahedral sheets terminating with a
• octahedral sheet at another external surface plane with fluorescer molecules having excitation wavelength between 200- 500 nm selectively attached to the coordinating cations on one of the said external surface planes wherein said particulate fluorescer has anisotropic characteristics.
• the invention provides a detergent
• composition comprising particulate fluorescer of the invention.
• the invention provides the use of the
• the invention provides a process of
• bipolar particulate fluorescer which precursor is an asymmetric 1:1 or 2:1:1 clay particle comprising
• alternating tetrahedral and octahedral sheets terminating with a tetrahedral sheet at one external surface plane and an octahedral sheet at another external surface plane comprising the steps of (a) contacting the precursor with a mineral acid (b) adding a fluorescer molecule to the mixture (c) adjusting the pH to a range of between 2 and 10 and (d) heating the solution mixture at a temperature 50 - 150 °C and (e) separating the solid product comprising bipolar particulate fluorescer .
• the invention provides a process for
• preparation of coated particle comprising the steps of (a) taking the solid bipolar fluorescer particle (b) adding it to a solvent containing the coating material at a temperature of 0°C to 100°C (c) stirring it for 10 minutes to 4 hours, (d) separating the coated particle, and (e) drying it at a
• the invention provides a cosmetic composition comprising particulate fluorescer of the invention and a cosmetically acceptable base.
• the invention provides the use of particulate fluorescer for improving skin appearance.
• the invention provides the use of particulate fluorescer for photoprotection of skin.
• characteristics according to the present invention is an asymmetric 1:1 or 2:1:1 clay particle having alternating tetrahedral and an octahedral sheets terminating with a
• Particle of 1:1 clay is particularly preferred as precursor.
• preferred 1 : 1 clays include kaolinite and serpentine subgroups of minerals.
• the species included within the kaolinite subgroup include, but are not limited to, kaolinite, dickite, halloysite and nacrite.
• the species within the serpentine subgroup include, but are not limited to chrysolite, lizardite, and amesite.
• preferred 2:1:1 clays include chlorite group of minerals. Chlorite is sometimes wrongly referred to as 2:2 clay by some mineralogists.
• the chlorite comprises tetrahedral-octahedral-tetrahedral sheets like 2:1 clays, with an extra weakly bound brucite like layer between tetrahedral layers.
• the tetrahedral sheet preferably comprises coordinating
• the tetrahedral sheet may also comprise isomorphously substituted coordinating tetrahedral cations which are not silicon.
• Isomorphously substituted coordinating tetrahedral cations include, but are not limited to, cations of aluminium, iron or boron.
• the octahedral sheet preferably comprises coordinating
• the octahedral sheet may also comprise isomorphously substituted coordinating octahedral cations which are not aluminium.
• Isomorphously substituted coordinating octahedral cations include cations of magnesium or iron.
• the fluorescer molecule is attached to the coordinating cations on the exterior side of one of the
• the fluorescer molecule is attached to coordinating cations on the exterior side of the tetrahedral sheet.
• the fluorescer molecule is attached to the coordinating cations on the exterior side of the octahedral sheet.
• coordinating cations on the exterior side of each of the tetrahedral and the octahedral surface sheets are attached to a fluorescer molecule, with the proviso that the fluorescer molecule attached to the coordinating cations on the exterior side of the tetrahedral surface sheet is not identical to the molecule attached to the coordinating cations on the exterior side of the octahedral surface sheet.
• the fluorescer molecule is preferably attached to the
• coordinating cations on the external surface of the octahedral surface plane and is not preferably attached to coordination cations of non-exterior tetrahedral or octahedral plane or on the interior side of the surface sheets.
• excitation of ultra violet (UV) and/or yellow light and emission of light in the blue region of the spectrum is
• emission in the brown/red (550-700 nm) region of the spectrum is preferred.
• the excitation in the UV region and emission outside the UV region, or even emission in the form of heat, is preferred. Further specifications of absorption and emission
• fluorescer ratio is between 1:0.001 and 1:0.1, more preferably between 1:0.01 and 1:0.05, most preferably about 1:0.018.
• any chemical reaction or series of reactions wherein a fluorescer molecule is attached selectively to coordinating cations on the exterior plane of either the tetrahedral or the octahedral surface plane of an asymmetric clay can be used to prepare the bipolar particulate fluorescer according to the present invention.
• the reaction is selective to only one of the exterior planes.
• selective is meant that more than 50% of the total fluorescer molecule is present on one of the exterior planes, preferably more than 75%, more preferably than 80%, still more preferably than 90%, even more preferably than 95%, or even more than 99%.
