Capsule composition

CN122803828APending Publication Date: 2026-09-22MICROENCAPSULATION CO LTD
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Patent Information

Application Number
CN202580017016.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2024-03-01
Filing Date
2025-02-27
Publication Date
2026-09-22

AI Technical Summary

Technical Problem

尽管可考虑仅增加基质的粘度以避免胶囊沉降,但这将必然损害胶囊组合物的可泵送性和可喷雾性

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Abstract

Disclosed herein is a capsule composition (1) comprising a matrix (2) and a plurality of capsules (3). Furthermore, a method for producing such a capsule composition, a perfume bottle comprising such a capsule composition and the use of such a perfume bottle are disclosed.
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Description

Technical Field

[0001] This disclosure pertains to the field of encapsulation technology, and particularly relates to capsule compositions, perfume bottles having such capsule compositions, uses of such perfume bottles, and methods for producing capsule compositions. Background Technology

[0002] Capsules are commonly used in a variety of applications to encapsulate target compounds. For example, they can be used as drug carriers to deliver and protect drugs, to protect flavor substances in food applications and release them under specific conditions (such as mechanical force or heating), or to deliver and protect fragrances in the perfume industry.

[0003] Perfumes may, for example, contain or consist of such capsule compositions. That is, the capsules encapsulate one or more fragrances and, for example, protect the fragrances from oxidation or evaporation. The capsules are suspended in a matrix, which typically contains an alcohol, such as ethanol. However, ethanol has certain disadvantages because it is harmful to the skin, especially if the skin is irritated or damaged, and it is generally not desired by perfume users. Perfumes are typically packaged in perfume bottles, which may consist of a base container and a nozzle unit mounted thereon. The nozzle unit may include a tube, a nozzle, and a pumping mechanism that allows the capsule composition to be drawn into the tube and expelled from the nozzle. A major problem with using capsule compositions in perfumes is avoiding capsule settling in the bottle. The time required for capsule phase separation, more specifically settling or emulsification, is considered one of the factors affecting the shelf life of the capsule composition. Settling or emulsification of capsules not only has undesirable aesthetic effects but can also lead to capsule aggregation and even capsule damage. Furthermore, if the capsules settle, the nozzle unit may apply the matrix only, or at least primarily, to the user's skin. However, because the fragrance is located within the capsule and not, or not solely, in the matrix, little or no fragrance is delivered to the user's skin. Furthermore, if the capsule breaks before application, an undesirable dose of fragrance will be applied. In contrast, if a capsule suspension in which the capsules are suspended and do not settle can be provided, a constant and predetermined amount of capsules and matrix can be drawn into the nozzle unit and applied to the user's skin. Providing a dispersion with satisfactory shelf life and / or uniformity is particularly difficult to achieve. While increasing the viscosity of the matrix alone could be considered to avoid capsule settling, this would necessarily compromise the pumpability and sprayability of the capsule composition. Summary of the Invention

[0004] The general objective of this disclosure is to advance the existing level of the encapsulation technology, particularly the technology of perfumes, and preferably to completely or at least partially overcome the disadvantages of the prior art. In an advantageous embodiment, a capsule composition is provided that has a long shelf life, i.e., avoiding or at least delaying the separation of the capsule from the matrix phase, particularly sedimentation. In a further advantageous embodiment, a capsule composition is provided that allows pumping and spraying via a nozzle unit of a perfume bottle. Furthermore, a capsule composition that can be applied as a mist via a nozzle unit of a perfume bottle, and preferably avoids application as a jet, is provided. In a particularly advantageous embodiment, these advantages are achieved simultaneously.

[0005] The general objective is achieved through the subject matter of the independent claims. Further advantageous embodiments are derived from the dependent claims and the overall disclosure.

[0006] In a first aspect, this disclosure relates to capsule compositions. In a second aspect, this disclosure relates to perfume bottles. In a third aspect, this disclosure relates to methods for producing capsule compositions. In a fourth aspect, this disclosure relates to the use of perfume bottles, or methods for generating mist using perfume bottles. In a fifth aspect, this disclosure relates to the use of capsule compositions as disclosed in any embodiment herein.

[0007] As generally understood herein, the term "comprising" is interpreted to mean that it includes those features following the term, but does not exclude the presence of other features, provided they do not render the claim unfeasible. On the other hand, if the phrase "consisting of..." is used, then there are no other features besides those following the phrase. As generally understood, if a range is provided herein, such as the form "X to Y" or "between X and Y", then the boundary values ​​X and Y are included in the scope of the claim, unless otherwise stated. Furthermore, range expressions 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 entire numerical range and include the boundary values ​​X and Y, unless otherwise stated.

[0008] The capsule composition may comprise a matrix and a plurality of capsules suspended in the matrix, or in some embodiments, consist of the matrix and the plurality of capsules. Thus, the matrix can be considered a continuous phase, and the plurality of capsules can be considered a dispersed phase suspended in the continuous phase. The matrix may contain a solvent. In some embodiments, the matrix may contain a polymer composition.

[0009] In particular, the capsule composition may be a capsule composition for use in perfumes and / or contain at least one fragrance. In some embodiments, the fragrance may be encapsulated inside the capsule and may optionally be present or form its liquid core.

[0010] In some embodiments, the capsule composition may have a content of ≤ (equal to or less than) 2.5·10 –9 The emulsification rate v is defined as m / s. This emulsification rate is defined by the following formula: in: g is the gravitational constant [9.81 m / s²]. 2 ]; r is the average radius of the capsule [m]; ρ 基质 The density of the matrix [kg / m³] 3 ]; ρ 胶囊 The average density of the capsule [kg / m³] 3 This can be the average density calculated based on capsule size; η 基质 For the matrix at 0.01 s –1 The shear viscosity [Pa·s] at the shear rate; Φ represents the volumetric filling rate of the capsules in the capsule composition [%).

[0011] As is generally understood, the viscosity and density provided in this article refer to viscosity and density at 20°C and atmospheric pressure.

[0012] The capsule radius r can be determined by staining the capsule with a dye to enhance the contrast between the oil core, the capsule and the surrounding medium, and then recording digital images with a microscope (Keyence VHX 7000) and determining the average size of the capsule with software.

[0013] matrix density ρ 基质 The density of the capsule, ρ, can be determined by averaging at least 10 replicates per 1 mL matrix. 胶囊 It can be calculated based on the volume ratio of the core to the shell, which is determined by the dimensions obtained from optical microscope images.

[0014] Apparent shear viscosity η measured only for the matrix 基质 It can be achieved in 0.01 s –1 The results were obtained from rotational rheological experiments at shear rates, as described in this paper.

[0015] Therefore, the matrix density and viscosity can be selected to achieve ≤ (equal to or less than) 2.5·10 –9 A milk separation rate of m / s has been found to be ideal for avoiding or at least delaying capsule sedimentation. Specifically, the capsules can have a separation rate of 959 kg / m³. 3 Up to 1010 kg / m 3 Especially 971 kg / m 3 Up to 1000 kg / m3 More importantly, 981 kg / m 3 Up to 995 kg / m 3 Capsule density ρ 胶囊 .

[0016] In some embodiments, the emulsification rate v of the capsule composition may be ≤ (equal to or less than) 2.0·10 –9 m / s, especially ≤ (equal to or less than) 1.3·10 –9 m / s, and more particularly ≤ (equal to or less than) 9.5·10 –10 m / s.

[0017] In some embodiments, the emulsification rate v of the capsule composition can be ≥ (equal to or greater than) 7.10. –11 m / s, especially ≥ (equal to or greater than) 9.10 –11 m / s, and especially ≥ (equal to or greater than) 10 –10 m / s.

[0018] In some embodiments, the emulsification rate v of the capsule composition can be 2.5-10. –9 m / s to 7.10 –11 Between m / s, especially 2.5·10 –9 m / s to 9.10 –11 Between m / s, especially 2.5·10 –9 m / s to 10 –10 The emulsification rate v of the capsule composition can be between 1.3 and 10 m / s. In some embodiments, the emulsification rate v of the capsule composition can be between 1.3 and 10 m / s. –9 m / s to 7.10 –11 Between m / s, especially 1.3·10 –9 m / s to 9.10 –11 Between m / s, especially 1.3·10 –9 m / s to 10 –10 The emulsification rate v of the capsule composition can be between 9.5 and 10 m / s. In some embodiments, the emulsification rate v of the capsule composition can be between 9.5 and 10 m / s. –10 m / s to 7.10 –11 Between m / s, especially 9.5·10 –10 m / s to 9.10 –11 Between m / s, especially 9.5·10 –10 m / s to 10 –10 Between m / s.

