Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/34—Alcohols
  • A61K8/347—Phenols
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q13/00—Formulations or additives for perfume preparations
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23K—FODDER
  • A23K20/00—Accessory food factors for animal feeding-stuffs
  • A23K20/10—Organic substances
  • A23K20/111—Aromatic compounds
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
  • A23L27/20—Synthetic spices, flavouring agents or condiments
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
  • A23L27/20—Synthetic spices, flavouring agents or condiments
  • A23L27/204—Aromatic compounds
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
  • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
  • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
• • 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
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
  • A61P17/00—Drugs for dermatological disorders
• • 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
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
  • C07C45/78—Separation; Purification; Stabilisation; Use of additives
  • C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
  • C11B9/00—Essential oils; Perfumes
  • C11B9/0061—Essential oils; Perfumes compounds containing a six-membered aromatic ring not condensed with another ring
• • 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
  • C11D3/50—Perfumes

Definitions

• the present invention relates to a process for preparing a composition comprising essentially a vanillin and ethyl vanillin compound.
• Vanillin or 4-hydroxy-3-methoxybenzaldehyde is a widely used product in many fields of application as a flavor and / or fragrance.
• vanillin is widely consumed in the food and feed industry but it also has applications in other areas such as for example, pharmacy or perfumery. It follows that it is a consumer product.
• Vanillin is very often associated with ethylvanillin or 3-ethoxy-4-hydroxybenzaldehyde because it is known that the presence of a small amount of ethyl vanillin makes it possible to exalt the vanishing properties and / or organoleptic properties of vanillin.
• Said compound is in the form of a white powder which has a melting point measured by differential scanning calorimetry of 60 ° C. ⁇ 2 ° C. different from that of vanillin and ethylvanillin respectively of 81 ° C. ⁇ 1 ° C. and 76 ° C ⁇ 1 ° C.
• FIG. 1 represents three curves corresponding to the different X-ray diffraction spectra of the new vanillin and ethyl vanillin compound, vanillin and ethyl vanillin.
• Another feature of said compound is that its X-ray diffraction pattern does not undergo significant change during prolonged storage.
• the 3 curves obtained are normally superimposed.
• curve corresponding to the X-ray diffraction spectrum obtained after a storage of 2 months is shifted by 5,000 shots / sec and that obtained after a storage of 5 months is shifted by 10,000 shots / sec.
• Figure 2 shows that there is no evolution of the compound of the invention after prolonged storage. There is no modification of the specific lines of the new vanillin / ethyl vanillin / ethylvanillin compound of vanillin / ethylvanillin molar ratio of 2
• Another characteristic of said compound is that it is a not or very little hygroscopic compound such as vanillin and ethyl vanillin.
• the hygroscopicity of said compound is determined by measuring its mass change after being held for 1 hour, at 40 ° C under air at 80% relative humidity.
• Said compound adsorbs less than 0.5% by weight of water, its content is preferably between 0.1 and 0.3% by weight of water. Said compound remains perfectly solid.
• this compound has good organoleptic properties and has a high aromatic power significantly higher than that of vanillin.
• the compound as defined and which is hereinafter referred to as “new compound” has specific properties which result in a lower caking ability compared to a vanillin and ethyl vanillin composition obtained by simple dry mix.
• the particular properties of the compound based on vanillin and ethyl vanillin as previously described are related to two parameters namely the molar ratio between vanillin and ethyl vanillin and the fact that there is a co-crystallization between vanillin and ethylvanillin in a specific crystalline form characterized by its melting point and its X-ray diffraction pattern.
• One of the routes of access to said compound resides in a process which consists in effecting the melting of the mixture of vanillin and ethylvanillin implemented in a molar ratio of 2 and then cooling the molten mixture by lowering the temperature to 50 °. C ⁇ 1 ° C, then the temperature is maintained until solidification of the mixture.
• Cooling is advantageously carried out in the absence of any agitation.
• the vanillin and ethylvanillin employed are charged in a molar ratio of 2, separately or in mixture, and the mixture is heated to a temperature which is chosen between 60 ° C. and 90 ° C. and which preferably between 70 ° C and 80 ° C.
• the molten product is transferred into any container, for example a stainless steel tray, which will easily recover the product after solidification.
