New granules based on sodium iminodisuccinate, their preparation processes and their uses in solid cosmetic compositions

Abstract

The present invention relates to a granule, comprising as components or consisting of: sodium iminodisuccinate, at least one alkylpolyglucoside, in which the alkyl chain is a carbon chain comprising from 4 to 20 carbon atoms, in particular 10 carbon atoms, said granule comprising a moisture content of 4.5 to 6%. (no figures)

Description

Title of the invention: New granules based on sodium iminodisuccinate, their preparation processes and their uses in solid cosmetic compositions Technical field

[0001] The present invention relates to novel granules based on sodium iminodisuccinate, their preparation processes and their uses in solid cosmetic compositions. State of the art

[0002] Sodium iminodisuccinate is a chelating agent widely used in the cosmetics industry and other sectors. It has the ability to form multiple bonds with a single metal ion, making it effective in neutralizing metal ions that can impair the stability and appearance of cosmetic products. Used as a stabilizing agent, it protects formulations from degradation due to metal ions present in water, helping to maintain the color, texture, and efficacy of products. Compared to other chelating agents, it is considered more environmentally friendly due to its biodegradability, and it is generally considered safe for use in cosmetic products, provided the concentration is appropriate. In addition to cosmetics, it is also used in other products such as detergents due to its chelating properties.

[0003] Alkyl polyglucosides, when used in granule form in the formulation of solid foaming products, have several advantages. Firstly, their handling and dosage are facilitated, which is essential to maintain the consistency of the formulation. In addition, granules offer better stability and a longer shelf life than liquid forms, which facilitates storage and transportation. Their incorporation into solid foaming products improves the efficiency of the foam produced and reduces packaging waste and the environmental impact associated with the transportation of liquid raw materials.In addition, dense granules offer additional benefits in an industrial setting, including reduced dust, making it easier to clean equipment and work areas, increased dosing accuracy for better quality control, and safer handling and storage, contributing to a healthier working environment. The cosmetics industry uses many surfactants in solid form, such as sodium stearate, sodium cocoyl sulfate, sodium lauryl sulfate, and sodium cocoyl isethionate.

[0004] The growing interest in waterless solid cosmetics, particularly foaming products certified according to the international COSMOS standard and with a high naturalness index, is explained by several factors. These products reduce water consumption and require less packaging, thus responding to environmental concerns and the "zero waste" trend. In addition, their increased concentration offers greater effectiveness and better value for money, while their practicality for travel and their alignment with a growing ecological awareness of consumers contribute to their appeal. Waterless cosmetics also make it possible to avoid the presence of preservatives in the compositions. The latter are likely to trigger skin sensitization or even an allergy.Preservatives are also responsible for the imbalance of the skin microbiome, as well as the disruption of the protective barrier of the dermis.

[0005] One of the problems to date is to find natural chemical compounds allowing the formation of granules intended for use in solid cosmetic compositions (without water).

[0006] One aspect of the present invention is to address the above problem and to use compounds having a very high naturalness index to form granules.

[0007] Another aspect of the invention is to provide a population of granules comprising particles based on sodium iminodisuccinate, in the form of stable powders, easily handled and adapted to the application for which said granules are intended.

[0008] Another aspect of the present invention is the use of the granules for formulating or preparing a solid cosmetic composition or a powder preparation to be dissolved in water.

[0009] Another aspect of the invention is to provide a cosmetic composition comprising such granules. Description of the invention.

[0010] The invention therefore relates to a granule, comprising as components or consisting of: - sodium iminodisuccinate, - at least one alkylpolyglucoside,

[0011] in which the alkyl chain is a carbon chain comprising from 4 to 20 carbon atoms, in particular 10 carbon atoms.

[0012] said granule comprising a humidity level of 4.5 to 6%.

[0013] The inventors have surprisingly discovered that it is possible to form a granule comprising sodium iminodisuccinate and an alkylpolyglucoside of stable manner, and that said granules are easily handled. In particular, it is unexpected that sodium riminodisuccinate acts as a heat-resistant bulking agent and avoids the caramelization process of the alkylpolyglucoside during the preparation process of said granule, in particular in a fluidized bed.

[0014] Sodium iminodisuccinate (C8H7NNa4O8, CAS: 144538-83-0) is a compound of the following formula:

[0015] [Chem.l] My My

[0016] It can be commonly produced from maleic anhydride and ammonia in the presence of a sodium hydroxide solution. This compound is the conjugate base of iminodisuccinic acid. It has four carboxylate functions, which form a neutrally charged compound with the aid of four sodium cations. It exists in the form of 3 epimers (R,R), (S,S) and (R,S). The present invention relates to granules formed solely by each of these 3 epimers, or mixtures of at least two of the epimers as described above. The present invention relates to granules comprising as components sodium (R,R) iminodisuccinate and an alkylpolyglucoside. The present invention relates to granules comprising as components sodium (S,S) iminodisuccinate and an alkylpolyglucoside. The present invention relates to granules comprising as components sodium (R,S) iminodisuccinate and an alkylpolyglucoside.The present invention relates to granules comprising as components sodium (R,R) iminodisuccinate, sodium (S,S) iminodisuccinate and an alkylpolyglucoside. The present invention relates to granules comprising as components sodium (R,R) iminodisuccinate, sodium (R,S) iminodisuccinate and an alkylpolyglucoside. The present invention relates to granules comprising as components sodium (S,S) iminodisuccinate, sodium (R,S) iminodisuccinate and an alkylpolyglucoside. The present invention relates to granules comprising as components sodium (R,R) iminodisuccinate, sodium (S,S) iminodisuccinate, sodium (R,S) iminodisuccinate and an alkylpolyglucoside. .

[0017] Alkylpolyglucoside is a polymer formed by acetals between glucoses and alkyl chains, and has structural similarities with glycolipids. It is produced from glucose and alcohol. It is a mild and biodegradable non-ionic surfactant. It is characterized by its degree of polymerization as well as by the length of the carbon chains. Its critical micelle concentration (CMC) is strongly influenced by the length of the alkyl chain relative to the number of glucoside groups. The value of said CMC decreases as the number of carbon atoms in the alkyl chain increases. It is relatively safe when ingested and has a very low degree of toxicity (median lethal dose (LD50) greater than 35 g / kg).

[0018] The expression “4 to 20 carbon atoms” means: 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 and 20 carbon atoms.

[0019] In a particular embodiment, the invention relates to a granule as defined above, comprising a single alkylpolyglucoside.

[0020] In a particular embodiment, the invention relates to a granule as defined above, comprising a mixture of alkylpolyglucosides, in particular comprising a mixture of two alkylpolyglucosides.

[0021] In a particular embodiment, the invention relates to a granule as defined above, in which the alkylpolyglucoside has a degree of polymerization of 1 to 5.

[0022] By "degree of polymerization from 1 to 5" is meant: from 1 to 1.2, from 1.2 to 1.4, from 1.4 to 1.6, from 1.6 to 1.8, from 1.8 to 2, from 2 to 2.2, from 2.2 to 2.4, from 2.4 to 2.6, from 2.6 to 2.8, from 2.8 to 3, from 3 to 3.2, from 3.2 to 3.4, from 3.4 to 3.6, from 3.6 to 3.8, from 3.8 to 4, from 4 to 4.2, from 4.2 to 4.4, from 4.4 to 4.6, from 4.6 to 4.8, from 4.8 to 5.

[0023] The term "heat-resistant filler" means a compound used to weight a preparation in order to give it volume without significantly changing its properties, and exhibiting resistance to thermal degradation up to a temperature between 100 and 170°C, thus ensuring its functionality under high-temperature processing or use conditions.

[0024] The expression "humidity level of 4.5 to 6%" means a humidity level: of 4.5 to 5%, of 5 to 5.5% and of 5.5 to 6%.

[0025] In a particular embodiment, the invention relates to a granule as defined above, comprising a crystallization initiator.

[0026] By "crystallization initiator" is meant a compound introduced into a fluidized bed process to promote or initiate crystallization. In particular, it makes it possible to provide nucleation sites from the beginning of the process to promote crystal formation, to adjust and refine the size of crystals during growth, to prevent particles from agglomerating and forming clumps, and to influence the rate of crystallization and the formation of specific crystalline phases.