[0019] In some embodiments, the capsule composition is in 0.01 s –1At certain shear rates, a shear stress τ, or yield stress, can be ≤ (equal to or less than) 50 Pa, particularly ≤ (equal to or less than) 25 Pa, more particularly ≤ (equal to or less than) 15 Pa, and even more particularly ≤ (equal to or less than) 10 Pa. This shear stress has been found advantageous because it allows for the provision of capsule compositions with satisfactory pumpability and sprayability. Yield stress is the minimum stress at which flow occurs.

[0020] The shear stress τ, or yield stress, can be determined using shear stress testing methods. Apparent shear viscosity, shear stress, and normal force can be determined in a rotational rheological experiment with a controlled shear rate [s]. –1 From 0.01 s –1 Change to 1000 s –1 Typically, once a stable value is determined over a 15-second time period, that value is taken. Shear viscosity can be measured, for example, according to ISO 3219-2:2021. The measurement can be performed, for example, on an MCR 501 (Anton Paar, Graz, Austria) equipped with a 50 mm cone-plate geometry or a 50 mm plate-plate geometry, to measure individual matrix or capsule compositions separately. The sample is placed on the plate using a cut plastic pipette, and the geometry is lowered until a gap of 0.0513 mm or 1 mm is achieved for the matrix or capsule composition, respectively. Excess sample is gently removed before starting the measurement. The measurement is performed at 20°C and ambient conditions (1 atm). Measurements for the matrix only are taken at 0.01 s. –1 The apparent shear viscosity at the applied shear rate was calculated by dividing the measured stress by the applied shear rate. The normal force used for sprayability was obtained from the same experiment but at 0.1 s. –1 The results were obtained at an increased shear rate (normal force test method).

[0021] Shear stress (e.g., yield stress), defined as the yield point, is the stress at which the capsule composition is subjected to shear stress for 0.01 s. –1 Measurement at the shear rate (shear stress test method).

[0022] In some embodiments, the capsule composition is in 0.01 s –1 The shear stress τ, or yield stress, at the shear rate can be ≥ 0.1 Pa, especially ≥ 0.5 Pa, and even more especially ≥ 1 Pa.

[0023] In some embodiments, the capsule composition is in 0.01 s –1The shear stress τ, or yield stress, at the shear rate can be between 50 Pa and 0.1 Pa, particularly between 50 Pa and 0.5 Pa, and even more particularly between 50 Pa and 1 Pa. In some embodiments, the capsule composition is at 0.01 s... –1 The shear stress τ, or yield stress, at the shear rate can be between 15 Pa and 0.1 Pa, particularly between 15 Pa and 0.5 Pa, and even more particularly between 15 Pa and 1 Pa. In some embodiments, the capsule composition is at 0.01 s –1 The shear stress τ, or yield stress, at the shear rate can be between 10 Pa and 0.1 Pa, especially between 10 Pa and 0.5 Pa, and even more especially between 10 Pa and 1 Pa.

[0024] In some embodiments, the capsule composition may be selected such that it reacts in 0.01 s. –1 The yield point at the shear rate (i.e., the point on the stress / strain curve where the material transitions from elastic to plastic deformation behavior, or the stress beyond which the fluid begins to flow) is between 0.1 Pa and 10 Pa, particularly between 1 Pa and 10 Pa. This yield point has been found advantageous because the resulting capsule compositions exhibit good pumpability and sprayability, while avoiding phase separation, particularly emulsification, of the capsules.

[0025] In some embodiments, the capsule composition is in 0.01 s –1 The yield point at the shear rate can be ≥0.1 Pa, especially ≥1 Pa, and even more especially ≥10 Pa.

[0026] In some embodiments, the capsule composition is in 0.01 s –1 The yield point at the shear rate can be between 50 Pa and 0.1 Pa, particularly between 50 Pa and 0.5 Pa, and even more particularly between 50 Pa and 1 Pa. In some embodiments, the capsule composition yields at 0.01 s... –1 The yield point at the shear rate can be between 15 Pa and 0.1 Pa, particularly between 15 Pa and 0.5 Pa, and even more particularly between 15 Pa and 1 Pa. In some embodiments, the capsule composition yields at 0.01 s⁻¹. –1 The yield point at the shear rate can be between 10 Pa and 0.1 Pa, especially between 10 Pa and 0.5 Pa, and even more especially between 10 Pa and 1 Pa.

[0027] In some embodiments, the matrix of the capsule composition is in the range of 0.1 s. –1Normal force F at shear rate N,0.1s –1 >(greater than) –0.1 N, particularly >(greater than) –0.10 N. This normal force of the matrix ensures satisfactory atomizability of the capsule composition. In particular, it allows the matrix (and fragrance) to be applied as a mist and avoids its application as a jet, especially when the capsule composition is used in a perfume bottle, such as one of the embodiments of the second aspect of this disclosure. In a particular embodiment, the matrix of the capsule composition has a sprayability of 0.1 s. –1 At a shear rate, a normal force F has a value greater than –0.08 N, particularly greater than –0.05 N, and even more particularly greater than –0.03 N. N,0.1s –1 The normal force can be determined, for example, according to the normal force testing method described herein.

[0028] In some implementations, the matrix is ​​in 0.1 s –1 Normal force F at shear rate N,0.1s –1 It can be ≤ (equal to or less than) –0.001 N, especially ≤ (equal to or less than) –0.005 N, and even more especially ≤ (equal to or less than) –0.01 N.

[0029] In some implementations, the matrix is ​​in 0.1 s –1 Normal force F at shear rate N,0.1s –1 The range can be between -0.1 N and -0.001 N, particularly between -0.1 N and -0.005 N, and even more particularly between -0.1 N and -0.01 N. In some embodiments, the matrix is ​​in the range of 0.1 s. –1 Normal force F at shear rate N,0.1s –1 The range can be between -0.08 N and -0.001 N, particularly between -0.08 N and -0.005 N, and even more particularly between -0.08 N and -0.01 N. In some embodiments, the matrix is ​​in the range of 0.1 s. –1 Normal force F at shear rate N,0.1s –1 It can be between -0.03 N and -0.001 N, especially between -0.03 N and -0.005 N, and even more especially between -0.03 N and -0.01 N.

[0030] It has ≤ (equal to or less than) 2.5·10 –9 The emulsification rate v in m / s and the shear stress τ ≤ (equal to or less than) 50 Pa and in 0.1 s –1At a shear rate, it has a normal force F greater than -0.1 N. N,0.1s –1 The capsule composition with the matrix is ​​particularly advantageous because this combination of parameters gives the capsule composition an excellent shelf life of one year or longer (i.e., the time required for the capsule to settle), while simultaneously possessing excellent atomizability and pumpability, allowing it to be applied to the user's skin, for example, as a mist rather than a jet, and ensuring that both the capsule and the matrix are drawn into the nozzle unit of the perfume bottle during pumping, particularly drawing in not only or primarily the matrix. Therefore, these three parameters can be satisfied by the capsule composition according to the first aspect in a particular embodiment, thereby achieving synergistic advantages, which allows for the provision of improved capsule compositions for perfumes.

[0031] In some embodiments, the capsule composition and / or solvent may be alcohol-free, particularly alkyl alcohols, such as C450. 1-12 Alkyl alcohols, such as ethanol.

[0032] In some implementations, the solvent may contain or consist of water.

[0033] In some embodiments, the matrix may contain at least one fragrance, particularly at least one water-soluble fragrance, which is dissolved in a solvent, particularly water.

[0034] In some embodiments, the matrix of the capsule composition may have a viscosity η between 80 Pa·s and 300 Pa·s, particularly between 100 Pa·s and 260 Pa·s, and even more particularly between 100 Pa·s and 230 Pa·s. 0.01 / s (in 0.01s) –1 (at the shear rate). As mentioned above, the viscosity is the viscosity at 20°C.

[0035] In some embodiments, the capsule composition also contains alkaline earth metal ions, particularly Mg. 2+ or Ca 2+ Ions. The alkaline earth metal ions may, for example, be contained in or dissolved in the matrix. Alternatively, the alkaline earth metal ions may also be contained in the capsule. The content of alkaline earth metal ions in the matrix can be considered as the alkaline earth metal ion matrix fraction, and the content of alkaline earth metal ions in the capsule can be considered as the alkaline earth metal ion capsule fraction. The alkaline earth metal ions in the matrix and the capsule can be the same or different, for example, the same or different types.

