CN1280486A - Use of substantially amorphous cellulose nanofibrils associated with a polyhydroxylated compound in cosmetic formulations - Google Patents

Use of substantially amorphous cellulose nanofibrils associated with a polyhydroxylated compound in cosmetic formulations Download PDF

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CN1280486A
CN1280486A CN98811698A CN98811698A CN1280486A CN 1280486 A CN1280486 A CN 1280486A CN 98811698 A CN98811698 A CN 98811698A CN 98811698 A CN98811698 A CN 98811698A CN 1280486 A CN1280486 A CN 1280486A
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fibril
cellulose
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C·威尔莱敏
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Rhodia Chimie SAS
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Rhone Poulenc Chimie SA
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    • 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
    • A61K8/11—Encapsulated compositions
    • 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
    • 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
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/027—Fibers; Fibrils
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/731—Cellulose; Quaternized cellulose derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
    • 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
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • 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
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/413—Nanosized, i.e. having sizes below 100 nm
    • 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
    • A61K2800/48—Thickener, Thickening system
    • 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
    • A61K2800/54—Polymers characterized by specific structures/properties
    • A61K2800/542—Polymers characterized by specific structures/properties characterized by the charge
    • A61K2800/5422—Polymers characterized by specific structures/properties characterized by the charge nonionic
    • 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
    • A61K2800/54—Polymers characterized by specific structures/properties
    • A61K2800/542—Polymers characterized by specific structures/properties characterized by the charge
    • A61K2800/5424—Polymers characterized by specific structures/properties characterized by the charge anionic
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q9/00—Preparations for removing hair or for aiding hair removal
    • A61Q9/04—Depilatories

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Molecular Biology (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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  • Dermatology (AREA)
  • Cosmetics (AREA)

Abstract

The invention concerns the use of substantially amorphous cellulose nanofibrils having a crystalline index not more than 50 % in dispersible dry form associated with at least a polyhydroxylated (polyOH) organic compound, as texturizing and/or reinforcing agent in cosmetic formulations. The invention further concerns the resulting cosmetic formulations.

Description

Receive the purposes of fibril in cosmetic formulations with the bonded amorphous cellulose basically of at least a polyhydroxylated compound
The present invention relates to be form, the degree of crystallinity that can be scattered in the cosmetic formulations be less than or equal to 50%, amorphous cellulose is received the purposes and the thus obtained preparation of fibril basically.
The present invention relates more specifically to be used for the novel thickening agent and/or the reinforcing agent of cosmetic formulations.
In meaning of the present invention, term " cosmetic formulations " is meant at appendix I (any cosmetics of those types of narrating in the cosmetics range specification table that are called the European catalogue No.76/768/EEC cosmetics catalogue, on July 25th, 1976.
Cosmetic composition generally is formulated into the multiple product type, described product type or be applied to hair, as foams, gelinite (particularly hair caring glue), conditioner, be used for forming hair or promote combing and/or the preparation of loosening, or rinsing preparation, or be applied to skin, as handwashing liquid and body lotion, regulate the product of moisture of skin, clean skin milk, cleansing composition, the depilatory product, the cream or the washing liquid that are used for sunlight and protection from ultraviolet rays, maintenance frost (care creams), prevent and treat the preparation of acne, the local analgesia agent, mascara, foundation cream or fingernail oil type cosmetic formulations, desire to be applied to the product of lip or other mucosa, lip pomade, other preparation of fancy soap class solid composite and same type.
Usually, except that one or more active component at intended application, the more general chemical compound of what is called that these various preparations also comprise some, the concrete effect of these chemical compounds are to give it with long-time stability (as antiseptic) and/or special pharmaceutical preparation form (as gel, cream, milk or washing liquid type).They generally are surfactant and/or dispersant, stabilizing agent, emulsifying agent, humidizer, gellant or thickening agent.
Representative as general stable and/or thickening agent can should be mentioned that hydrocolloid such as Xanthane-Rhodicare that Acusol772 Acusol771, fermentation obtain especially Glue and succinoglycan such as Rh é ozan , cellulose derivative such as hydroxypropyl cellulose or carboxymethyl cellulose or guar gum and derivant thereof, they are used alone or in combination.
One of purpose of the present invention provides a kind of novel thickening agent and/or the reinforcing agent that have advantageous property concerning the rheological characteristic of preparing cosmetics compositions.More specifically, it is a kind ofly to receive the reagent of fibril based on amorphous cellulose basically, and the described degree of crystallinity of receiving fibril is less than or equal to 50%, and the described fibril of receiving is and can be scattered in the dry-form that contains in the medium.
Native cellulose generally always is filamentous.These fibrils are known materials, and they have been proposed to be used in the structure of improving their residing media particularly.Under the situation of fluid media (medium), they improve its viscosity, even its rheological characteristic.
Receive various sources of fibril, as derive from plant, antibacterial, fungus or amebicide.
In Plant fiber or cell wall, receive and generally have strong association force between the fibril.In described cell wall, can distinguish the main secondary wall that obtains in by timber, be the primary wall of representative instance with the parenchyma.Parenchymatous example is made up of beet pulp, Citrus (Fructus Citri Limoniae, Fructus Citri tangerinae orange, grapefruit) and most fruits and vegetable.In secondary wall, these fibrils are height-oriented sheet arranges, thereby forms indissociable fiber.They are extremely several microns aggregate form of tens nanometers usually.These aggregations are made up of the monomer fibril that can not loosen in the process that homogenizes of carrying out under not causing broken condition.
