Composition of cellulose acetate particles or particles containing cellulose acetate and method for producing such particles

Abstract

The invention relates to a composition of cellulose acetate particles or of particles containing cellulose acetate, wherein the particles have, in particular, an average d50 particle diameter of from 80 nm to 300 µm, and wherein – in relation to the total mass of the composition – at least 45 wt.% of the cellulose acetate particles or the particles containing cellulose acetate are partially spherical and, in particular, hemispherical, and wherein the cellulose acetate particles or the particles containing cellulose acetate have, in particular, an average coefficient of friction of from 0.5 to 3.0.

Description

[0001] Composition of cellulose acetate particles or of particles containing cellulose acetate and method for producing such particles

[0002] Description

[0003] The present invention relates generally to care and cosmetic products, in particular in the form of a preferably cosmetic agent which remains on the skin or hair after application instead of being washed off (so-called "leave-on product").

[0004] The invention further relates to microparticles based on cellulose acetate, which serve as a functional filler in a care and / or cosmetic product, in particular in a cosmetic product which remains on the skin or hair after use.

[0005] Microplastics are used in many cosmetic and personal care products, especially skincare products. Microplastics are generally defined as plastic particles smaller than 5 mm. Often, these particles are so small that they are barely visible to the naked eye.

[0006] On the other hand, the environmentally damaging consequences of microplastics are well known. Microplastic particles, which are intended to serve as "gentle abrasives" in scrubs and other skincare products, for example, enter the sea via wastewater systems after their use and ultimately the food chain.

[0007] Microplastics, particularly those made of polyethylene (PE) and polypropylene (PP), are currently used in cosmetic products such as scrubs and deodorants. Due to their chemical resistance and the fact that they are colorless, odorless, and tasteless, they are also used not only as "gentle abrasives" but also as stabilizers and fillers. Polyethylene and polypropylene, in particular, are not biodegradable, and because of their small particle size of less than 5 mm, the microplastics that enter wastewater via cosmetics cannot be adequately removed in wastewater treatment plants. As a result, they enter the environment, especially our waterways. In the ocean, these microplastic particles are ingested by marine organisms and thus ultimately enter our food chain.

[0008] For precautionary reasons and to minimize risk, some EU member states have already implemented measures at the national level to regulate the use of microplastics. In particular, cosmetic manufacturers are striving to eliminate the use of microplastics in the future and instead use suitable alternatives. This also applies to leave-on products such as creams, lotions, eyeshadows, lipsticks, etc., which primarily end up in household waste through makeup removal. In fact, these products will no longer be allowed to be sold from October 2029 onwards if they contain intentionally added, solid microplastics.

[0009] The object of the present invention is to provide a cosmetic product that exhibits comparable efficacy to polyethylene or polypropylene even without the use of microplastic particles in cosmetic products as a substitute for these alternatives. In particular, the alternative particles should be biodegradable in water and inexpensive to produce.

[0010] This problem is solved according to the invention in particular by the subject matter of independent claim 1.

[0011] Accordingly, the invention relates in particular to a composition of cellulose acetate particles or of particles containing cellulose acetate, wherein the particles have a particularly average d50 particle diameter of 80 nm to 300 pm, and wherein - based on the total mass of the composition - at least 45 wt. %, of the cellulose acetate particles or the particles containing cellulose acetate are semi-spherical and in particular hemispherical.

[0012] The cellulose acetate particles or the particles containing cellulose acetate preferably have a coefficient of friction of 0.5 to 3.0, and even more preferably a coefficient of friction of 1.3 to 2.7. According to embodiments of the composition according to the invention, the cellulose acetate particles or the particles containing cellulose acetate have an oil absorption capacity of 30 ml to 1,500 ml, preferably an oil absorption capacity of 180 ml to 500 ml, and even more preferably an oil absorption capacity of 50 ml to 290 ml of linseed oil per 100 g of dry particles.

[0013] Preferably, the cellulose acetate particles or the particles containing cellulose acetate have a bulk density of, in particular, 100 g / l to 480 g / l, preferably 120 g / l to 280 g / l, particularly preferably 130 g / l to 240 g / l and particularly preferably between 130 g / l and 185 g / l.

[0014] According to embodiments of the composition according to the invention, the cellulose acetate of the cellulose acetate particles or the cellulose acetate of the particles containing cellulose acetate has a total acetyl substitution degree of 0.7 to 2.9, and in particular a total acetyl substitution degree of 1.8 to 2.6.

[0015] In particular, the cellulose acetate particles or the particles containing cellulose acetate have a particularly average coefficient of friction of 1.3 to 2.7.

[0016] According to realizations of the composition according to the invention, at least 65 wt.% of the cellulose acetate particles or the particles containing cellulose acetate are semi-spherical and in particular hemispherical, based on the total mass of the composition.

[0017] Alternatively or additionally, at least 35 wt% of the cellulose acetate particles or the particles containing cellulose acetate have a hollow shape with a semi-spherical pit, based on the total mass of the composition.

[0018] In particular, it is advantageous that the cellulose acetate particles or the particles containing cellulose acetate have a contact angle of 100° to 155°.