• the chemical reaction or series of reactions wherein the same fluorescer molecule attached to coordinating cations of both the surface sheets, viz octahedral and tetrahedral, are therefore not preferred.
• the particle has two spatially distinct exterior faces having distinct surface characteristics. It is envisaged that by selecting specific fluorescer molecule having specific group, and
• the invention provides a process for preparing a bipolar particulate fluorescer which precursor is an asymmetric 1:1 or 2:1:1 clay particle having alternating tetrahedral and octahedral sheets terminating with a
• octahedral sheet at another external surface plane comprising the steps of contacting the precursor with a mineral acid, adding a fluorescer molecule to the mixture, adjusting the pH of the solution in a range_between 2 to 10, heating the mixture to a temperature of 50 - 150 °C, and separating the solid product comprising bipolar particulate fluorescer.
• a pressure vessel is preferred.
• the raw clay is treated with a mineral acid preferably hydrochloric acid.
• the hydrochloric acid is used in a concentration range of 0.01 (N) to 1 (N) , preferably about 0.1 (N) .
• the clay particle with the acid is then stirred. The stirring is typically done for 10-60 minutes, preferably about 30 minutes.
• the fluorescer molecules are then added in a concentration of 0.001 to 30 percent of the total weight of the dispersion, preferably 0.01 to 5%.
• the pH of the system is preferably adjusted to the desired pH as explained below.
• the reaction may be conducted in two different pH ranges.
• the clay particle is treated with 0.1 N HC1.
• NaOH is added to increase the pH above 8.
• this dispersion mixture is heated, preferably for 4-8 hours, preferably about 6 hours with stirring at 70-90°C, preferably about 80°C.
• the solid product comprising the bipolar particulate fluorescer particles is separated after washing it repeatedly with water and solvent.
• the solvent is preferably a ketone, most preferably acetone.
• the kaolinite clay particle is treated with 0.1 N HC1. Then alkali is added to adjust the pH to between 2 to 4. After that the desired fluorescer molecule is added. Then this solution mixture is heated for 4-8 hours, preferably about 6 hours with stirring at 70-90°C, preferably about 80°C. Finally the solid product comprising the bipolar particulate fluorescer particles is separated after washing it repeatedly with water and solvent, preferably acetone. Heating the solution
• the solution After adding the fluorescer molecule and adjusting the pH of the dispersion, the solution is preferably heated for between 1 to 10 hours, preferably 4 to 8 hrs and more preferably about 6 hrs while stirring at 50°C to 150°C preferably 70°C to 90°C more preferably at 80°C.
• the dispersion mixture is preferably centrifuged to obtain the bipolar fluorescer particle as residue. Then it is preferably washed with water and subsequently with a ketone solvent (e.g. acetone) . After that it is dried in an oven to get the final product.
• a ketone solvent e.g. acetone
• fluorescer molecule is attached to the coordinating cations of the octahedral sheet preferable by covalent bonding.
• the particulate fluorescer made by this process has different wettability characteristics for two external surface planes.
• the invention provides a bipolar particulate fluorescer coated with a coating material having a refractive index in the range of 1.3 to 2 preferably of 1.3 to 1.6.
• the selected coating material is preferably transparent to light in the wavelength range of 200 to 800 nm and is
• This coating material preferably has a surface energy between 10-200 ergs/cm 2 , preferably between 20 - 50 ergs/cm 2 .
• coating materials are aluminum hydroxide, fatty acid, silicone, polysaccharides and their derivatives.
• the coating process may be carried out either in an aqueous or a non-aqueous solvent.
• the preferred solvents include water, acetone, ethanol and/or hexane .
• the process of making coated fluorescer particles preferably comprises the following steps:
• aqueous or non-aqueous medium and optionally heating it to 25°C to 100°C to get the coating material dissolved in the solvent
• the coated particle made from this process has uniform coating and uniform surface behaviour.
• the present invention provides a detergent composition for improved whiteness of the fabrics and textiles.
• the particulate fluorescer is preferably delivered to the fabric by a detergent composition.
• This detergent composition is made by usual way of making any detergent formulation.
• the emission wavelength of the fluorescer molecule is
• wavelength of the fluorescer molecule is preferably between 290-400 nm and more preferably between 345-355 nm.
• This molecule is selected from the classes of Stilbene
• Tinopal CBSXTM Tinopal CBSXTM, Benzthiazaole
• the particulate fluorescer is preferably incorporated in 0.01% to 10% by weight of the detergent composition. More preferred amount is from 0.1% to 5% by weight of the composition.