• This container is preheated between 70 and 80 ° C before receiving the molten mixture.
• the molten mixture is cooled to a temperature of 50 ° C. ⁇ 1, by regulating the cooling temperature by any known means.
• the cooling is preferably carried out in the absence of any agitation.
• the solidified mixture obtained can then be shaped according to various techniques, including grinding.
• cooling to a temperature below 50 ° C. ⁇ 1, for example 20 ° C. makes it possible to accelerate the solidification process of the molten mixture, but the crystallization is heterogeneous with the coexistence of different crystalline phases, some of which are unstable at ambient temperature or very hygroscopic. This results in an important caking storage of vanillin - ethylvanillin mixture crystallized under such conditions.
• FIG. 3 represents the X-ray diffraction spectrum of an equimolar vanillin-ethyl vanillin mixture, melted at 70.degree. ° C, then crystallized by rapid cooling to 20 ° C.
• FIG. 4 shows the evolution of this spectrum over a storage period of 3 weeks at 22 ° C., proving that the phases thus crystallized are unstable and evolve rapidly, causing the caking of the product.
• This product has a melting point of 48 ° C ⁇ 1 and is very hygroscopic: in 1 hour at 40 ° C and under air at 80% relative humidity, it adsorbs more than 4% water by weight and becomes deliquescent.
• the objective of the present invention is to provide a method that is transposable on an industrial scale, making it possible to obtain essentially the new vanillin and ethyl vanillin compound of vanillin / ethyl vanillin molar ratio of 2.
• Another object of the invention is that it leads to a composition comprising it which has the improved properties as mentioned above.
• a process for the preparation of a composition essentially comprising a compound based on vanillin and ethyl vanillin in a vanillin / ethyl vanillin molar ratio of 2, characterized in that it comprises a co-granulation operation of vanillin and ethylvanillin implemented in powder form and in such quantities that the vanillin / ethyl vanillin molar ratio is at least equal to 2, conducted at a temperature between 50 ° C and 57 ° C, followed by an operation to bring the temperature of the resulting composition to room temperature.
• composition essentially comprising a compound based on vanillin and ethyl vanillin means a composition comprising at least 80% by weight of a mixture of the new vanillin / ethyl vanillin compound of the vanillin / ethyl vanillin molar ratio. 2 and vanillin: vanillin represents less than 20% by weight of said mixture.
• new vanillin / ethyl vanillin compound is meant the compound in anhydrous form and its hydrates.
• Co-granulation is understood to mean an operation which consists, from vanillin and ethyl vanillin powders, of obtaining the novel compound of the invention in the form of granules.
• granulation is meant the shaping of a powder in the form of granules. According to the invention, it has been found that the new vanillin and ethyl vanillin compound is easily obtained by this co-granulation method.
• vanillin and ethyl vanillin are used in the following proportions:
• the proportions are advantageously as follows:
• a homogeneous mixture of vanillin and ethyl vanillin powders is firstly made.
• said powders are charged separately or in mixture in a mixer-granulator and subjected to stirring.
• the stirring conditions are chosen so that there are no significant shears.
• the stirring conditions advantageously vary between 0.2 and 1 m / s at the end of the blades.
• This temperature is defined as being lower than the melting temperature of the new vanillin and ethyl vanillin compound which, measured by differential scanning calorimetry, is 60 ° C ⁇ 2 ° C.
• the co-granulation temperature is advantageously chosen between 50 and 57 ° C, preferably between 50 and 55 ° C.
• the mixture of vanillin and ethyl vanillin powders is brought from room temperature to the co-granulation temperature which is chosen as previously described.
• ambient temperature is generally meant a temperature of between 15 and 25 ° C.
• the temperature rise is preferably carried out progressively, for example 1 ° C. every 3 minutes.
• the mixture is stirred at this temperature for a sufficient time in order to obtain the transformation of the reagents into the expected new compound.
• the duration of this isothermal stage is determined as a function of the co-granulation temperature chosen.
• the duration of the plateau advantageously varies between 5 minutes and 1 hour and, preferably, between 20 minutes and 40 minutes. It should be noted that the upper limit is not critical but for reasons of productivity, a duration of at most 1 hour is preferably chosen.
