Capsule composition
Patent Information
- Authority / Receiving Office
- AU · AU
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2025-02-27
- Publication Date
- 2026-08-06
AI Technical Summary
Capsule compositions used in perfumes face issues with sedimentation, leading to aesthetic and functional problems, such as agglomeration and uneven fragrance delivery, and increasing viscosity to prevent sedimentation compromises pumpability and sprayability.
A capsule composition with specific density, viscosity, and shear stress parameters is developed, ensuring minimal creaming velocity and maintaining pumpability and sprayability, while avoiding sedimentation, using a matrix without alcohol and incorporating alkaline earth metal ions and chelating agents to enhance stability and fragrance release.
The composition provides a long shelf life, consistent fragrance delivery, and excellent pumpability and sprayability, allowing for uniform application as a mist without jetting, thereby enhancing user experience and product stability.
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Abstract
Description
[0001] Capsule Composition
[0002] Field of disclosure
[0003] The present disclosure lies in the field of encapsulation technology and relates in particular to a capsule composition, a perfume vial with such a capsule composition, a use of such a perfume vial and a method for producing a capsule composition.
[0004] Background, prior art
[0005] Capsules are commonly used for various different applications to encapsulate compounds of interest. For example, they can be used as pharmaceutical carriers for delivering and protecting drugs, in food applications to protect a flavor and release this flavor under specific conditions, such a mechanical force or heating, or also in the perfume industry to deliver and protect fragrances.
[0006] A perfume may for example comprise or consist of such a capsule composition. That is, the capsules encapsulate one or more fragrances and protect the fragrance for example from oxidation or evaporation. The capsules are suspended in a matrix which often contains alcohol, e.g. ethanol. Ethanol has however certain disadvantages, as it is harmful to the skin, in particular if the skin is irritated or damaged, and is further generally not desired by perfume users. Perfumes are commonly filled in a perfume vial which may consist of a base container and a nozzle unit mounted thereto. The nozzle unit may comprise a tube, a nozzle and a pumping mechanism which allows to suck the capsule composition into the tube and expel it from the nozzle. A major problem with capsule compositions being used in perfumes is to avoid that the capsule sediment in the vial. The time required for capsules to phase separate, more specifically sediment or cream, is considered as one of the factors of the shelf life of the capsule composition. Sedimentation or creaming of the capsules has not only disadvantageous aesthetic effects, but it also leads to capsule agglomeration and even capsule damage. Further, if the capsules sediment, the nozzle unit may only or at least majorly apply the matrix onto the user’s skin. However, since the fragrances are in the capsule and not or not only in the matrix, no or only a little portion of fragrances is delivered to the user’s skin. Further, if the capsules break before being applied, an undesired dosage of the fragrance will be applied. In contrast, if a suspension of capsules can be provided in which the capsules float and do not sediment, a constant and predetermined amount of capsules and matrix can be sucked into the nozzle unit and applied to the user’s skin. Providing dispersions with a satisfying shelf life and / or homogeneity is particularly hard to achieve. Although one may consider to merely increase the viscosity of the matrix to avoid sedimentation of the capsules, this will necessarily impair pumpability and sprayability of the capsule composition.
[0007] Summary of disclosure
[0008] It is the general object of the present disclosure to advance the state of the art in the field of encapsulation technology, in particular perfume technology, and preferably to overcome the disadvantages of the prior art fully or at least partly. In advantageous embodiments, a capsule composition is provided which has a long shelf life, i.e. avoids, or at least delays that capsules phase separate from the matrix, in particular sediment. In further advantageous embodiments, a capsule composition is provided which allows to be pumped and sprayed via a nozzle unit of a perfume vial. Further, a capsule composition is provided which can be applied via a nozzle unit of a perfume vial as a mist and avoids preferably to be applied as a jet. In particularly favorable embodiments these advantages are achieved concomitantly.
[0009] The general object is achieved by the subject-matter of the independent claims. Further advantageous embodiments follow from the dependent claims and the overall disclosure.
[0010] In a first aspect, the present disclosure relates to a capsule composition. In a second aspect, the present disclosure relates to a perfume vial. In a third aspect, the present disclosure relates to a method for producing a capsule composition. In a fourth aspect, the present disclosure relates to a use of a perfume vial, respectively a method for generating a mist with a perfume vial. In a fifth aspect of the disclosure refers to the use of a capsule composition as disclosed in any of the embodiments herein.
[0011] It is generally understood herein that the term “comprising” is interpreted as meaning that it includes those features following this term, but that it does not exclude the presence of other features, as long as they do not render the claim unworkable. On the other hand, if the wording "consist of" is used, then no further features are present apart from the ones following said wording. It is generally understood that if a range is provided herein, for example in the format “X to Y” or “between X and Y”, the boundary values X and Y are included in the claimed range, unless noted otherwise. Furthermore, the range formulations used herein, such as “X to Y”, “between X and Y”, “between X or Y”, are interchangeable and have the same meaning and scope. Such ranges extend over their full numerical range and include the boundary values X and Y unless noted otherwise.
[0012] The capsule composition may comprise, or in some embodiments consist of, a matrix and a plurality of capsules, which are suspended in the matrix. Thus, the matrix can be seen as the continuous phase and the plurality of capsules as the dispersed phase being suspended in the continuous phase. The matrix may comprise a solvent. The matrix may in some embodiments comprise a polymer composition.
[0013] In particular, the capsule composition may be a capsule composition for perfumes and / or comprise at least one fragrance. The fragrance may in some embodiments be encapsulated inside the capsules and may optionally be present or form their liquid core.
[0014] In some embodiments, the capsule composition may have a creaming velocity v of < (equal or less than) 2.5- 10-9m / s. The creaming velocity is defined by the following formula: wherein g is the gravitational constant [9.81 m / s2] r is the average radius of the capsules [m]
[0015] Pmatrix is the density of the matrix [kg / m3]
[0016] Pcapsuies is the average density of the capsules [kg / m3], which can be a calculated average density based on the capsule dimensions;
[0017] Hmatrix is the shear viscosity of the matrix at a shear rate of 0.01 s-1[Pa-s] is the volume packing of the capsules [%] in the capsule composition.
[0018] It is generally understood that the viscosities and densities as provided herein refer to the viscosities and densities at 20°C and at atmospheric pressure.
[0019] The capsule radius rmay be determined by staining the capsules with a dye to increase the contrast between the oil core, the capsule, and the surrounding media, and subsequently record a digital image with a microscope (Keyence VHX 7000) and determine the average dimensions of the capsules with a software.
[0020] The matrix density pmatnx may be determined gravimetrically averaging at least 10 repetitions of 1 mL of matrix. The capsule density Pcapsuie can be calculated based on the volume ratio of the core and the shell taken from the dimensions determined from light microscopy images.
[0021] The apparent shear viscosity rjmatrixmeasured for the matrix only may be taken from the rotational rheology experiments at a shear rate 0.01 s-1, as described herein.
[0022] Thus, the matrix density and viscosity may be selected such that the creaming velocity of < (equal or less than) 2.5- 10-9m / s is achieved. Such a creaming velocity has been found ideal to avoid or at least to delay that the capsules sediment. In particular, the capsules may have a capsule density pCaPsuies of 959 kg / m3to 1010 kg / m3, in particular 971 kg / m3to 1000 kg / m3, more particular 981 kg / m3to 995 kg / m3. In certain embodiments, the creaming velocity v of the capsule composition may be < (equal or less than) 2.0- 10-9m / s, in particular < (equal or less than) 1.3- 10-9m / s, more particular < (equal or less than) 9.5- 10-10m / s.
[0023] In some embodiments the creaming velocity v of the capsule composition may be > (equal or larger than) 7- 10-11m / s, in particular s (equal or larger than) 9 10-11m / s, more particular > (equal or larger than) 10-1° m / s.
[0024] In some embodiments the creaming velocity v of the capsule composition may be between
[0025] 2.5- 10-9m / s and 7- 10-11m / s, in particular between 2.5-10-9m / s and 9-10-11m / s, more particular between 2.5- 10-9m / s and 10-10m / s. In some embodiments the creaming velocity v of the capsule composition may be between 1 .3-10-9m / s and 7- 10-11m / s, in particular between 1.3- 10-9m / s and 9- 10-11m / s, more particular between 1.3- 10-9m / s and 10-10m / s. In some embodiments the creaming velocity v of the capsule composition may be between
[0026] 9.5- 1 O-10m / s and 7- 10-11m / s, in particular between 9.5-1 O-10m / s and 9- 10-11m / s, more particular between 9.5- 10-1° m / s and 10-10m / s.