[0036] In a matrix, alkaline earth metal ions can induce gel formation, for example, by reacting with a gelling agent. Therefore, alkaline earth metal ions can be considered gel inducing agents or crosslinking agents configured to react with the gelling agent in the matrix or polymer composition.

[0037] In capsules, alkaline earth metal ions can also be used as gelation inducers. As will be further described below, the capsule may comprise a shell made of a matrix forming agent, which reacts with alkaline earth metal ions (e.g., Ca²⁺). 2+ It forms a matrix, especially a water-insoluble matrix.

[0038] In some embodiments, alkaline earth metal ions, particularly Ca, are contained (e.g. dissolved) in the matrix of the capsule composition. 2+ The amount of ions is between 0.01 wt.% and 2.0 wt.%, particularly between 0.01 wt.% and 1.0 wt.%, and even more particularly between 0.01 wt.% and 0.5 wt.%. This amount can be considered as the matrix fraction of alkaline earth metal ions. This concentration has been found to be particularly advantageous because it helps to provide optimal viscosity and emulsification rate for the capsule composition.

[0039] In some embodiments, alkaline earth metal ions, particularly Ca, are present in the capsule composition. 2+ The total amount of ions is greater than that of alkaline earth metal ions, especially Ca, contained (e.g., dissolved) in the matrix. 2+ The amount of ions. The total amount of alkaline earth metal ions can be, for example, composed of the sum of the matrix fraction and the capsule fraction of alkaline earth metal ions.

[0040] In some embodiments, alkaline earth metal ions, particularly Ca, are present in the capsule composition (i.e., throughout the entire capsule composition). 2+ The total amount of ions can be between 0.01 wt.% and 2.0 wt.%, particularly between 0.01 wt.% and 1.0 wt.%, and even more particularly between 0.01 wt.% and 0.5 wt.%.

[0041] In some embodiments, the capsule composition (particularly the matrix) also comprises a chelating agent. In specific embodiments, the chelating agent may be configured to chelate alkaline earth metal ions, such as those present in the capsule composition and / or the capsule. For example, the chelating agent may be configured to chelate Ca... 2+Ions. Suitable chelating agents may be citrates (e.g., sodium citrate or any other suitable citrate), citric acid, EDTA (ethylenediaminetetraacetic acid), EGTA (ethylene glycol-bis(β-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 softening agents and can be used to fine-tune matrix parameters, such as viscosity. Furthermore, chelating agents can soften capsule shells containing alkaline earth metal ions. This can help ensure that the capsule breaks down in the nozzle unit, thereby releasing the target compound (e.g., fragrance) when the capsule composition is applied to the user's skin via a perfume bottle (e.g., a perfume bottle described according to an embodiment of the second aspect of this disclosure).

[0042] In some embodiments, the amount of chelating agent in the capsule composition (particularly in the matrix) is between 0.05 wt.% and 0.5 wt.%, particularly between 0.05 wt.% and 0.4 wt.%, for example between 0.05 wt.% and 0.25 wt.%, and more particularly between 0.15 wt.% and 0.4 wt.%. These wt.% values ​​refer to the amount in the capsule composition, with the total capsule composition representing 100 wt.%. The addition of a chelating agent (particularly in this amount) causes the capsule to soften, which results in a low bursting force, thereby contributing to improved sprayability.

[0043] In some embodiments, the capsule composition (particularly the matrix) also contains an alkali metal salt, particularly NaCl, for example, NaCl alone.

[0044] In some embodiments, the amount of alkali metal salt (particularly NaCl) contained in the matrix (with a matrix of 100 wt.%, the following ranges are relative to this) is between 0.02 wt.% and 0.4 wt.%, particularly between 0.02 wt.% and 0.2 wt.%, and even more particularly between 0.02 wt.% and 0.1 wt.%. In some embodiments, the amount of alkali metal salt (particularly NaCl) contained in the matrix (with a matrix of 100 wt.%, the following ranges are relative to this) is between 0.05 wt.% and 0.4 wt.%, particularly between 0.05 wt.% and 0.2 wt.%, and even more particularly between 0.05 wt.% and 0.1 wt.%. These wt.% values ​​refer to the amount in the matrix, where the total matrix represents 100 wt.%.

[0045] In some embodiments, the polymer composition comprises or consists of one or more polymers. In particular, the polymer may be configured to react with a gelation inducing agent (e.g., alkaline earth metal ions (e.g., Ca)). 2+When ions react, a gel is formed. Therefore, the polymer can be considered a gelling agent. In some embodiments, the polymer composition comprises or consists of at least one negatively charged polymer. The negatively charged polymer may be a polymer containing one or more negatively charged moieties (e.g., hydroxyl groups or carboxylate groups).

[0046] In some embodiments, the polymer composition comprises or consists of at least one polysaccharide. The polysaccharide may exist as a gel, particularly as a mixture of the polysaccharide and an alkaline earth metal ion (e.g., Ca). 2+ The gel contains ions.

[0047] In some embodiments, at least one polysaccharide may be selected from one or more of the following: gellan gum (especially low-acyl gellan gum), alginate, carrageenan, xanthan gum, pectin, starch (especially modified starch), chitin, glycogen, galactopolysaccharide, cellulose, amylose, and inulin. In certain embodiments, at least one polysaccharide may be selected from gellan gum (also known as gelatan gum) and xanthan gum (also known as xanthan gum). In some embodiments, gellan gum (especially low-acyl gellan gum) and xanthan gum may be the only polysaccharide and / or gelling agent in the matrix.

[0048] In some embodiments, the amount of polymer composition contained in the matrix is ​​between 0.02 wt.% and 0.40 wt.%, particularly between 0.02 wt.% and 0.35 wt.%, particularly between 0.02 wt.% and 0.30 wt.%, particularly between 0.03 wt.% and 0.25 wt.%, and even more particularly between 0.04 wt.% and 0.20 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0049] In some embodiments, the amount of polymer composition included in the matrix is ​​between 0.10 wt.% and 0.40 wt.%, particularly between 0.20 wt.% and 0.35 wt.%, particularly between 0.20 wt.% and 0.30 wt.%, particularly between 0.20 wt.% and 0.25 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0050] In some embodiments, the amount of one or more polymers (particularly a gelling agent) contained in the matrix and configured to form a gel upon gelation with a gel inducing agent is between 0.02 wt.% and 0.40 wt.%, particularly between 0.02 wt.% and 0.35 wt.%, particularly between 0.02 wt.% and 0.30 wt.%, particularly between 0.03 wt.% and 0.25 wt.%, and even more particularly between 0.04 wt.% and 0.20 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0051] In some embodiments, the amount of one or more polymers (particularly a gelling agent) contained in the matrix and configured to form a gel upon gelation with a gel inducing agent is between 0.10 wt.% and 0.40 wt.%, particularly between 0.20 wt.% and 0.35 wt.%, particularly between 0.20 wt.% and 0.30 wt.%, particularly between 0.20 wt.% and 0.25 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0052] In some embodiments, the amount of one or more polymers (particularly gelling agents) included in the matrix may be between 0.10 wt.% and 0.40 wt.%, particularly between 0.10 wt.% and 0.30 wt.%, particularly between 0.10 wt.% and 0.25 wt.%, particularly between 0.15 wt.% and 0.25 wt.%, and even more particularly between 0.15 wt.% and 0.22 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0053] In some embodiments, the amount of at least one polysaccharide contained in the matrix is ​​between 0.02 wt.% and 0.40 wt.%, particularly between 0.02 wt.% and 0.35 wt.%, particularly between 0.02 wt.% and 0.30 wt.%, particularly between 0.03 wt.% and 0.25 wt.%, and even more particularly between 0.04 wt.% and 0.20 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0054] In some embodiments, the amount of at least one polysaccharide in the matrix may be between 0.10 wt.% and 0.40 wt.%, particularly between 0.10 wt.% and 0.30 wt.%, particularly between 0.10 wt.% and 0.25 wt.%, particularly between 0.15 wt.% and 0.25 wt.%, and even more particularly between 0.15 wt.% and 0.22 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0055] In some embodiments, the amount of at least one negatively charged polymer in the matrix is ​​between 0.02 wt.% and 0.40 wt.%, particularly between 0.02 wt.% and 0.35 wt.%, particularly between 0.02 wt.% and 0.30 wt.%, particularly between 0.03 wt.% and 0.25 wt.%, and even more particularly between 0.04 wt.% and 0.20 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0056] In some embodiments, the amount of at least one negatively charged polymer in the matrix may be between 0.10 wt.% and 0.25 wt.%, particularly between 0.15 wt.% and 0.25 wt.%, and even more particularly between 0.15 wt.% and 0.22 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0057] In some embodiments, the polymer composition of the matrix contains, or is composed of, two gelling agents (particularly two polysaccharides).