[0027] In a particular embodiment, the invention relates to a granule as defined above, in which said crystallization initiator is chosen from precrystallized sodium iminodisuccinate, or at least one precrystallized alkylpolyglucoside.

[0028] By "precrystallized" is meant that the sodium iminodisuccinate or alkylpolyglucoside is in crystalline form with a size of the order of several hundred to a thousand micrometers.

[0029] In a particular embodiment, the invention relates to a granule as defined above, in which said crystallization initiator is chosen from SiO2, Na2 SO4, CaCO3, TiO2, Al2O3, ZrO2, Fe2O3, Ba2SO4 and MgO.

[0030] It is possible to use as crystallization initiator microbeads made of materials such as silica, alumina or polymers, particles made of metal oxides, small quantities of impurities, or even zeolite, in particular SiO2. The choice of SiO2 as crystallization initiator makes it possible to obtain granules of a size of the order of several hundred to a thousand micrometers.

[0031] In a particular embodiment, the invention relates to a granule as defined above, in which said crystallization initiator is present in an amount of 1% to 10%, in particular 1 to 5%, relative to the mass of said granule.

[0032] In a particular embodiment, the invention relates to a granule as defined above, in which the alkyl chain is a carbon chain comprising from 4 to 12 carbon atoms.

[0033] The expression “4 to 12 carbon atoms” designates: 4, 5, 6, 7, 8, 9, 10, 11 and 12 carbon atoms.

[0034] When the granule has as a component an alkylpolyglucoside in which the alkyl chain is a carbon chain comprising from 4 to 12 carbon atoms then the granule is detergent or solubilizing, non-foaming and sequestering.

[0035] By "detergent" we mean the property of separating impurities and cleaning.

[0036] By "solubilizer" we mean the property of making soluble or more soluble the impurities and dirt.

[0037] The term "non-foaming" refers to the property of preventing foam formation. The term "sequestering" refers to the property of a compound to form complexes with metal ions, thereby reducing their availability in the solution. This action prevents the metal ions from reacting with other compounds present, improving cleaning efficiency, granule stability and preventing deterioration of the granule's physicochemical properties.

[0038] In a particular embodiment, the invention relates to a granule as defined above, in which the alkyl chain is a carbon chain comprising from 12 to 20 carbon atoms.

[0039] The expression “12 to 20 carbon atoms” means: 12, 13, 14, 15, 16, 17, 18, 19 and 20 carbon atoms.

[0040] When the granule has as a component an alkylpolyglucoside in which the alkyl chain is a carbon chain comprising from 12 to 20 carbon atoms, then the granule is foaming and has lower detergency properties than those of the granules comprising as a component an alkylpolyglucoside in which the alkyl chain is a carbon chain comprising from 4 to 12 carbon atoms.

[0041] In a particular embodiment, the invention relates to a granule as defined above, in which the alkyl chain is a carbon chain comprising from 4 to 12 carbon atoms, or in which the alkyl chain is a carbon chain comprising from 12 to 20 carbon atoms.

[0042] In a particular embodiment, the invention relates to a granule as defined above, comprising as component: - an alkylpolyglucoside in which the alkyl chain is a carbon chain comprising from 4 to 12 carbon atoms;

[0043] and - an alkylpolyglucoside in which the alkyl chain is a carbon chain comprising 12 to 20 carbon atoms.

[0044] In this embodiment, the granule is detergent or solubilizing, foaming and sequestering.

[0045] In a particular embodiment, the invention relates to a granule as defined above, in which: - the mass percentage of said alkylpolyglucoside is 80% relative to the mass of the granule; and - the mass percentage of sodium iminodisuccinate is 20% relative to the mass of the granule.

[0046] In this embodiment, the granule is composed solely of of alkylpolyglucoside and sodium iminodisuccinate, at a mass ratio of 4:1 in the granule.

[0047] When the mass percentage of said alkylpolyglucoside is less than 80% relative to the mass of the granule, then the granule will have a moisture uptake value of less than 12% at 20°C in thirty minutes. The granule has the ability to absorb less water, providing greater stability for products that may be degraded in the presence of water.

[0048] When the mass percentage of said alkylpolyglucoside is greater than 80% relative to the mass of the granule, then the granule is amorphous.

[0049] As another example, the mass percentage of said alkylpolyglucoside is 50% relative to the mass of the granule and the mass percentage of sodium iminodisuccinate is 50% relative to the mass of the granule.

[0050] In a particular embodiment, the invention relates to a granule as defined above, in which: - the mass percentage of said alkylpolyglucoside is 79% relative to the mass of the granule; - the mass percentage of sodium iminodisuccinate is 20% relative to the mass of the granule; and - the mass percentage of a crystallization initiator is 1% relative to the mass of the granule.

[0051] In a particular embodiment, the invention relates to a granule as defined above, in which: - the mass percentage of said alkylpolyglucoside is 79% relative to the mass of the granule; - the mass percentage of sodium iminodisuccinate is 20% relative to the mass of the granule; and - the mass percentage of SiO2 is 1% relative to the mass of the granule.

[0052] In a particular embodiment, the invention relates to a granule as defined above, the size of which varies from 310 μm to 1260 μm.

[0053] By "from 310 pm to 1260 pm" is meant: from 310 to 360 pm, from 360 to 410 pm, from 410 to 460 pm, from 460 to 510 pm, from 510 to 560 pm, from 560 to 610 pm, from 610 to 660 pm, from 660 to 710 pm, from 710 to 760 pm, from 760 to 810 pm, from 810 to 860 pm, from 860 to 910 pm, from 910 to 960 pm, from 960 to 1010 pm, from 1010 to 1060 pm, from 1060 to 1110 pm, 1110 pm to 1160 pm.

[0054] By way of example and in a non-limiting manner, it is possible to measure the size of the granule using a Mastersizer 3000 granulometer from the company Malvem Panalytical, equipped with an air pressure dispersion module.

[0055] In a particular embodiment, the invention relates to a granule as defined above, the surface roughness of which is between 7 and 9 μm.

[0056] By "surface roughness" is meant the morphological characteristic of the granule. It quantifies the difference between the peaks and troughs present on the surface of said granule. It relates to a characteristic depth of the striations or asperities crisscrossing the surface of the granule.

[0057] By way of example and in a non-limiting manner, it is possible to measure the surface roughness of the granule with a 3D VK-X160K confocal laser scanning microscope from the company Keyence.

[0058] In a particular embodiment, the invention relates to a granule as defined above, said granule having a wet dissolution time of 245 to 255 seconds for a mass of 20 g of granules in 200 mL of water.

[0059] By “dissolution” is meant the passage from the solid phase of the granule to the aqueous phase.

[0060] By way of example and in a non-limiting manner, it is possible to measure the wet dissolution time by adding 20 g of granules to 200 mL of water while stirring using a magnetic bar at 21°C.

[0061] In a particular embodiment, the invention relates to a granule as defined above, said granule having a glass transition temperature of 22 to 38°C, in particular 30°C.

[0062] By "glass transition temperature" is meant the temperature corresponding to a transition of the material, passing from a rubbery state below this temperature, to a glassy state above this temperature.

[0063] By way of example and in a non-limiting manner, the glass transition temperature for a granule consisting of 80% decylglucoside and 20% sodium iminodisuccinate is 30°C.

[0064] In a particular embodiment, the invention relates to a granule as defined above:

[0065] whose size varies from 310 pm to 1260 pm,

[0066] and / or

[0067] whose surface roughness is between 7 and 9 pm,

[0068] and / or

[0069] whose wet dissolution time is between 245 and 255 seconds for a mass of 20 g of granules in 200 mL of water

[0070] and / or

[0071] whose glass transition temperature is from 22 to 38°C, in particular 30°C.

[0072] In a particular embodiment, the invention relates to a granule as defined above, in which said alkylpolyglucoside is decylglucoside.

[0073] In this embodiment, the carbon chain of the alkylpolyglucoside comprises 10 carbon atoms. This gives the granule a detergency compatible with the use of the product on the skin or scalp, as well as foaming properties that are visually acceptable to the consumer.