[0019] According to embodiments of the composition according to the invention, the cellulose acetate particles or the particles containing cellulose acetate have a specific surface area of ​​1.5 m². 2 / g up to 9.99 m 2 / g. In particular, the cellulose acetate particles or the particles containing cellulose acetate have a specific surface area of ​​1.5 m². 2 / g up to 10.0 m 2 / g, preferably a specific surface area of ​​3.0 m² 2 / g up to 9.0 m 2 / g, or even more preferably a specific surface area of ​​4.0 m² 2 / g up to 8.0 m 2 / g, on.

[0020] In preferred embodiments of the invention, at least 35 wt.% of the cellulose acetate particles or the particles containing cellulose acetate have an open porosity of 5 to 95% and preferably an open porosity of 10 to 90%, based on the total mass of the composition.

[0021] In this context in particular, it has proven advantageous that - based on the total mass of the composition - at least 35 wt.% of the cellulose acetate particles or the particles containing cellulose acetate have an open porosity of 5 to 95%.

[0022] The cellulose acetate particles or the particles containing cellulose acetate exhibit, in particular, a biodegradability after 15 to 280 days of not less than 60 wt% according to ASTM D6691 (date of filing) in seawater.

[0023] Alternatively or additionally, the cellulose acetate particles or the particles containing cellulose acetate show a degradation rate after 6 months of not less than 60 wt% according to ASTM D6691 (date of filing).

[0024] In this context, it is advantageous for the cellulose acetate particles or the particles containing cellulose acetate, which exhibit biodegradability in seawater, to have a weight-average molecular weight of 80,000 or less.

[0025] In preferred embodiments of the composition according to the invention, the cellulose acetate particles or the particles containing cellulose acetate, which exhibit biodegradability in seawater, have a weight-average molecular weight of 80,000 or less, preferably a weight-average molecular weight of 75,000 or less, and even more preferably a weight-average molecular weight of 70,000 or less. In particular, the cellulose acetate particles or the particles containing cellulose acetate have a density of 1.20 g / cm³ to 1.35 g / cm³, preferably a density of 1.25 g / cm³ to 1.35 g / cm³, and even more preferably a density of 1.25 g / cm³ to 1.30 g / cm³.

[0026] On the other hand, it has been shown that according to embodiments of the composition according to the invention, the cellulose acetate particles or the particles containing cellulose acetate have a maximum solubility in water at pH 7.0, 20 °C, 1 bar, of 0 g / l to 0.5 g / l, preferably of 0 g / l to 0.2 g / l, particularly preferably of 0 g / l to 0.08 g / l.

[0027] Further advantageous properties and / or parameters of the cellulose acetate particles or the particles containing cellulose acetate of the composition according to the invention are listed below:

[0028] • the cellulose acetate particles or the particles containing cellulose acetate have a density of 1.20 g / cm3 to 1.35 g / cm3; and / or

[0029] • The cellulose acetate particles or the particles containing cellulose acetate have a maximum solubility in water at pH 7.0, 20 °C, 1 bar, of 0 g / l to 0.5 g / l, preferably of 0 g / l to 0.2 g / l, particularly preferably of 0 g / l to 0.08 g / l.

[0030] Due to the previously discussed properties of the cellulose acetate particles or the particles containing cellulose acetate, the composition according to the invention can be used in particular as follows:

[0031] (i) as a carrier system for an active ingredient; and / or

[0032] (ii) as an absorbent for impurities; and / or

[0033] (iii) as a filter medium; and / or

[0034] (iv) as a cleaning agent; and / or

[0035] (v) as dry shampoo; and / or

[0036] (vi) as a sunscreen; and / or

[0037] (vii) as a functional filler for cosmetics and / or detergents; and / or (viii) as a pigment substitute; and / or

[0038] (ix) as a dispersing agent. The cellulose acetate particles or the particles containing cellulose acetate, which in the composition according to the invention are used, for example, in a care and / or cosmetic product as functional fillers, have a key function in the development of cosmetics, especially skin-correcting ones. They determine whether formulations cover imperfections and even out irregular skin tones without appearing mask-like and unnatural.

[0039] Specifically, cellulose acetate particles, or particles containing cellulose acetate, are suitable for achieving individual skin tone corrections in skincare and / or cosmetic products. These functional fillers bring freshness, transparency, and skin tone into perfect harmony, providing an invisible color correction. Their small particle size creates a pleasantly soft feeling on the skin.

[0040] Furthermore, the cellulose acetate particles, or particles containing cellulose acetate, minimize shine, guarantee optimal coverage with maximum transparency, and subtly even out uneven skin tones. In particular, the cellulose acetate particles, or particles containing cellulose acetate, are suitable for removing and / or concealing skin depressions, especially wrinkles.

[0041] Since cellulose acetate particles, or particles containing cellulose acetate, can be combined with a variety of other components, especially raw materials, the richness of cosmetic formulations is increased. Cellulose acetate particles, or particles containing cellulose acetate, are particularly well-suited for makeup products or other cleansing, care, and / or cosmetic products in liquid and powder form.

[0042] In particular, the present invention also relates to a cosmetic formulation comprising a composition of cellulose acetate particles or of particles containing cellulose acetate of the aforementioned type. According to preferred embodiments, the cosmetic formulation is an emulsion, in particular an O / W or a W / O emulsion, with a viscosity at a shear rate of 10 s⁻¹ and at 20°C of 0.01 Pas to 100,000 Pas, particularly preferably of 0.1 Pas, in particular 2.5 Pas, to 10,000 Pas.