[0058] In some embodiments, the polymer composition of the matrix comprises or consists of gellan gum and xanthan gum.

[0059] In a particular embodiment, the amount of xanthan gum contained in the matrix is ​​between 0.02 wt.% and 0.25 wt.%, particularly between 0.02 wt.% and 0.20 wt.%, and even more particularly between 0.03 wt.% and 0.15 wt.%. These wt.% refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0060] In a particular embodiment, the amount of xanthan gum contained in the matrix is ​​between 0.02 wt.% and 0.10 wt.%, particularly between 0.03 wt.% and 0.10 wt.%. These wt.% refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0061] In some embodiments, the amount of gellan gum contained in the matrix is ​​between 0.02 wt.% and 0.20 wt.%, particularly between 0.05 wt.% and 0.15 wt.%, and even more particularly between 0.10 wt.% and 0.15 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0062] In some embodiments, the amount of gellan gum contained in the matrix is ​​between 0.02 wt.% and 0.17 wt.%, particularly between 0.02 wt.% and 0.09 wt.%, and particularly between 0.02 wt.% and 0.08 wt.%. These wt.% values ​​refer to the amount in the matrix, with the total matrix representing 100 wt.%.

[0063] In some implementations, the amount of xanthan gum contained in the matrix is ​​less than the amount of gellan gum contained in the matrix.

[0064] In some embodiments, the capsule composition (particularly the matrix) further comprises one or more antifreeze agents. The antifreeze agent may be configured to lower the melting point of the capsule composition, particularly below 0°C, and more particularly below –10°C. Suitable antifreeze agents may be, for example, glycerol. In some embodiments, the amount of antifreeze in the capsule composition is 1 wt.% to 15 wt.%, particularly 1 wt.% to 10 wt.%, and more particularly 1 wt.% to 6 wt.%. These wt.% values ​​refer to the amount in the capsule composition, with the total capsule composition representing 100 wt.%. In some embodiments, the capsule composition comprises two, particularly exactly two, antifreeze agents. In some embodiments, the capsule composition may comprise glycerol and propylene glycol as two antifreeze agents. In particular, the two antifreeze agents may be present in equal amounts (e.g., the same wt.%). In some embodiments, the two antifreeze agents together in the capsule composition may be present in amounts of 1 wt.% to 15 wt.%, particularly 1 wt.% to 10 wt.%, and more particularly 1 wt.% to 6 wt.%. For example, if the total amount of the two antifreeze agents is 1 wt.%, then in embodiments where they are present in equal amounts, each can be present in an amount of 0.5 wt.%. It has been observed that the use of two antifreeze agents, and particularly glycerol and propylene glycol together, avoids capsule breakage at low temperatures (e.g., below the freezing point). For example, although glycerol can be used alone, it has been observed that capsule compositions combining two antifreeze agents (e.g., glycerol and propylene glycol) achieve better emulsification properties.

[0065] In some embodiments, the capsule composition comprises a pH adjuster. The pH adjuster is configured to adjust the pH of the capsule composition. For example, Brønsted acid or Brønsted base can be used as the pH adjuster. The pH adjuster can be, for example, a buffer system or buffer. For example, lactic acid can be added as a pH adjuster. Other pH adjusters that can be used are phytic acid, ascorbic acid, or Tris (tris(hydroxymethyl)aminomethane). In some embodiments, the pH adjuster is present such that the pH of the capsule composition is between pH 4 and 6, particularly between pH 4.5 and 5.5, and especially pH 5. In some embodiments, the amount of the pH adjuster in the capsule composition is between 0.1 and 2 wt.%, particularly 0.5 to 1 wt.%.

[0066] In some embodiments, the capsule composition, and particularly the matrix, may contain one or more preservatives, such as propylene glycol, alkyl parabens (e.g., propylparaben or methylparaben), diazoalkylurea, chlorphenesin (CAS 104-29-0), ethylhexylglycerin, phenoxyethanol, and / or hexanediol. In some embodiments, the amount of preservative in the capsule composition may be between 0.1 wt.% and 3 wt.%, particularly between 0.3 wt.% and 2.2 wt.%, and more particularly between 0.4 wt.% and 1.9 wt.%. These wt.% values ​​refer to the amount in the capsule composition, where the total capsule composition represents 100 wt.%.

[0067] In some embodiments, the capsule composition, and particularly the matrix and / or capsule, may contain dyes, particularly water-soluble dyes.

[0068] In some embodiments, the capsule composition, and particularly the matrix and / or capsule, may contain a moisturizing agent, such as hyaluronic acid (e.g., 0.5 wt.% to 2 wt.%, i.e., wt.% of the capsule composition) or panthenol (1 wt.% to 5 wt.%, i.e., wt.% of the capsule composition), or glycerin or lactic acid.

[0069] In some embodiments, the capsules of the plurality of capsules have an average capsule diameter, particularly an average maximum diameter, of 150 µm to 3000 µm, particularly 200 µm to 2500 µm, more particularly 250 µm to 2000 µm, more particularly 500 µm to 2000 µm, and even more particularly 750 µm to 1500 µm. In some embodiments, the capsules of the plurality of capsules have an average capsule diameter, particularly an average maximum diameter, of 150 µm to 3000 µm, particularly 200 µm to 3000 µm, more particularly 250 µm to 3000 µm, more particularly 500 µm to 3000 µm, and even more particularly 750 µm to 3000 µm. The term "maximum diameter" refers to the longest line between the outer sides of the capsule relative to the wall / shell portion, which typically extends through the center of the capsule. The capsule diameter can be obtained from an optical microscopic image of the capsule. The capsule may particularly have a spherical shape in any other embodiment described herein or herein.

[0070] In some embodiments, each of the plurality of capsules has a capsule diameter of 150 µm to 3000 µm, particularly 200 µm to 2500 µm, more particularly 250 µm to 2000 µm, more particularly 500 µm to 2000 µm, and even more particularly 750 µm to 1000 µm, particularly the maximum diameter. The term "maximum diameter" refers to the longest line between opposing wall portions of the capsule, which typically extends through the center of the capsule.

[0071] In some embodiments, the capsules of the capsule composition have an iso-size distribution with respect to their capsule diameter (particularly the maximum capsule diameter) having a coefficient of variation of 10% or less, particularly 8% or less, and even more particularly 5% or less. Those skilled in the art will understand that the coefficient of variation can be calculated as the ratio of the standard deviation σ to the mean μ (i.e., the average capsule size of the component's capsules).

[0072] In some embodiments, the amount of capsules in the capsule composition is at least 10 wt.%, particularly at least 15 wt.%, particularly at least 20 wt.%, particularly at least 30 wt.%. These values ​​are relative to the capsule composition (capsule composition is 100 wt.%). In some embodiments, the remaining wt.% (i.e., 100 wt.% – wt.% of capsules) is the amount of matrix.

[0073] In some embodiments, the amount of capsules in the capsule composition is up to 70 wt.%, particularly up to 60 wt.%, particularly up to 55 wt.%, particularly up to 50 wt.%. These values ​​are relative to a capsule composition (capsule composition is 100 wt.%). In some embodiments, the remaining wt.% (i.e., 100 wt.% – wt.% of capsules) is the amount of matrix. An amount of 60 wt.% or less, and particularly 50 wt.% or less of capsules avoids contact between capsules, thereby preventing capsule aggregation and damage over time.

[0074] In some embodiments, the amount of capsules in the capsule composition is from 10 wt.% to 65 wt.%, particularly from 20 wt.% to 60 wt.%, and even more particularly from 25 wt.% to 55 wt.%. These values ​​are relative to a capsule composition (100 wt.%). In some embodiments, the remaining wt.% (i.e., 100 wt.% – wt.% of capsules) is the amount of matrix.

