A stable three-phase emulsion system for use as a solid perfume and a method for preparing the same

Abstract

The invention relates to a stable three-phase (oil / water / oil) emulsion system containing chitosan molecules, which is obtained by dispersing oil in water, and again by dispersing these two phases in oil, using physical chemistry, colloid chemistry, and interfacial chemistry, and to a method for preparing said system.

Description

[0001] DESCRIPTION

[0002] A STABLE THREE-PHASE EMULSION SYSTEM FOR USE AS A SOLID PERFUME AND A METHOD FOR PREPARING THE SAME

[0003] Technical Field of the Invention

[0004] The invention relates to a stable three-phase (oil / water / oil) emulsion system containing chitosan molecules, which is obtained by dispersing oil in water, and again by dispersing these two phases in oil, using physical chemistry, colloid chemistry, and interfacial chemistry, and to a method for preparing said system. The system traps the perfume essence inside and provides its release over an extended period. Furthermore, the presence of chitosan in the system prevents degradation of the emulsion system due to its antimicrobial and anti-inflammatory properties.

[0005] State of the Art

[0006] Perfumes used in cosmetics are complex mixtures composed of hundreds of ingredients that give the product its unique scent. Fragrances and perfumes are used in a wide range of consumer products, including fine perfumes and creams applied directly to the skin, lotions, detergents, perfumes in solid or liquid form used in many other personal care and household products. Unlike traditional liquid perfumes, solid perfumes are products derived from a mixture of beeswax, oils and essential oils and have superior technical properties compared to liquid perfumes in different areas such as ease of use, portability and skin health. For instance, solid perfumes are compact and durable, allowing them to be easily carried in a pocket, bag, or wallet, whereas liquid perfumes are more fragile and harder to transport due to their glass bottles. In addition, solid perfumes can be applied in the desired amount as they are applied directly. However, with liquid perfumes, due to the spray mechanism, a large amount of perfume is used, which causes the product to run out more quickly.

[0007] Perfume production generally involves obtaining an extract of the perfume raw material, either in the form of an essential oil (in case of natural origin) or in concentrated form. However, in order to provide innovative formulations and product diversity in perfume production, emulsions, especially those containing a combination of aqueous and oil phases, are used in the present art as they offer several advantages such as stabilization, skin compatibility and controlled release of perfume ingredients. Emulsions, which are widely used in many industries, especially in the food, cosmetics, pharmaceutical and chemical industries, are heterogeneous systems with a homogeneous appearance, formed by the dispersion of two immiscible liquids within each other. Dispersed droplets (globules) in the emulsion constitute the dispersed phase, while the other liquid forms the continuous phase

[0001] . There are four different types of emulsions: oil-in-water (O / W), water-in-oil (W / O), W / O / W and O / W / O. In oil-in-water (W / O) systems, oil droplets are dispersed in water, with the continuous phase being water and the dispersed phase being oil. In water-in-oil (W / O) systems, water droplets are dispersed in oil, with the continuous phase being oil and the dispersed phase being water. In W / O / W emulsion systems, water droplets are dispersed in oil, and these oil droplets are again dispersed in an aqueous phase. In O / W / O emulsion systems, the first oil phase is dispersed in aqueous phase, and this aqueous phase is dispersed in an outer oil phase. O / W / O systems are also used for the controlled and slow release of active ingredients (e.g., drugs or biological molecules), as they allow the gradual release of active ingredients trapped in the inner aqueous or first oil phase into the external environment. In the state of the art, in the perfume production techniques, O / W / O (oil-in- water- 1 and oil-in-water-2) systems are more preferred than W / O / W systems. O / W / O emulsions enable a more controlled release of fragrance components located in different phases from the second continuous oil phase, allowing the scent to last longer. The outer oil phase slows down the release of fragrance components through the intermediate aqueous (dispersed) phase.