[0043] In principle, it is conceivable that the cosmetic formulation contains, as an additional component, at least one polyol or at least one thickener selected from the group of polysaccharides, proteins, polyacrylates or silicates.

[0044] In a preferred embodiment, the cosmetic formulation contains as an additional component at least two nitrogen-containing active ingredients and / or at least one thickener from the group of polysaccharides and / or at least one polyol and / or at least one hydrosol and has a turbidity of at least 60% and a total transmission of at least 80% when 3% of the cellulose acetate particles or the particles containing cellulose acetate are added, and / or has a turbidity of at least 98% and a total transmission of at least 60% when 9% of the cellulose acetate particles or the particles containing cellulose acetate are added.

[0045] According to one aspect of the present invention, the cellulose acetate particles or the particles containing cellulose acetate, which are used as particularly functional fillers in the composition according to the invention, are produced by a process which comprises the following process steps.

[0046] (a) Dissolving cellulose acetate with a total degree of acetyl substitution of 0.7 or more and 2.9 or less in acetone or an acetone-containing solvent;

[0047] (b) Spraying the acetonic cellulose acetate solution at 50 °C or more and 165 °C or less; and

[0048] (c) Removal of residual acetone from the cellulose acetate particles or from the particles containing cellulose acetate;

[0049] (d) optionally and in particular instead of process step (c) carrying out a basic hydrolysis of the acetate groups to adjust biodegradability with subsequent aqueous washing. The saponification proceeds according to the reaction equation (A) given below: Saponification according to reaction equation (A):

[0050] 4x

[0051]

[0052] The hydroxide ion initially acts as a highly nucleophilic base. The final step, the elimination of the acetate group, is irreversible. This permanently shifts the saponification equilibrium in favor of the products.

[0053] The process may further include the process step of washing the cellulose acetate particles formed in process step (b) or the particles containing cellulose acetate.

[0054] To control particle properties, especially for the production of spherical particles or shape-regulated, aspherical particles, a spraying process is therefore used in particular.

[0055] In particular, hemispherical particles with uniform grain size can be produced. Additionally, biconvex and hemispherical shapes, as well as mushroom-shaped and partially defective spherical (concave) particles, can be produced. The principle of producing the particles according to the invention consists of dissolving solutions of cellulose acetate in a solvent, in particular acetone or an acetone-containing solvent, and then removing the solvent (acetone). The spray method is particularly suitable for this purpose. In this process, the particles are produced by spraying the acetone-containing cellulose acetate solution from a fine nozzle under high pressure.

[0056] The particle size can be adjusted by the spray mass flow rate during spray drying and / or by the spray concentration. A high spray mass flow rate results in smaller particle sizes, while a high spray concentration results in larger particles.

[0057] However, the drying conditions, especially the volume flow rate of the drying air, also have a significant influence. The higher the volume flow rate of the drying air, the smaller the particles.

[0058] Accordingly, in realizations of the process according to the invention, it is provided that in process step (b) the acetone cellulose acetate solution is sprayed with a hot gas stream, wherein a volume flow of the hot gas is set depending on a desired mean particle size of the cellulose acetate particles to be produced or the particles containing cellulose acetate, wherein in particular a higher volume flow of the hot gas is set if a smaller mean particle size is desired for the cellulose acetate particles to be produced or for the particles containing cellulose acetate.

[0059] In this context, it is advisable to regulate the temperature of the hot gas, in particular so that before or during the injection of the acetone cellulose acetate solution into the hot gas stream, the hot gas stream has a temperature between approximately 50 °C and approximately 165 °C.

[0060] Preferably, the temperature of the hot gas is controlled, in particular such that after the acetonic cellulose acetate solution is sprayed into the hot gas stream, it has a temperature between about 30 °C and about 150 °C.

[0061] Alternatively or additionally, in realizations of the process according to the invention, it is provided that, depending on a desired average particle size of the cellulose acetate particles to be produced or the particles containing cellulose acetate, in process step b) the acetone cellulose acetate solution is passed through at least one nozzle serving as an atomizer with a correspondingly adapted spray mass flow and with a correspondingly adapted spray concentration, wherein the nozzle preferably has a nozzle opening of 0.5 to 5.5 and in particular of about 1.0 to 3.0 mm.

[0062] In this context, it is advantageous that, in order to produce cellulose acetate particles or particles containing cellulose acetate with a particularly average d50 particle diameter of about 80 nm to about 250 pm, the acetone cellulose acetate solution is passed in process step b) at a nozzle pressure of 1.5 bar to about 8 bar through at least one nozzle serving as an atomizer with a nozzle opening of 0.5 to 5.5 mm and in particular of about 1.0 to 3.0 mm.

[0063] Alternatively or additionally, in realizations of the inventive method, it is provided that, for the production of the cellulose acetate particles or the particles containing cellulose acetate with a particularly medium d50 particle diameter of about 1.5 bar to about 8 bar, the material is passed through at least one nozzle serving as an atomizer with a nozzle opening of about 0.5 mm to about 5.5 mm and in particular of about 1.0 mm to 3.0 mm.

[0064] The proportion of cellulose acetate in the acetone cellulose acetate solution prior to spraying the acetone cellulose acetate solution in process step b) should preferably be 1.0 wt.% to about 25.0 wt.%, preferably about 1.5 wt.% to about 20 wt.%.