[0075] In some embodiments, the amount of capsules in the capsule composition is from 10 wt.% to 60 wt.%, particularly from 10 wt.% to 55 wt.%, and even more particularly from 15 wt.% to 50 wt.%. These values ​​are relative to the capsule composition (100 wt.%). In some embodiments, the remaining wt.% (i.e., 100 wt.% – wt.% of the capsules) is the amount of matrix.

[0076] In some embodiments, each capsule comprises a shell (i.e., a capsule shell). In some embodiments, the shell may encapsulate a liquid core. The liquid core may be, in particular, an oil core. The oil core may contain one or more liquid oils. It should be understood that the term "liquid" refers to a state under normal conditions (1 atm and 20°C). Typically, the shell completely surrounds the oil core peripherally. The shell may be configured such that the oil core remains inside the shell. The oil core of the capsule may be arranged in a core compartment surrounded and defined by the shell. The diameter of the core compartment of the capsule (e.g., the maximum distance relative to the shell portion) is from 100 µm to 2500 µm, particularly from 350 µm to 1500 µm, and more particularly from 500 µm to 900 µm.

[0077] The shell can be made from a shell matrix (particularly a water-insoluble matrix), i.e., the shell is a water-insoluble matrix shell. In a particular embodiment, the shell may comprise or consist of a matrix forming agent (e.g., a polysaccharide) and a gelation inducing agent (e.g., an alkaline earth metal ion). The matrix forming agent and the gelation inducing agent can be configured to react together to form a shell matrix, such as a water-insoluble matrix. For example, the matrix forming agent can be ionically bonded to a gelation inducing agent to form a shell matrix, such as a water-insoluble matrix. As a representative example, a polysaccharide (e.g., alginate) can be reacted with an alkaline earth metal ion (which may typically be Mg2+). 2+Ca 2+ or Sr 2+ Especially Ca 2+ ( ) Forming ionic bonds. The capsule may be a capsule and may be obtained as described in the applicant's WO 2022 106 361 A1, which is incorporated herein by reference in its entirety. Water solubility may, for example, refer to solubility in water at a maximum of 40°C (particularly a maximum of 30°C).

[0078] The capsule can have 935 kg / m 3 Up to 1010 kg / m 3 Especially 965 kg / m 3 Up to 999 kg / m 3 The density.

[0079] In some embodiments, the capsule has a shell thickness of 50 µm to 350 µm, particularly 65 µm to 275 µm, and more particularly 80 to 200 µm.

[0080] In some implementations, the oil core volume is 30% to 60% of the total capsule volume, particularly 40% to 60%.

[0081] In some embodiments, the capsule contains at least one target compound. The target compound may, in particular, be a fragrance. A fragrance may, for example, be a compound configured to bind to receptors in the human nasal cavity and thereby trigger signal transmission through the human olfactory system. The capsule may also contain a variety of different fragrances, such as a perfume formulation.

[0082] In some embodiments, the target compound (particularly one or more fragrances) may be arranged in a liquid core (particularly an oil core). An oil core is advantageous because the vast majority of the target compound, and particularly the fragrance, is soluble in the oil phase but insoluble in the aqueous phase. Therefore, the target compound, particularly one or more fragrances, can dissolve in the oil of the oil core. Thus, the fragrance (and therefore the liquid core) can be encapsulated in a capsule shell.

[0083] As described above, the capsule of the capsule composition may contain a core, such as a liquid core. In some embodiments, the core (e.g., liquid core) contains 50 wt.% or more, particularly 75 wt.% or more, particularly 85 wt.% or more of the target compound, particularly one or more flavorings. These wt.% refer to the content of the core (e.g., liquid core) (its total content is 100 wt.%).

[0084] One or more oils in the oil core may be selected from medium-chain triglycerides (MCT), menthol, vegetable oils (e.g., sunflower oil, olive oil, castor oil, low-erucic acid rapeseed oil, soybean oil, peanut oil), isopropyl myristate, Iso ESuper (CAS 54464-57-2), Hedione (CAS 246-495-9), linalool (CAS 78-70-6), and dipentene (138-86-3).

[0085] The second aspect of this disclosure relates to a perfume bottle. The perfume bottle may include a base container. The perfume bottle may also include a capsule composition, particularly as described in any embodiment herein, for example, with respect to the first aspect.

[0086] The perfume bottle may also include a nozzle unit. The nozzle unit can be mounted to the perfume bottle, particularly in a releasable manner and / or in a form-locking and / or force-locking manner. Typically, the nozzle unit is threadedly connected to a base container. The base container may include an opening, particularly a single opening, which is closed by the nozzle unit. For example, the base container may include a threaded element surrounding the opening. The nozzle unit may also include a threaded element that engages with the threaded element of the base container, thereby achieving a form-locking connection.

[0087] In some embodiments, the nozzle unit includes a nozzle. The nozzle is configured to convert the capsule composition into a mist, which may be discharged specifically from the nozzle. In some embodiments, the nozzle unit may also include a tube (e.g., a polymer or metal tube) extending from the nozzle into the capsule composition disposed in a base container. The tube may be connected to the nozzle unit. In some embodiments, the tube may extend to the bottom portion of the base container, particularly from the nozzle. The tube may have the shape of a hollow cylinder, particularly a hollow circular cylinder.

[0088] In some implementations, the tube may have a diameter of 0.19 mm. 2 Up to 1.77 mm 2 Especially 0.50 mm 2 Up to 1.13 mm 2 The cross-sectional opening area. Typically, the cross-sectional opening area can be within this range along the entire length of the pipe.

[0089] In some embodiments, the tube may have a diameter of 200 µm to 2000 µm, particularly 500 µm to 1500 µm, and even more particularly 800 µm to 1200 µm. Typically, the tube diameter may be within this range along the entire length of the tube.

[0090] In some embodiments, the nozzle unit includes a pumping mechanism. This pumping mechanism can be configured to pump the capsule composition into the nozzle and, more particularly, to expel it from the nozzle. The pumping mechanism can be any pumping mechanism capable of performing this function. For example, a crimp-type pumping mechanism can be used. In some embodiments, a crimp-type pumping mechanism may include a pump body and a pump head removable within the pump body. Furthermore, it may include a piston that moves against a biasing element (e.g., a spring) toward the base body of the perfume bottle. Movement of the piston can create overpressure in the base body and / or base container, and when the piston is forced back to its original position, its contents (e.g., the capsule composition) are forced into the tube and expelled from the nozzle. Suction may also be generated in the base body and / or base container. Alternatively, the pumping mechanism may include a retractable element that can be pressed and retracted to provide overpressure in the base body and / or base container and force the capsule composition into the tube and nozzle.

[0091] A third aspect of this disclosure relates to a method for producing capsule compositions, particularly capsule compositions as described in any embodiment herein (e.g., an embodiment of the first aspect).

[0092] The method may include dissolving a polymer composition in a solvent to form a matrix (dissolution step). The method may also include adding multiple capsules to the matrix, particularly under mixing (e.g., stirring) (capsule addition step).

[0093] In some embodiments, dissolving the polymer composition can be achieved by heating the solvent and / or the mixture of the polymer composition and the solvent at temperatures above 20°C, particularly above 25°C, more particularly above 40°C, and even more particularly above 60°C. Heating can be performed to ensure complete dissolution of the polymer composition in the solvent. However, in some embodiments, heating can be performed up to 100°C, more particularly up to 80°C. Therefore, it is preferable to perform heating at temperatures of 70 to 90°C.

[0094] It should be understood that the components used in the method may be the same as those described above with respect to the first aspect of this disclosure. For example, it is clear that the polymer composition may comprise or consist of one or more polymers, and / or the solvent may be water.

[0095] In some embodiments, heating the solvent and / or the polymer composition mixed with the solvent may be performed at heating intervals, such as 1 to 30 minutes, to form the matrix. It should be understood that the solvent and / or mixture is maintained at the corresponding temperature during these heating intervals. In some embodiments, after the heating interval, the matrix is ​​cooled, particularly to ambient temperature. Ambient temperature refers to the temperature of the surrounding environment, such as 20°C to 25°C. For example, the matrix may be actively cooled by a suitable cooling device, or it may be allowed to cool to ambient temperature on its own. Both the heating and cooling steps can be sub-steps of the dissolution step.