[0027] The capsule composition may in some embodiments have a shear stress T, respectively yield stress, at a shear rate of 0.01 s-1of < (equal or less than) 50 Pa, in particular < (equal or less than) 25 Pa, more particular < (equal or less than) 15 Pa, even more particular of < (equal or less than) 10 Pa. Such a shear stress has been found to be beneficial as it allows to provide capsule compositions with satisfying pumpability and sprayability. The yield stress is the minimum stress at which flow occurs.
[0028] The shear stress T, respectively yield stress, can be determined according to the shear stress test method:
[0029] The apparent shear viscosity, shear stress and normal force can be determined in a shear rate controlled rotational rheology experiment varying the applied shear rate [s-1] from 0.01 s-1to 1000 s’1. Typically, the values may be taken as soon as a stable value over a time period of 15 s is determined. The shear viscosity may for example be measured according to ISO 3219-2:2021 ). The measurements can for example be performed on a MCR 501 (Anton Paar, Graz, Austria) equipped with a 50 mm cone-plate geometry or a 50 mm plateplate geometry for measuring the matrix alone or the capsule composition, respectively. The samples are placed with a cut plastic pipette onto the plate, the geometry is lowered until a gap of 0.0513 mm or 1 mm is reached for the matrix or the capsule composition, respectively. The excess sample is trimmed gently before starting the measurement. The measurements are conducted at 20°C and at ambient conditions (1 atm). The apparent shear viscosity is measured for the matrix only at a shear rate of 0.01 s’1, and is calculated by dividing the measured stress by the applied shear rate. The normal force for sprayability is taken from the same experiment but at an elevated shear rate of 0.1 s-1(normal force test method).
[0030] The shear stress (e.g. yield stress), defined as yield point is measured at a shear rate of 0.01 s-1exerted on the capsule composition (shear stress test method).
[0031] In some embodiments the shear stress T, respectively yield stress, at a shear rate of 0.01 s-1of the capsule composition may be > (equal or larger than) 0.1 Pa, in particular > (equal or larger than) 0.5 Pa, more particular > (equal or larger than) 1 Pa.
[0032] In some embodiments the shear stress T, respectively yield stress, at a shear rate of 0.01 s-1of the capsule composition may be between 50 Pa and 0.1 Pa, in particular between 50 Pa and 0.5 Pa, more particular between 50 Pa and 1 Pa. In some embodiments the shear stress T, respectively yield stress, at a shear rate of 0.01 s-1of the capsule composition may be between 15 Pa and 0.1 Pa, in particular between 15 Pa and 0.5 Pa, more particular between 15 Pa and 1 Pa. In some embodiments the shear stress T, respectively yield stress, at a shear rate of 0.01 s-1of the capsule composition may be between 10 Pa and 0.1 Pa, in particular between 10 Pa and 0.5 Pa, more particular between 10 Pa and 1 Pa.
[0033] In some embodiments, the capsule composition may be selected such that its yield point (being the point in the stress / strain curve where the material transitions from elastic to plastic deformation behavior, respectively the stress above which fluids begin to flow) at a shear rate of 0.01 s-1is between 0.1 and 10 Pa, in particular between 1 and 10 Pa. Such a yield point has been found to be beneficial as the resulting capsule composition show good pumpability and sprayability, while avoiding phase separation, in particular creaming, of the capsules.
[0034] In some embodiments the yield point at a shear rate of 0.01 s-1of the capsule composition may be > (equal or larger than) 0.1 Pa, in particular > (equal or larger than) 1 Pa, more particular s (equal or larger than) 10 Pa.
[0035] In some embodiments the yield point at a shear rate of 0.01 s-1of the capsule composition may be between 50 Pa and 0.1 Pa, in particular between 50 Pa and 0.5 Pa, more particular between 50 Pa and 1 Pa. In some embodiments the yield point at a shear rate of 0.01 s-1of the capsule composition may be between 15 Pa and 0.1 Pa, in particular between 15 Pa and 0.5 Pa, more particular between 15 Pa and 1 Pa. In some embodiments the yield point at a shear rate of 0.01 s-1of the capsule composition may be between 10 Pa and 0.1 Pa, in particular between 10 Pa and 0.5 Pa, more particular between 10 Pa and 1 Pa.
[0036] In some embodiments, the matrix of the capsule composition has a normal force FN,o.is“1at a shear rate of 0.1 s-1of > (more than) -0.1 N, in particular of > (more than) -0.10 N. Such a normal force of the matrix ensures a satisfying sprayability of the capsule compositions. In particular, it allows to apply the matrix (and the fragrance) as a mist and avoids to apply it as a jet, in particular when the capsule composition is used in a perfume vial, such as one of the embodiments of the second aspect of the disclosure. In particular embodiments, the matrix of the capsule composition has a normal force FN, o.is“1at a shear rate of 0.1 s-1of > (more than) -0.08 N, in particular of > (more than) -0.05 N, more particular of > (more than) -0.03 N. The normal force can for example be determined according to the normal force test method as described herein.
[0037] In some embodiments the normal force FN, o.is“1at a shear rate of 0.1 s-1of the matrix may be < (equal or smaller than) -0.001 N, in particular < (equal or smaller than) -0.005 N, more particular < (equal or smaller than) -0.01 N. In some embodiments the normal force FN, o.is“1at a shear rate of 0.1 s-1of the matrix may be between -0.1 N and -0.001 N, in particular between -0.1 N and -0.005 N, more particular between -0.1 N and -0.01 N. In some embodiments the normal force FN, o.is“1at a shear rate of 0.1 s-1of the matrix may be between -0.08 N and -0.001 N, in particular between -0.08 N and -0.005 N, more particular between -0.08 N and -0.01 N. In some embodiments the normal force FN, o.is“1at a shear rate of 0.1 s-1of the matrix may be between -0.03 N and -0.001 N, in particular between -0.03 N and -0.005 N, more particular between -0.03 N and -0.01 N.
[0038] A capsule composition having a creaming velocity v of < (equal or less than) 2.5- 10-9m / s and a shear stress T of < (equal or less than) 50 Pa and a matrix having a normal force FN, o.is“1at a shear rate of 0.1 s-1of more than -0.1 N is particularly advantageous, because such a combination of parameters provides a capsule composition with excellent shelf life (i.e. the time required for capsule sedimentation) of 1 year or more, but at the same time has an excellent sprayability and pumpability, such that it can for example be applied as a mist and not as a jet to the skin of a user and such that during pumping both the capsules and the matrix are sucked into the nozzle unit of a perfume vial and in particular not only or not majorly the matrix. Thus, these three parameters may in particular embodiments be fulfilled by a capsule composition according to the first aspect, thereby enabling a synergistic advantage which allows to provide an improved capsule composition for perfumes.
[0039] In some embodiments, the capsule composition and / or the solvent may be free of an alcohol, in particular an alkyl alcohol, such as C1-12 alkyl alcohols, e.g. ethanol.
[0040] In some embodiments, the solvent may comprise or consist of water.
[0041] In some embodiments the matrix may comprise at least one fragrance, in particular at least one water soluble fragrance, which is dissolved in the solvent, in particular water. In some embodiments, the matrix of the capsule composition may have viscosity n0 01 / s(at a shear rate of 0.01 s-1) of between 80 and 300 Pa-s, in particular of between 100 and 260 Pa-s, more particular of between 100 and 230 Pa-s. As noted above, the viscosity is the viscosity at 20 °C.
[0042] In some embodiments, the capsule composition further comprises alkaline earth metal ions, in particular Mg2+or Ca2+ions. The alkaline earth metal ions may for example be comprised, respectively dissolved in, the matrix. Additionally, or alternatively, it may also be possible that the alkaline earth metal ions are comprised in the capsule. The content of the alkaline earth metal ions in the matrix may be considered as the alkaline earth metal ion matrix fraction and the content of the alkaline earth metal ions in the capsules may be considered as the alkaline earth metal ion capsule fraction. The alkaline earth metal ions in the matrix and the capsules may be the same or different, e.g. the same or different kind.