[0065] In implementations of the process according to the invention, it is provided that the acetone cellulose acetate solution contains at least one pharmaceutical and / or cosmetic active ingredient.

[0066] The at least one active ingredient may in particular be at least one of the following active ingredients:

[0067] Retinoids and especially retinol, zinc salts such as zinc gluconate;

[0068] Laminaria saccharina extracts; • Wild yam extracts;

[0069] • Triclosan;

[0070] • Hyaluronic acid;

[0071] • Phenoxyethanol;

[0072] • Octoxyglycerin;

[0073] • Octanoylglycine;

[0074] • Clove extracts;

[0075] • Caprylyl glycol;

[0076] • Azelaic acid;

[0077] • o-Hydroxy acids, such as lactic acid or glycolic acid; β-Hydroxy acids, especially salicylic acid and its derivatives such as 5-n-octanoylsalicylic acid;

[0078] • Ursolic acid;

[0079] • Panthenol;

[0080] • Niacinamide; and / or

[0081] • Octo pirox.

[0082] Additionally or alternatively, the acetone cellulose acetate solution may contain at least one nitrogen-containing additive, such as polyvinylpyrrolidone, urea, allantoin, diethylhexyl butamido triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, diethylamino hydroxybenzoyl hexyl benzoate, etc. It is also conceivable that the acetone cellulose acetate solution contains at least one other polysaccharide ester.

[0083] Alternatively or additionally to at least one active ingredient, the composition according to the invention can also contain pigments or fillers, powders made from natural organic materials such as starch powder, in particular cross-linked or non-cross-linked corn, wheat or rice starch, silicone resin microbeads, silicon dioxide, alkaline earth metal oxides, metal oxides such as iron oxide, titanium dioxide, zinc oxide or aluminum oxide, mica, talc, sericite, boron nitride, clays and mixtures thereof.

[0084] The following section describes in more detail, with reference to the examples discussed below. To produce the cellulose acetate particles or the particles containing cellulose acetate, spray drying in an acetone solution of cellulose acetate is carried out.

[0085] Example of process conditions:

[0086] 1 mm nozzle, dual-flow nozzle or rotating disc, nozzle gas nitrogen

[0087] Pressure 0 - 15 bar

[0088] Air inlet temperature 50 - 165 °C

[0089] Air / product outlet temperature 30 - 65 °C

[0090]

[0091] Observed properties of the cellulose acetate particles produced in this way or of the cellulose acetate-containing particles of spray-dried materials:

[0092] • significantly higher oil absorption than with ground material;

[0093] • good sebum absorption; and

[0094] • Increased sun protection factor.

[0095] The previously discussed properties of the cellulose acetate particles or the particles containing cellulose acetate were determined as follows:

[0096] Contact angle measurement:

[0097] For contact angle measurements, double-sided adhesive tape was applied to a glass slide. To create a uniform coating, 0.2 g of particles were placed on the tape and spread with a spatula. A glass slide was then placed on top of the particle layer to press and compact it. Any remaining particles were carefully tapped off. Static contact angles of water droplets on the samples were determined using a droplet shape analyzer (DSA30, Krüss GmbH, Hamburg, Germany).

[0098] A needle with an outer diameter of 0.31 mm was used to apply the water droplets. The needle was moved close to the surface of the particle layer, and a 6.5 g droplet of distilled water was dispensed onto the surface. The contact angle was recorded at 0 and 15 s. At least 10 data points were recorded for each sample.

[0099] Bulk density:

[0100] The measurement was carried out according to DIN ISO 697 (as of the date of registration).

[0101] Specific surface area:

[0102] The specific surface area of ​​the cellulose acetate particles was measured on a Micrometrics TriStar II 3020 using nitrogen as the adsorption gas. The measurement was performed according to DIN ISO 9277 (as of the filing date).

[0103] Density:

[0104] The density of the cellulose acetate particles was measured using a helium pycnometer. The measurement was performed according to DIN 51913:2001-05 (as of the filing date).

[0105] Friction coefficient measurements:

[0106] The coefficient of friction of the cellulose acetate particles was determined by measuring the angle of repose. For this purpose, the powder was heaped into a mound on a cylindrical test specimen using a funnel. The angle of repose was then measured at three different points. The coefficient of friction was calculated from the mean angle of repose: coefficient of friction p = tan (angle of repose).

[0107] Determination of oil and sebum uptake:

[0108] Oil and sebum absorption were determined according to DIN EN ISO 787-5 (as of the filing date). Gloss measurements:

[0109] The gloss was determined using a Skin-Glossymeter GL 200 from Courage + Khazaka electronic GmbH.

[0110] Turbidity and total transmission:

[0111] The turbidity and total transmittance were determined using a Haze Gard i from Byk-Gardner GmbH. For this purpose, the particles were incorporated into a hydrogel. The finished gel was then applied as a 120 µm thick film onto a transparent foil and measured with the Haze Gard i after a drying time of 15 minutes.

[0112] Nomenclature:

[0113] The number in the cellulose acetate designations (Cellulose acetate SP 10) refers to the d50 value in micrometers (pm).

[0114] In the following examples, aspects of the present invention are described by way of example, without the invention, the scope of which is evident from the entire description and the claims, being limited to the embodiments mentioned in the examples.