[0096] In some embodiments, the matrix is ​​stirred before the capsules are added, and particularly after heating and optionally after cooling, for example in an optional additional stirring step. Specifically, the matrix is ​​stirred using a dissolving pan. In some embodiments, stirring makes the matrix homogenized. This breaks down the gel, which reduces the viscosity of the matrix, thereby allowing for satisfactory pumpability and sprayability.

[0097] Specifically, the polymer can be configured to react with a gelation inducing agent (e.g., alkaline earth metal ions such as Ca) 2+ A gel is formed during the ionic reaction. Therefore, the polymer can be a gelling agent, or the polymer composition can contain a gelling agent. The gelling agent can be configured to form a gel, particularly when reacting with a gelation inducing agent.

[0098] In some embodiments, one or more preservatives, such as those described above, are added. In some embodiments, the one or more preservatives may be added after mixing (i.e., after an optional additional mixing step), and preferably before adding the capsules. In addition to or as a substitute for preservatives, at least one antifreeze agent, particularly those described above, may be added.

[0099] In some embodiments, the polymer composition comprises or consists of at least one negatively charged polymer. The negatively charged polymer may contain one or more negatively charged moieties (e.g., hydroxyl (-O) groups). – ) or carboxylate (-COO) –The polymer composition comprises or consists of at least one gelling agent. In some embodiments, the polymer composition comprises or consists of at least one polysaccharide. The polysaccharide may be present as a gelling agent configured to form a gel upon reaction with a gelling 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 (especially modified starch), chitin, glycogen, galactopolysaccharide, cellulose, amylose, and inulin. In a particular embodiment, the at least one polysaccharide may be selected from gellan gum (also known as gelatan gum) and xanthan gum (also known as xanthan gum). In some embodiments, gellan gum and xanthan gum may be the only polysaccharide and / or gelling agent in the polymer composition.

[0100] In some embodiments, a gelation inducing agent is added, particularly to the solvent, for example, before or after the addition of the polymer composition, or before or after the addition of the plurality of capsules. The gelation inducing agent may, for example, comprise alkaline earth metal ions. In specific examples, the gelation inducing agent may comprise alkaline earth metal salts, such as CaCl2 or MgCl2. In some embodiments, the gelation inducing agent is added while the solvent is heated (e.g., above 20°C, particularly above 25°C, and even more particularly above 40°C). This avoids the formation of agglomerated particles.

[0101] In some embodiments, the gelation inducer may be added after and / or during heating and / or before cooling, i.e., before the cooling step described above.

[0102] In some embodiments, a gelation inducer (e.g., CaCl2) may be added as an aqueous solution, for example, a solution of 0.1 M to 1 M, particularly 0.25 M to 0.75 M.

[0103] In some embodiments, a chelating agent is added, particularly to the solvent, for example, before or after the addition of the polymer composition, or before or after the addition of the plurality of capsules. The chelating agent may be configured to chelate alkaline earth metal ions, such as alkaline earth metal ions present in the capsule composition and / or capsules. The chelating agent may be a chelating agent as described above. In particular, the chelating agent may be added after mixing (i.e., after an optional additional mixing step).

[0104] In some embodiments, the polymer composition, solvent, and the plurality of capsules, and optionally a gelation inducing agent and a chelating agent, are selected and / or selected in amounts such that the capsule composition may have a concentration of ≤ (equal to or less than) 2.5 × 10⁻⁶. –9 m / s, especially ≤ (equal to or less than) 1.3·10 –9 m / s, and more particularly ≤ (equal to or less than) 9.5·10 –10The emulsion rate v is m / s.

[0105] In some embodiments, the polymer composition, solvent, and said plurality of capsules, and optionally a gelation inducing agent and a chelating agent, are selected and / or selected in such amounts that the capsule composition is gelled in 0.01 s. –1 At a shear rate, it can have a shear stress τ ≤ (equal to or less than) 50 Pa, especially less than 25 Pa, more especially less than 15 Pa, and even more especially less than 10 Pa.

[0106] In some embodiments, the polymer composition, solvent, and said plurality of capsules, and optionally a gelation inducing agent and a chelating agent, are selected and / or selected in such amounts that the capsule composition is gelled in 0.01 s. –1 It has a yield point (i.e., the point in the stress / strain curve where the material changes from elastic deformation behavior to plastic deformation behavior, or the stress above which the fluid begins to flow) at a shear rate of 0.1 to 15 Pa, especially 0.1 to 10 Pa, and even more especially 1 to 10 Pa.

[0107] In some embodiments, the polymer composition and solvent, and optionally a gelation inducing agent and chelating agent, are selected and / or selected in amounts such that the matrix reacts in 0.1 s. –1 At shear rates, a normal force F can be greater than –0.1 N, and especially greater than –0.10 N. N,0.1s –1 .

[0108] In a specific implementation plan, the method may include the following steps: a. Dissolving the polymer composition in a solvent to form a matrix, particularly by mixing the polymer composition and the solvent, for example under stirring, wherein the dissolution optionally includes i. Heating a mixture of solvent and / or polymer composition with a matrix, particularly with continuous heating intervals, to form a matrix; ii. Optionally add a gelling inducer to the formed matrix; iii. The resulting matrix is ​​then cooled, particularly to ambient temperature, such as 20°C to 25°C, wherein the cooling may be carried out, especially after the addition of the gelling inducer; b. The stirred, and particularly cooled, matrix. This stirring may be an additional and / or further stirring step. For example, the stirring may be carried out by stirring the matrix formed in a dissolving pan. In some embodiments, stirring is performed to homogenize the matrix; c. Optionally add one or more preservatives and / or at least one antifreeze and / or at least one chelating agent; d. Add multiple capsules.

[0109] The designations a., b., c., d. and i., ii., iii. in some embodiments may 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. Furthermore, 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 is not necessarily the case. In some embodiments, for example, step c. may be performed after step d. It is also possible that the gelling inducer in sub-step ii. may be added during step i.

[0110] The fourth aspect of this disclosure relates to the use of perfume bottles, such as the use of perfume bottles as described in any embodiment herein (e.g., the second aspect of this disclosure). This use can also be considered as a method of generating a mist or a method of applying a mist to a subject.

[0111] Perfume bottles can be used to generate mist. The mist may specifically comprise or consist of a matrix portion and a capsule portion. In particular, the mist may contain one or more fragrances, that is, one or more fragrances that may be contained in the capsule, or its liquid core. The mist may also contain oil from the liquid oil core of the capsule. As understood, mist differs from a jet. A jet is a continuous flow of liquid, while mist may comprise or consist of multiple droplets, such as droplets of submicron (less than 1000 micrometers) size. Droplet size may be diameter, such as the maximum diameter of the droplet. In particular, droplets may have a droplet size of less than 800 µm, especially less than 400 µm, and even more particularly less than 200 µm.

[0112] In some embodiments, the mist may be discharged from the nozzle of the nozzle unit. In some embodiments, the mist may be applied to the subject, for example, by applying it to the subject's skin.

[0113] In some embodiments, mist generation involves guiding a portion of the capsule composition (particularly capsules and matrix) into a nozzle unit, particularly into a tube and thereby into a nozzle.

[0114] In some embodiments, the capsule ruptures within a nozzle unit (e.g., in a tube and / or nozzle). In some embodiments, the ruptured capsule is ejected from the nozzle unit (specifically, the nozzle) as capsule fragments. The advantage of rupturing the capsule within the nozzle unit is that the target compound (e.g., fragrance) is released only shortly before the mist is applied to the subject. This ensures consistent formulation and avoids degradation of the target compound. Therefore, in specific embodiments, the capsule may contain a fragrance, which may be released during capsule rupture and ejected from the nozzle unit (e.g., the nozzle), particularly as part of the generated mist.

[0115] The fifth aspect of this disclosure relates to the use of capsule compositions as disclosed in any embodiment herein, particularly for the application of fragrances to a user's skin or for the production of perfumes. Attached Figure Description

[0116] The disclosure described herein will be more fully understood from the detailed description given below and the accompanying drawings, which should not be construed as limiting the disclosure described in the appended claims. The drawings show: Figure 1 Microscopic image of a capsule composition according to one embodiment of the present disclosure; Figure 2 A perfume bottle according to one embodiment of this disclosure; Figure 3 The difference between jet spray and mist spray is shown in the photo (left) and the diagram (right); Figure 4 Shear rate / shear stress diagrams for different samples. Detailed Implementation

[0117] Figure 1 A capsule composition 1 comprising a matrix 2 and a plurality of capsules 3 is shown. Each capsule 3 comprises a shell encapsulating a liquid oil core. The liquid oil core contains an oil and a target compound, such as one or more fragrances.