In meaning of the present invention, the cellulose fibril of being considered is to be essentially amorphous cellulose to receive fibril (CNF), preferably derives from the cell with primary wall.
Cellulose of the present invention receive fibril advantageously by at least about 80%, the cell acquisition formed of preferred 85wt% primary wall at least.
Amorphous basically cellulose that the present invention uses is received fibril thereby preferably have at least 80% cell with primary wall.
Opposite with secondary wall cellulose fibril discussed above, cellulose is received the diameter of fibril and mostly is several nanometers most, and it is the filament outward appearance, confirms and can loosen at described filament of the stage of homogenizing.
Their preferred sections are about 2 to about 10nm, and more preferably about 2 to about 4nm.
In meaning of the present invention, the fibril of being considered of receiving is the amorphous basically fibril of receiving of what is called, and is opposite with so-called crystalline state fibril.
Term " amorphous state basically " is meant that the degree of crystallinity of fibril received of qualification is less than or equal to 50%.According to concrete replacement scheme of the present invention, this degree of crystallinity is 15 to 50%, is more preferably less than 50%.
It is particularly advantageous with respect to the crystalline state microfibril that these amorphous basically celluloses are received fibril, its reason is that they are dispersible in water-bearing media, give the rheological characteristic of its highly special shear thinning type, and to heat or in medium, be stable with macroion load.Receiving fibril hanging down this height effectiveness that shows under the quantity by cellulose, in fact is by being caused in the fabulous rheological characteristic behavior that they showed aspect pour point and the shear thinning ability.
According to preferred version of the present invention, cellulose used in the present invention is received the fibril surface and is loaded with separately or mixes carboxylic acid and the acidic polysaccharose that exists.
Term " carboxylic acid " is meant common carboxylic acid and salt thereof.These acid are preferably selected from alduronic acid, more especially galacturonic acid and/or Portugal (grape) alduronic acid.
As acidic polysaccharose, can should be mentioned that pectin, more especially comprise polygalacturonic acid.These acidic polysaccharoses can be the form of mixtures with hemicellulose.
In fact, these fibrils of receiving with area load thing are not to obtain with sour and simple mixing of polysaccharide by the described fibril of receiving.And relate to the close combination received between this chemical compound of two types that method directly obtained of fibril by being used for preparing.This is that promptly described acid can not separate from fiber fully with polysaccharide, but remains on the surface of described fiber because the type of this preparation method is such, thereby gives its extremely special performance.Importantly requiring emphasis, separate fully from these acid and/or polysaccharide as then receiving fibril, and then add described acid and/or polysaccharide to acquisition like this receiving in the fibril, is to reproduce these identical performances.
More particularly, the objective of the invention is to that these celluloses are received fibril uses with the redispersible form of solid with at least a polyhydroxylated (many OH) organic compound.
Thereby, theme of the present invention be with at least a polyhydroxylated (many OH) but organic compound combine, degree of crystallinity be less than or equal to 50%, that be the drying dispersing morphology, basically amorphous cellulose receive fibril in cosmetic formulations as the purposes of thickening agent and/or reinforcing agent.
In meaning of the present invention, thickening agent is the reagent that has stable and thickening power in comprising its cosmetic composition.
Within the scope of the invention, reinforcing agent is to improve this reagent is added into the mechanical performance of compositions wherein with wet or dry-form reagent.
In addition, also observe compositions of the present invention even in comprising the water-bearing media of surfactant, also can be used as emulsifying agent and stabilizing agent.
Being dry-form uses the cellulose that combines with at least a (many OH) to receive fibril, be favourable economically not only with regard to for example storing and transporting, and also be favourable from the angle of technology, because use the redispersible form of described drying can prepare aqueous suspension with high-load dried active material.
In cosmetic composition, use this cellulose that is dry redispersible form to receive fibril, unexpectedly confirm it is favourable in many aspects as thickening agent and/or reinforcing agent.
For example, under the concrete condition of the cosmetic formulations of the dermal application that is used for the cream type, for example, notice that the skin penetration amount of described preparation significantly increases.In the application process of these preparations, do not observe on the surface of skin " phenomenon of soaping ".At last, cellulose of the present invention is received fibril and is given very softish skin sense, and the effect of tension and protection skin surface is arranged, and also has humidification.
About the concrete condition of hair caring preparation, add the cellulose combine with at least a polyhydroxy organic compound and receive fibril and strengthened the moulding effect.
The use of the compositions that described and dissolved water-soluble, film-forming polymers or dispersive water-insoluble film forming polymer form causes producing a kind of film forming matter, this material shows the good adhesion with cutin base thing, has both also nonadherent cosmetics sensations of non-greasy.
The water-soluble, film-forming polymers that the present invention uses can be:
-have a synthetic water-soluble, film-forming polymers of low glass state conversion temperature Tg (preferably being less than or equal to 20 ℃);
-or natural origin (polysaccharide that is obtained by cellulose), its Tg are generally more than or equal to 40 ℃ water-soluble, film-forming polymers.
For example can should be mentioned that poly-(vinyl alcohol), hydroxyethyl-cellulose, the plain ether of universal fibre, guar gum or carob in cosmetics.