[0043] In the matrix, the alkaline earth metal ions may induce gel formation, for example by reacting with a gelation agent. Thus, the alkaline earth metal ions may be considered as gelation inducing agents or cross-linkers which are configured to react with a gelation agent of the matrix, respectively the polymer composition.
[0044] In the capsules, the alkaline earth metal ions may also serve as gelation inducing agent. As will be further described below, the capsules may comprise a shell being made from a matrix forming agent which forms a matrix, in particular a water insoluble matrix, with alkaline earth metal ions such as Ca2+.
[0045] In some embodiments, the amount of alkaline earth metal ions, in particular the Ca2+ions, being comprised, e.g. dissolved, in the matrix of the capsule composition is between 0.01 wt.% to 2.0 wt.%, in particular between 0.01 wt.% and 1.0 wt.%, more particular between 0.01 wt.% and 0.5 wt.%. This amount may be considered as the alkaline earth metal ion matrix fraction. Such a concentration has been found particularly advantageous, because it may help to provide an optimal viscosity and creaming velocity of the capsule composition. In some embodiments, the total amount of alkaline earth metal ions, in particular Ca2+ions, in the capsule composition is larger than the amount of alkaline earth metal ions, in particular the Ca2+ions, being comprised, e.g. dissolved, in the matrix. The total amount of alkaline earth metal ions may for example consist of the sum of the amount of the alkaline earth metal ion matrix fraction and the alkaline earth metal ion capsule fraction.
[0046] In some embodiments, the total amount of alkaline earth metal ions, in particular Ca2+ions, in the capsule composition, i.e. the whole capsule composition, may be between 0.01 wt.% to 2.0 wt.%, in particular between 0.01 wt.% and 1.0 wt.%, more particular between 0.01 wt.% and 0.5 wt.%.
[0047] In some embodiments, the capsule composition, particularly the matrix, further comprises a chelating agent. In particular embodiments, the chelating agent may be configured to chelate alkaline earth metal ions, such as the alkaline earth metal ions present in the capsule composition and / or the capsules. For example, the chelating agent may be configured to chelate Ca2+ions. A suitable chelating agent may be a citrate, such as sodium citrate or any other suitable citrate, citric acid, EDTA (ethylenediaminetetraacetic acid), EGTA (ethylene glycol-bis(P-aminoethyl ether)-N,N,N',N'-tetraacetic acid)), EDDS (ethylenediamine-N,N'-disuccinic acid), salts of these or any other suitable chelating agents. Chelating agents can act as softener and may be used to fine tune parameters of the matrix, such as the viscosity. Further, the chelating agents can soften capsule shells which comprise alkaline earth metal ions. This can be advantageous to ensure that the capsules break in the nozzle unit and thus that the compound of interest, e.g. the fragrance(s), are released when the capsule composition is applied onto the skin of a user by means of a perfume vial, e.g. a perfume vial as described in the embodiments according to the second aspect of the disclosure.
[0048] In some embodiments, the amount of chelating agent of the capsule composition, in particular in the matrix, is between 0.05 wt.% and 0.5 wt.%, in particular between 0.05 wt.% and 0.4 wt.%, e.g. between 0.05 wt.% and 0.25 wt.%, more particular between 0.15 wt.% and 0.4 wt.%. These wt.% values refer to the amount in the capsule composition, the total capsule composition representing 100 wt.%. The addition of a chelating agent, in particular in such an amount, leads to capsule softening, which leads to low rupture force and thus helps to improve sprayability.
[0049] In some embodiments, the capsule composition, particularly the matrix, further comprises an alkali metal salt, in particular NaCI, for example only NaCI.
[0050] In some embodiments, the amount of the alkali metal salt, in particular NaCI, comprised in the matrix (the matrix being 100 wt.% to which the following ranges relate to), is between 0.02 wt.% and 0.4 wt.%, in particular between 0.02 wt.% and 0.2 wt.%, more particular between 0.02 wt.% and 0.1 wt.%. In some embodiments, the amount of the alkali metal salt, in particular NaCI, comprised in the matrix (the matrix being 100 wt.% to which the following ranges relate to), is between 0.05 wt.% and 0.4 wt.%, in particular between 0.05 wt.% and 0.2 wt.%, more particular between 0.05 wt.% and 0.1 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0051] In some embodiments, the polymer composition comprises or consists of one or more polymers. In particular, the polymers may be configured to form a gel upon reacting with a gelation-inducing agent, such as alkaline earth metal ions (e.g. Ca2+ions). Thus, the polymers may be considered as gelation agents. In some embodiments, the polymer composition comprises or consists of at least one negatively charged polymer. A negatively charged polymer may be a polymer comprising one or more negatively charged moieties, such as hydroxylates or carboxylates.
[0052] In some embodiments, the polymer composition comprises or consists of at least one polysaccharide. The polysaccharide may be present as a gel, in particular a gel comprising the polysaccharide and alkaline earth metal ions, such as Ca2+ions.
[0053] In some embodiments, the at least one polysaccharide may be selected from one or more of the following: gellan gum, in particular low acyl gellan gum, alginate, carrageenan, xanthan gum, pectin, starch, in particular modified starches, chitin, glycogen, galactogen, cellulose, amylose and inulin. In particular embodiments, the at least one polysaccharide may be selected from gellan gum (also known as gellan) and xanthan gum (also known as xanthan). In certain embodiments, gellan gum, in particular low acyl gellan gum, and xanthan gum may be the only polysaccharides and / or gelation agents in the matrix.
[0054] In some embodiments, the amount of the polymer composition comprised in the matrix is between 0.02 wt.% and 0.40 wt.%, in particular between 0.02 wt.% and 0.35 wt.%, in particular between 0.02 wt.% and 0.30 wt.%, in particular between 0.03 wt.% and 0.25 wt.%, more particular between 0.04 wt.% and 0.20 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0055] In some embodiments, the amount of the polymer composition comprised in the matrix is between 0.10 wt.% and 0.40 wt.%, in particular between 0.20 wt.% and 0.35 wt.%, in particular between 0.20 wt.% and 0.30 wt.%, in particular between 0.20 wt.% and 0.25 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0056] In certain embodiments, the amount of the polymer / polymers, in particular gelation agents, comprised in the matrix which is / are configured to form a gel upon reacting with a gelationinducing agent gel is between 0.02 wt.% and 0.40 wt.%, in particular between 0.02 wt.% and 0.35 wt.%, in particular between 0.02 wt.% and 0.30 wt.%, in particular between 0.03 wt.% and 0.25 wt.%, more particular between 0.04 wt.% and 0.20 wt.%, These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0057] In certain embodiments, the amount of the polymer / polymers, in particular gelation agents, comprised in the matrix which is / are configured to form a gel upon reacting with a gelationinducing agent gel is between 0.10 wt.% and 0.40 wt.%, in particular between 0.20 wt.% and 0.35 wt.%, in particular between 0.20 wt.% and 0.30 wt.%, in particular between 0.20 wt.% and 0.25 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%. In certain embodiments, the amount of the polymer / polymers, in particular gelation agents, comprised in in the matrix may be between 0.10 wt.% and 0.40 wt.%, in particular 0.10 wt.% to 0.30 wt.%, in particular between 0.10 wt.% and 0.25 wt.%, in particular between 0.15 wt.% and 0.25 wt.%, more particular between 0.15 wt.% and 0.22 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0058] In certain embodiments, the amount of the at least one polysaccharide comprised in the matrix is between 0.02 wt.% and 0.40 wt.%, in particular between 0.02 wt.% and 0.35 wt.%, in particular between 0.02 wt.% and 0.30 wt.%, in particular between 0.03 wt.% and 0.25 wt.%, more particular between 0.04 wt.% and 0.20 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0059] In certain embodiments, the amount of the at least one polysaccharide in the matrix may be between 0.10 wt.% and 0.40 wt.%, in particular between 0.10 wt.% and 0.30 wt.%, in particular between 0.10 wt.% and 0.25 wt.%, in particular between 0.15 wt.% and 0.25 wt.%, more particular between 0.15 wt.% and 0.22 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0060] In certain embodiments, the amount of the at least one negatively charged polymer of the matrix is between 0.02 wt.% and 0.40 wt.%, in particular between 0.02 wt.% and 0.35 wt.%, in particular between 0.02 wt.% and 0.30 wt.%, in particular between 0.03 wt.% and 0.25 wt.%, more particular between 0.04 wt.% and 0.20 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0061] In certain embodiments, the amount of the at least one negatively charged polymer in the matrix may be between 0.10 wt.% and 0.25 wt.%, in particular between 0.15 wt.% and 0.25 wt.%, more particular between 0.15 wt.% and 0.22 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0062] In some embodiments, the polymer composition of the matrix comprises or consists of two gelation agents, in particular two polysaccharides. In some embodiments, the polymer composition of the matrix comprises or consists of gellan gum and xanthan gum.