[0008] The patent application KR20160067478A in the state of the art relates to the formulations in solid form at room temperature, which comprise bead emulsion particles, and to their pharmaceutical use as well as their use in perfume formulations. It is stated that said particles may be O / W / O type emulsions, and that chitosan is used in the formulation as an antioxidant and free radical scavenger. However, the system may not be fully 3- phased. The presence of the active substance in one of the phases does not mean that this substance will be dispersed as a different phase, because this depends on the structure of said substance, i.e. whether it dissolves or disperses in the environment in which it is present. Since this study is prepared as a general formulation intended for similar applications, the exact definition of the system remains ambiguous. Another patent application KR102548433B1 in the state of the art discloses a multiple emulsion for sequential release of functional ingredients and a cosmetic composition comprising the same. The composition uses chitosan as amphiphilic polymer and jojoba oil in the oil phase. The document states that the described three-phase W / O / W-type emulsion can be used as a fragrance essence. In this context, the sequential release of functional ingredients is intended so that the skin-whitening and anti-wrinkle agents are released in a controlled manner, effectively penetrating the skin while minimizing irritation.

[0009] The limitations and inadequacies of the solutions in the state of the art, skin irritation and allergic reactions caused by the perfumes, the low persistence time of the fragrance, the degradation of emulsion systems over time, as well as the use of non-natural materials and alcoholic ingredients, have made it necessary to develop an improvement in the relevant technical field.

[0010] Brief Description and Objects of the Invention

[0011] The invention describes a stable three-phase (oil / water / oil) emulsion system containing chitosan molecules, which is obtained by dispersing oil in water, and again by dispersing these two phases in oil, using physical chemistry, colloid chemistry, and interfacial chemistry, and a method for preparing said system. In the system containing chitosan and perfume essence acording to the invention, the essence is released over an extended period, and degradation of the emulsion is prevented.

[0012] The object of the invention is to obtain a perfume with long-lasting scent. In the emulsion system according to the invention, the essence is contained in both the innermost first oil phase (disperse phase) and the outer second oil layer (continuous phase-medium), and the separation of the phases with chitosan, that is, the stability and permanence of the phases are ensured, and the perfume is released at two different speeds in a longer time, that is, in a longer time.

[0013] An object of the invention is to obtain a natural-content perfume that does not cause skin irritation or allergic reactions. Since the perfume components according to the invention are organic ingredients such as coconut, avocado, argan, or jojoba oil, and also contain chitosan, the final perfume does not cause skin reactions like those triggered by alcohol- based or chemically formulated products.

[0014] Another object of the invention is to prevent the degradation of the emulsion system. In the oil / water / oil emulsion system according to the invention, the aqueous phase contains chitosan. Thus, the presence of chitosan provides essential natural protection against degradation of the emulsion system due to its antimicrobial and anti-inflammatory properties.

[0015] Description of the Figures

[0016] Figure 1. Solid perfume system according to the invention.

[0017] Figure 2. FTIR results of the solid perfume system according to the invention.

[0018] Detailed Description of the Invention

[0019] The invention relates to a stable three-phase (oil / water / oil) emulsion system containing chitosan molecules, which is obtained by dispersing oil in water, and again by dispersing these two phases in oil, using physical chemistry, colloid chemistry, and interfacial chemistry, and to a method for preparing said system. The system traps the perfume essence inside and provides its release over an extended period. Furthermore, the presence of chitosan in the system prevents degradation of the emulsion system due to its antimicrobial and anti-inflammatory properties. When used as a solid perfume, this emulsion system provides fragrance longevity for up to 10 hours.