Equally, opposite with general thickening agent, cellulose of the present invention is received fibril does not influence the cosmetics performance of the preparation that has added them.Advantageously, do not observe depression effect (curbing effect) or loss of gloss, and resistance to water is not seen decline to some extent for described compositions.
Have again, confirmed the flavouring effect.
As mentioned above, receive the described cellulose that carries out in the fibril process at the preparation cellulose and receive combining of fibril and at least a (many OH), but have the advantage that makes that they can the drying dispersing morphology be prepared.The potential advantage of the cosmetic formulations that this yes preparation is corresponding is particularly because high-load active component and provide bigger elasticity for preparation.
Described polyhydroxylated (many OH) organic compound is preferably selected from carbohydrate and derivant and polyhydric alcohol.
As the representative of these carbohydrates, can should be mentioned that C especially 3-6, preferred C 5Or C 6Ring or straight chain monosaccharide, as fructose, mannose, galactose, sucrose, talose, gulose, allose, altrose, idose, Arabic candy, xylose, lyxose and ribose, oligosaccharide, as maltose and lactose, polysaccharide, as starch, cellulose, xanthan gum and guar gum, and their fat derivant, as sucrose fatty acid ester, alcohol sugar is as Sorbitol and mannitol, acid sugar as Portugal (grape) saccharic acid, alduronic acid and galacturonic acid and salt thereof and ether sugared as the cellulose methyl-, ethyl-, carboxymethyl-, ethoxy-and hydroxypropyl-ether.
About polyhydric alcohol, they can be glycerol, tetramethylolmethane, propylene glycol, ethylene glycol especially and/or gather (vinyl alcohol).
Receiving fibril and using under the concrete condition of carbohydrate and derivant thereof with being amorphous cellulose basically, the more special carboxylation cellulose that should be mentioned that, preferred carboxy methylation cellulose, the latter also represents with CMC.
The polymer that cellulose is made up of the glucose monomer unit: the degree of polymerization can change in wide region.Described carboxylation group is introduced wherein by monoxone and fibrin reaction in itself known mode.Its substitution value is then corresponding to the carboxymethyl group number of every glucose unit.Theoretical maximum substitution value is 3.These carboxylation celluloses were considered to have high substituted degree at its substitution value numerical value greater than 0.95 o'clock, and its substitution value is considered to have low degree of substitution when being lower than this numerical value.
Thereby, be suitable for be wherein the carboxylation content of cellulose more than or equal to 5wt% and be less than or equal to the high-quality carboxy methylation cellulose of 30wt%, or carboxylation content of cellulose 10 to 30wt% low quality carboxy methylation cellulose more especially wherein.
For identical quality, confirm in addition can further reduce it with respect to receiving the ratio of fibril by the carboxy methylation cellulose that tends to select to have high substituted degree.
This fibrid element is received fibril and the cellulosic mixture of carboxylation and is disclosed in especially among application PCT/FR9701291 (publication number WO98/02487) and the PCT/FR9701290 (publication number WO98/02486).
This polyhydroxylated (many OH) organic compound is preferably selected from carboxymethyl cellulose, HANSHENGJIAO, Guar beans, Sorbitol, sucrose and its mixture.
The cosmetic formulations that the present invention obtained is preferably with the many OH of (many OH) * 100/[()+(CNF)] weight ratio is more than or equal to 5% and be less than or equal to 50%, be preferably greater than or equal 5% and be less than or equal to 30% and comprise that polyhydroxylated chemical compound (one or more) and cellulose receive fibril.
According to favourable form of the present invention, they comprise that the cellulose that is with carboxymethyl cellulose with high degree (CMC) combining form receives fibril, (CMC) * 100/[(CMC)+(CNF)] weight ratio is more than or equal to 5% and be less than or equal to 25%.
Also the polyhydroxylated derivant of another kind can be combined with CMC, described derivant is for instance as sucrose, propylene glycol or poly-(ethylene glycol).Under this concrete condition, (CMC) * the many OH of 100/[() Amount to+ (CNF)] then significantly decline of weight ratio.
About receiving the quantity of fibril and (many OH) by the cellulose that the present invention uses, obviously they depend on institute at pharmaceutical dosage form and/or the purpose effect of cosmetic formulations, for example, humidification or as in the preparation that loses hair or feathers to the protective effect of epidermis.
Thereby the quantity that is adopted with liquid preparation compares, and the quantity of the thickening agent of the present invention that exists in cream types of drug preparation form is bigger.
Cellulose receive the quantity of mixture of fibril and many OH preferably adjust to make described receive fibril exist ratio be about cosmetic formulations 0.1 to 20wt%, more preferably about 0.15 to 5wt%.
As an illustration, it is 0.11 to 40% that the cellulose that can advise for the preparation of preparation cream type is received the concentration range of fibril and (many OH), can advise that concentration is 0.11 to 10% for the preparation of preparation kind of liquid.For the many OH of (many OH) * 100/[()+(CNF)] the suggestion numerical value of weight ratio is for more than or equal to 5% and be less than or equal to 50%.