• the composition obtained is cooled to a temperature below 40 ° C.
• the composition is allowed to cool with stirring and under an inert atmosphere to a temperature below 40 ° C, preferably to a temperature below 35 ° C.
• the lower limit of the cooling temperature is advantageously ambient temperature.
• a composition comprising the new vanillin / ethyl vanillin compound is recovered.
• a mixer which is advantageously a mixer with plowshares or a ribbon mixer (s).
• This mixer is advantageously provided with a double envelope in order to ensure the various heat transfers by circulating a coolant in the double jacket.
• the heat transfer fluid may be water maintained at a higher temperature, for example from 2 to 5 ° C., at the chosen co-granulation temperature or any other coolant, for example a silicone oil.
• the temperature of the coolant in this case the water is generally chosen at a lower temperature, for example 2 to 5 ° C at the chosen cooling temperature.
• composition obtained according to the process of the invention comprises at least 80% by weight, preferably at least 90% by weight of a mixture of the new vanillin / ethyl vanillin compound and vanillin.
• composition obtained comprises less than 20% by weight, preferably less than 10% by weight of other crystalline phases of the vanillin / ethyl vanillin phase diagram and possibly vanillin: this mixture is hereinafter referred to as "other crystalline phases”. .
• compositions obtained can comprise:
• compositions of the invention include:
• the vanillin is less than 20% by weight, preferably less than 14% by weight of said mixture.
• mixtures obtained can comprise:
• the preferred mixtures have the following composition:
• composition obtained is in the form of granules whose size varies, for example, between 200 and 10,000 ⁇ and preferably between 500 ⁇ and 1 ⁇ .
• the particle size expressed by the median diameter (dso) varies from 200 ⁇ to 1,000 ⁇ and is preferably between 500 ⁇ and 800 ⁇ .
• the median diameter is defined as being such that 50% by weight of the particles have a diameter greater than or less than the median diameter.
• the grinding operation can be carried out in conventional equipment such as a vane mill, a pin mill, a granulator.
• the composition of the invention has a flowability index after 24 hours of storage at 40 ° C. under air at 80% relative humidity under a normal stress of 2400 Pa varying between 0.degree. , 05 and 0.6.
• a small amount of water may be present in the nitrogen. It may represent from 1 to 5% by weight of nitrogen, preferably from 2 to 3% by weight of nitrogen.
• the humidification of the nitrogen flow can be ensured by bubbling in the water.
• the mixing of the powders is started under wet nitrogen, then the temperature is gradually increased and when the latter is greater than or equal to 44 ° C. and less than 49 ° C. dry nitrogen is introduced.
• dry nitrogen is meant a stream of nitrogen comprising less than 0.5 g, preferably less than 0.3 g of water per kg of nitrogen.
• the temperature of the composition obtained is brought to room temperature as previously described.
• composition obtained has an X-ray diffraction spectrum which comprises the characteristic lines as illustrated in FIG.
• a whiter color composition is obtained and more quickly because the isothermal stage can be shortened. For example, following a rise in temperature under dry nitrogen, an isothermal plateau at 52 ° C for a duration of 2 hours is desirable. If the rise in temperature is carried out under wet nitrogen, an isothermal plateau at 52 ° C for a period of 30 minutes is sufficient.
• the process of the invention is applicable to vanillin and ethyl vanillin produced by any chemical synthesis, regardless of the starting substrate. It is also suitable for the vanillin obtained according to the biochemical processes, in particular microbiological fermentation processes, in particular ferulic acid.
• the invention does not exclude the use of one or more excipients with the composition of the invention
• the amount of excipient (s) can be very variable and it can represent from 0.1 to 90% of the weight of the final mixture.
• the excipient may be introduced, in whole or in part, at the end of the preparation of the composition of the invention or during the preparation of the composition of the the invention.
• the total amount of excipient (s) may be introduced during the preparation of the composition of the invention or added at the end of the preparation of the composition of the invention. It is also possible to split the quantities used during preparation or after preparation,
• the excipient is added by dry mixing with the composition of the invention obtained.
• the excipient may be incorporated in the process for obtaining the composition of the invention, for example during the step of co-granulation of the vanillin and ethyl vanillin mixture.
• excipients which can be used which are given without limitation are given below.