[0020] The stable three-phase (oil / water / oil) emulsion system (30 ml) according to the invention comprises an inner-first oil phase, an aqueous phase containing chitosan, and an outer- second oil phase containing a carrier oil and additional essences. In one embodiment of the invention, it comprises an inner-first oil phase at 15%-30% of the emulsion volume, an aqueous phase between 23.5%-30.5% of the emulsion volume, which comprises 2% chitosan solution, and an outer-second oil phase containing 44-62% of the emulsion volume of carrier oil and additional essences. In another embodiment of the invention, which is the same as the first one, it comprises an inner-first oil phase at 20% of the emulsion volume, an aqueous phase at 27% of the emulsion volume, which comprises 2% chitosan solution, and an outer-second oil phase at 53% of the emulsion volume, which comprises a carrier oil and additional essences. The systems comprises soy wax which is additionally added in an amount corresponding to ! of the total emulsion. This amount is not included in the percentage calculations. It is added separately for the purpose of solidifying the emulsion system. The carrier oils mentioned here may be coconut, avocado, argan or jojoba oil. In addition to soy wax, beeswax and jojoba wax can also be used. Preferably, the aqueous phase constitutes 23.5%-30.5% (optimally 27%) of the total emulsion volume, and this ratio may be adjusted to achieve the desired consistency of the solid perfume. In another embodiment of the invention, the emulsion system according to the invention comprises an inner-first oil phase with essence, an aqueous phase with chitosan, and an outer-second oil phase with carrier oil and essence (in the same ratios as the first embodiment), as well as propolis, vitamin E, and Na- benzoate. These components are added as extras and are not included in the percentage calculations. Propolis is added to the aqueous phase in an amount of 1 -3 ml, vitamin E is added to the oil phase in a ratio of 1 .0%-1 .5%, and Na-benzoate is added to the aqueous phase in an amount of less than <0.1%, providing additional antimicrobial and preservative properties to the product.

[0021] The pH of the emulsion system according to the invention is 5.5, and the essence is present in the outermost second oil phase with its molecules dispersed, while the innermost core constitutes the entire first oil phase. As a result of these two different presences, the fragrance is released in two different ways (kinetics). The stability and longevity of the phases in the emulsion system are ensured by chitosan which is a natural material. Unlike current techniques, no synthetic surfactants are used in the invention. The emulsion stability provided by surfactants by entering the interfaces is achieved by chitosan thanks to its large molecules by staying between the drops in the medium and preventing film drainage. In other words, oil or water drops are unable to merge or coalesce.

[0022] The method for preparing the stable three-phase (oil / water / oil) emulsion system according to the invention comprises the following process steps: i. mixing 5-7 ml of essence with 4-12.2 ml of an aqueous phase containing 2% chitosan solution to prepare the oil / water emulsion system, ii. mixing the prepared oil / water emulsion system with 14-18 ml of coconut oil, which forms the outer-second oil phase and also contains additional essences, iii. melting 8-12 grams of soy wax in a separate container, iv. adding the melted wax to the oil / water / oil emulsion system and mixing with a probe for 20-30 seconds, v. pouring the resulting final mixture into molds for freezing and allowing it to solidify for 3-5 minutes.

[0023] In an embodiment of the invention, the method for preparing the stable three-phase (oil / water / oil) emulsion system according to the invention comprises the following process steps: i. mixing 6 ml of essence with 8.0 ml of an aqueous phase containing chitosan solution to prepare the oil / water emulsion system, ii. mixing the prepared oil / water emulsion system with 16 ml of coconut oil, which forms the outer-second oil phase and also contains additional essences, iii. melting 10 grams of soy wax in a separate container, iv. adding the melted wax to the oil / water / oil emulsion system and mixing with a probe for 20-30 seconds, v. pouring the resulting final mixture into molds for freezing and allowing it to solidify for 3-5 minutes.

[0024] In the method according to the invention, the aqueous phase mentioned in process step (i) consists of a 1.0-3.0% (optimally %2) chitosan solution prepared by dissolving in a 1 .5-2.5% (optimally %2) acetic acid solution. Additionally, the amount of soy wax mentioned in process step (iii) is not included in the percentage calculation of the emulsion system. It is added separately and serves the purpose of solidifying the emulsion system.

[0025] According to the FTIR results shown in Figure 2, the spectrum of the emulsion displays a combination of characteristic bands of coconut oil, essence and chitosan. The C-H stretching vibrations in the range of 3000-2800 cm-1confirm the presence of both coconut oil and the essence. The C=O stretching vibrations in the range of 1750-1700 cm-1indicate the carbonyl groups of coconut oil and the essence. The amide bands in the range of 1650-1550 cm-1and the broad OH and NH bands in the range 3500-3200 cm-1indicate the presence of chitosan. In the ranges of 1600-1500 cm-1and 1300-1200 cm-1, the vibrations of the common organic functional groups of the essence and chitosan are present. In conclusion, the overall spectrum confirms the presence of each component within the emulsion and reflects the characteristic FTIR bands of all components.