Cellulose of the present invention is received outside the polyhydroxylated compound of the redispersible solid composite of fibril divided by last qualification, also can comprise at least a additive that helps that is selected from following material:
General formula is (R 1R 2N) chemical compound of COA, wherein R 1Or R 2Identical or different, represent hydrogen or C 1-10, preferred C 1-5Alkyl, A are represented hydrogen, C 1-10, preferred C 1-5Alkyl or radicals R `1R `2N, wherein R `1Or R `2Identical or different, represent hydrogen or C 1-10, preferred C 1-5Alkyl; With
Anion, nonionic or amphoteric surfactant, these two kinds are helped additive to be used alone or as a mixture.
As the representative of these surfactants, can should be mentioned that those that below this paper, point out especially.
Be to be noted that these help additive with (many OH) but for example the fortifying fibre element that is used in combination of carboxymethyl cellulose receive the shear thinning performance of fibril behind redispersion.
About (R 1R 2N) chemical compound of COA type, the preferred chemical compound that comprises two amide functional groups that uses.The preferred carbamide that uses is as helping additive.
According to specific embodiments of the present invention, these amorphous basically celluloses receive that the solid redispersible composition of fibril comprises carboxylation cellulose with high substituted degree and as at least a chemical compound that is selected from surfactant that helps additive.
When cellulose of the present invention is received fibril and one or more polyhydroxylated chemical compound and above-mentioned when helping additive to combine with one or more, polyhydroxylated chemical compound and help content of additive more than or equal to receiving fibril, polyhydroxylated chemical compound and help the 5wt% of weight of additive and be less than or equal to 30wt%.
The fibril of receiving used in the present invention can be obtained by disclosed the whole bag of tricks in the document.
Can should be mentioned that disclosed method in European patent application EP-A-726356 especially.
Wherein to the serosity that derives from plant with primary wall promptly through processed, by ensiling preservation or the wet pulp liquid such as the beet pulp of taking off pectin through part, after extracting sucrose in advance, carry out this processing procedure by approach well known.More particularly, acid or the alkalescence extraction of the first step is adopted in this processing, when finishing, it reclaims first kind of solid residue, also can carry out for second step to described first kind of solid residue under alkali condition subsequently extracts, reclaim second kind of solid residue, the two kinds of residues that are made of cellulosic material that merge wash bleaching then, the third solid residue that obtains when bleaching stage finishes dilutes, then the suspension that obtains is diluted, to reach amount of dry matter is 2 to 10wt%, at last, carry out homogenization step, comprising at least one circulation that described diluted suspension is carried out.
This homogenization step is corresponding to any mixing, grinding operation or any high mechanical shearing operation, make described cell suspending liquid one or the hole by minor diameter repeatedly subsequently, make described suspension stand pressure drop and the high speed shear effect of 20mPa at least, carry out high deceleration subsequently and impact.The homogenize of described cellulose suspension obtains by passing for several times, and the number of times that passes can be 1 to 20 time, is preferably 2 to 5 times, till obtaining steady suspension.
About the detailed rules in each stage of this processing, can be with reference to the description of above-mentioned application.
Just now Xu Shu method makes the fibril of receiving can obtain to maintain on its surface carboxylic acid and/or polysaccharide.
Under the cellulose that the present invention uses is received the situation of fibril, carry out homogenize before the stage or after carrying out the homogenize circulation the general for example the polyhydroxylated chemical compound of carboxylation cellulose type be incorporated in the above-mentioned preparation rules.
Be to be noted that this alternative method form is disclosed among the international patent application No.PCT/FR 97/01291 (publication number is WO 98/02487), if necessary can be with reference to the document.
The cellulose that is added with polyhydroxylated chemical compound is received the preparation method of fibril, in the phase I, comprise, add the polyhydroxylated chemical compound that at least a portion considers in the fibril suspension and also can add and help additive (one or more) to receiving through at least one homogenize circulation.Then, in second stage, carry out the suspension after the interpolation like this is carried out the exsiccant stage.
In fact, can according to three kinds of selectable forms add the polyhydroxylated chemical compounds of at least a portion and may exist help additive (one or more):
-can when the homogenize stage finishes and preferably, in described suspension, add through behind at least one concentration step,
-or when the described homogenize stage finishes, in described suspension, add through before at least one concentration step at described suspension, or
-adding before the stage or therebetween in homogenize, at this moment described serosity has passed through the circulation at least one homogenize stage.
Described enriching stage (one or more stage) can be undertaken by any general means, till the dry extract that obtains about 35wt%.More particularly, described dry extract content is 5 to 25wt%.
Before proper drying stage, advantageously to forming through spissated suspension, promptly by extruding or pelletize.Certainly the temperature of drying stage is chosen as the decomposition that makes restriction carboxylic acid, acidic polysaccharose, hemicellulose, polyhydroxylated chemical compound and (as suitably) help additive.More especially 30 to 80 ℃, be preferably 30 to 60 ℃.
The drying stage that is undertaken by universal means makes the moisture that keeps minimum 3wt% with respect to prepared solid weight.More especially, the weight of the water that is kept is 10 to 30wt%.This embodiment does not allow above receiving the fibril limit of redispersion fully.
The resulting cellulose of mixture that obtains by above-mentioned rules by redispersion in water is received the fibril suspension, and advantageously it is for being at least 1s -1The viscosity numerical value that shear rate showed corresponding to the undried stage and neither contain polyhydroxylated chemical compound do not contain yet the cellulose that helps additive receive the fibril suspension viscosity numerical value at least 50%.