[0074] In a particular embodiment, the invention relates to a granule as defined above, in which: - the mass percentage of decylglucoside is 79% relative to the mass of the granule; - the mass percentage of sodium iminodisuccinate is 20% relative to the mass of the granule; and - the mass percentage of SiO2 is 1% relative to the mass of the granule.

[0075] In a particular embodiment, the invention relates to a granule as defined above, in which the naturalness index of the components of said granule is 1.

[0076] The term "naturalness index" means an index determined according to the ISO 16128 standard (part 2), codifying the calculations and indices of components and products for determining the naturalness of a cosmetic composition.

[0077] The ISO 16128 standard provides an international definition of naturalness, by setting guidelines for natural and organic cosmetics, as well as for their components. This standard provides a calculation model for establishing the percentage of components of natural origin, and therefore the naturalness index or percentage of naturalness, of a cosmetic composition from the naturalness indices of the raw materials forming said composition.

[0078] The calculation of the naturalness index of a cosmetic component is generally established and communicated by the supplier of the raw material.

[0079] When the naturalness index is 0, then the cosmetic composition or component is of purely synthetic origin.

[0080] When the naturalness index is 1, then the cosmetic composition or component is of purely natural origin.

[0081] The invention also relates to a population of granules as defined above.

[0082] Another subject of the invention is a population of granules comprising granules as defined above, in which the particle size varies from 310 pm to 1260 pm and having a median particle size of 800 pm.

[0083] By “granule population” is meant a set formed by at least several hundred granules having properties as defined above.

[0084] The term "granulometric size" refers to the size of the granules within the population.

[0085] By "from 310 pm to 1260 pm" is meant: from 310 to 360 pm, from 360 to 410 pm, from 410 to 460 pm, from 460 to 510 pm, from 510 to 560 pm, from 560 to 610 pm, from 610 to 660 pm, from 660 to 710 pm, from 710 to 760 pm, from 760 to 810 pm, from 810 to 860 pm, from 860 to 910 pm, from 910 to 960 pm, from 960 to 1010 pm, from 1010 to 1060 pm, from 1060 to 1110 pm, 1110 pm to 1160 pm.

[0086] By "median particle size" is meant the average particle size diameter, such that 50% of the granules of said population have a diameter greater than said average diameter and 50% of the particles of said composition have a diameter less than said average diameter.

[0087] The average particle size diameter can be measured by laser diffraction or by sieving. By way of example and in a non-limiting manner, it is possible to measure the median particle size using a Mastersizer 3000 particle size analyzer from the company Malvern Panalytical, equipped with an air pressure dispersion module.

[0088] In a particular embodiment, the invention relates to a population of granules as defined above, in which the SPAN value of the granules is less than 0.95; said SPAN value being calculated according to the following formula:

[0089] [Math.l] SPAN D(9()%>ZX10%) ZX50%)

[0090] in which D(90%), D(50%) and D(10%) represent the diameters for which respectively 90%, 50% and 10% of the population of granules has a diameter less than this value.

[0091] The SPAN value of a granule population is an index of dispersion of granule size in the population.

[0092] In the case of a SPAN value less than 0.5, said population is considered monodisperse.

[0093] In the case of a SPAN value of 0.5 to 1, said population is considered polydisperse.

[0094] In a particular embodiment, the invention relates to a population of granules as defined above, in which the particle size varies from 310 μm to 1260 μm and having a median particle size of 800 μm, in particular in which the SPAN value of the granules is less than 0.95; said SPAN value being calculated according to the following formula:

[0095] [Math.2] SPAN / )(50%)

[0096] in which D(90%), D(50%) and D(10%) represent the diameters for which respectively 90%, 50% and 10% of the population of granules has a diameter less than this value.

[0097] In a particular embodiment, the invention relates to a population of granules as defined above, in which the moisture uptake value is from 12% to 14% by total mass of the population of granules in an atmosphere comprising 80% humidity at 20°C in thirty minutes.

[0098] Moisture uptake is measured as % moisture uptake relative to the starting humidity.

[0099] Moisture uptake reflects the hygroscopic nature of a powder, or the ability of a powder to absorb water and then dissolve. By extension, this method indirectly indicates the speed of dissolution of the compounds in a powder.

[0100] By way of example and in a non-limiting manner, the moisture uptake is measured in an ICH110 climatic chamber from the company Memmert GmbH. The population of granules is stored in the climatic chamber for a period of thirty minutes. The mass of the sample was detected and the change in morphology of the sample was evaluated optically and under a microscope.

[0101] In a particular embodiment, the invention relates to a population of granules as defined above, in which the water activity value is from 0.20 to 0.24 at 25°C.

[0102] The term "water activity" refers to the water vapor pressure of a gaseous atmosphere in equilibrium with the medium (here, the granule population) divided by the saturated vapor pressure of this atmosphere at the same temperature. This represents the amount of free water available for biological reactions. Bacteria do not grow at a water activity below 0.7. Above a water activity of 0.7 the granule population is rapidly degraded because the conditions are favorable to the growth of bacteria, molds and other microorganisms.

[0103] With respect to the present invention, the population of granules can be stored for a period of at least 18 months without risk of being degraded by microorganisms, provided that the population of granules is stored in a hermetically sealed environment.

[0104] By way of example and in a non-limiting manner, the water activity of a population of granules can be determined using an AQUALab 3 TE water activity meter from the company Decagon Devices.

[0105] In a particular embodiment, the invention relates to a population of granules as defined above, in which the flow function of said population of granules is comprised from 63 to 73, in particular 68.

[0106] The expression "flow function", otherwise designated ffc, designates the flow function of a population of granules, and is the ratio between the maximum principal stress, ob that the population of granules can undergo without changing consolidation and the maximum stress, fc, supported by the population of granules on a free surface, developed for this state of consolidation. It is calculated according to the formula:

[0107] [Math.3] / c

[0108] It is possible to classify granule populations according to the ffC and qualify the flow behavior of a granule population ([Fig.l]). A flow function of 10 or more is considered free.

[0109] With respect to the present invention, the granule population exhibits free flow. By "free flow" is meant that the granules can flow fairly easily and without encountering significant resistance. The granule population has an easy movement capacity.

[0110] By way of example and in a non-limiting manner, the flow function can be determined using a Dietmar schulze® brand Ring Shear Tester RST-XS.s device.

[0111] In a particular embodiment, the invention relates to a population of granules as defined above, in which the specific surface area is from 3 to 9 m2 / kg.

[0112] By "specific surface area" is meant a measure of the total surface area of ​​the granules per unit mass.

[0113] By way of example and in a non-limiting manner, it is possible to measure the specific surface area of ​​a population of granules using a Mastersizer 3000 granulometer from the company Malvern Panalytical, equipped with an air pressure dispersion module.

[0114] In a particular embodiment, the invention relates to a population of granules as defined above:

[0115] wherein the moisture uptake value is from 12% to 14% by total mass of the granule population in an atmosphere comprising 80% humidity at 20°C in thirty minutes,

[0116] and / or

[0117] in which the water activity value is from 0.20 to 0.24 at 25°C,

[0118] and / or

[0119] wherein the flow function of said granule population is comprised from 63 to 73, in particular 68.

[0120] and / or

[0121] in which the specific surface area is from 3 to 9 m2 / kg.

[0122] In a particular embodiment, the invention relates to a population of granules as defined above, in which: • the apparent density is between 1.28 and 1.34 g / cm3, measured with a Helium pycnometer. • or in which the packed density is between 700 and 715 kg / m3, in particular 712 kg / m3; said packed density value being measured with a Dietmar schulze® brand Ring Shear Tester RST-XS.s device.

[0123] By "apparent density" is meant the ratio of the mass of a quantity of granule population divided by the volume it occupies.

[0124] By "packed density" is meant the ratio of the mass of a quantity of granule population divided by the volume it occupies after a step of compacting / packing said granule population.

[0125] By way of example and in a non-limiting manner, the density can be measured by using a container of known volume, and filling it with the population of granules. The excess population of granules is removed in order to obtain a straight edge.