• a first type of excipients are fatty substances.
• fatty acids optionally in the form of salts or esters.
• the fatty acids used are generally long-chain saturated fatty acids, that is to say having a chain length of between about 9 and 21 carbon atoms such as, for example, capric acid, lauric acid , tridecyl acid, myristic acid, palmitic acid, stearic acid, behenic acid.
• acids are in salified form and mention may in particular be made of calcium or magnesium stearate.
• fatty acid esters mention may in particular be made of glyceryl stearate, isopropyl palmitate, cetyl palmitate and isopropyl myristate.
• esters of glycerol and of long-chain fatty acids such as glycerol monostearate, glycerol monopalmitostearate, glycerol palmitostearate, ethylene glycol palmitostearate, polyglycerol palmitostearate, palmitostearate of glycerol can be mentioned more specifically.
• polyglycol 1500 and 6000 glycerol monolinoleate; optionally mono- or diacetylated glycerol esters of long-chain fatty acids such as monoacetylated or diacetylated monoglycerides and mixtures thereof; the semisynthetic glycerides.
• a fatty alcohol whose carbon atom chain is between about 16 and 22 carbon atoms such as, for example, myristyl alcohol, palmityl alcohol, stearyl alcohol.
• polyoxyethylenated fatty alcohols resulting from the condensation with ethylene oxide in a proportion of from 6 to 20 moles of ethylene oxide per mole, of linear or branched fatty alcohols having from 10 to 20 carbon atoms such as, for example, coconut alcohol, tridecanol or myristyl alcohol.
• waxes such as microcrystalline waxes, white wax, carnauba wax, paraffin wax.
• sugars such as, for example, glucose, sucrose, fructose, galactose, ribose, maltose, sorbitol, mannitol, xylitol, lactitol, maltitol; inverted sugars: glucose syrups and sucroglycerides derived from fatty oils such as coconut oil palm oil, hydrogenated palm oil and hydrogenated soybean oil; sucroesters of fatty acids such as sucrose monopalmitate, sucrose monodistearate and sucrose distearate.
• fatty oils such as coconut oil palm oil, hydrogenated palm oil and hydrogenated soybean oil
• sucroesters of fatty acids such as sucrose monopalmitate, sucrose monodistearate and sucrose distearate.
• polysaccharides mention may be made, inter alia, of the following products and their mixtures:
• starches derived in particular from wheat, maize, barley, rice, cassava or potato, native, pregelatinized or modified, and more particularly native corn starches rich in amylose, pregelatinized maize starches, modified corn starches, modified waxy maize starches, pregelatinized waxy maize starches, modified waxy maize starches, in particular OSSA / octenylsuccinate sodium starch,
• cellulose its ethers, especially methylcellulose, ethylcellulose, methylethylcellulose, hydroxypropylcellulose; or its esters, in particular carboxymethylcellulose or carboxyethylcellulose optionally in soded form,
• gums such as carrageenan gum, Kappa or Iota carrageenan, pectin, guar gum, locust bean gum, and xanthan gum, alginates, gum arabic, acacia gum, agar -agar,
• a maltodextrin having a degree of hydrolysis measured by "equivalent dextrose” or D.E less than 20 and preferably between 5 and 19 and more preferably between 6 and 15 is chosen.
• flour especially wheat flour (native or pregel); starches, especially potato starch, Toloman starch, cornstarch, cornflour, sago or tapioca.
• gelatin preferably having a jelly strength measured with a 100, 175 and 250 Bloom gelometer. It can come either from the acid treatment of pork and ossein skins, or the alkaline treatment of cattle and bone skins.
• the invention does not exclude the addition of an additional amount of vanillin or ethyl vanillin.
• composition of the invention can be used in many fields of application, inter alia, in the food and pharmaceutical field, and in the perfume industry.
• a preferred field of application for the implementation of the composition of the invention is that of biscuit and pastry, and more particularly:
• the basic elements present in the mixtures intended for the aforementioned industries are the proteins (gluten) and the starch which are most often brought by the wheat flour.
• ingredients such as sucrose, salt, eggs, milk, fatty substances, possibly chemical yeasts (sodium bicarbonate or other artificial yeasts) or organic yeasts and flours are added to the flour.