Certainly, amorphous basically area load material (preferably being loaded with acid) is arranged, with polyhydroxylated chemical compound and also can receive fibril to be used to the cosmetic formulations that the present invention obtains with the cellulose that helps additive to combine with at least a blended form of carrier compatible with hair, skin or sun-proof application.
Term " compatible with the application on hair and/or skin " is meant that at this this carrier does not destroy the outward appearance of hair and/or skin or it is had a negative impact, skin and/or eyes and/or scalp is not produced stimulation.
Another theme of the present invention is a cosmetic formulations, but wherein as thickening agent and/or reinforcing agent adopt amorphous basically, be drying dispersing morphology and the bonded cellulose of at least a polyhydroxylated compound defined above and receive fibril.These preparations also can comprise the additive of above definition.
Cosmetic formulations of the present invention preferably contains the mixture of a kind of carrier or several carriers, and its concentration that exists in described preparation is about 0.5 to 99.5%, is more preferably 5 to 90%.
The carrier compatible with preparation of the present invention for example comprise in spray, foams, tonic, gel, shampoo or the agent of emulsion-type hair care employed those.
Certainly, suitably the selection of carrier depend on described preparation at concrete application.(for example conditioner, the agent of emulsion-type hair care) is unsuitable for the preparation that will rinse after using remaining to be remained on the carrier that is suitable in the applied lip-deep preparation (for example spray, foams, washing liquid, tonic or gel).
Thereby the carrier that can use is simple or complicated, and can comprise the product that is usually used in hair, skin or sun care preparations preparation in a large number.
Thereby can be also can add solubilizing agent with dissolving or disperse used active component such as C 1-6Alcohol and composition thereof, the particularly water of ethanol, isopropyl alcohol or propylene glycol and composition thereof.
Advantageously, receive fibril with the bonded cellulose of at least a polyhydroxy organic compound and show excellent compatibility with the alcohols solubilizing agent.These celluloses are received the architecture advances performance of fibril and are not affected adversely in water/pure medium.
Equally, they have more in what is called and still keep its performance in the rodent medium, and the described promptly very tart medium of rodent medium that has more for example has the cream of 'alpha '-hydroxy acids, or alkaline medium, as depilation preparation or permanent wave solution.
The embodiment 2 and 3 that provides below this paper has narrated with the bonded cellulose of at least a many OH and received the favourable character that fibril shows in cosmetic applications.
CNF by the present invention's preparation confirms that advantageously for the cosmetics medium be fabulous structural agent, and keeps their performance not change in time.Their thickening ability is greater than microcrystal-state cellulose.
Also can mix one or more in mutually at the fat that contains the separated attitude of water with CNF of the present invention and be selected from softening agent in the following material: mineral oil is (as Marcol 82 ), vegetable oil or derive from marine oil, halogenated hydrocarbons, linalool, ester (as the tetradecanoic acid isopropyl esters) and polysiloxanes (particularly encircle dimethicone and dimethicone and derivant and hexamethyldisiloxane) and derivant or the mixture compatible with cosmetic applications.
When described cosmetic formulations is the form of spray, nourishing washing liquid, gel or foams, preferred solvent comprise water, ethanol, Y 7175 derivant, and composition thereof.The solvent that in these mixture, uses mutually miscible or immiscible.Aerosol spray and foams also can use any propellant that can produce the product that is fine spraying of homogeneous or foam form.For instance, can should be mentioned that dimethyl ether, propane, normal butane or iso-butane.
Under cosmetic formulations desired to be used for situation that surface local uses, described carrier must have the good comfort energy, with all other component compatibility and be fully harmless.
These carriers can be a variety of forms, emulsion, foams or spray type etc.For example, the carrier that is the emulsion form comprises polysiloxanes Bao Shui, Water-In-Oil, oil-in-water and polysiloxanes bag O/w emulsion.These emulsions have covered very wide range of viscosities, for example under 25 ℃ from 100 to 20000mPa.s.These emulsions also can be disengaged with the spray form by using the pressurization of mechanical pump class device or propellant gas.
The form that these carriers also can be foams is disengaged.
Except above-mentioned carrier, cosmetic formulations of the present invention also can comprise be used for disperseing, the surfactant of emulsifying, dissolving or the stable particularly softening or all cpds that the requirement of wettability the subject of knowledge and the object of knowledge is used.They are anionic, nonionic, cationic, amphoteric ion type or amphoteric.As the example of these chemical compounds, more special should be mentioned that:
-anion surfactant is as alkyl sulfonate esters, alkyl sodium sulfate ester, alkyl sodium sulfate amide and saturated or unsaturated fatty acid salt;
-non-ionic surface active agent is as polyoxyalkylene alkylphenol, glucamide (glucosamides), glucamide (glucamide) or by the deutero-glycerol amide of N-alkylamine, polyoxyalkylene C 8-22Aliphatic alcohol, the product that obtains by oxirane and hydrophobic compound condensation or the product that obtains by expoxy propane and propylene glycol condensation, amine oxide, alkyl polyglycoside and their polyoxyalkylene derivative, C 8-20Fatty acid amide and ethoxylated fatty acid, amide, amine or amido amine (amidoamines);
-both sexes or amphoteric ionic surfactant, as those of betaine-type, as the amphoteric derivatives of two propionates of condensation product, cocoyl both sexes acetate (cocoamphoacetates) and cocoyl both sexes diacetate, alkyl both sexes propionate or the both sexes of betanin, sulfobetaines, amido alkyl betaine and sulfobetaines, alkyl sulfobetaines, fatty acid and protein hydrolysate or alkyl polyamine.