[0115] The stickiness, spreadability, hardness, and firmness of the cosmetic formulations were determined using the Texture Analyzer from Stable Micro Systems. A 5 kg load cell was used for the measurements. Lipsticks were measured using the penetration test and the lipstick rack. Creams were analyzed with the spreadability rack.

[0116] The nomenclature used to evaluate the emulsion comparison examples regarding "stability" is based on the following requirements. A "good" rating for stability means that the emulsion remains stable for at least one month at room temperature and 40°C. "Stable" in this context means that no oil or water separation occurs, the emulsion's appearance remains homogeneous, and there are no changes in viscosity, color, or odor. The nomenclature used to evaluate the lipstick examples regarding "stability" is based on the following requirements. A "good" rating for stability means that no separation occurs after two hours at 60°C, the lipstick's appearance remains intact, and the lipstick shows no color changes. The hardness value is an average of three different measurements taken with the Texture Analyzer.The method used with the texture analyzer was based on ASTM method D1321-95 (as of the filing date). The mean value was then converted to a percentage, using the comparison example as a reference. The stickiness value is an average of three different measurements taken with the texture analyzer. This value was also then converted to a percentage, again using the comparison example as a reference.

[0117] The nomenclature used to evaluate the eyeshadow samples regarding "stability" is based on the following requirements. A "good" rating for stability means that the eyeshadows do not completely disintegrate during the Texture Analyser penetration test and that the eyeshadow's appearance remains intact, with no color bleeding or oil stains visible beforehand.

[0118] The evaluation of the baby powder and the mineral face powder was carried out according to ISO 787-5 (as of the filing date).

[0119] The synthetic sebum consists of 17% fatty acid, 44.7% triglyceride, 25% wax monoester (jojoba oil) and 12.4% squalene.

[0120] The SPF (sun protection factor) was determined according to ISO 24444 (as of the filing date).

[0121] Example 1, Comparative Example 1 and Comparative Example VI: Lipstick

[0122] The formulations listed in Table 1 were produced and their stability, appearance, stickiness and hardness were evaluated.

[0123] Table 1 according to Example 1: Formulation and results of Example 1, Comparison Example 1 and Comparison Example VI, Lipstick with Cellulose Acetate Example 1 VI VV1 Cocos nucifera L. 34 34 34 Simmondsia chinensis seed oil 18 18 18 Cellulose acetate SP 10 7 0 0 Cellulose 0 0 7 Iron Oxide Red, CI 77491 7 7 7 Mica, Titanium Dioxide, CI 77491, CI 7 7 7 75470

[0124] Cera Flava 8 8 8 Theobroma Cacao Seed butter 2 2 2 Copernicia Cerifera (Carnauba) Cera 4 4 4 Lanolin 6 6 6 Butyrospermum Parkii Butter 5 5 5

[0125] Stability good bad good Appearance Homogeneous, Homogeneous, Homogeneous, hard soft hard Stickiness 72% 100% 87% Hardness 6% increased 0 3% increased

[0126]

[0127] Example 2, Comparison Example 2 and Comparison Example V2: Oil-in-Water Facial Cream

[0128] The formulations listed in Table 2 were prepared and their stability, appearance, stickiness, spreadability, and strength were evaluated. Table 1 according to Example 2: Formulation and results of Example 2, Comparison Example 2, and Comparison Example V2, oil-in-water face cream with cellulose acetate.

[0129] Example 2 V2 VV2 Butyrosperum parkii butter 4.0 4.0 4.0 Cethyl palmitate 1.0 1.0 1.0 Myristyl Myristate 3.0 3.0 3.0 Octyldodecanol 2.0 2.0 2.0 Helianthus annuus seed

[0130] oil 3.0 3.0 3.0 Glyceryl Citrate / Lac-tate / Linoleate / Oleate 3.0 3.0 3.0 Urea 4.0 4.0 4.0 Aqua 68.6 68.6 68.6 Glycerin 4.0 0.0 0.0 Xanthan gum 0.3 0.3 0.3 Cellulose acetate SP 10

[0131] 4.0 0 0 Polymethyl Methacrylate 0 0 4.0

[0132] Panthenol 2.5 2.5 2.5 Ethanol 2.0 2.0 2.0 Geranium 0.35 0.35 0.35 Tocopherol 0.7 0.7 0.7 Potassium sorbate 0.25 0.25 0.25 Magnesium ascorbyl

[0133] phosphates 0.5 0.5 0.5 Trisodium citrate dihydrate 0.64 0.64 0.64 Citric acid anhydrate

[0134]

[0135] 0.16 0.16 0.16 Stability good good good Appearance homogeneous homogeneous Stickiness

[0136] -17.57g / SD 0.5 -14.79g / SD 0.11 -19.45g / SD 0.46 Spreadability 14.lg*sec / 12.08g*sec / SD 15.45g*sec / SD

[0137] SD 0.48 0.09 0.557 Strength 25.81g / SD

[0138] 28

[0139]

[0140] 1.09 22.69g / SD 0.76 .55g / SD 0.49

[0141] Example 3, Comparison Example 3, Comparison Example V3 and Comparison Example VV3: Baby powder

[0142] The formulations listed in Table 3 were prepared and their absorption capacity for linseed oil (oil absorption), sebum and water was evaluated.