[0126] In a particular embodiment, the invention relates to a population of granules as defined above, in which the elementary composition of said granules is comprised: • from 63.5 to 71.58% carbon; • from 22.51 to 28.35% in oxygen; • from 5.18 to 7.72% sodium; and • from 0 to 1.18% silicon,

[0127] the percentages being expressed in mass relative to the total mass

[0128] of the granule population.

[0129] The expression “elemental composition” designates the quantitative determination of the chemical elements constituting the population of granules.

[0130] Silicon may be present in the elemental composition of the population of granules when said population has been prepared by a fluidized bed, and a crystallization initiator (SiO2) has been introduced at less than 5% relative to the mass of the population of granules, to initiate the crystallization of the other components of the granule.

[0131] By way of example and in a non-limiting manner, the elemental composition of a granule population can be determined using energy dispersive X-ray spectroscopy by a Supra 55 VP microscope from the company Zeiss.

[0132] The invention also relates to the use of a population of granules as defined above.

[0133] Another object of the invention is the use of a population of granules as defined above, as surfactant.

[0134] The expression “surfactant” designates a chemical compound capable of reducing the interfacial tension between two liquids, a liquid and a gas, or a liquid and a solid.

[0135] It is known in the prior art that surfactants are amphiphilic compounds, having both a hydrophilic group and a hydrophobic group, but can be conventionally characterized by the hydrophilic-lipophilic balance (HLB).

[0136] In a particular embodiment, the invention relates to the use of a population of granules as defined above, as a surfactant of hydrophilic character.

[0137] In a particular embodiment, the invention relates to the use of a population of granules as defined above, for the formulation or preparation of a solid cosmetic composition, a solid detergent composition, in particular a dishwasher detergent or a detergent capsule, a solid descaling composition, in particular a powder descaling agent, a solid cleaning composition, in particular a multi-purpose cleaner, a clothing cleaner, a dishwashing cleaner, a surface cleaner or a sanitary cleaner or a powder preparation to be dissolved in water or as a surfactant for one of the solid compositions mentioned above

[0138] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a waterless facial cleansing bar, said waterless facial cleansing bar comprising from 70 to 90% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 5 to 15% of coconut oil, from 3 to 7% of beeswax, from 2 to 4% of vegetable glycerin and from 1 to 3% of a fragrance, in particular lavender essential oil, said percentages being expressed as a percentage by mass of the composition.

[0139] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a waterless facial cleansing bar, said waterless facial cleansing bar comprising 80% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 10% of coconut oil, 5% of beeswax, 3% of vegetable glycerin and 2% of a fragrance, in particular lavender essential oil, said percentages being expressed as a mass percentage of the composition.

[0140] Another subject of the invention relates to a process for preparing a cosmetic composition in the form of a waterless facial cleansing bar, comprising at least the following steps: i. melt beeswax and coconut oil in a bain-marie to obtain a mixture of wax and oil, ii. adding granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention to the mixture of wax and oil, to obtain a mixture of wax, oil and granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, iii. vegetable glycerin and fragrance are added to the mixture of wax, oil and granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, followed by rigorous stirring, to obtain a homogeneous mixture of wax, oil, alkylpolyglucoside and sodium iminodisuccinate according to the invention, vegetable glycerin and fragrance, iv. the homogeneous mixture of wax, oil, granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, vegetable glycerin and fragrance is poured into bar-shaped molds and left to harden until a cosmetic composition is obtained in the form of a waterless facial cleansing bar.

[0141] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a solid shampoo, said solid shampoo comprising from 60 to 80% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 15 to 25% of mild surfactant, in particular sodium cocoyl isethionate, from 3 to 7% of shea butter, from 2 to 4% of hydrolyzed rice protein and from 1 to 3% of a fragrance, in particular peppermint essential oil, said percentages being expressed as a percentage by mass of the composition.

[0142] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a solid shampoo, said solid shampoo comprising 70% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 20% of mild surfactant, in particular sodium cocoyl isethionate, 5% of shea butter, 3% of hydrolyzed rice protein and 2% of a fragrance, in particular peppermint essential oil, said percentages being expressed as a percentage by mass of the composition.

[0143] Another subject of the invention relates to a process for preparing a cosmetic composition in the form of a solid shampoo, comprising at least the following steps: i. mixing granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, and mild surfactant, to obtain a paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, and surfactant, ii. shea butter is incorporated into the paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention and surfactant, to obtain a paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, surfactant and shea butter, iii. hydrolyzed rice protein and fragrance are incorporated into the alkylpolyglucoside and sodium iminodisuccinate granule paste according to the Invention of surfactant and shea butter, followed by mixing, for obtaining a paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the Invention, surfactant, shea butter, hydrolyzed rice protein and fragrance, iv. the paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, surfactant, shea butter, hydrolyzed rice protein and fragrance is pressed and allowed to harden until a cosmetic composition in the form of a solid shampoo is obtained.

[0144] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a moisturizing shower bar, said moisturizing shower bar comprising from 50 to 70% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 15 to 25% of cocoa butter, from 7 to 13% of sweet almond oil, from 3 to 7% of beeswax, from 2 to 4% of honey and from 1 to 3% of fragrance, in particular vanilla essential oil, said percentages being expressed as a percentage by mass of the composition.

[0145] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a moisturizing shower bar, said moisturizing shower bar comprising 60% alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 20% cocoa butter, 10% sweet almond oil, 5% beeswax, 3% honey and 2% fragrance, in particular vanilla essential oil, said percentages being expressed as a percentage by mass of the composition.

[0146] Another subject of the invention relates to a process for preparing a cosmetic composition in the form of a moisturizing shower bar, comprising at least the following steps: i. melt beeswax, shea butter and sweet almond oil in a bain-marie to obtain a mixture of beeswax, shea butter and sweet almond oil, ii. the granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, honey and fragrance are added to the mixture of beeswax, shea butter and sweet almond oil, followed by mixing, to obtain a homogeneous mixture of beeswax, shea butter, sweet almond oil, granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, honey and fragrance, iii. the homogeneous mixture of beeswax, shea butter, sweet almond oil, alkylpolyglucoside granules and sodium iminodisuccinate according to the invention, honey and fragrance is poured into bar-shaped molds and left to harden until a cosmetic composition in the form of a moisturizing shower bar is obtained.

[0147] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a solid non-melting soap bar, said solid non-melting soap bar comprising from 50 to 80% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 15 to 25% of shea butter, from 5 to 15% of coconut oil, from 2 to 4% of beeswax and from 1 to 3% of fragrance, in particular lavender essential oil, said percentages being expressed as a percentage by mass of the composition.

[0148] Alkylpolyglucoside, shea butter and coconut oil provide gentle and moisturizing cleansing for the skin, while beeswax helps keep the cosmetic composition in a solid bar form. Lavender essential oil adds a soothing fragrance to the composition.

[0149] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a solid non-melting soap bar, said solid non-melting soap bar comprising 65% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 20% of shea butter, 10% of coconut oil, 3% of beeswax and 2% of fragrance, in particular lavender essential oil, said percentages being expressed as a percentage by mass of the composition.

[0150] Another subject of the invention relates to a process for preparing a cosmetic composition in the form of a solid soap bar without melting, comprising at least the following steps: i. mixing granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, shea butter, coconut oil and beeswax in a container, to obtain a homogeneous paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, shea butter, coconut oil and beeswax, ii. fragrance, in particular lavender essential oil, is added, followed by mixing, to obtain a homogeneous paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, shea butter, coconut oil, beeswax and fragrance, iii. the homogeneous paste of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, shea butter, coconut oil, beeswax and fragrance is loaded into an extruder capable of forming bars, and allowed to harden until a cosmetic composition is obtained in the form of a solid soap bar without melting.

[0151] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a soap enriched with alkylpolyglucoside, said soap comprising from 60 to 80% of saponified oils, in particular olive oil, coconut oil or palm oil, from 15 to 25% of alkylpolyglucoside granules and iminodisuccinate. of sodium according to the Invention, from 3 to 7% of vegetable glycerin, from 2 to 4% of distilled water and optionally from 1 to 3% of fragrance, in particular essential oil, said percentages being expressed as a percentage by mass of the composition.