• surfactants may also be included in the detergent composition.
• zwitterionic surfactant or combinations thereof may be used in the detergent composition.
• the surfactants of the surfactant system may be chosen from the surfactants described well known textbooks like "Surface Active Agents" Vol. 1, by Schwartz & Perry, Interscience 1949, Vol. 2 by Schwartz, Perry & Berch, Interscience 1958, and/or the current edition of
• the surfactant is preferably incorporated to 50% by weight of the detergent composition, preferably at least 10% or even more than 15%, while generally less than 40% and even less than 30%. Although any concentration of surfactant may be used, suitable concentration is in the range of 0.5 to 3 grams per liter of the water after dissolution of the detergent
• composition into 10-60 liters of water for washing.
• builders may also be included in the detergent composition.
• Preferred builders include alkali metal
• the builder is preferably incorporated in 10% to 50% by weight of the detergent composition.
• Preferably 0% to 10% minors may also be incorporated in the detergent composition. These minors include perfumes, colours, pH modifier etc.
• the detergent composition is suitable for any kind of laundry applications like hand-wash, machine-wash (with horizontal axis or vertical axis) and for any kind of fabric like cotton, polyester, polycotton etc.
• detergent composition is meant a composition for treatment or cleaning of fabric and includes compositions for use during main wash or for use during the rinse stage e.g. fabric
• sunscreen / skin brightening elements are preferably selected from p-Aminobanzoic acid, padimate 0TM, Phenylbenzimidazole sulphonic acid, cinoxate, Dioxybenzone, Oxybenzone, Homosalate, Menthyl anthranilate, Octocrylene, Octyl methoxycinnamate, Octyl salicylate, Sulisobenzone,
• the preferred emission depends on the intended use.
• the emission is preferably in the form of heat (or even as simple reflection of the radiation) .
• excitation in the range of 360-500nm is preferred; emission, the emission may be in any part of the visible light spectrum, preferably between 400 and 700 nm, more preferably between 400 and 600 nm, still more preferably between 400 and 550 nm.
• the excitation is preferably in the range of 360-500nm and emission is preferably in the range 500-700 nm, more preferably 550-700 nm, most preferably 600-700 nm.
• the excitation is preferably at a wavelength in the range of 200-400 nm and emission in any form, including visible light (360-800nm) and/or heat.
• the particulate fluorescer is preferably incorporated in 0.05% to 10% by weight of the skin composition. More preferred amount is from 0.1% to 10%; most preferred amount is from 0.2 % to 5 % by weight of the composition.
• Useful inorganic sun-blocks may also be additionally used in the compositions of the present invention. These include, for example, zinc oxide, iron oxide, silica, such as fumed silica, and titanium dioxide.
• the total amount of sun block that is preferably incorporated in the composition according to the invention is from 0.1 to 5% by weight of the composition.
• a combination of particulate fluorescer and inorganic sun-block may be incorporated for better protection of skin which will cover a wide range of the UV and visible light spectra.
• the skin cosmetic composition preferably comprises a
• composition cosmetically acceptable vehicle to act as a diluent, dispersant or carrier for other materials present in the composition, so as to facilitate their distribution when the composition is applied to the skin.
• concentrations of these in vanishing cream base is generally from 5%-25% by weight C 1 2-C20 fatty acids and 0.1%-10% by weight fatty acid soap.
• emollients emollients, solvents, humectants, thickeners and powders.
• Examples of each of these types of vehicles can be used singly or as mixtures of one or more vehicles.
• compositions of the present invention may comprise a wide range of other optional components like antioxidants, binders, biological additives, buffering agents, colorants, thickeners, polymers, astringents, fragrance, humectants, opacifying agents, conditioners, exfoliating agents, pH adjusters,
• compositions may be "leave ons", where the product is left to deliver actives/provide benefits on human substrate e.g. skin (including surfaces on face, hands, body, hair, lips, under arms) .
• Suitable leave-on compositions include skin creams, lotions, gels, hair treatment products, deodorants and
• Such personal care compositions also include "wash-off" products for cleaning surfaces of human body e.g. soaps, body wash, face wash, hand wash and shampoos.
• the Tinopal reacted particles were visible in fluorescence mode while the untreated clays were not visible.
• the results of image analysis are presented in table 1.
• the average grey scale intensity of the reacted particles is more than 150 while the background values are less than 10.
• Untreated clays had similar values as background.