[0143] Table 3 according to Example 3: Formulation and results of Example 3, Comparison Example 3, Comparison Example V3 and commercially available Comparison Example VV3.

[0144] Example 3 V3 VV3 VVV3

[0145] 90.5 0 0 0 Cellulose acetate SP 10

[0146] Oryza Sativa Starch 8.5 99.4 0 0 Cellulose 0 99.4 0 Tale >90

[0147] Zinc acetate 0.15 0.15 0.15

[0148] Sodium benzaote 0.15 0.15 0.15

[0149] Tricalcium phosphate 0.3 0.3 0.3

[0150] Oil absorption [ml / 100g] 226 82 191 69 Sebum absorption 197 84 185 72 [ml / 100g]

[0151] Water absorption 280 99 252 89

[0152] [ml / 100g]

[0153]

[0154] Example 4 and Comparative Example 4: Mineral Facial Ointment

[0155] The formulations listed in Table 4 were prepared and their absorption behavior of linseed oil (oil absorption) and artificial sebum was evaluated.

[0156] Table 4 according to Example 4: Formulation and results of Example 4 and Comparative Example 4, Mineral face powder with cellulose acetate

[0157] Example 4 V4 Cellulose acetate SP 10 60 0 Distarch phosphate 0 60 Magnesium stearate 2 2 Zinc Oxide, CI 77947 4 4

[0158] CI 77891, CI 77491, CI 77492, CI 9 9 77499

[0159] Limnanthes alba (Meadowfoam) Seed Oil 4 4

[0160] Appearance: Homogeneous; Oil absorption [ml / 100g]: 160; Sebum absorption [ml / 100g]: 154; 108

[0161]

[0162]

[0163] 5.1, 5.2 and 5.3: Sunscreen

[0164] Three sunscreens were produced, containing the following raw materials:

[0165] 5.1 Sonnencreme:

[0166] Aqua, Diethylhexyl Carbonate, Butylene Glycol Dicaprylate / Dicaprate, Dibutyl Adipate, Titanium dioxide, Zinc Oxide, PEG-30 Dipolyhyxroxystearate, Alcohol denat., Isonyl Isononanoate, Glycerin, Pentaerythrityl Tetra-di-t-Butyl Hydroxyhydrocinnamate, Triethoxycaprylylsilane, Aluminium Oxide, Stearic Acid, Magnesium Sulfate, Trisodium Ethylenediamine, Phenoxyethanol, Cellulose acetate SP 10.

[0167] 5.2 Sonnencreme:

[0168] Aqua, Diethylhexyl Carbonate, Butylene Glycol Dicaprylate / Dicaprate, Dibutyl Adipate, Titanium dioxide, Zinc Oxide, PEG-30 Dipolyhyxroxystearate, Alcohol denat., Isonyl Isononanoate, Glycerin, Pentaerythrityl Tetra-di-t-Butyl Hydroxyhydrocinnamate, Triethoxycaprylylsilane, Aluminium Oxide, Stearic Acid, Magnesium Sulfate, Trisodium Ethylenediamine, Phenoxyethanol, Cellulose acetate SP 18.

[0169] 5.3 Sonnencreme:

[0170] Aqua, Diethylhexyl Carbonate, Butylene Glycol Dicaprylate / Dicaprate, Dibutyl Adipate, Titanium dioxide, Zinc Oxide, PEG-30 Dipolyhyxroxystearate, Alcohol denat., Isonyl Isononanoate, Glycerin, Pentaerythrityl Tetra-di-t-Butyl Hydroxyhydrocinnamate, Triethoxycaprylylsilane, Aluminum Oxide, Stearic Acid, Magnesium Sulfate, Trisodium Ethylenediamine, Phenoxyethanol. Table 5 according to Example 5: Results of the SPF measurements

[0171] 5.1 Sunscreen SPF 23.1

[0172] 5.2 Sunscreen SPF 28.8

[0173] 5.3 Sunscreen SPF 17.1

[0174]

[0175] Example 6 and commercially available comparison example V6: Dry shampoo

[0176] Table 6 according to Example 6: The formulations listed in Table 6 were prepared and their washing effect was evaluated based on gloss measurements. The exact composition of the commercially available comparison example V6 cannot be specified, as it is not known in detail.

[0177] Example 6 V6

[0178] Cellulose acetate SP 18

[0179] 35

[0180] Oryza Sativa (Rice)

[0181] Starch 17

[0182] Kaolin X

[0183] 9

[0184] Hydrated Silica X

[0185] 4

[0186] Talc X

[0187] 4

[0188] Zea mays starch X

[0189] 13

[0190] Triticum vulgare (Wheat)

[0191] Starch 17

[0192]

[0193] Table 7 according to Example 6: Results of the gloss measurement

[0194] Shine without drying. Shine with dry shampoo. Shampoo action.

[0195] 6 3.23 2.80

[0196] V6 3.42 2.29

[0197]

[0198] Example 7 and commercially available comparison example 7: Dry shampoo with PVP as an additive

[0199] Table 8 according to Example 7: The formulations listed in Table 7 were prepared and their washing effect was evaluated based on gloss measurements. The exact composition of the commercially available comparison example V7 cannot be specified, as it is not known in detail.