Also can there be conditioner.
Wherein can should be mentioned that, with title season hydroxyethyl-cellulose and those of more well-known synthetic source, as season hydroxyethyl-cellulose-2, season hydroxyethyl-cellulose-7 and season hydroxyethyl-cellulose-10, the cationic derivant of polysaccharide, as the cocodimonium hydroxyethyl-cellulose, melon ear hydroxypropyl trimonium chloride or hydroxypropyl melon ear hydroxypropyl trimonium chloride, or non-volatile polyorganosiloxane ramification, as amodimethicone, Cyclomethicone or water insoluble and be nonvolatile organopolysiloxane, as oil, resin or glue, for example diphenyl SKTV-M.
Described cosmetic formulations also can comprise the polymer with filming performance, and they have been used for the fixative effect.These polymer exist with 0.01 to 10% concentration usually, are preferably 0.5 to 5%.They are following type preferably: the copolymer of the copolymer of polyvinylpyrrolidone, polyvinylpyrrolidone and methyl methacrylate, polyvinylpyrrolidone and vinyl acetate, poly-(ethylene glycol terephthalate)/poly-(ethylene glycol) copolymer or sulfonation p-phthalic acid copolyester polymer.
Described cosmetic formulations also can comprise the content that shields and be about 0.01 to 10wt%; preferred about polymeric derivative of 0.1 to 5wt% is as cellulose derivative, be grafted to polyvinyl ester, polyvinyl alcohol, sulfonation p-phthalic acid copolyester polymer, ethoxylation monoamine or polyamines and ethoxylated amine polymer on the polyolefin backbone.
Also wetting agent can be incorporated in the described cosmetic formulations.These reagent especially can should be mentioned that glycerol, propylene glycol, carbamide, collagen, gelatin and softening agent for instance, described softening agent is selected from alkyl monoglyceride, alkyl glycerol diester or triglyceride usually, as oil or their hydroderivating thing, mineral oil or paraffin oil, glycol, fatty acid ester or the polysiloxanes that extracts from plant and vegetable.
Also add one or more aromatic, coloring agent and/or opacifier such as pigment in these chemical compounds usually.
For protecting skin and/or hair not to be subjected to sunlight and UV radiation damage; can in these preparations, add sunscreen; but the described radiating organic compound of sunscreen strong absorption UV or be the inorganic particle of nano-particle state is as zinc oxide, titanium dioxide or cerium oxide.
The active component that has the cosmetics performance merely as vitamin, 'alpha '-hydroxy acids, botanical derivative or marine product extract can be incorporated into comprise the CNF that is used for the treatment of purpose as described in the preparation.
Equally, CNF is the preferred thickener of depilation preparation, as the medium based on thioglycol acid calcium.
Appendix VII according to the cosmetics regulations, generally antiseptic is incorporated in these compositionss described antiseptic such as p-Hydroxybenzoate, sodium benzoate or the general any chemical reagent that prevents antibacterial or mycete propagation in cosmetic composition with 0.01 to 3wt% quantity.
At last, described cosmetic formulations also can comprise multiviscosisty or gel polymer, as the Garbopol that is sold by Goodrich The Acusol772 Acusol771 of type, cellulose derivative, as hydroxypropyl cellulose or carboxymethyl cellulose, guar gum and derivant thereof, as hydroxypropyl guar gum, JaguarHP for example , carob, thorn pod tannic extract or cassia gum, HANSHENGJIAO is as Rhodicare , succinoglycan, alginate, carrageenin, chitin derivative or any other have the polysaccharide of thickening power.
Obviously, the estimation of the selection of these described so-called generalization compounds and their respective amount and the type of designed preparation are that gel, cream, emulsion, spray, washing liquid etc. and required agreeable property are directly related.These adjust in fact just cosmetics allotment personnel's routine operation problem.
Cosmetics of the present invention can be favourable be used for hair caring, sun-proof, skin protection and cosmetic field.
The embodiment that below provides only is used for illustration purpose, is not to mean limitation of the present invention.
Embodiment 1
The preparation cellulose is received the mixture of fibril and carboxymethyl cellulose
With substitution value is that 1.2 carboxymethyl cellulose (derives from the CMC Blanose of Aqualon 12M8P) be dissolved in the distilled water.
Subsequently described solution is added to and comprise 2.3% cellulose and receive disperseing in the mother solution with the fibril of receiving of 14000 rev/mins of pre-homogenize (every 100g dispersion liquid 1 minute) of fibril with Ultra-Turrax.The mixture that merges coagulates oar with 1000 rev/mins with loosing and stirred 30 minutes.
The addition of carboxymethyl cellulose is that cellulose is received the 15wt% of fibril and carboxymethyl cellulose gross weight.
Subsequently described mixture is poured in the dish, dry then, promptly being dried to solids content under 40 ℃ in the aerofluxus baking oven is 92%, measures the water yield by the Karl-Fischer method and monitors.
The mixture crossed of mill-drying sieves through 500 μ m then subsequently.