[0152] This formulation combines the cleansing properties of saponified oils with the gentle benefits (ability to cleanse the skin effectively while providing a soft skin feel) of alkylpolyglucoside and sodium iminodisuccinate granules. The added vegetable glycerin has moisturizing properties for the skin, while the essential oils can add a pleasant fragrance for the consumer

[0153] By way of example and in a non-limiting manner, the cosmetic composition may be in the form of a soap enriched with alkylpolyglucoside, said soap comprising 70% saponified oils, in particular olive oil, coconut oil or palm oil, 20% granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, 5% vegetable glycerin, 3% distilled water and optionally 2% fragrance, in particular essential oil, said percentages being expressed as a percentage by mass of the composition.

[0154] Another subject of the invention relates to a process for preparing a cosmetic composition in the form of soap enriched with alkylpolyglucoside, comprising at least the following steps: i. a solution of caustic lye and liquid saponified oil is brought into contact and mixed to obtain a homogeneous mixture of caustic lye and oil,

[0155] said step of bringing into contact a solution of caustic lye and liquid saponified oil comprising beforehand at least the following steps: a. a solution of lye and caustic soda is mixed with distilled water at a temperature of 30 to 40°C to obtain a caustic lye solution,

[0156] and at least the following steps: a. melting saponified oil in a heat-resistant container to obtain boiling saponified oil, b. the boiling saponified oil is cooled to a temperature of 40 to 50°C, to obtain liquid saponified oil, i. adding granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, and vegetable glycerin to the homogeneous mixture of caustic lye and oil, followed by mixing, to obtain a homogeneous mixture of caustic lye, oil, alkylpolyglucoside and sodium iminodisuccinate according to the invention, and vegetable glycerin, ii. optionally, fragrance, in particular essential oil, is added to the homogeneous mixture of caustic lye, oil, granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, and vegetable glycerin, followed by mixing, to obtain a homogeneous mixture of caustic lye, oil, granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, vegetable glycerin and essential oil, iii. the homogeneous mixture of caustic lye, oil, granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, and vegetable glycerin or the homogeneous mixture of caustic lye, oil, granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, vegetable glycerin and essential oil is poured into a soap mold, and left to harden for a period of 24 to 48 hours, to obtain a hard mixture in the form of soap, iv. the hard mixture is cut into soap form, to obtain bars of hard mixture in soap form, v. drying for a period of at least 4 weeks, to obtain a cosmetic composition in the form of soap enriched with alkylpolyglucoside.

[0157] By way of example and in a non-limiting manner, the powder to be dissolved in water may be in the form of a facial cleansing powder, said facial powder comprising from 40 to 60% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 25 to 35% of oat flour, from 10 to 20% of coconut milk powder and from 3 to 7% of chamomile powder, said percentages being expressed as a percentage by mass of the composition.

[0158] By way of example and in a non-limiting manner, the powder to be dissolved in water may be in the form of a facial cleansing powder, said facial powder comprising 50% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 30% of oat flour, 15% of coconut milk powder and 5% of chamomile powder, said percentages being expressed as a percentage by mass of the composition.

[0159] Another subject of the invention relates to a method for preparing a powder to be dissolved in water in the form of a facial cleansing powder, comprising at least one step of mixing granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, oat flour, coconut milk powder and chamomile powder, to obtain the powder to be dissolved in water in the form of a facial cleansing powder.

[0160] By way of example and in a non-limiting manner, the powder to be dissolved in water may be in the form of dry shampoo powder, said dry shampoo powder comprising from 30 to 50% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 25 to 35% of arrowroot powder, from 15 to 25% of hibiscus powder and 7 to 13% of rosemary powder, said percentages being expressed as a percentage by mass of the composition.

[0161] By way of example and in a non-limiting manner, the powder to be dissolved in water may be in the form of dry shampoo powder, said dry shampoo powder comprising 40% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 30% of arrowroot powder, 20% of hibiscus powder and 10% of rosemary powder, said percentages being expressed as a percentage by mass of the composition.

[0162] Another subject of the invention relates to a process for preparing a powder to be dissolved in water in the form of dry shampoo powder, comprising at least one step of mixing granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, arrowroot powder, hibiscus powder and rosemary powder, to obtain the powder to be dissolved in water in the form of dry shampoo.

[0163] By way of example and in a non-limiting manner, the powder to be dissolved in water may be in the form of a foaming bath powder, said foaming bath powder comprising from 40 to 60% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, from 20 to 40% of sodium bicarbonate, from 10 to 20% of oat milk powder and from 3 to 7% of fragrance, in particular lavender essential oil, said percentages being expressed as a percentage by mass of the composition.

[0164] By way of example and in a non-limiting manner, the powder to be dissolved in water may be in the form of a foaming bath powder, said foaming bath powder comprising 50% of alkylpolyglucoside and sodium iminodisuccinate granules according to the invention, 30% of sodium bicarbonate, 15% of oat milk powder and 5% of fragrance, in particular lavender essential oil, said percentages being expressed as a percentage by mass of the composition.

[0165] Another subject of the invention relates to a process for preparing a powder to be dissolved in water in the form of a foaming bath powder, comprising at least one step of: i. mixture of granules of alkylpolyglucoside and sodium iminodisuccinate according to the invention, sodium bicarbonate and oat milk powder, in order to obtain a mixture of granules of alkylpolyglucoside and sodium iminodisuccinate, sodium bicarbonate and oat milk powder, ii. addition of fragrance, in particular lavender essential oil to the mixture of alkylpolyglucoside granules and sodium iminodisuccinate according to the Invention, sodium bicarbonate and oat milk powder, followed by mixing, to obtain the foaming bath powder.

[0166] In a particular embodiment, the invention relates to a use of a population of granules as defined above, as a surfactant, or for the formulation or preparation of a solid cosmetic composition or a powder preparation to be dissolved in water.

[0167] The invention also relates to a cosmetic composition comprising said population of granules as defined above.

[0168] Another subject of the invention is a cosmetic composition, comprising from 5 to 80%, in particular from 10 to 60%, relative to the mass of the composition, of the above-mentioned population of granules as defined above.

[0169] By "5 to 80%" is meant: from 5 to 10%, from 10 to 15%, from 15 to 20%, from 20 to 25%, from 25 to 30%, from 30 to 35%, from 35 to 40%, from 40 to 45%, from 45 to 50%, from 50 to 55%, from 55 to 60%, from 6 to 65%, from 65 to 70%, from 70 to 75%, from 75 to 80%.

[0170] The granule and the population of granules can be prepared according to a preparation method as described below. This preparation method consists of spray drying.

[0171] The description teaches a method of preparing a granule as defined above, comprising the steps of: a. introduction of sodium iminodisuccinate and at least one alkylpolyglucoside into a fluidized bed reactor, the proportion of all the alkylpolyglycosides being at least equal to the proportion of sodium iminodisuccinate, said proportion being expressed as a mass percentage, b. drying the sodium iminodisuccinate and all the alkylpolyglycosides in a fluidized bed reactor at temperatures up to 150°C, preferably 50°C.

[0172] The granule and the population of granules can be prepared according to a preparation method as defined above, in which the proportion of all the alkylpolyglycosides is greater than the proportion of sodium iminodisuccinate.

[0173] The granule and the population of granules may be prepared according to a preparation method as defined above as defined above, in which the proportion of all the alkylpolyglycosides and the proportion of sodium iminodisuccinate are in a ratio of 7:3 to 9:1.

[0174] The granule and the population of granules can be prepared according to a preparation method as defined above as defined above, in which the introduction of all the alkylpolyglycosides is carried out from a liquid phase, before the introduction of the sodium iminodisuccinate in solid form.

[0175] The granule and the population of granules can be prepared according to a preparation method as defined above as defined above, in which all of the alkylpolyglycosides and the sodium iminodisuccinate are introduced from a common liquid phase or each from an independent liquid phase into the fluidized bed reactor.

[0176] The granule and the population of granules may be prepared according to a preparation method as defined above as defined above, in which a coating is applied to the granule with a coating reagent during the method, preferably using sodium iminodisuccinate as the coating reagent.