• the higher intensity of the Tinopal-clay particles indicates the fluorescence of the particles while the intensity of the untreated particles being similar to the back ground indicates absence of fluorescence.
• FTIR transformed infrared
• the objective in this experiment is to determine whether the fluorescent molecule is bound to the clay surface. If the fluorescent molecule is attached with Kaolinite it would result in a shift of the spectra which is a reflection of the micro-environment of the fluorescent molecule.
• the fluorescence spectrum exhibits that pure Kaolinite as expected does not have any fluorescence peak.
• the max of the molecular Tinopal species is at 432 nm while the Tinopal-clay has a max at 460 nm.
• Binding of a fluorescer ligand to a substrate is usually accompanied by a spectral shift. The shift in the spectra in this case suggests that the fluorescer is bound to the clay surface.
• a fluorescer molecule has a larger dipole moment in the excited state. Upon excitation the clay surface can either relax or reorient the dipole moment, which lowers the energy of the exited state. This lowering of energy results in shifting of the emission peak to longer wavelengths.
• Example 4 Characterization of Tinopal-clay deposited fabrics: Effect of fabric specificity Swatches (10X1 Ocm) of cotton (WFK10A) and polyester (WFK 30A) were loaded with 0.5ml of 0.00432 gms/litre of Tinopal CBSX and dried at ambient temperature in the dark. Swatches (10X1 Ocm) of cotton (WFK10A) and polyester (WFK 30A) were loaded with 0.5ml of 20 gms/litre of particulate fluorescer of Example 1 and dried.
• the fluorescence spectroscopes of the fabrics were determined using a Shimadzu RF 5301 PC fluorescence spectrophotometer by placing the fabrics onto a black template at an angle of 45 degree .
• Reflectance spectroscopy of the particles provides information regarding the back scattering of the particles which is an important parameter governing photo protection involving particles. This experiment was performed by spreading 5 mg of the particles onto a circular area of 1.5 cm radius and
• Example 6 Skin cream formulation with Tinopal clay particles
• Example 7 Efficacy of the Tinopal reacted clay with respect to the unreacted clay in terms of their UV protection
• Amigel Alban Muller International
• a vegetable based gelling agent derived from the yeast of Sclerotium rolfsii is used as a gelling agent.
• 2% w/v of gellent was slowly added to deionized water under magnetic stirring and it was stirred for 1-2 hours to develop enough viscosity.
• Tinopal reacted clay was capable of absorbing much more UV light than unreacted clay or base gel.
• Example 8 Coating process for bipolar fluorescer particles In non-aqueous solvent
• O.Olg of cellulose acetate was dissolved in 25 ml of acetone. 0. lg of particulate fluorescer was dispersed by mixing it in a vortex mixer. The solution was then stirred until all the acetone was volatilized. The coated particles were dried in an air oven at 40°C for 1 hour.
• 1% to 5% by weight of starch solution was prepared at 80°C. lg of particulate fluorescer was dispersed in 30 ml of the starch solution. The solution was then stirred for about 1 to 2 hour. After that the solution was cooled down to room temperature (25°C) . The coated particles were separated from the solution by centrifugation and then dried it in an air oven at 40°C for an hour.
• Example 9 Comparison of retention between molecular fluorescer versus fluorescer particle of the invention.
• Tinopal CBSX is taken as the molecular fluorescer for this purpose and Tinopal CBSX reacted clay particle is the fluorescer particle of the invention (see above for synthesis) .
• ImL of lOgpL Tinopal CBSX solution is dosed over hydroxyapatite tile (15mm x 15mm x 5 mm; ex IFGL Bio Ceramics Ltd 15.; a common model tooth surface) and kept for 1 min. 19mL of deionized water is added to this and rinsed for 1 min in shaker bath (Orbital Shaking Incubator Model ACM-22065-I) at 180 rpm. The rinsing step is repeated twice with 20 mL of deionized water each. Then reflectance spectroscopy is used to determine the concentration of Tinopal CBSX on the tiles.
• Tinopal CBSX is removed after rinsing .
• ImL of 5gpL Tinopal CBSX-clay suspension is dosed over hydroxyapatite tile and kept for lmin. 19mL of deionized water is added to this and rinsed for 1 min in shaker bath (Orbital Shaking Incubator Model ACM-22065-I) at 180 rpm. The rinsing step is repeated twice with 20 mL of deionized water each. Then reflectance spectroscopy is used to determine the concentration of Tinopal CBSX on the tiles.

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• 2010
  • 2010-08-30 WO PCT/EP2010/062616 patent/WO2011036029A1/en active Application Filing
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