[0063] In particular embodiments, the amount of xanthan gum comprised in the matrix is between 0.02 wt.% and 0.25 wt.%, in particular between 0.02 wt.% and 0.20 wt.%, more particular between 0.03 wt.% and 0.15 wt.%. These wt.% refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0064] In particular embodiments, the amount of xanthan gum comprised in the matrix is between 0.02 wt.% and 0.10 wt.%, in particular between 0.03 wt.% and 0.10 wt.%. These wt.% refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0065] In certain embodiments, the amount of gellan gum comprised in the matrix is between 0.02 wt.% and 0.20 wt.%, in particular between 0.05 wt.% and 0.15 wt.%, more particular between 0.10 wt.% and 0.15 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0066] In certain embodiments, the amount of gellan gum comprised in the matrix is between 0.02 wt.% and 0.17 wt.%, in particular 0.02 wt.% and 0.09 wt.%, in particular between 0.02 wt.% and 0.08 wt.%. These wt.% values refer to the amount in the matrix, the total matrix representing 100 wt.%.
[0067] In some embodiments, the amount of xanthan gum comprised in the matrix is less than the amount of gellan gum in the matrix.
[0068] In some embodiments, the capsule composition, in particular the matrix, additionally comprises one or more anti-freezing agents. The anti-freezing agent may be configured to lower the melting point of the capsule composition, in particular below 0 °C, more particular below -10 °C. A suitable anti-freezing agent may for example by glycerol. In certain embodiments, the amount of the anti-freezing agent in the capsule composition is 1 wt.% to 15 wt.%, in particular 1 wt.% to 10 wt.%, more particular 1 wt.% to 6 wt.%. These wt.% values refer to the amount in the capsule composition, the total capsule composition representing 100 wt.%. In some embodiments, the capsule composition comprises 2, in particular exactly 2, anti-freezing agents. In some embodiments, the capsule composition may comprise glycerol and propylene glycol as two anti-freezing agents. In particular, the 2 anti-freezing agents may be present in the same amounts (e.g. the same wt. %). Together, the 2 anti-freezing agents may in some embodiments be present in the capsule composition in an amount of is 1 wt.% to 15 wt.%, in particular 1 wt.% to 10 wt.%, more particular 1 wt.% to 6 wt.%. For example, if the amount of the 2 anti-freezing agents together is 1 wt.%, each of them may be present in an amount of 0.5 wt.% in embodiments in which they are present in the same amounts. It has been observed that using 2 anti-freezing agents and in particular glycerol and propylene glycol together, cold temperatures, e.g. below freezing point, capsule breaking is avoided. For example, even though glycerol alone can be used, it has been observed that the better creaming properties can be achieved for the capsule composition with the combination of 2 anti-freezing agents, such as glycerol and propylene glycol.
[0069] In some embodiments, the capsule composition comprises a pH adjustment agent. A pH adjustment agent is configured to adjust the pH of the capsule composition. For example, a Bronsted acid or Bronsted base can be used as pH adjustment agent. A pH adjustment agent may for example be a buffer system, respectively a buffer. For example, lactic acid may be added as pH adjustment agent. Other pH adjustment agents which may be used are phytic acid, ascorbic acid or Tris (tris(hydroxymethyl)aminomethane). In some embodiments, a pH adjustment agent is present such that the pH of the capsule composition is between pH 4 and 6. In particular pH 4.5 to 5.5, in particular pH 5. In some embodiments, the amount of the pH adjustment in the capsule composition is between 0.1 to 2 wt.%, in particular 0.5 to 1 wt.%.
[0070] In some embodiments, the capsule composition and in particular the matrix, may comprise one or more preservatives, such as propylene glycol, alkyl parabens, such as propylparaben or methylparaben, diazolidinyl urea, chlorphenesin (CAS 104-29-0), ethylhexylglycerin, phenoxyethanol and / or hexandediol. In certain embodiments, the amount of preservative in the capsule composition may be between 0.1 wt.% and 3 wt.%, in particular between 0.3 wt.% and 2.2 wt.%, more particular between 0.4 wt.% and 1.9 wt.%. These wt.% values refer to the amount in the capsule composition, the total capsule composition representing 100 wt.%.
[0071] In some embodiments, the capsule composition and in particular the matrix and / or the capsules may comprise a dye, in particular a water soluble dye.
[0072] In some embodiments, the capsule composition and in particular the matrix and / or the capsules may comprise a humectant, such as hyaluronic acid (e.g. 0.5 wt.% to 2 wt.%, i.e. of the capsule composition) or panthenol (1 wt.% to 5 wt.%, i.e. of the capsule composition), or glycerin or lactic acid.
[0073] In some embodiments, the capsules of the plurality of capsules have an average capsule diameter, in particular average maximum diameter, of 150 pm to 3000 pm, in particular 200 pm to 2500 pm, more particular 250 pm to 2000 pm, more particular 500 pm to 2000 pm, even more particular 750 pm to 1500 pm. In some embodiments, the capsules of the plurality of capsules have an average capsule diameter, in particular average maximum diameter, of 150 pm to 3000 pm, in particular 200 pm to 3000 pm, more particular 250 pm to 3000 pm, more particular 500 pm to 3000 pm, even more particular 750 pm to 3000 pm. The term “maximum diameter” refers to the longest line between the outside of opposing wall / shell sections of the capsule, which typically extends through the center of the capsule. The capsule diameter can be obtained from light microscopy images of the capsules. The capsules may in this, or any other embodiment described herein, particularly have a spherical shape.
[0074] In some embodiments, each capsule of the plurality of capsules has a capsule diameter, in particular maximum diameter, of 150 pm to 3000 pm, in particular 200 pm to 2500 pm, more particular 250 pm to 2000 pm, more particular 500 pm to 2000 pm, even more particular 750 pm to 1000 pm. In some embodiments, each capsule of the plurality of capsules has a capsule diameter, in particular maximum diameter, of 150 pm to 3000 pm, in particular 200 pm to 3000 pm, more particular 250 pm to 3000 pm, more particular 500 pm to 3000 pm, even more particular 750 pm to 3000 pm. The term “maximum diameter” refers to the longest line between opposing wall sections of the capsule, which typically extends through the center of the capsule.
[0075] In some embodiments, the capsules of the capsule composition have an equal size distribution with respect to their capsule diameter, in particular maximum capsule diameter, with a coefficient of variation of 10% or less, in particular 8% or less, more particular of 5% or less. The skilled person understands that the coefficient of variation may be calculated by the ratio of the standard deviation o to the mean p, i.e. the average capsule size of the capsules of the assembly.
[0076] In some embodiments, the amount of capsules in the capsule composition is at least 10 wt.%, in particular at least 15 wt.%, in particular at least 20 wt.%, in particular at least 30 wt.%. These values refer to the capsule composition (the capsule composition being 100 wt.%). In some embodiments, the remaining wt.% (i.e. 100 wt.% - the wt.% of the capsules) is the amount of the matrix.
[0077] In some embodiments, the amount of capsules in the capsule composition is at most 70 wt.%, in particular at most 60 wt.%, in particular at most 55 wt.%, in particular at most 50 wt.%. These values refer to the capsule composition (the capsule composition being 100 wt.%). In some embodiments, the remaining wt.% (i.e. 100 wt.% - the wt.% of the capsules) is the amount of the matrix. A capsule amount of 60 wt.% or less, and in particular 50 wt.% or less, avoids that capsules contact each other and thus avoids capsule agglomeration and damage over time.