[0177] The granule and the population of granules can be prepared according to a preparation method as defined above as defined above, in which at the end of step c), the granule obtained is cooled until it reaches a temperature of 25°C.

[0178] By way of example and in a non-limiting manner, the method according to the invention can be carried out in a spray fluidized bed granulator of the AGT 400 type from the company Valortecs, equipped with a fluidized bed reactor, a filtration chamber with polyester filter cloth, a wet washer, a sieve (200 μm / 1000 μm), a grinder from the company Retsch GmbH (750 μm) and a Verderflex Smart N40 feed pump marketed by Verder (10 mm). The granule can be produced under the conditions as defined below:

[0179] [Tableauxl] Inlet temperature 76 - 6 b Inlet air flow rate: 1000 -1200 msih Outlet temperature: 43 - 48 "C Nozzle (type / position) Two-fluid nozzle / B2 Product temperature: 53 'C Atomizing pressure 2 0 bar Outlet temperature: 60 SG Atomizing air tak temperature: 25X Solids content of magnet: eawofi 45 Separator air: 17-20mVh Feed rate: 200 ÿmm

[0180] Table 1. Operating conditions of the fluidized bed reactor

[0181] Sodium iminodisuccinate (Baypure® CX 100, batch: CHASME2128) has been introduced into the fluidized bed reactor at a rate of 20% by mass relative to the total mass of the granule obtained, using a 500 pm sieve, which made it possible to obtain a fluidized bed mass of approximately 6 mbar. The addition of 80% by mass relative to the total mass of the granule obtained of decylglucoside (AC 2000, batch: 230515ACO4B) has was carried out at 47°C with a feed rate of approximately 200 g / min. Discharge began after 2 h (approximately 5 mbar) and a yield of 15.5 kg of final product was obtained, with a moisture content of 5.13%. In a subsequent step, the granules were sieved to 500-1000 pm. Fractions containing granules smaller than 500 pm and larger than 1000 pm were separated and continuously recycled by pulverization via a mill from Retsch GmbH.

[0182] By way of example and in a non-limiting manner, the method according to the invention can be carried out under the conditions as defined below:

[0183] [Tables2] Inlet temperature; 65 - 66 'C Inlet air flow: 1200 Outlet temperature: 45 - 47 Nozzle (type / position) Two-fluid nozzle / S2 Product temperature: 4743 X Atomizing pressure 2.5-3.2 bar Outlet temperature: 68 'C Atomizing air temperature: 2 SX Solid content of the feed: approx. 45 Separator air: 17 - 26m% Feed rate: 200 - 380 g» min

[0184] Table 2. Operating conditions of the fluidized bed reactor

[0185] A liquid preparation was formed from 20 kg (10.1 kg solids) of decylglucoside (AC 2000, batch: 230515ACO4B) with 7.3 kg (2.5 kg solids) of sodium iminodisuccinate (Baypure® CX 100, batch: CHASME2128) heated to 60°C. This liquid preparation was injected into the fluidized bed reactor with moderate stirring, spray granulation proceeded stably at drying temperatures close to 50°C and by continuously recycling the granule fractions of sizes less than 500 pm and greater than 1000 pm by means of a mill from the company Retsch GmbH to stabilize the mass of the bed and increase the drying surface for granulation. Description of figures

[0186] [Fig. 1] is a graph of the classification of powder behavior as a function of the value of the flow function. The abscissa axis corresponds to the maximum principal stress, in kPa, and the ordinate axis corresponds to the maximum stress supported by the granule population on a free surface in kPa.

[0187] [Fig.2] represents 4 photographs taken using a confocal laser scanning microscope of a granule containing sodium iminodissucinate and decylglucoside according to example 1. Panel a) corresponds to a magnification of 10, panel b) corresponds to a magnification of 20, panel c) corresponds to a magnification of 50 and panel d) corresponds to a magnification of 100.

[0188] [Fig. 3] is a photograph taken using a scanning electron microscope of a granule containing sodium iminodissucinate and decylglucoside according to Example 1, at a magnification of 304, with a current of 5 kV, an aperture size of 30 pm and a working distance (distance between the sample and the objective lens) of 6 mm.

[0189] [Fig.4] is a scanning electron microscope image of a granule containing sodium iminodissucinate and decylglucoside according to Example 1, at a magnification of 250, with a current of 5 kV, an aperture size of 30 pm and a working distance of 6 mm.

[0190] [Fig.5] is a photograph taken using a scanning electron microscope of a granule containing sodium iminodissucinate and decylglucoside according to Example 1, at a magnification of 1490, with a current of 5 kV, an aperture size of 30 pm and a working distance of 6 mm.

[0191] [Fig.6] is a scanning electron microscope image of a granule containing sodium iminodissucinate and decylglucoside according to Example 1, at a magnification of 250, with a current of 5 kV, an aperture size of 30 pm and a working distance of 6 mm.

[0192] [Fig.7] is a scanning electron microscope image of a granule containing sodium iminodissucinate and decylglucoside according to Example 1, at a magnification of 323, with a current of 5 kV, an aperture size of 30 pm and a working distance of 6 mm.

[0193] [Fig.8] is a graph of the distribution of granule size within the population (in percentage) as a function of granule size (in micrometers) obtained with the Fraunhofer method (triplicate).

[0194] [Fig.9] is a graph of the distribution of granule size within the population (in percentage) as a function of granule size (in micrometers) obtained with the Mie method (triplicate).

[0195] [Fig. 10] represents an energy dispersive X-ray spectroscopy analysis with a scanning electron microscope of the granule population according to Example 1.

[0196] [Fig. 11] represents a differential scanning calorimetry graph during heating of a population of granules according to Example 1. The x-axis corresponds to the temperature in °C, and the y-axis corresponds to the flux of heat, in mW / mg. (a) corresponds to the glass transition temperature, at 29.5 °C. Zone (b) corresponds to the evaporation of water. Zone (c) corresponds to the melting of the granules.

[0197] [Fig. 12] shows a differential scanning calorimetry graph during cooling. The x-axis corresponds to the temperature in °C, and the y-axis corresponds to the heat flux, in mW / mg. The change in heat flux suggests recrystallization. Examples

[0198] EXAMPLE 1 Granule comprising as component sodium iminodisuccinate and decylglucoside

[0199] The granule consists of 80% decylglucoside and 20% sodium iminodisuccinate, the percentages being expressed as a mass percentage relative to the mass of the granule. It contains 4.64% moisture.

[0200] EXAMPLE 2 Analysis of the size distribution and specific surface area of ​​a population of granules according to Example 1

[0201] The analysis is carried out using a Mastersizer 3000 granulometer from Malvern Panalytical, equipped with an air pressure dispersion module. The distribution of granule size densities according to Fraunhofer methods (KKL Ho, IW Kellaway, R Tredree, Particle Size Analysis of Nebulized Aerosols Using Fraunhofer Laser Diffraction and Inertial Compaction Methods, J. ofPharmacy and Pharmacology, 38, Dec 1986, 26). This method is based on the far-field observation of the diffraction pattern by a diffracting object, such as particles in the sample. In the case of the Mastersizer 3000 granulometer, the Fraunhofer method uses a detector located at a relatively small angle to the propagation axis of the light beam. This configuration allows to measure relatively small scattering angles and to obtain information on the size of particles in the sample) and Mie (Genc S, Icoz K, Erdem T., 2023, Numerical analysis and experimental verification of optical scattering from microplastics., R. Soc.Open Sci.10: 230586). This method is based on calculations of infinite sums of spherical harmonics independent of the electron intensity and the exact nature of the particle. It is often used to characterize larger particles or for broader particle size distributions. In the case of the Mastersizer 3000 particle size analyzer, the Mie method can be used to analyze samples with different optical properties or for larger particles is shown in Figures 8 and 9 respectively. The measurement results can be found in Table 3.

[0202] [Tables3] Fraunhofer method Mie method dio,3[qm] 474 477 d50,3 [qm] 730 751 d90j3 [qm] 1130 1167 d3j2[qm] 693 708 SPAN 0.897 0.922

[0203] Table 3. Size distribution and SPAN value according to example 2

[0204] The two methods used provide complementary information on the particle size distribution of the granules analyzed, thus allowing better characterization of the properties of said granules.