It is that the ratio redispersion of 0.43wt% is in distilled water that resulting powder is received fibril and carboxymethyl cellulose with cellulose.Coagulating oar with loosing stirred 5 minutes or 30 minutes with 1000 rev/mins.This dispersion liquid is used for following embodiment.
Embodiment 2
In pure medium with the behavior of the blended CNF of CMC
For this reason, the CNF/CMC mixture that will prepare in embodiment 1 under shear action is scattered in the water, adds or do not add the alcohol of being considered then.
So the composition of two kinds of moisture/pure media of preparation is listed among the following table I.The viscosity of these media and control media (water) estimated in the viscometer of use Brookfield LVT type.
The results are shown in the Table I.
Table I
CNF 85/15 CMC 0.43% that adds
Viscosity, Pa.s 10% ethanol 10% propylene glycol Distilled water
??1s -1 ????0.8 ??0.85 ????0.60
??100s -1 ????0.04 ??0.04 ????0.035
Embodiment 3
With the behavior of the blended CNF of CMC in acidity or alkaline medium
The CNF mixture of embodiment 1 preparation is incorporated into to be buffered in pH be in 4 or 9 the water.With respect to containing 1% buffer medium that has added the microcrystal-state cellulose of CMC, estimate the rheological behaviour of this medium.In Table II, provided the viscosity that changes in time.
Table II
Thickening agent Viscosity, Pa.s 1s -1?????????????????????????????100s -1It pH=4 pH=9 pH=4 pH=9
0.43% adduction CNF85/15CMC 1 day 5 days ????0.35 ????0.35 ????0.55 ????0.65 ????0.015 ????0.015 ????0.02 ????0.02
1% is added with the microcrystal-state cellulose of CMC 1 day 5 days ????0.02 ????0.02 ????0.03 ????0.03
Notice the CNF for preparing by the present invention confirms it is the fabulous thickening agent of cosmetics medium, and can keep its performance not change in time.Their thickening ability is greater than microcrystal-state cellulose.
Embodiment 4
Cosmetic formulations of the present invention
These preparations comprise the CNF/CMC mixture of embodiment 1 preparation.
1) has the cream of 'alpha '-hydroxy acids
Component wt%
The A phase
□cetearyl?alcohol????????????????????8
diethylamine hexadecanyl phosphate 2
eicosylene/PVP copolymer 2
neopentanoic acid octyl dodecanol ester 10
Mirasil DM300: dimethicone 1
The B phase
□CNF/CMC?????????????????????????????0.2
propylene glycol 5
water is in right amount to 100
The C phase
'alpha '-hydroxy acids 5
The D phase
triethanolamine 1.8
The E phase
The antiseptic is an amount of
2) be used for the slight remover of health
Component wt%
The A phase
water is in right amount to 100
The B phase
□CNF/CMC???????????????????????????????1
The C phase
lauryl magnesium sulfate 8.5
cocoyl sodium sarcosinate 1.0
55% sodium hydroxide 0.50
diethylamine lauramide 2.0
stearic acid 1.0
Geropon AC78 : cocoyl ethylenehydrinsulfonic acid sodium 13
The D phase
gathers (oxirane) 20
The E phase
The antiseptic is an amount of
aromatic and coloring agent are an amount of
3) depilatory solution
Component wt%
The A phase
□CNF/CMC???????????????????????????????0.5
water is in right amount to 100
The B phase
propylene glycol 5
The C phase
mineral oil and lanolin alcohol 5
polysorbate80 and acetic acid cetyl ester and acetylation 2
Lanolin alcohol
PEG-100 stearate and tristerin 2
The D phase
thioglycol acid calcium 5
calcium hydroxide 6
The E phase
antiseptic, coloring agent, aromatic are in right amount to 100
Embodiment 5
With the behavior of the blended CNF of CMC as the film-forming polymer dispersant reinforcing agent
The purpose of present embodiment is to show that the fibril of receiving that makes up with at least a (many OH) also can be used as reinforcing agent.
Use the Rhodopas DS1003 film forming latex of selling by Rhodia (aqueous dispersion of acrylate copolymer) to carry out this test, the glass transition temperature Tg of described latex is 12 ℃, film-forming temperature TMF is lower than 5 ℃, the solids content of described dispersion liquid is 50%, and the particle size of described latex is 0.1 μ m.The pH of described dispersion liquid approximates 8.
The cellulose that will be in embodiment 1 obtains from dry powder is received the fibril dispersion liquid and is used for present embodiment.
The preparation that can be used as moisture nial polish base material
The following two kinds of preparations that limit of preparation based on DS 1003 latex:
F1 (contrast): 30wt%1003 latex+70wt% water is benchmark in the total formulation weight;
F2 (the present invention): the CNF+69wt% water that 30wt%1003 latex+1wt% obtains in embodiment 1 is benchmark in the total formulation weight.
The pH of medium is adjusted to 7.
The viscosity that F1 showed is less than 10mPa.s, and the viscosity of F2 is about 4500mPa.s.Use the viscometer (3,10 rev/mins of rotors) of Brookfield LVT type to estimate described viscosity.
The results are shown in the Table III.