[0118] Figure 2 A perfume bottle 10 is shown, comprising a base container 11 and a nozzle unit 12. The nozzle unit 12 includes a tube 14 and a nozzle 13 through which a capsule composition, or a ruptured capsule composition, can be discharged from the perfume bottle 10. The nozzle unit 12 also includes a pumping mechanism, which in this embodiment is a press-fit type. It includes a pump body 15 and a pump head 16, the pump head 16 being movable into the pump body 15 by being pushed downward toward the base container 11. Furthermore, it includes a piston 17, which, together with the pump head 16, can move toward the base body 11 against a biasing element 18 (e.g., a spring). The movement of the piston 17 creates overpressure in the base body and / or the base container, and when the piston is forced back to its original position, the capsule composition is forced into the tube 14, then through the nozzle 13, and discharged as a mist. Typically, as they pass through nozzle unit 12 (e.g., through tube 14 and nozzle 13), capsules 3 rupture and break apart, thereby releasing their contents, such as spices arranged in a liquid oil core.

[0119] Figure 3 This illustrates the difference between the jet and mist emitted from a perfume bottle nozzle. Figure 3 Figure a shows a jet containing one or more continuous liquid flows, while Figure 3b illustrates the generation of fog, as in some application embodiments of this disclosure. The fog comprises multiple droplets with a droplet size less than 800 micrometers, particularly less than 400 µm, and even more particularly less than 200 µm. The droplet size can be determined, for example, by laser diffraction or image analysis, particularly laser diffraction.

[0120] Figure 4 Shear rate / shear stress diagrams are shown for five different capsule compositions (samples 10, 8, 7, 4 and 9). Example

[0121] General Instructions Kelcogel CG-LA (CAS 71010-52-1) is available from CP Kelco. Keltrol CG-T (CAS 11138-66-2) is available from CP Kelco.

[0122] To produce samples, polymers (e.g., Kelcogel and Keltrol) are dissolved in water (amounts are shown in the table below). The mixture is then heated to 80°C to achieve dissolution. A crosslinking agent (e.g., CaCl2) is then added while stirring, and the mixture is allowed to cool without mixing to induce gelation. The mixture is then stirred to break up the gel (e.g., through a dissolving pan) until the mixture is homogeneous. Other additives (e.g., sodium citrate, preservatives, sodium chloride, hexanediol, or water-soluble flavoring) are then added. Subsequently, multiple capsules are added while stirring.

[0123] Capsules having an oil core containing a target compound (e.g., a fragrance) can be obtained by the method described in WO 2022 106 361 A1 (application number PCT / EP2021 / 081705), which is incorporated herein by reference in its entirety and particularly with respect to the formulations disclosed therein in Tables 1, 2, and 3. After production, the capsules are separated (e.g., from any remaining continuous phase) and used as described above. If the oil core shell contains one or more target compounds (e.g., a fragrance), these target compounds are present in the oil phase used. It should be understood that any possible oil phase can be used.

[0124] All rheological measurements were performed on an MCR 501 (Anton Paar, Graz, Austria), equipped with either a 50 mm cone-plate geometry or a 50 mm plate-plate geometry for measuring individual matrix or capsule compositions, respectively. The sample was placed on the plate using a cut plastic pipette, and the geometry was lowered until a gap of 0.0513 mm or 1 mm was achieved for the matrix or capsule composition, respectively. Excess sample was gently removed before starting the measurement. The measurements were performed at 20°C and ambient conditions (1 atm).

[0125] Apparent shear viscosity, shear stress, and normal force were all determined in a rotational rheological experiment with a controlled shear rate [s]. –1 From 0.01 s –1 Change to 1000 s –1 The shear viscosity can be measured, for example, according to ISO 3219-2:2021.

[0126] Measurements were taken only on the matrix at a shear rate of 0.01 s⁻¹. –1 The apparent shear viscosity was calculated by dividing the measured stress by the applied shear rate. The critical normal force for sprayability was determined by the same experiment but at 0.1 s-1. –1 This was obtained under increased shear rates.

[0127] Shear stress (i.e., yield stress), defined as the yield point, is the stress at which the capsule composition is subjected to shear stress for 0.01 s. –1 Measured at the shear rate.

[0128] Emulsion rate was calculated based on Stokes' law modified by Richardson-Zaki (source: ISBN 3-527-30743-5): 9.81 m / s was used in all cases. 2 The gravitational constant g.

[0129] The capsule radius r was determined by staining the capsule with a dye to enhance the contrast between the oil core, the capsule, and the surrounding medium, followed by recording digital images with a microscope (Keyence VHX 7000) and determining the average size of the capsule using software.

[0130] matrix density ρ 基质 The density of the capsule, ρ, is determined by averaging over weight in at least 10 replicates of 1 mL of matrix. 胶囊 The volume ratio of the core to the shell is calculated based on the dimensions determined from optical microscope images.

[0131] Apparent shear viscosity η measured only for the matrix 基质 From 0.01 s –1 The results were obtained from rotational rheological experiments at shear rates.

[0132] The capsule volume fill rate Φ is approximated by formulating the capsule composition using only wt.% of sieved and drained capsules (without any excess surrounding medium).

[0133] Sample 1 The following tables provide different capsule compositions. These tables show the matrix composition and the wt.% of the components.

[0134] To produce the capsule composition of Sample 1, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 570 µm, an average capsule diameter of 770 µm, and a weight of 983 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0135] Sample 2 To produce the capsule composition of Sample 2, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 570 µm, an average capsule diameter of 820 µm, and a weight of 983 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0136] Sample 3 To produce the capsule composition of Sample 3, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 570 µm, an average capsule diameter of 770 µm, and a weight of 983 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0137] Sample 4 To produce the capsule composition of Sample 4, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 600 µm, an average capsule diameter of 860 µm, and a weight of 967 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0138] Sample 5 To produce the capsule composition of Sample 5, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 560 µm, an average capsule diameter of 670 µm, and a weight of 980 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0139] Sample 6 To produce the capsule composition of Sample 6, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 570 µm, an average capsule diameter of 820 µm, and a weight of 983 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0140] Sample 7 To produce the capsule composition of Sample 7, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 570 µm, an average capsule diameter of 820 µm, and a weight of 983 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0141] Sample 8 To produce the capsule composition of Sample 8, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 680 µm, an average capsule diameter of 800 µm, and a weight of 981 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0142] Sample 9 To produce the capsule composition of Sample 9, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 580 µm, an average capsule diameter of 820 µm, and a weight of 985 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0143] Sample 10 To produce the capsule composition of Sample 10, the matrix mentioned above was mixed with the oil-core capsules prepared as described above. The capsules have an oil core with an average diameter of 600 µm, an average capsule diameter of 860 µm, and a weight of 967 kg / m³. 3 The density. The capsules are mixed with the matrix to achieve a volumetric filling ratio Φ of 50% in the capsule composition.

[0144] The table below shows data on emulsion analysis obtained for seven different samples: entry sample Milk analysis Emulsion separation rate v [m / s] <![CDATA[at 0.01 s –1 η [Pa·s]]]> 1 Sample 1 ++ 8.8E-10 229 2 Sample 2 ++ 2.0E-09 101 3 Sample 3 + 1.6E-09 151 4 Sample 4 - 1.2E-08 250 5 Sample 5 - 1.4E-08 14.4 6 Sample 6 - 3.2E-09 62.9 7 Sample 7 - 3.7E-09 54.5 Samples with a + or ++ rating in terms of emulsification showed a satisfactory shelf life of 1 year or longer.

[0145] The table below shows the results obtained for five different samples at 0.01 s. –1 Data on shear stress at shear rate: entry sample Pumpability <![CDATA[At 0.01 s –1 Shear stress at shear rate [Pa] <!-- 18 -->]]> 1 Sample 10 + 13.5 2 Sample 4 + 22.4 3 Sample 7 ++ 6.7 4 Sample 8 + 22.9 5 Sample 9 ++ 3.4 Samples with a + rating indicate satisfactory pumpability of both the capsules and the matrix, while samples with a ++ rating indicate excellent pumpability of both the capsules and the matrix, where the matrix and capsules are pumped substantially uniformly, resulting in little or no capsule residue in the perfume bottle. To test pumpability, a perfume bottle with a press-fit pumping mechanism, a nozzle unit, and a tube was used. The bottle was cylindrical with a volume of 12 ml, and the tube had a circular cross-section with a diameter of 900 µm and a length of 25 mm. The perfume bottle was filled with 10 mL of the capsule composition and emptied by repeatedly starting the pumping mechanism. Satisfactory pumpability was defined as at least a portion of the capsules being pumped and expelled from the nozzle. Excellent pumpability was achieved when the number of capsules remaining in the perfume bottle was less than 4 wt.% of the original capsule composition.