[0205] dioj3corresponds to the particle size diameter such that 10% of the granules in said population have a diameter less than this value. D50j3corresponds to the particle size diameter such that 50% of the granules in said population have a diameter less than this value. DQ0.3corresponds to the particle size diameter such that 90% of the granules in said population have a diameter less than this value. The value d3j2is a measure of the particle size distribution that represents the equivalent diameter to which 32% of the mass of the granules is less. More precisely, this means that 32% of the total mass of the particles in the sample have an equivalent diameter less than or equal to d3>2

[0206] The value of Sv (6.422 m2 / kg), it represents the specific surface area of ​​the sample, measured in square meters per kilogram. Specific surface area is a measure of the total surface area of ​​particles per unit mass. In the cosmetic context, this can be important because a higher specific surface area can influence properties such as absorption, adhesion and interaction with other components of the formulation.

[0207] EXAMPLE 3 Analysis of the apparent density of a population of granules according to Example 1

[0208] The apparent density of the granule population was determined using the AccuPyc 1330 helium pycnometer from Micromeritics. The measurement was repeated 6 times and the results are shown in Table 4.

[0209] [Tables4] Measurement number Apparent density (g / cm3) 1 1.3233 2 1.3210 3 1.3202 4 1.3200 5 1.3196 6 1.3196 Mean 1.3206 Derivation around the mean 0.0014

[0210] Table 4. Measurement results (average values) of packed density.

[0211] EXAMPLE 4 Analysis of the surface roughness of a population of granules according to Example 1

[0212] The surface roughness of the granule population was studied with a 3D confocal laser scanning microscope type VK-X160K from the company Keyence and the results are shown in Table 5. Pictures were taken of 5 different particles at 4 different magnifications (10x, 20x, 50x and 100x see [Fig.2]).

[0213] [Tables5] Surface roughness (pm) Granule 1 7.73 Granule 2 9.36 Granule 3 7.32 Granule 4 8.43 Average 8.21 Deviation around average 0.78

[0214] Table 5. Measurement results (average values) of surface roughness.

[0215] EXAMPLE 5 Scanning electron microscopy of a population of granules according to Example 1

[0216] The microscope used is the Supra 55 VP from Zeiss. In scanning electron microscopy, the surface of the sample of the granule population is scanned with a finely focused electron beam in a grid. Secondary electrons and backscattered electrons are generated in each point of the grid. For the measurement, the particles were fixed on a sample holder and sputtered with gold. The resulting images are shown in Figures 3 to 7.

[0217] EXAMPLE 6 Energy Dispersive X-ray Spectroscopy of a Population of Granules According to Example 1

[0218] The microscope used is the Supra 55 VP from the Zeiss company and the results are shown in Table 6. Three granules were analyzed and were fixed on a sample holder and sprayed with gold. Gold is not part of the intrinsic composition of the sample but is added artificially to improve the quality imaging and analysis. [Fig. 10] shows one of the spectra. In addition to C and O, Na and Si were also detected. Gold is found on the sample due to sputtering

[0219] [Tableauxô] Mass percentage of each element CO Na Si Average 67.53 25.43 6.45 0.59 Derivation around the average 4.03 2.92 1.27 0.59

[0220] Table 6. Measurement results (average values) of elemental composition

[0221] In calculating the mass percentages of each element, the mass of the sample before and after sputtering with gold was taken into account. Since gold artificially increases the total mass of the sample, it was excluded from the atomic mass calculations, as it is not part of the intrinsic composition of the sample.

[0222] EXAMPLE 7 Analysis of the flow function of a population of granules according to Example 1

[0223] The flow function of the granule population was studied with a Dietmar schulze® Ring Shear Tester RST-XS.s device. A flow function of 68 is obtained.

[0224] A value of 68 suggests good fluidity and relatively easy movement of the granules. In general, the higher the value of the flow function, the freer the granule population is to flow.

[0225] EXAMPLE 8 Analysis of the water activity of a population of granules according to Example 1

[0226] The water activity of the granule population was studied with the AQUALab 3 TE water activity meter from Decagon Devices. The measurement is carried out at 24.8°C and is 0.226.

[0227] EXAMPLE 9 Analysis of the moisture uptake of a population of granules according to Example 1

[0228] A 0.878 g sample of a granule population is introduced into an ICH110 climatic chamber from Memmert GmbH. The climatic chamber has an atmosphere at 20°C at a humidity level of 80%. The sample remained in the climatic chamber for 30 minutes, and has a mass of 0.999 g. The mass difference between the initial mass and the mass after exposure to humidity is 0.121 g (0.999 g - 0.878 g). To calculate the moisture uptake, divide this mass difference by the initial mass of the sample, then multiply by 100 to obtain The percentage of moisture regain is 13.78%, which indicates the ability of the granule sample to absorb moisture under specific conditions.

[0229] EXAMPLE 10 Determination of the wet dissolution time of a granule according to Example 1

[0230] 20 gr of granules are added to 200 mL of water at 21°C in a beaker under stirring with a magnetic bar until the granules are visually completely dissolved. The experiment is carried out three times, the granules are completely dissolved in 250 s, 246 s and 255 s respectively. EXAMPLE 11 Waterless Facial Cleansing Bar

[0231] Cosmetic composition in the form of a waterless facial cleansing bar comprising 80% alkylpolyglucoside and sodium iminodissucinate granules, 10% coconut oil, 5% beeswax, 3% vegetable glycerin and 2% lavender essential oil, said percentages being expressed as a percentage by mass of the composition. EXAMPLE 12 Solid shampoo

[0232] Cosmetic composition in the form of a solid shampoo comprising 70% of alkylpolyglucoside and sodium iminodissucinate granules, 20% of mild surfactant, in particular sodium cocoyl isethionate, 5% of shea butter, 3% of hydrolyzed rice protein and 2% of a fragrance, in particular peppermint essential oil, said percentages being expressed as a percentage by mass of the composition. EXAMPLE 13 Moisturizing Shower Bar

[0233] Cosmetic composition in the form of a moisturizing shower bar comprising 60% alkylpolyglucoside and sodium iminodisuccinate granules, 20% cocoa butter, 10% sweet almond oil, 5% beeswax, 3% honey and 2% vanilla essential oil, said percentages being expressed as a percentage by mass of the composition. EXAMPLE 14 Soap enriched with alkylpolyglucoside

[0234] Cosmetic composition in the form of soap enriched with alkylpolyglucoside comprising 70% saponified oils, in particular olive oil, coconut oil or palm oil, 20% granules of alkylpolyglucoside and sodium iminodisuccinate, 5% vegetable glycerin, 3% distilled water and 2% essential oil, said percentages being expressed as a percentage by mass of the composition. EXAMPLE 15 Facial Cleansing Powder

[0235] Powder to be dissolved in water in the form of a facial cleansing powder comprising 50% alkylpolyglucoside granules and sodium iminodisuccinate, 30% oat flour, 15% coconut milk powder and 5% chamomile powder, said percentages being expressed as a percentage by mass of the composition. EXAMPLE 16 Dry Shampoo Powder

[0236] Powder to be dissolved in water in the form of dry shampoo powder comprising 40% alkylpolyglucoside and sodium iminodisuccinate granules, 30% arrowroot powder, 20% hibiscus powder and 10% rosemary powder, said percentages being expressed as a percentage by mass of the composition. EXAMPLE 17 Foaming Bath Powder

[0237] Powder to be dissolved in water in the form of dry shampoo powder comprising 50% alkylpolyglucoside and sodium iminodisuccinate granules, 30% sodium bicarbonate, 15% oat milk powder and 5% lavender essential oil, said percentages being expressed as a percentage by mass of the composition.