Table III
F1????????????????F2
The film forming outward appearance is the film forming semi-transparent film not
Persoz hardness (second)-49
Adhesion 00 (do not have and separate)
Persoz hardness is determined according to NFT standard 30-016: under the room temperature dry surpass 8 days after onboard three differences measure hardness.Each measured value is corresponding to the meansigma methods of 3 measurements.What the result showed is that the pendulum vibration is from 12 ° of times (in second) that damping to 4 ° angle in angle is required.
" hardness " of this time with film increases.
Adhesion to matrix is determined by the cross-hatching test according to iso standard 2409: prepare film on steel plate.Described test comprise use cutter with 2 row at interval 6 vertical lines of 1mm draw reticule, blended rubber band this grid of tearing.Grading range (does not have and separates) to 4 (separating about 50% grid) from 0.
Preparation F2 comprises the CNF that contains additive of the present invention, thereby corresponding to the material that can be used as moisture paint base.The preparation F2 that is obtained is stable.Having pseudoplastic said preparation is easy to be coated in the substrate.Described film has good adhesion and better elastic, and it feels that both non-greasy was also non-glued.

Claims (16)

  1. With at least a polyhydroxylated (many OH) but organic compound is bonded, degree of crystallinity is less than or equal to 50%, be the drying dispersing morphology, basically amorphous cellulose receive fibril in cosmetic formulations as the purposes of thickening agent and/or reinforcing agent.
  2. 2. the purposes of claim 1 is characterized in that described polyhydroxylated (many OH) organic compound is selected from sugar and derivant and polyhydric alcohol.
  3. 3. the purposes of claim 2 is characterized in that described sugar is preferably selected from C 3-6Ring-type or straight chain monosaccharide, oligosaccharide, polysaccharide and derivative of fatty acid thereof such as sucrose fatty acid ester, pure sugar, sour sugar and ether sugar.
  4. 4. each purposes in the claim 1 to 3 is characterized in that described polyhydroxylated (many OH) organic compound is preferably selected from carboxymethyl cellulose, HANSHENGJIAO, guar gum, Sorbitol, sucrose and composition thereof.
  5. 5. each purposes in the claim 1 to 4 is characterized in that degree of crystallinity is 15 to 50%, preferably less than 50%.
  6. 6. each purposes in the claim 1 to 5 is characterized in that described cellulose receives fibril and have at least 80% cell that has a primary wall.
  7. 7. each purposes in the claim 1 to 6, it is characterized in that described cellulose receive fibril from preferred by the cell of forming at least about 80% primary wall.
  8. 8. as each purposes in the claim 1 to 7, it is characterized in that described cellulose receives fibril and be loaded with independent or blended carboxylic acid and acidic polysaccharose.
  9. 9. each purposes in the claim 1 to 8 is characterized in that described polyhydroxylated compound and sodium cellulosate fibril are with the many OH of (many OH) * 100/[()+(CNF)] weight is more than or equal to 5% and be less than or equal to 50% and mix.
  10. 10. the purposes of claim 9 is characterized in that institute (many OH) * many OH of 100/[()+(CNF)] weight ratio is more than or equal to 5% and be less than or equal to 30%.
  11. 11. each purposes in the claim 4 to 10 is characterized in that described cellulose receives the carboxymethyl cellulose (CMC) of fibril and high substituted degree with (CMC) * 100/[(CMC)+(CNF)] weight ratio is more than or equal to 5% and be less than or equal to 25% and mix.
  12. 12. each purposes in the aforementioned claim, it is characterized in that adjusting cellulose receive the quantity of fibril and (many OH) mixture make described receive the fibril usage ratio be cosmetic formulations 0.1 to 20wt%.
  13. 13. the purposes of claim 12 is characterized in that the described usage ratio of receiving fibril is 0.15 to 5wt%.
  14. 14. each purposes in the aforementioned claim is characterized in that described cellulose receives fibril and (many OH) and mix with at least a additive that helps, the described additive that helps is selected from:
    General formula is (R 1R 2N) chemical compound of COA, wherein R 1Or R 2Identical or different, represent hydrogen or C 1-10, preferred C 1-5Alkyl, A are represented hydrogen, C 1-10, preferred C 1-5Alkyl or R `1R `2N, wherein R `1Or R `2Identical or different, represent hydrogen or C 1-10, preferred C 1-5Alkyl; With
    Anion, nonionic or amphoteric surfactant, these help additive to be used alone or as a mixture.
  15. 15. the purposes of claim 14 is characterized in that polyhydroxylated chemical compound and helps content of additive to receive fibril, polyhydroxylated chemical compound and to help the weight of additive be that benchmark is more than or equal to 5wt% and be less than or equal to 30wt%.
  16. 16. cosmetic formulations, it is characterized in that comprising as each qualification in the claim 1 to 13 of thickening agent and/or reinforcing agent blended with at least a polyhydroxylated compound, but amorphous cellulose that is the drying dispersing morphology is received fibril basically, and as suitably, described cellulose is received fibril and is also mixed with the additive of at least a claim 14 or 15.
CN98811698A 1997-10-21 1998-09-22 Use of substantially amorphous cellulose nanofibrils associated with a polyhydroxylated compound in cosmetic formulations Pending CN1280486A (en)

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AU9269998A (en) 1999-05-10
FR2769836B1 (en) 2000-03-10
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AU746945B2 (en) 2002-05-09
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EP1024782A1 (en) 2000-08-09

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