[0146] The table below shows the matrix of 11 different capsule compositions measured at 20°C in 0.1 s. –1 Normal force F at shear rate N,0.1s –1 : entry sample Sprayability <![CDATA[at 0.1 s –1 F under N,0.1s –1 [N]]]> 1 Sample 1 ++ -0.036 2 Sample 2 ++ -0.009 3 Sample 3 ++ -0.012 4 Sample 6 ++ -0.037 5 Sample 2 ++ -0.010 6 Sample 7 ++ -0.033 7 Sample 4 - -0.108 Samples with a sprayability score of ++ have the potential to generate a mist using a perfume bottle (such as the perfume bottle with a press-fit pump mechanism described herein). In contrast, samples marked with – only result in a jet of spray. The same perfume bottle used was employed for the pumpability test.

[0147] The table below shows a comparison of emulsification heights observed after 5 freeze-thaw cycles using 15 wt.% of the indicated antifreeze in the same capsule composition throughout. wt.% is given relative to the total capsule composition. One freeze-thaw cycle consists of freezing the capsule composition at –10°C for 24 h and then thawing it at 40°C for 24 h.

[0148] Tag list .

Claims

1. A capsule composition comprising a matrix and a plurality of capsules dispersed in the matrix, wherein the matrix comprises a solvent and a polymer composition; wherein the capsule composition has a particle size distribution of 2.5 × 10⁻⁶. –9 The emulsification rate v is m / s, and the capsule composition is in the range of 0.01 s. –1 The matrix has a shear stress τ equal to or less than 50 Pa at a shear rate, and the matrix is ​​in the range of 0.1 s⁻¹. –1 At a shear rate, it has a normal force F greater than -0.1 N. N,0.1s –1 .

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 content equal to or less than 1.3·10 –9 m / s, especially equal to or less than 9.5·10 –10 The emulsion rate v is measured in m / s.

4. The capsule composition according to any one of the preceding claims, wherein the capsule composition is in 0.01 s –1 It has a shear stress τ equal to or less than 10 Pa at a shear rate.

5. The capsule composition according to any one of the preceding claims, wherein the matrix of the capsule composition is in the range of 0.01 s. –1 It has a viscosity η between 80 and 300 Pa·s at shear rates.

6. The capsule composition according to any one of the preceding claims, wherein the capsule composition further comprises alkaline earth metal ions, particularly Ca... 2+ .

7. The capsule composition according to claim 6, wherein the capsule composition contains alkaline earth metal ions, particularly Ca, in the matrix of the capsule composition. 2+ The amount of ions is from 0.01 wt.% to 2.0 wt.%, particularly from 0.01 wt.% to 1.0 wt.%, and even more particularly from 0.01 wt.% to 0.5 wt.%.

8. The capsule composition according to claim 6 or 7, wherein the alkaline earth metal ions, particularly Ca, in the capsule composition... 2+ The total amount of ions is greater than that of alkaline earth metal ions, especially Ca, contained in the matrix. 2+ The amount of ions; and / or the alkaline earth metal ions, particularly Ca2+, in the capsule composition. 2+ The total amount of ions is 0.01 wt.% to 2.0 wt.%, particularly 0.01 wt.% to 1.0 wt.%, and even more particularly 0.01 wt.% to 0.5 wt.%.

9. The capsule composition according to any one of the preceding claims, wherein the capsule composition further comprises a chelating agent, particularly a chelating agent configured to chelate alkaline earth metal ions.

10. The capsule composition according to claim 9, wherein the amount of chelating agent in the capsule composition is between 0.05 wt.% and 0.5 wt.%, particularly between 0.05 wt.% and 0.25 wt.%.

11. The capsule composition according to any one of the preceding claims, wherein the polymer composition comprises at least one polymer configured to form a gel, particularly when reacting with a gelation inducing agent, particularly at least one polysaccharide and / or at least one negatively charged polymer.

12. The capsule composition according to claim 11, wherein the at least one polysaccharide is selected from one or more of gellan gum, alginate, carrageenan, xanthan gum, pectin, starch, especially modified starch, chitin, glycogen, galactopolysaccharide, cellulose, amylose and inulin.

13. The capsule composition according to any one of the preceding claims, wherein the amount of the polymer composition contained in the matrix, particularly at least one polymer configured to form a gel, particularly at least one polysaccharide and / or at least one negatively charged polymer, is between 0.02 wt.% and 0.40 wt.%, particularly between 0.02 wt.% and 0.30 wt.%, particularly between 0.03 wt.% and 0.25 wt.%, particularly between 0.04 wt.% and 0.20 wt.%.

14. The capsule composition according to any one of the preceding 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.%, particularly between 0.02 and 0.09 wt.%, particularly 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.%, particularly between 0.03 wt.% and 0.08 wt.%.

16. The capsule composition according to any one of the preceding claims, wherein the capsule composition further comprises one or more antifreeze agents configured to lower the melting point of the capsule composition, such as glycerin and / or propylene glycol.

17. The capsule composition according to any one of the preceding claims, wherein each of the capsules has a capsule diameter of 150 µm to 3000 µm, particularly 200 µm to 2500 µm, more particularly 250 µm to 2000 µm, more particularly 500 µm to 2000 µm, and even more particularly 750 µm to 1500 µm.

18. The capsule composition according to any one of the preceding claims, wherein the capsules of the capsule composition have an iso-size distribution with a coefficient of variation of 10% or less, particularly 8% or less, more particularly 5% or less, with respect to their capsule diameter.

19. The capsule composition according to any one of the preceding claims, wherein the amount of capsules in the capsule composition is from 10 wt.% to 65 wt.%, particularly from 20 wt.% to 60 wt.%, and even more particularly from 25 wt.% to 55 wt.%.

20. The capsule composition according to any one of the preceding claims, wherein the capsule comprises a shell encapsulating a liquid core, particularly an oil core.

21. The capsule composition according to any one of the preceding claims, wherein the capsule comprises the target compound, particularly a fragrance.

22. The capsule composition according to claims 20 and 21, wherein the target compound is disposed in the liquid core.

23. A perfume bottle (10) comprising a base container (11) and a nozzle unit (12), wherein the base container (11) contains a capsule composition (1) according to any one of the preceding claims.

24. The perfume bottle of claim 23, wherein the nozzle unit comprises a nozzle and a tube extending from the nozzle into the capsule composition.

25. The perfume bottle of claim 23 or 24, wherein the nozzle unit comprises a pumping mechanism configured to pump the capsule composition into and through the nozzle.

26. A method for producing a capsule composition according to any one of claims 1 to 22, the method comprising the following steps: - The polymer composition is dissolved in a solvent to form a matrix, wherein the dissolution of the polymer composition is preferably carried out by heating the solvent at a temperature above 20°C for a continuous heating time interval; - Add multiple capsules to the matrix, especially under stirring.

27. The method of claim 26, wherein after the heating time interval, the substrate is cooled, particularly to ambient temperature.

28. The method of claim 26 or 27, wherein the polymer composition comprises at least one gelling agent configured to form a gel.

29. The method of claim 28, wherein a gelation inducing agent, particularly an alkaline earth metal ion, is added, especially before or during the heating time interval, wherein the gelation inducing agent is configured to form a gel together with the gelling agent.

30. The use of a perfume bottle for producing a mist according to any one of claims 23 to 25, wherein the mist particularly comprises a matrix portion and a capsule portion.

31. The use according to claim 30, wherein the capsule ruptures within the nozzle unit, particularly within the nozzle, and preferably exits from the nozzle as capsule fragments.

32. The use according to claim 31, wherein the capsule contains a fragrance, and wherein the fragrance is released and discharged from the nozzle unit during capsule rupture, particularly as part of the generated mist.

Citation Information

Patent Citations

  • Encased oil core microcapsules

    WO2022106361A1