[0238] EXAMPLE 18 Formulation for a multi-purpose cleaner

[0239] Alkylpolyglucoside / sodium iminodisuccinate mixture (80 / 20): 75%

[0240] Sodium carbonate (improves cleaning efficiency, adjusts pH): 5%

[0241] Sodium percarbonate (source of hydrogen peroxide, bleaching and disinfectant): 10%

[0242] Enzymes (e.g., amylase and protease to break down organic stains): 2%

[0243] Perfume (for olfactory pleasure): 1%

[0244] Anti-caking agents (e.g., silica): 2%

[0245] Solvent: 5% 1. Mixing the Dry Ingredients: • Start by mixing the sodium carbonate, sodium percarbonate, and anti-caking agents (silica) in a mixer suitable for powder until a homogeneous dissolution is obtained. 2. Adding Enzymes: • Gently incorporate the enzymes (amylase and protease) into the dry mixture to avoid damaging them, while continuing to mix at low speed. 3. Integration of the Mixture of alkylpolyglucoside and sodium iminodisuccinate: • Gradually add the powdered alkylpolyglucoside and sodium iminodisuccinate mixture to the mixture while mixing to ensure even dispersion. 4. Adding Liquids: • Introduce the solvent and fragrance into the mixture. If the solvent is a liquid, it may require special equipment to be effectively incorporated into the powder without causing clumping. 5. Final Mix: • Continue mixing until the mixture is homogeneous. Mixing time may vary depending on the mixer used.

[0246] EXAMPLE 19 Formulation for a Powder Descaler

[0247] Alkylpolyglucoside / sodium iminodisuccinate mixture (80 / 20): 70%

[0248] Sodium citrate (additional chelating agent): 10%

[0249] Sodium bicarbonate (slightly abrasive effect, adjusts pH): 10%

[0250] Sodium percarbonate (source of hydrogen peroxide, for whitening action): 5%

[0251] Perfume: 2%

[0252] Anti-caking agents: 3% 1. Mixing the Bases: • Mix the sodium bicarbonate, sodium citrate, and sodium percarbonate with the anti-caking agents. 2. Integration of the mixture of alkylpolyglucoside and sodium iminodisuccinate: • Add the mixture of alkylpolyglucoside and sodium iminodisuccinate powder and mix until smooth. 3. Perfume: • Add the fragrance at the end of the mixing process to avoid excessive volatilization.

[0253] EXAMPLE 20 Formulation for a dishwasher detergent

[0254] Alkylpolyglucoside / sodium iminodisuccinate mixture (80 / 20): 70%

[0255] Sodium citrate (chelating agent, improves effectiveness against limescale deposits): 10%

[0256] Sodium percarbonate (source of hydrogen peroxide, bleaching agent): 10%

[0257] Enzymes (protease and lipase to break down proteins and fats): 4%

[0258] Anti-foam agents (to prevent excessive foaming): 1%

[0259] Solvent (in particular, propylene glycol to improve solubility): 2%

[0260] Perfume: 1%

[0261] Anti-caking agents: 2% 1. Mixing the Dry Ingredients:#

[0262] Mix the sodium citrate, sodium percarbonate, and anti-foaming agents with the anti-caking agents. 1. Adding the Enzymes and the mixture of alkylpolyglucoside and sodium iminodisuccinate:

[0263] Incorporate the enzymes thoroughly, followed by the alkylpolyglucoside and sodium iminodisuccinate mixture, and continue mixing until evenly distributed. 1. Integration of Liquids:#

[0264] Add the solvent and perfume, taking care to ensure a homogeneous dispersion without causing agglomeration.

[0265] EXAMPLE 21 Formulation for a detergent capsule Main Compartment (Solid Phase)

[0266] • Mixture of alkylpolyglucoside and sodium iminodisuccinate (80 / 20): 30% • Sodium carbonate (pH adjuster, cleaning aid): 20% • Sodium citrate (chelating agent): 15% • Sodium percarbonate (bleaching agent releasing hydrogen peroxide): 20% • Enzymes (protease, amylase, lipase, for different stains): 5% • Anti-caking agents (to keep the powder loose): 5% • Perfume: 1% • Food coloring (for aesthetics, optional): 1% • Solvent (Polyethylene glycol) (for capsule formation): 3%

[0267] Secondary Compartment (Liquid Phase) • Additional alkylpolyglucoside (extra gentle cleanser): 50% • Solvent (Ethyl alcohol or propylene glycol): 25% • Water (for dilution): 24% • Perfume: 1% Preparation process

[0268] 1. Preparation of the Phases: Prepare the solid and liquid phases separately. For the solid phase, mix all the dry ingredients thoroughly until completely homogeneous. For the liquid phase, mix the alkylpolyglucoside with the solvent and water, then add the perfume. 2. Encapsulation: Use specific equipment to encapsulate the two phases in a water-soluble film (usually polyvinyl alcohol (PVA)). The encapsulation technology must allow for the creation of separate compartments for the solid and liquid phases if necessary. 3. Drying: Capsules must be dried to ensure film integrity and prevent capsules from sticking together. Drying time and temperature depend on the specific formulation and encapsulation equipment. 4. Packaging: Once dried, the capsules are packed in containers or bags that protect from humidity and water before use.

Claims

Claims

1. Granule, comprising as components or consisting of: - sodium iminodisuccinate, - at least one alkylpolyglucoside, in which the alkyl chain is a carbon chain comprising from 4 to 20 carbon atoms, in particular 10 carbon atoms, said granule comprising a humidity level of 4.5 to 6%.

2. A granule according to claim 1, wherein the alkyl chain is a carbon chain having 4 to 12 carbon atoms, or wherein the alkyl chain is a carbon chain having 12 to 20 carbon atoms.

3. Granule according to one of claims 1 to 2, in which: - the mass percentage of said alkylpolyglucoside is 80% relative to the mass of the granule; and - the mass percentage of sodium iminodisuccinate is 20% relative to the mass of the granule.

4. Granule according to one of claims 1 to 3, the size of which varies from 310 pm to 1260 pm, and / or the surface roughness of which is from 7 to 9 pm, and / or the wet dissolution time of which is from 245 to 255 seconds for a mass of 20 g of granules in 200 mL of water and / or the glass transition temperature of which is from 22 to 38°C, in particular 30°C.

5. Granule, according to one of claims 1 to 4, in which said alkylpolyglucoside is decylglucoside.

6. A population of granules comprising granules according to one of claims 1 to 5, wherein the particle size varies from 310 pm to 1260 pm and having a median particle size of 800 pm, in particular wherein the SPAN value of the granules is less than 0.95; said SPAN value being calculated according to the following formula: [Math.4] ÆV “ D(50%) in which D(90%), D(50%) and D(10%) represent the diameters for which respectively 90%, 50% and 10% of the population of granules has a diameter less than this value.

7. A granule population according to claim 6, wherein the moisture uptake value is from 12% to 14% by total mass of the granule population in an atmosphere comprising 80% humidity at 20°C in thirty minutes, and / or wherein the water activity value is from 0.20 to 0.24 at 25°C, and / or wherein the flow function of said granule population is from 63 to 73, in particular 68. and / or wherein the specific surface area is from 3 to 9 m2 / kg.

8. Population of granules according to one of claims 6 or 7, in which: • the apparent density is between 1.28 and 1.34 g / cm3, measured with a Helium pycnometer. • or in which the packed density is between 700 and 715 kg / m3, in particular 712 kg / m3; said packed density value being measured with a Dietmar schulze® brand Ring Shear Tester RST-XS.s device.

9. Population of granules according to one of claims 6 to 8, in which the elemental composition of said granules is comprised: • from 63.5 to 71.58% in carbon; • from 22.51 to 28.35% in oxygen; • from 5.18 to 7.72% in sodium; and • from 0 to 1.18% in silicon, the percentages being expressed by mass relative to the total mass of the population of granules.

10. Use of a population of granules according to one of claims 6 to 9, for the formulation or preparation of a solid cosmetic composition, a solid detergent composition,

11. in particular a dishwasher detergent or detergent capsule, a solid descaling composition, in particular a powder descaling agent, a solid cleaning composition, in particular a multi-purpose cleaner, a clothing cleaner, a dishwashing cleaner, a surface cleaner or a sanitary cleaner, or a powder preparation to be dissolved in water or as a surfactant in one of the above-mentioned solid compositions. Cosmetic composition, comprising from 5 to 80%, in particular from 10 to 60%, relative to the mass of the composition, of the above population of granules according to one of claims 6 to 9.

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