[0078] In some embodiments, the amount of capsules in the capsule composition is 10 wt.% to 65 wt.%, in particular 20 wt.% to 60 wt.%, more particular 25 wt.% to 55 wt.%. These values refer to the capsule composition (the capsule composition being 100 wt.%). In some embodiments, the remaining wt.% (i.e. 100 wt.% - the wt.% of the capsules) is the amount of the matrix. In some embodiments, the amount of capsules in the capsule composition is 10 wt.% to 60 wt.%, in particular 10 wt.% to 55 wt.%, more particular 15 wt.% to 50 wt.%. These values refer to the capsule composition (the capsule composition being 100 wt.%). In some embodiments, the remaining wt.% (i.e. 100 wt.% - the wt.% of the capsules) is the amount of the matrix.
[0079] In some embodiments the capsules each comprise a shell (i.e. a capsule shell). The shell may in some embodiments encase a liquid core. The liquid core may in particular be an oil core. The oil core may comprise one or more liquid oils. It is understood that the term “liquid” refers to the state at normal conditions (1 atm. and 20 °C). Typically, the shell peripherally completely surrounds the oil core. The shell may be configured such that the oil core is retained inside the shell. The oil core of the capsules may be arranged in a core compartment being encompassed and delimited by the shell. The diameter of the core compartment of the capsules, e.g. the maximum distance of opposing shell portions, of 100 pm to 2500 pm, in particular 350 pm to 1500 pm, more particular 500 pm to 900 pm.
[0080] The shell may be made from a shell matrix, in particular a water insoluble matrix, that is the shell is a water insoluble matrix shell. In particular embodiments, the shell may comprise or consist of a matrix forming agent, such as a polysaccharide, and a gelation-inducing agent, such as alkaline earth metal ions. The matrix forming agent and the gelation-inducing agent may be configured to react together to form the shell matrix, e.g. water insoluble matrix. For example, the matrix forming agent may undergo an ionic bond with the gelation-inducing agent to form the shell matrix, e.g. water insoluble matrix. As a representative example, a polysaccharide, such as an alginate may form an ionic bond with alkaline earth metal ions, which may generally be Mg2+, Ca2+or Sr2+, in particular Ca2+. The capsules may be capsules and may be obtained as described in WO 2022 106361 A1 of the applicant, which is included by reference in its entirety. The water solubility may for example refer to the solubility in water at maximum 40 °C, in particular at maximum 30 °C.
[0081] The capsules may have a density of 935 kg / m3to 1010 kg / m3, in particular 965 kg / m3to 999 kg / m3. In some embodiments, the capsules have a shell thickness of the shell of 50 pm to 350 pm , in particular 65 pm to 275 pm, more particular 80 to 200 pm.
[0082] In some embodiments, the volume of the oil core with reference to the total capsule volume is 30% to 60%, in particular 40% to 60%.
[0083] In some embodiments, the capsules comprise at least one compound of interest. The compound of interest may in particular be a fragrance. A fragrance may for example be a compound which is configured to bind to a receptor within the human nasal cavity and triggering thereby the transmission of a signal through the olfactory system of the human. It may also be possible that the capsules comprise a plurality of different fragrances, such as a perfume formulation.
[0084] In some embodiments, the compound of interest, in particular the one or more fragrances, may be arranged in the liquid core, in particular the oil core. An oil core is advantageous, because the vast majority of compounds of interest and in particular fragrances, are soluble in an oil phase and not in an aqueous phase. Thus, the compound of interest, in particular the one or more fragrances, may be dissolved in the oil of the oil core. Thus, the fragrance (and therefore also the liquid core) may be encapsulated by the capsule shell.
[0085] As noted above, the capsules of the capsule composition may comprise a core, e.g. a liquid core. In some embodiments, the core, e.g. liquid core, comprises 50 wt.% or more, in particular 75 wt.% or more, in particular 85 wt.% or more of the compound of interest, in particular the one or more fragrances. These wt.% refers to the content of the core, e.g. liquid core (its whole content being 100 wt.%.
[0086] The one or more oils of the oil core may be selected from medium-chain triglyceride (MCT), menthol, vegetable oil, such as sunflower oil, olive oil, castor oil, canola (rapeseed) oil, soybean oil, peanut oi, isopropyl myristate, Iso E Super (CAS 54464-57-2), Hedione (CAS 246-495-9) , Linalool (CAS 78-70-6), Dipentene (138-86-3). The second aspect of the present disclosure relates to a perfume vial. The perfume vial may comprise a base container. The perfume vial may also comprise a capsule composition, in particular a capsule composition as described in any of the embodiments herein, such as with respect to the first aspect.
[0087] The perfume vial may also comprise a nozzle unit. The nozzle unit may be mounted to the perfume vial, in particular releasably mounted and / or in a form locking and / or force locking manner. Typically, the nozzle unit may be threaded on the base container. The base container may comprise an opening, in particular only a single opening, which is closed by the nozzle unit. For example, the base container may comprise a thread element which encompasses the opening. The nozzle unit may also comprise a thread element which engages with the thread element of the base container such that a form-locking connection is realized.
[0088] In some embodiments, the nozzle unit comprises a nozzle. The nozzle may be configured to transform the capsule composition into a mist which may particularly be expelled from the nozzle. In some embodiments, the nozzle unit may also comprise a tube, such as a polymer or metal tube, which extends from the nozzle into the capsule composition being arranged in the base container. The tube may be connected to the nozzle unit. In some embodiments, the tube may extend to a bottom portion of the base container, in particular from the nozzle. The tube may have the shape of a hollow cylinder, in particular a hollow circular cylinder.
[0089] In some embodiments, the tube may have a cross-sectional open area of 0.19 mm2to 1.77 mm2in particular 0.50 mm2to 1.13 mm2. Typically, the cross-sectional open area may be in this range along the whole tube length.
[0090] In some embodiments, the tube may have a tube diameter of 200 to 2000 pm, in particular 500 pm to 1500 pm, more particular 800 pm to 1200 pm. Typically, the tube diameter may be in this range along the whole tube length. In some embodiments, the nozzle unit comprises a pumping mechanism. The pumping mechanism may be configured for pumping the capsule composition into the nozzle and particularly further expel it from the nozzle. The pumping mechanism may be any pump mechanism which can fulfill this function. For example, a crimp type pumping mechanism can be used. A crimp type pumping mechanism may in certain embodiments comprise a pump body and pump head which can be moved into the pump body. Further, it may comprise a piston which can be moved towards the base body of the perfume vial against a biasing element such as a spring. By movement of the piston, an overpressure in the base body and / or base container may be generated and when the piston is forced to return in its original position its content (e.g. capsule composition) is forced into the tube and out of the nozzle. It may also be possible that a suction in the base body and / or base container is generated. Alternatively, the pumping mechanism may comprise a collapsible element which can be pressed and collapsed thereby providing an overpressure in the base body and / or base container and forcing the capsule composition into the tube and the nozzle.
[0091] A third aspect of the present disclosure relates to a method for producing a capsule composition, in particular a capsule composition as described in any of the embodiments herein, such as the embodiments of the first aspect.
[0092] The method may comprise dissolving a polymer composition in a solvent to form a matrix (dissolving step). The method may further comprise adding a plurality of capsules to the matrix, in particular under mixing, such as stirring (capsule addition step).
[0093] Dissolving the polymer composition may in some embodiments be performed by heating the solvent and / or the mixture of the polymer composition and solvent, above 20 °C, in particular above 25 °C, more particular above 40 °C, even more particular above 60 °C. Heating may be performed such that the polymer composition is completely dissolved in the solvent. However, heating may be performed in some embodiments up to at most 100 °C, more particular at most 80 °C. Thus, preferably, heating may be performed to a temperature of 70 to 90 °C. It is understood that the components used in the method may be the same as described herein above with respect to the first aspect of the disclosure. For example, it is clear that the polymer composition may comprise or consist of one or more polymers and / or that the solvent may be water.
[0094] In some embodiments, heating the solvent and / or the mixture of the polymer composition and solvent, may be performed for a heating time interval to form the matrix, such as 1 to 30 min. It is understood that the corresponding temperature to which the solvent and / or mixture is heated is maintained during the heating time interval. In certain embodiments, after the heating interval, the matrix is cooled, in particular to ambient temperature. The ambient temperature refers to the temperature of the surrounding environment, e.g. 20 °C to 25 °C. For example, the matrix may be actively cooled by suitable cooling means or it may be allowed to cool to ambient temperature by itself. The heating and cooling step may both be sub-steps of the dissolving step.