[0200] Example 6 V7

[0201] Cellulose acetate SP+PVP

[0202] 35

[0203] Oryza Sativa (Rice)

[0204] Starch 17

[0205] Kaolin X

[0206] 9

[0207] Hydrated Silica X

[0208] 4

[0209] Talc X

[0210] 4

[0211] Zea mays starch X

[0212] 13

[0213] Triticum vulgare (Wheat)

[0214] Starch 17

[0215]

[0216] Table 8 according to Example 7: Results of the gloss measurement

[0217] Shine without drying. Shine with dry shampoo. Shampoo action.

[0218] 6 4.76 3.68

[0219] V7 3.42 2.29

[0220]

Claims

Patent claims 1. Composition of cellulose acetate particles or of particles containing cellulose acetate, wherein the particles have a particularly average d50 particle diameter of 80 nm to 300 pm, and wherein - based on the total mass of the composition - at least 45 wt. %, of the cellulose acetate particles or the particles containing cellulose acetate are semi-spherical and in particular hemispherical, and wherein the cellulose acetate particles or the particles containing cellulose acetate have a particularly average coefficient of friction of 0.5 to 3.

0.

2. Composition according to claim 1, wherein the cellulose acetate particles or the particles containing cellulose acetate have a particularly medium oil absorption capacity of 30 ml to 1,500 ml, preferably a particularly medium oil absorption capacity of 180 ml to 500 ml and even more preferably a particularly medium oil absorption capacity of 50 ml to 290 ml linseed oil per 100 g dry particles.

3. Composition according to claim 1 or 2, wherein the cellulose acetate particles or the particles containing cellulose acetate have a particularly average bulk density of 100 g / l to 480 g / l, preferably 120 g / l to 280 g / l, particularly preferably 130 g / l to 240 g / l and particularly preferably between 130 g / l and 185 g / l.

4. Composition according to any one of claims 1 to 3, wherein the cellulose acetate of the cellulose acetate particles or the cellulose acetate of the particles containing cellulose acetate contains a total acetylsubsti- exhibiting a degree of substitution of 0.7 to 2.9, and preferably exhibiting a total acetyl substitution degree of 1.8 to 2.6, and more preferably exhibiting a total acetyl substitution degree of 2.0 to 2.

6.

5. Composition according to any one of claims 1 to 4, wherein the cellulose acetate particles or the particles containing cellulose acetate have a particularly average coefficient of friction of 1.3 to 2.

7.

6. Composition according to any one of claims 1 to 5, wherein - based on the total mass of the composition - at least 65 wt.% of the cellulose acetate particles or the particles containing cellulose acetate are semi-spherical and in particular hemispherical.

7. Composition according to any one of claims 1 to 6, wherein - based on the total mass of the composition - at least 35 wt% of the cellulose acetate particles or the particles containing cellulose acetate have a hollow shape with a semi-spherical pit.

8. Composition according to any one of claims 1 to 7, wherein the cellulose acetate particles or the particles containing cellulose acetate have a contact angle of 100° to 155°.

9. Composition according to any one of claims 1 to 8, wherein the cellulose acetate particles or the particles containing cellulose acetate have a specific surface area of ​​1.5 m² 2 / g up to 10.0 m 2 / g, preferably a specific surface area of ​​3.0 m² 2 / g up to 9.0 m 2 / g, or even more preferably a specific surface area of ​​4.0 m² 2 / g up to 8.0 m 2 exhibit / g.

10. Composition according to any one of claims 1 to 9, wherein - based on the total mass of the composition - at least 35 wt% of the cellulose acetate particles or the particles containing cellulose acetate have an open porosity of 5 to 95% and preferably an open porosity of 10 to 90%.

11. Composition according to any one of claims 1 to 10, wherein the cellulose acetate particles or the particles containing cellulose acetate show a biodegradability after 15 to 280 days of not less than 60 wt% according to ASTM D6691 (date of filing) in seawater.

12. Composition according to any one of claims 1 to 11, wherein the cellulose acetate particles or the particles containing cellulose acetate show a degradation rate after 6 months of not less than 60 wt% according to ASTM D6691 (date of filing).

13. Composition according to claim 12, wherein the cellulose acetate particles or particles containing cellulose acetate, which exhibit biodegradability in seawater, have a weight-average molecular weight of 80,000 or less, preferably a weight-average molecular weight of 75,000 or less, and more preferably a weight-average molecular weight of 70,000 or less.

14. Composition according to any one of claims 1 to 13, wherein the cellulose acetate particles or the particles containing cellulose acetate have a density of 1.20 g / cm3 to 1.35 g / cm3, preferably a density of 1.25 g / cm3 to 1.35 g / cm3 and more preferably a density of 1.25 g / cm3 to 1.30 g / cm3.

15. Composition according to any one of claims 1 to 14, wherein the cellulose acetate particles or the particles containing cellulose acetate have a maximum solubility in water at pH 7.0, 20 °C, 1 bar, of 0 g / l to 0.5 g / l, preferably of 0 g / l to 0.2 g / l, particularly preferably of 0 g / l to 0.08 g / l.

16. Cosmetic formulation comprising a composition of cellulose acetate particles or of particles containing cellulose acetate according to any one of claims 1 to 15.

17. Cosmetic formulation according to claim 16, wherein the cosmetic formulation is an emulsion, in particular an O / W or a W / O emulsion, with a viscosity at a shear rate of 10 s-1 and at 20°C of 0.01 Pas to 100,000 Pas, particularly preferably of 0.1 Pas, in particular 2.5 Pas, to 10,000 Pas.