[0026] Industrial Applicability of the Invention

[0027] The invention relates to a stable three-phase (oil / water / oil) emulsion system containing chitosan molecules, which is obtained by dispersing oil in water, and again by dispersing these two phases in oil, using physical chemistry, colloid chemistry, and interfacial chemistry, and to a method for preparing said system, and is industrially applicable.

[0028] The invention is not limited to the above descriptions, and a person skilled in the art can easily come up with different embodiments of the invention. These should be considered within the scope of protection claimed in the appended claims.

[0029] REFERENCES

[0030] [1] Gungor, O., Zungur, A., Kog, M., & Kaymak-ertekin, F. (2013, June 1). Emulsiyonlarm ozellikleri ve Emulsifikasyon Ko§ullannm Aroma ve Yaglann Mikroenkapsulasyonu uzerine Etkisi. Akademik Gida.

Claims

CLAIMS1 . A three-phase (oil / water / oil) emulsion system, characterized in that it comprises an inner-first oil phase, an aqueous phase containing 2% chitosan solution, and an outer-second oil phase containing a carrier oil and additional essences.

2. An emulsion system according to claim 1 , characterized in that it comprises an inner-first oil phase at 15%-30% of the emulsion volume, an aqueous phase between 23.5%-30.5% of the emulsion volume, which comprises 2% chitosan solution, and an outer-second oil phase containing 44-62% of the emulsion volume of carrier oil and additional essences.

3. An emulsion system according to claim 2, characterized in that it comprises an inner-first oil phase at 20% of the emulsion volume, an aqueous phase at 27% of the emulsion volume, which comprises 2% chitosan solution, and an outer- second oil phase at 53% of the emulsion volume, which comprises a carrier oil and additional essences.

4. An emulsion system according to any one of claims 1 -3, characterized in that the carrier oils are coconut oil, avocado oil, argan oil or jojoba oil.

5. An emulsion system according to any one of claims 1 -4, characterized in that it comprises soy wax, beeswax or jojoba wax in an amount corresponding to 14 of the total emulsion.

6. An emulsion system according to any of the preceding claims, characterized in that it comprises propolis at 1 -3 ml of an aqueous phase, vitamin E at 1.0-1.5% of the oil phase, and Na-benzoate at <0.1 % of the aqueous phase.

7. Use of an emulsion system according to any of the preceding claims as a solid perfume.

8. A method for preparing a three-phase (oil / water / oil) emulsion system, characterized in that it comprises the following process steps: i. mixing 5-7 m of essence with 4-12.2 ml of an aqueous phase containing chitosan solution to prepare the oil / water emulsion system,ii. mixing the prepared oil / water emulsion system with 14-18 ml of coconut oil, which forms the outer-second oil phase and also contains additional essences, iii. melting 8-12 grams of soy wax in a separate container, iv. adding the melted wax to the oil / water / oil emulsion system and mixing with a probe for 20-30 seconds, v. pouring the resulting final mixture into molds for freezing and allowing it to solidify for 3-5 minutes.

9. A method according to claim 8, characterized in that it comprises the following process steps: i. mixing 6 ml of essence with 8.0 ml of an aqueous phase containing chitosan solution to prepare the oil / water emulsion system, ii. mixing the prepared oil / water emulsion system with 16 ml of coconut oil, which forms the outer-second oil phase and also contains additional essences, iii. melting 10 grams of soy wax in a separate container, iv. adding the melted wax to the oil / water / oil emulsion system and mixing with a probe for 20-30 seconds, v. pouring the resulting final mixture into molds for freezing and allowing it to solidify for 3-5 minutes.

10. A method according to claim 8 or 9, characterized in that the aqueous phase mentioned in process step (i) consists of a 1.0-3.0% chitosan solution prepared by dissolving in a 1 .5-2.5% acetic acid solution.1 1. A method according to claim 10, characterized in that the aqueous phase mentioned in step (i) consists of a 2% chitosan solution prepared by dissolving in a 2% acetic acid solution.

12. A three-phase (oil / water / oil) emulsion system prepared by the method according to claim 11 .

13. An emulsion system according to claim 12 for use as a solid perfume.

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