[0095] In some embodiments, the matrix is stirred, e.g. in an optional additional stirring step, before the capsules are added and in particular after the heating and optionally after cooling. In particular, the matrix is stirred with a dissolver disc. In certain embodiments, stirring is performed such that the matrix becomes homogenous. Thereby, the gel is broken, which reduces the viscosity of the matrix and thereby allows to achieve a satisfying pumpability and sprayability.
[0096] In particular the polymers may be configured to form a gel upon reacting with a gelationinducing agent, such as alkaline earth metal ions (e.g. Ca2+ions). Thus, the polymer may be a gelation agent, respectively the polymer composition may comprise a gelation agent. The gelation agent may be configured to form a gel, in particular upon reaction with a gelation-inducing agent.
[0097] In some embodiments, one or more preservatives are added, such as a preservative as described herein above. The one or more preservatives may in some embodiments be added after mixing, i.e. the optional additional mixing step, and preferably before the capsules are added. In addition to the preservatives or also alternatively thereto, at least one anti-freezing agent may be added, in particular an anti-freezing agent as described herein above.
[0098] In some embodiments, the polymer composition comprises or consists of at least one negatively charged polymer. A negatively charged polymer may be a polymer comprising one or more negatively charged moieties, such as hydroxyl (-O-) or carboxylates (-COO-). In certain embodiments, the polymer composition comprises or consists of at least one gelation agent. In some embodiments, the polymer composition comprises or consists of at least one polysaccharide. The polysaccharide may be present as a gelation agent being configured to form a gel upon reaction with a gelation-inducing agent. In some embodiments, the at least one polysaccharide may be selected from one or more of the following: gellan gum, alginate, carrageenan, xanthan gum, pectin, starch, in particular modified starches, chitin, glycogen, galactogen, cellulose, amylose and inulin. In particular embodiments, the at least one polysaccharide may be selected from gellan gum (also known as gellan) and xanthan gum (also known as xanthan). In certain embodiments, gellan gum and xanthan gum may be the only polysaccharides and / or gelation agents in the polymer composition.
[0099] In some embodiments, a gelation-inducing agent is added, in particular to the solvent e.g. before or after the polymer composition has been added, or before or after adding the plurality of capsules. The gelation-inducing agent may for example comprise alkaline earth metal ions. The gelation-inducing agent may in specific examples comprise alkaline earth metal salts, such as CaCh or MgCh. In some embodiments, the gelation-inducing agent is added when the solvent is heated (e.g. above 20 °C, in particular above 25 °C, more particular above 40 °C). This avoids the formation of agglomerated granulates.
[0100] In some embodiments, the gelation-inducing agent may be added after or during heating and / or before cooling, i.e. before the cooling step described above. In certain embodiments, the gelation-inducing agent, such as CaCl2, may be added as an aqueous solution, such as a 0.1 to 1 M, in particular 0.25 to 0.75 M solution.
[0101] In some embodiments, a chelating agent is added, in particular to the solvent e.g. before or after the polymer composition has been added, or before or after adding the plurality of capsules. The chelating agent may be configured to chelate alkaline earth metal ions, such as the alkaline earth metal ions present in the capsule composition and / or the capsules. The chelating agent may be a chelating agent as described herein above. In particular, the chelating agent may be added after mixing, i.e. the optional additional mixing step.
[0102] In some embodiments, the polymer composition, the solvent and the plurality of capsules, and optionally also the gelation inducing-agent and the chelating agent, are selected such that and / or in such an amount that the capsule composition may have a creaming velocity v of < (equal or less than) 2.5 10-9m / s, in particular < (equal or less than) 1.3- 10-9m / s, more particular < (equal or less than) 9.5- 10-10m / s.
[0103] In some embodiments, the polymer composition, the solvent and the plurality of capsules, and optionally also the gelation inducing-agent and the chelating agent, are selected such that and / or in such an amount that the capsule composition may have a shear stress T at a shear rate of 0.01 s-1of < (equal or less than) 50 Pa, in particular less than 25 Pa, more particular less than 15 Pa, even more particular of less than 10 Pa.
[0104] In some embodiments, the polymer composition, the solvent and the plurality of capsules, and optionally also the gelation inducing-agent and the chelating agent, are selected such that and / or in such an amount that the capsule composition has yield point (being the point in the stress / strain curve where the material transitions from elastic to plastic deformation behavior, respectively the stress above which fluids begin to flow) at a shear rate of 0.01 s-1of 0.1 to 15 Pa, in particular of 0.1 to 10 Pa, more particular of 1 to 10 Pa.
[0105] In some embodiments, the polymer composition and the solvent, and optionally also the gelation inducing-agent and the chelating agent, are selected such that and / or in such an amount that the matrix may have a normal force FN,o.is“1at a shear rate of 0.1 s-1of > (more than) -0.1 N, in particular > (more than) -0.10 N.
[0106] In specific embodiments, the method may comprise the steps of: a. Dissolving a polymer composition in a solvent to form a matrix, in particular by mixing the polymer composition and the solvent, e.g. under stirring, wherein dissolving optionally comprises i. Heating the solvent and / or the mixture of the polymer composition and the matrix, in particular for a heating interval, to form the matrix; ii. Optional addition of a gelation-inducing agent to the formed matrix; ill. Subsequent cooling of the formed matrix, in particular to ambient temperature, such as 20 °C to 25 °C, wherein cooling may particularly be performed after addition of the gelation-inducing agent; b. Stirring the formed, and in particular cooled, matrix. This stirring may be an additional and / or another stirring step. For example, this stirring may be performed by stirring the formed matrix with a dissolver disc. In certain embodiments, stirring is performed such that the matrix becomes homogenous; c. Optionally adding one or more preservatives and / or at least one anti-freezing agent and / or at least one chelating agent; d. Adding the plurality of capsules.
[0107] The designations a., b. c. d. and i. ii. ill. may in some embodiments indicate the order of steps. That is, in some embodiments, step a. is performed before step b., step b. is performed before step c., and step c. may be performed before step d.. Further, in specific embodiments sub-step i. may be performed before sub-step ii., and sub-step ii. may be performed before sub-step iii. However, this does not necessarily have to be the case. In certain embodiments, for example, step c. may be performed after step d. It may also be possible that the gelation inducing-agent in sub-step ii. may be added during step i..
[0108] A fourth aspect of the present disclosure relates to the use of perfume vial, such as a perfume vial as described in any of the embodiments herein, e.g. the second aspect of the disclosure. The use may also be considered as a method for generating a mist or a method of applying a mist on a subject.
[0109] The perfume vial may be used to generate a mist. The mist may in particular comprise or consist of portions of the matrix and the capsules. In particular, the mist may comprise one or more fragrances, i.e. the one or more fragrances which may have been comprised in the capsules, respectively their liquid core. The mist may also comprise the oil of the liquid oil core of the capsules. As understood, a mist is not the same as a jet. A jet is a constant stream of liquid, while a mist may comprise or consist of a plurality of droplets, such a submicron (less than 1000 micrometers) sized droplets. The droplet size may be the diameter, e.g. the maximum diameter of a droplet. In particular, the droplets may have a droplet size of less than 800 pm, in particular less than 400 pm, more particular less than 200 pm.
[0110] In some embodiments, the mist may be expelled from the nozzle of the nozzle unit. In some embodiments, the mist may be applied on a subject, such as on the skin of a subject.
[0111] In some embodiments, the generation of the mist comprises to guide a portion of the capsule composition, particularly capsules and matrix, into the nozzle unit, particularly into the tube and from there to the nozzle.
[0112] In some embodiments, the capsules are ruptured within the nozzle unit, such as in the tube and / or in the nozzle. In some embodiments the ruptured capsules are expelled from the nozzle unit, in particular the nozzle as capsule fragments. Rupturing of the capsules in the nozzle unit has the advantage that the compounds of interest, such as the fragrances, are only released shortly before applying the mist onto a subject. This ensures that a constant formulation is applied and avoids deterioration of the compound(s) of interest. Thus, in specific embodiments, the capsules may comprise a fragrance and the fragrance may be liberated during rupturing of the capsules and expelled from the nozzle unit, e.g. the nozzle, in particular as part of the generated mist.
[0113] A fifth aspect of the disclosure refers to the use of a capsule composition as disclosed in any of the embodiments herein, in particular for applying a fragrant to a user’s skin or for producing a perfume.