18. Cosmetic formulation according to claim 16 or 17, wherein the cosmetic formulation contains as an additional component at least one polyol or at least one thickener selected from the group of polysaccharides, proteins, polyacrylates or silicates.

19. Cosmetic formulation according to one of claims 16-18, wherein the cosmetic formulation contains as an additional component at least two nitrogen-containing active ingredients and / or at least one thickener from the group of polysaccharides and / or at least one polyol and / or at least one hydrosol and has a turbidity of at least 60% and a total transmission of at least 80% when 3% of the cellulose acetate particles or the particles containing cellulose acetate are added, and / or has a turbidity of at least 98% and a total transmission of at least 60% when 9% of the cellulose acetate particles or the particles containing cellulose acetate are added.

20. Use of the composition according to any one of claims 1 to 15 or of a cosmetic formulation according to any one of claims 16-19 as (i) a carrier system for an active ingredient; and / or (ii) Absorbents for impurities, in particular filter media; and / or (iii) Cleaning agents; and / or (iv) dry shampoo; and / or (v) sunscreens; and / or (vi) functional filler for cosmetics and / or detergents; and / or (vii) pigment substitute and / or dispersing agent.

21. Method for the production of cellulose acetate particles or particles containing cellulose acetate, in particular a composition of Cellulose acetate particles or particles containing cellulose acetate according to any one of claims 1 to 15, wherein the method comprises: (a) Dissolving cellulose acetate with a total degree of acetyl substitution of 0.7 or more and 2.9 or less, preferably with a total degree of acetyl substitution of 1.8 or more and 2.6 or less, and more preferably with a total degree of acetyl substitution of 2.0 or more and 2.6 or less, in acetone or in an acetone-containing solvent; (b) Spraying the acetonic cellulose acetate solution at 50 °C or more and 165 °C or less; and (c) Removal of residual acetone from the cellulose acetate particles or particles containing cellulose acetate.

22. Method according to claim 21, wherein the process further comprises the process step of washing the cellulose acetate particles formed in process step b) or the particles containing cellulose acetate.

23. Method according to claim 21 or 22, wherein the process further comprises the process step of basic hydrolysis of the cellulose acetate particles formed in process step b) or particles containing cellulose acetate.

24. Method according to one of claims 21-23, wherein in process step (b) the acetone cellulose acetate solution is sprayed with a hot gas stream, wherein a volume flow of the hot gas is adjusted depending on a desired mean particle size of the cellulose acetate particles to be produced or the particles containing cellulose acetate, wherein in particular a higher volume flow of the hot gas is adjusted if a smaller mean particle size is desired for the cellulose acetate particles to be produced or for the particles containing cellulose acetate.

25. Method according to claim 24, wherein the temperature of the hot gas is regulated in particular such that before or during the injection of the acetonic cellulose acetate solution into the hot gas stream, the hot gas stream has a temperature between about 50 °C and about 165 °C.

26. Method according to claim 25, wherein the temperature of the hot gas is regulated in particular such that, after the acetonic cellulose acetate solution is sprayed into the hot gas stream, the hot gas stream has a temperature between about 30 °C and about 150 °C.

27. Method according to any one of claims 21 to 26, wherein, depending on a desired mean particle size of the cellulose acetate particles to be produced or of the particles containing cellulose acetate, in process step b) the acetone cellulose acetate solution is passed through at least one nozzle serving as an atomizer with a correspondingly adapted spray mass flow and with a correspondingly adapted spray concentration, wherein the nozzle preferably has a nozzle opening of 0.5 to 5.5 and in particular of about 1.0 to 3.0 mm.

28. Method according to claim 27, wherein, in order to produce cellulose acetate particles or particles containing cellulose acetate with a particularly average d50 particle diameter of about 80 nm to about 300 pm, the acetone cellulose acetate solution is passed in process step b) at a nozzle pressure of 1.5 bar to about 8 bar through at least one nozzle serving as an atomizer with a nozzle opening of 0.5 to 5.5 mm and in particular of about 1.0 to 3.0 mm; and / or wherein, in order to produce cellulose acetate particles or particles containing cellulose acetate with a particularly average d50 particle diameter of about 5 pm to about 100 pm, the acetone cellulose acetate solution is passed in process step b) at a nozzle pressure of about 1.5 bar to about 8 bar through at least one nozzle serving as an atomizer with a nozzle opening of about 0.5 mm to about 5.5 mm and in particular of about 1.0 mm to 3.0 mm.

29. Method according to any one of claims 21 to 28, wherein the proportion of cellulose acetate in the acetone cellulose acetate solution prior to spraying the acetone cellulose acetate solution in process step b) is 1.0 wt.% to about 25.0 wt.%, preferably about 1.5 wt.% to about 20 wt.%.

30. Method according to any one of claims 21 to 29, wherein the acetone cellulose acetate solution contains at least one active ingredient, in particular a pharmaceutical active ingredient and / or a cosmetic active ingredient, and / or UV filters.

31. Method according to any one of claims 21 to 30, wherein the acetonic cellulose acetate solution comprises at least one additive, in particular a nitrogen-containing additive.

32. Method according to any one of claims 21 to 31, wherein the acetonic cellulose acetate solution contains at least one second polysaccharide ester.

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