• composition according to the invention is carried out during manufacture, according to the desired product and is conducted according to the conventional techniques of the field in question (see in particular JL KIGER and JC KIGER - Modern Techniques of Biscuit, Pastry - Bakery industry and craft, DUNOD, Paris, 1968, Volume 2, pp. 231 and following).
• the composition of the invention is introduced into the fatty substances that are involved in the preparation of the dough.
• composition of the invention is introduced in an amount of 0.005 to 0.2 g per kg of dough.
• composition of the invention is quite suitable for use in the field of chocolate and whatever the form of implementation. work: chocolates in plates, chocolates of cover, fodder for chocolates.
• cocoa paste It can be introduced during conching, that is to say the mixing of the cocoa paste with the various ingredients, including flavorings, or after conching, by implementation in cocoa butter.
• composition of the invention is used according to the type of chocolate, at a rate of 0.0005 g to 0.1 g per 1 kg of finished product: the highest contents found in chocolate for cover.
• composition of the invention is the manufacture of sweets of all kinds: sugared almonds, caramels, nougats, boiled sweets, melting sweets and others.
• composition of the invention introduced depends on the more or less pronounced taste that is sought. Thus, the use doses can vary between 0.001% and 0.2%.
• composition of the invention is well suited for uses in the dairy industry and more particularly in flavored and gelled milks, desserts, yogurt, ice cream and ice cream.
• the aromatization is done by simple addition of the composition of the invention, in one of the mixing stages required during the preparation of the product.
• compositions to be used are generally low of the order of 0.02 g per 1 kg of finished product.
• composition of the invention in the food field is the preparation of vanillin sugar, that is to say the impregnation of the sugar with these, in a content of about 7 g expressed relative to to 1 kg of finished product.
• composition of the invention may also be used in various drinks and include, among others, grenadine and chocolate drinks.
• the composition of the invention may be implemented at a rate of 6 g per ton of butter.
• Another field of application of the composition of the invention is the animal feed, especially for the preparation of feed meal for calves and pigs.
• the recommended content is about 0.2 g per kg of flour to be flavored.
• composition of the invention can find other applications as a masking agent, for the pharmaceutical industry (masking the drug odor) or for other industrial products (of the rubber, plastic, rubber ...) .
• perfuming compositions are meant mixtures of various ingredients such as solvents, solid or liquid carriers, fixatives, various odorous compounds, etc., in which is incorporated the composition of the invention, which is used to provide various types of of finished products, the sought-after fragrance.
• Fragrance bases are preferred examples of perfuming compositions in which the composition of the invention can be advantageously used in a proportion of from 0.1% to 2.5% by weight.
• the bases for perfume can be used for the preparation of many scented products such as, for example, toilet waters, perfumes, aftershave lotions; toilet and hygiene products such as bath or shower gels, deodorant or antiperspirant products, whether in the form of sticks or lotions, talcs or powders of any kind; hair products such as shampoos and hair products of all types.
• scented products such as, for example, toilet waters, perfumes, aftershave lotions
• toilet and hygiene products such as bath or shower gels, deodorant or antiperspirant products, whether in the form of sticks or lotions, talcs or powders of any kind
• hair products such as shampoos and hair products of all types.
• composition of the invention is the field of soap. It can be used at a content of 0.3% to 0.75% of the total mass to be perfumed. Generally, it is associated in this application with benzoin resinoid and sodium hyposulphite (2%).
• composition according to the invention can find many other applications, in particular in air fresheners or any maintenance product.
• physico-chemical characteristics of the compositions of the invention are determined according to the following methods:
• the melting point of the composition of the invention is measured by differential scanning calorimetry.
• the measurement is carried out using a Mettler differential analyzer DSC822e under the following conditions:
• the temperature programming is started and the fusion profile is obtained on a thermogram.
• the melting temperature is defined from a thermogram produced under the preceding operating conditions.
• the onset temperature is selected: temperature corresponding to the maximum slope of the melting peak.
• the X-ray diffraction spectrum of the composition of the invention is determined using the X'Pert Pro MPD PANalytical device equipped with an X 'Celerator detector, under the following conditions:
• composition of the invention has the characteristic of less motter storage which is evidenced by the determination of the flowability index of the powder.