[0114] Brief description of the figures
[0115] The herein described disclosure will be more fully understood from the detailed description given herein below and the accompanying drawings which should not be considered limiting to the disclosure described in the appended claims. The drawings are showing:
[0116] Fig. 1 a microscopic image of a capsule composition according to an embodiment of the disclosure;
[0117] Fig. 2 a perfume vial according to an embodiment of the disclosure;
[0118] Fig. 3 illustrates the difference between a jet spray and a mist spray in a photograph
[0119] (left) and a schematic drawing (right);
[0120] Fig. 4 a shear rate / shear stress diagram for different samples.
[0121] Exemplary embodiments
[0122] Fig 1 shows a capsule composition 1 comprising a matrix 2 and a plurality of capsules 3. Capsules 3 comprise each a shell which encases a liquid oil core. The liquid oil core contains an oil and a compound of interest, such as one or more fragrances. Fig. 2 shows a perfume vial 10 comprising base container 1 1 and a nozzle unit 12. Nozzle unit 12 comprises tube 14 and nozzle 13 through which the capsule composition, respectively the ruptured capsule composition, can be expelled from perfume vial 10. Nozzle unit 12 further comprises a pumping mechanism, which is in this embodiment of the crimp type. It comprises pump body 15 and pump head 16 which can be moved into pump body 15 by pushing it downwards towards base container 11 . Further, it comprises piston 17 which can be moved towards base body 1 1 together with pump head 16 against biasing element 18 such as a spring. By movement of piston 17, an overpressure in the base body and / or base container may be generated and when the piston is forced to return in its original position the capsule composition is forced into tube 14 and then through nozzle 13 and expelled therefrom as a mist. Typically, on their way through nozzle unit 12, e.g. through tube 14 and nozzle 13, the capsules 3 are ruptured and break, thereby releasing their contents, such as a fragrance being arranged in the liquid oil core.
[0123] Fig. 3 shows the difference between a jet and a mist exiting a nozzle of a perfume vial. While in Fig. 3a a jet is shown, which comprises one or more continuous liquid streams, Fig. 3b shows the generation of a mist as it is the case in certain use embodiments of the disclosure. The mist comprises a plurality of droplets, with droplet sizes below 800 micrometers, in particular less than 400 pm, in particular less than 200 pm. The droplet size may for example be determined by laser diffraction or image analysis, in particular laser diffraction.
[0124] Fig. 4 shows a shear rate / shear stress diagram for 5 different capsule compositions (samples 10, 8, 7, 4 and 9).
[0125] Examples
[0126] General
[0127] Kelcogel CG-LA (gellan gum, CAS 71010-52-1 ) can be obtained from CP Kelco. Keltrol CG-
[0128] T (xanthan gum, CAS 1 1138-66-2) can be obtained from CP Kelco. To produce the samples the polymers (e.g. Kelcogel and Keltrol) are dissolved in water (amounts, see tables below). The mixture is then heated to 80 °C to achieve solubilization. Then a cross-linker (e.g. CaCh) is added while stirring and the mixture is allowed to cool without mixing to induce gelling. Then, the mixture is mixed to break the gel, e.g. by a dissolver disk until the mixture is homogeneous. Other additives (such as sodium citrate, preservatives, sodium chloride, hexanediol, or water soluble fragrances) are then added. Thereafter, the plurality of capsules is added under stirring.
[0129] Capsules having an oil core which includes a compound of interest, such as a fragrance can be obtained by the methods described in WO 2022 106 361 A1 (application number PCT / EP2021 / 081705) which is included herein by reference in its entirety and in particular with respect to the recipes disclosed therein with respect to table 1 , 2 and 3. After production, the capsules are isolated (e.g. separated from any remaining continuous phase) and used as described above. If the oil core shell contains one or more compounds of interest, such as a fragrance, the one or more compounds of interest are present in the oil phase used. It is understood that any possible oil phase can be used.
[0130] All rheological measurements were performed on a MCR 501 (Anton Paar, Graz, Austria) equipped with a 50 mm cone-plate geometry or a 50 mm plate-plate geometry for measuring the matrix alone or the capsule composition, respectively. The samples were placed with a cut plastic pipette onto the plate, the geometry was lowered until a gap of 0.0513 mm or 1 mm was reached for the matrix or the capsule composition, respectively. The excess sample was trimmed gently before starting the measurement. The measurements were conducted at 20 °C and at ambient conditions (1 atm).
[0131] The apparent shear viscosity, shear stress and normal force were all determined in a shear rate controlled rotational rheology experiment varying the applied shear rate [s-1] from 0.01 s-1to 1000 s’1. The shear viscosity may for example be measured according to ISO 3219- 2:2021 ). The apparent shear viscosity is measured for the matrix only at a shear rate of 0.01 s-1and is calculated by dividing the measured stress by the applied shear rate. The critical normal force for sprayability is taken from the same experiment but at an elevated shear rate of 0.1 S’1.
[0132] The shear stress (i.e. yield stress), defined as yield point is measured at a shear rate of 0.01 s-1exerted on the capsule composition.
[0133] The creaming velocity is calculated based on the Stoke’s law adjusted by Richardson-Zaki (Source: ISBN 3-527-30743-5):
[0134] The gravitational constant g of 9.81 m / s2is used for all cases.
[0135] The capsule radius r is determined by staining the capsules with a dye to increase the contrast between the oil core, the capsule, and the surrounding media, and subsequently record a digital image with a microscope (Keyence VHX 7000) and determine the average dimensions of the capsules with a software.
[0136] The matrix density pmatrix is determined gravimetrically averaging at least 10 repetitions of 1 mL of matrix. The capsule density Pcapsuie is calculated based on the volume ratio of the core and the shell taken from the dimensions determined from light microscopy images.
[0137] The apparent shear viscosity p matrix measured for the matrix only is taken from the rotational rheology experiments at a shear rate 0.01 s’1.
[0138] The capsule volume packing is approximated by formulating the capsule composition using the wt.% ratio of sieved and drained capsule only, not having any excess surrounding media. Sample 1
[0139] In the following tables, different capsule compositions are provided. The tables show the composition and wt.% of the components of the matrix. To produce the capsule composition of sample 1 , the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 570 pm, an average capsule diameter of 770 pm, a density 983 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved. Sample 2
[0140] To produce the capsule composition of sample 2, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 570 pm, an average capsule diameter of 820 pm, a density 983 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved.
[0141] Sample 3 To produce the capsule composition of sample 3, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 570 pm, an average capsule diameter of 770 pm, a density 983 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved. Sample 4
[0142] To produce the capsule composition of sample 4, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 600 pm, an average capsule diameter of 860 pm, a density 967 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved.
[0143] Sample 5 To produce the capsule composition of sample 5, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 560 pm, an average capsule diameter of 670 pm , a density 980 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved. Sample 6
[0144] To produce the capsule composition of sample 6, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 570 pm, an average capsule diameter of 820 pm, a density 983 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved. Sample 7
[0145] To produce the capsule composition of sample 7, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 570 pm, an average capsule diameter of 820 pm, a density 983 kg / m3.
[0146] The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved.
[0147] Sample 8 To produce the capsule composition of sample 8, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 680 pm, an average capsule diameter of 800 pm, a density 981 kg / m3. The capsules were mixed with the matrix such that a volume packing <D of 50% of the capsules on the capsule composition is achieved. Sample 9
[0148] To produce the capsule composition of sample 9, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 580 pm, an average capsule diameter of 820 pm, a density 985 kg / m3.
[0149] The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved.
[0150] Sample 10 To produce the capsule composition of sample 10, the matrix mentioned above has been mixed with oil core capsules prepared as described above. The capsules have an oil core of average diameter 600 pm, an average capsule diameter of 860 pm, a density 967 kg / m3. The capsules were mixed with the matrix such that a volume packing of 50% of the capsules on the capsule composition is achieved. The following table shows the data on creaming obtained for 7 different samples:
[0151] Samples having a + or ++ in creaming show a satisfying shelf life of 1 year or more.
[0152] The following table shows the data on shear stress at a shear rate of 0.01 s-1obtained for 5 different samples: Samples having a + showed satisfying pumpability of both the capsules and the matrix, sample having a ++ showed excellent pumpability both the capsules and the matrix with essentially even pumping of matrix and capsules and thus no or almost no capsule left over in the perfume vial. For testing pumpability a perfume vial having a crimp type pumping mechanism with a nozzle unit and a tube. The vial has a cylinder shape with dimensions volume 12 ml and the tube has a circular cross section with diameter 900 pm and has a length of 25 mm. The perfume vial was filled with 10 mL of the capsule composition and emptied by repeatedly activating the pumping mechanism. Satisfying pumpability means that at least a certain portion of the capsules is pumped and expelled from the nozzle. An excellent pumpability was achieved when the remaining capsules in the perfume vial were less than 4 wt.% of the original capsule composition.
[0153] The following table shows the normal force FN, o.is“1at a shear rate of 0.1 s-1of the matrix of 11 different capsule compositions measured at 20 °C:
[0154] With samples having a ++ in sprayability it was possible to create a mist with a perfume vial, such as the one described herein, having a crimp type pumping mechanism. In contrast, samples denoted by - resulted only in jet spraying. The same a perfume vial as for the pumpability test has been used.
[0155] The following table shows a comparison of using 15 wt.% of the indicated anti-freezing agents in always the same capsule composition and the observed creaming height after 5 cycles of freeze-thawing. The wt.% are given with respect to the total capsule composition. One freeze-thawing cycle comprised maintaining the capsule composition at -10 °C for 24 h for freezing and then at 40 °C for 24 h for thawing.
[0156] List of designations 1 capsule composition
[0157] 2 matrix
[0158] 3 capsule
[0159] 10 perfume vial
[0160] 11 base container 12 nozzle unit
[0161] 13 nozzle
[0162] 14 tube
[0163] 15 pump bods
[0164] 16 pump head 17 piston
[0165] 18 biasing element
Claims
Claims1 . A capsule composition comprising a matrix and a plurality of capsules being dispersed in the matrix, wherein the matrix comprises a solvent and a polymer composition; wherein the capsule composition has a creaming velocity v of equal or less than 2.5- 10-9m / s, and wherein the capsule composition has a shear stress T at a shear rate of 0.01 s-1of equal or less than 50 Pa, and wherein the matrix has a normal force FN, O.IS“1at a shear rate of 0.1 s-1of more than -0.1 N.
2. The capsule composition according to claim 1 , wherein the solvent is water.
3. The capsule composition according to claim 1 or 2, wherein the capsule composition has a creaming velocity v of equal or less than 1 .3- 10-9m / s, in particular of equal or less than 9.5- 10-10m / s.
4. The capsule composition according to any of the previous claims, wherein the capsule composition has a shear stress T at a shear rate of 0.01 s-1of equal or less than 10 Pa.
5. The capsule composition according to any of the previous claims, wherein the matrix of the capsule composition has viscosity q at a shear rate of 0.01 s-1of between 80 and 300 Pa-s.
6. The capsule composition according to any of the previous claims, wherein the capsule composition further comprises alkaline earth metal ions, in particular Ca2+.
7. The capsule composition according to claim 6, wherein the amount of alkaline earth metal ions, in particular the Ca2+ions, being comprised in the matrix of the capsule composition is 0.01 wt.% to 2.0 wt.%, in particular 0.01 wt.% to 1.0 wt.%, more particular 0.01 wt.% to 0.5 wt.%.
8. The capsule composition according to claim 6 or 7, wherein the total amount of alkaline earth metal ions, in particular Ca2+ions, in the capsule composition is larger than the mount of alkaline earth metal ions, in particular the Ca2+ions, being comprised in the matrix; and / or wherein the total amount of alkaline earth metal ions, in particular Ca2+ions, in the capsule composition is 0.01 wt.% to 2.0 wt.%, in particular 0.01 wt.% to 1 .0 wt.%, more particular 0.01 wt.% to 0.5 wt.%.
9. The capsule composition according to any of the previous claims, wherein the capsule composition further comprises a chelating agent, in particular a chelating agent being configured to chelate alkaline earth metal ions.
10. The capsule composition according to claim 9, wherein the amount of the chelating agent in the capsule composition is between 0.05 wt.% and 0.5 wt.%, in particular between 0.05 wt.% and 0.25 wt.%.
11. The capsule composition according to any of the previous claims, wherein the polymer composition comprises at least one polymer being configured to form a gel, in particular upon reaction with a gelation-inducing agent, in particular at least one polysaccharide and / or at least one negatively charged polymer.
12. The capsule composition according to claim 1 1 , wherein the at least one polysaccharide is selected from one or more of gellan gum, alginates, carrageenan, xanthan gum, pectin, starch, in particular modified starches, chitin, glycogen, galactogen, cellulose, amylose and inulin.
13. The capsule composition according to any of the previous, wherein the amount of the polymer composition comprised in the matrix, in particular the at least one polymer being configured to form a gel, in particular the at least one polysaccharide and / or the at least one negatively charged polymer, is between 0.02 wt.% and 0.40 wt.%, in particular 0.02 wt.% and 0.30 wt.%, in particular between 0.03 wt.% and 0.25 wt.%, in particular between 0.04 wt.% and 0.20 wt.%.
14. The capsule composition according to any of the previous claims, wherein the polymer composition comprises gellan gum and xanthan gum.
15. The capsule composition according to claim 14, wherein the amount of gellan gum in the capsule composition is between 0.02 wt.% and 0.17 wt.%, in particular between 0.02 and 0.09 wt.%, in particular between 0.02 wt.% and 0.08 wt.%; and / or wherein the amount of xanthan gum in the capsule composition is between 0.02 wt.% and 0.09 wt.%, in particular between 0.03 wt.% and 0.08 wt.%.
16. The capsule composition according to any of the previous claims, wherein the capsule composition additionally comprises one or more anti-freezing agents being configured to lower the melting point of the capsule composition, such as glycerol and / or propylene glycol.
17. The capsule composition according to any of the previous claims, wherein the capsules each have a capsule diameter of 150 pm to 3000 pm, in particular 200 pm to 2500 pm, more particular 250 pm to 2000 pm, more particular 500 pm to 2000 pm, even more particular 750 pm to 1500 pm.
18. The capsule composition according to any of the previous claims, wherein the capsules of the capsule composition have an equal size distribution with respect to their capsule diameter with a coefficient of variation of 10% or less, in particular 8% or less, more particular of 5% or less.
19. The capsule composition according to any of the previous claims, wherein the amount of capsules in the capsule composition is 10 wt.% to 65 wt.%, in particular 20 wt.% to 60 wt.%, more particular 25 wt.% to 55 wt.%.
20. The capsule composition according to any of the previous claims, wherein the capsules comprise a shell encasing a liquid core, in particular oil core.
21. The capsule composition according to any of the previous claims, wherein the capsules comprise a compound of interest, in particular a fragrance.
22. The capsule composition according to claims 20 and 21 , wherein the compound of interest is arranged in the liquid core.
23. A perfume vial (10) comprising a base container (11 ) and a nozzle unit (12), wherein the base container (11) contains the capsule composition (1) according to any of the previous claims.
24. The perfume vial according to claim 23, wherein the nozzle unit comprises a nozzle and a tube extending from the nozzle into the capsule composition.
25. The perfume vial according to claim 23 or 24, wherein the nozzle unit comprises a pumping mechanism being configured for pumping the capsule composition into and through the nozzle.
26. Method for producing a capsule composition according to any of claim 1 to 22, the method comprising the steps:- Dissolving a polymer composition in a solvent to form a matrix, wherein dissolving the polymer composition is preferably conducted by heating the solvent above 20 °C for a heating time interval;- Adding a plurality of capsules to the matrix, in particular under stirring.
27. The method according to claim 26, wherein after the heating time interval, the matrix is cooled, in particular to ambient temperature.
28. The method according to claim 26 or 27, wherein the polymer composition comprises at least one gelation agent being configured to form a gel.
29. The method according to claim 28, wherein a gelation-inducing agent, in particular alkaline earth metal ions, is added, in particular before or during the heating time interval, wherein the gelation inducing agent is configured to form a gel together with the gelation agent.
30. Use of a perfume vial according to any of claims 23 to 25 to generate a mist comprising in particular portions of the matrix and portions of the capsules.
31. The use according to claim 30, wherein the capsules are ruptured within the nozzle unit, in particular the nozzle, and are preferably expelled from the nozzle as capsule fragments.
32. The use according to claim 31 , wherein the capsules comprise a fragrance and wherein the fragrance is liberated during rupturing of the capsules and expelled from the nozzle unit, in particular as part of the generated mist.