• the flowability of powders is a technical concept well known to those skilled in the art. For further details, reference may be made in particular to "Standard Shear Testing Technique for Particulate Materials Using the Jenike Shear Cell", published by "The Institution of Chemical Engineers", 1989 (ISBN: 0 85295 232 5).
• the flowability index is measured in the following manner.
• the flowability of the powders is measured by shearing a sample in an annular cell (marketed by D. Schulze, Germany).
• the shear points required to plot the flow of the sample are obtained for 4 normal stresses lower than the stress of the precision, typically 480 Pa, 850 Pa, 2050 Pa and 3020 Pa.
• the ratio between the normal stress in the principal direction and the cohesive force is a nondimensional number called "i, flowability index".
• Another series of measurements is performed with a cell that has been stored for 24 hours at 40 ° C and 80% relative humidity under a normal stress of 2400 Pa.
• Example 1 In the examples, the percentages mentioned are expressed by weight. Example 1
• VA vanillin
• EVA ethylvanillin
• a circulation of wet nitrogen is established in the mixer with a flow rate of 200 l / h.
• the humidification of the nitrogen stream is ensured by bubbling in water maintained at 40 ° C. so as to obtain 25 g of water per kg of nitrogen.
• the feed line between the water bath and the mixer is maintained at 45 ° C so as to avoid any condensation in the pipes.
• the temperature of the coolant circulating in the jacket is increased gradually so that the temperature of the powder mixture follows a ramp of + 0.3 ° C / min.
• the water bath moistening the flow of nitrogen is short-circuited so as to supply the mixer with a circulation of dry nitrogen (less than 0.5 g of water / kg of nitrogen).
• 15 g of Tixosil 365 silica are introduced into the mixer.
• the temperature of the product is raised from 49.5 ° C to 52 ° C to + 0.2 ° C / min and is then maintained at 52 ° C for 30 minutes.
• the heating of the coolant is then stopped and, by natural cooling, the temperature of the product is reduced to 30 ° C.
• the stirring and the circulation of nitrogen are stopped.
• the mixer is drained.
• the product is sieved at 800 ⁇ ; the passer is 56% by weight of the total mass.
• the refusal at 800 ⁇ is milled using a grinder Quadro Comill equipped with a grid of 800 ⁇ .
• the 2 fractions are then combined and the mixture is homogenized to give the final product.
• the melting point of the granules is determined by differential scanning calorimetry as previously described.
• the thermogram obtained has a main peak which corresponds to the new vanillin / ethyl vanillin compound.
• the melting temperature (Tonset) corresponding to the maximum slope of the peak is 59.5 ° C.
• the flowability index and the caking index, measured as previously described with the aid of an annular cell, are 5.70 and 0.09, respectively.
• the increase in the final co-granulation temperature makes it possible to eliminate the isothermal stage guaranteeing the complete transformation of the vanillin-ethyl vanillin mixture in the new compound.
• the growth of the granules is more important since, at the mixer outlet, the passing at 800 ⁇ represents only 27% of the total mass, which forces to grind 73% of the product.
• the product obtained After milling the refusal at 800 ⁇ and mixing the two fractions, the product obtained has a flowability index of 6.30 and a caking index of 0.10.
• Example 1 The procedure of Example 1 is repeated with the only difference that the 15 g of Tixosil 365 silica are replaced by 150 g of Roquette IT12 maltodextrin.
• the passing at 800 ⁇ represents 55% of the total mass.
• the product obtained After milling the refusal at 800 ⁇ and mixing the two fractions, the product obtained has a flowability index of 5.90 and a caking index of 0.12.
• a composition is prepared in the form of granules comprising 50% by weight of the granules prepared according to Example 1 and 50% by weight of Roquette IT6 maltodextrin.
• the mixing operation of about 5 minutes is carried out at room temperature under ambient air in the plow mixer with a rotation speed of 60 rpm.
• the mixture thus obtained has a flowability index of 8.80 and a caking index of 0.62.

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• 2010
  • 2010-02-24 FR FR1000747A patent/FR2956661B1/fr not_active Expired - Fee Related
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  • 2011-02-21 EP EP11705518A patent/EP2538802A1/de not_active Withdrawn
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