Water-oil microbead bi-phase system containing microfibrous cellulose and its preparation and use

Abstract

The present application relates to the field of cosmetic technology, and provides a water-oil microbead two-phase system containing microfibrous cellulose, and preparation and application thereof, the viscosity of the system is not less than 90 mPa.s; the water-oil two-phase system includes oil phase with density of 0.95-1.10 g / cm 3 The oil phase is suspended in the water phase containing microfibrous cellulose in the form of microbeads; the mass content of the microfibrous cellulose in the water-oil two-phase system is 0.03-0.075%. The present application realizes the water-oil two-phase system with high transparency, uniform dispersion of oil phase, avoidance of water-oil stratification, aesthetics and stable performance of the system and other performances by optimizing the amount of microfibrous cellulose, giving full play to its supporting capacity in the water-oil two-phase system of the present application, and combining the synergistic control of the density of the oil phase and the viscosity of the system.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to a water-oil microsphere biphase system containing microfibrillated cellulose and its preparation and application. Background Technology

[0002] Water-oil microbead technology is commonly used in the skincare industry. It is a technology that encapsulates, suspends, or stores oil-based active ingredients in the form of microbeads in an aqueous substrate. It has the advantages of good fluidity, strong moisturizing ability, and high stability of active ingredients. The skin feels smooth and non-greasy upon contact with the skin, and it is currently favored by more and more consumers.

[0003] Currently, some products are prepared by encapsulating oil-soluble active ingredients (such as retinol, vitamin E, and plant essential oils) in extremely small phospholipid vesicles, microcapsules, or porous polymer microspheres. Other products require shaking before use, during which countless tiny water-in-oil or oil-in-water droplets (temporary emulsions) are formed. These products naturally separate into two or more distinct layers when left to stand, typically with an oil phase on top and a water phase below. The oil phase layer itself is a macroscopic "oil droplet" or "oil layer," commonly found in shake-and-use toners, essences, and makeup removers. Currently, some serums, after adding stabilizers such as carbomer, xanthan gum, and gellan gum, can maintain the stability of water-in-oil droplet microbeads under static conditions, presenting a crystal-bubble effect. However, carbomer has significant ionic sensitivity and can undergo protonation reactions with some functional ingredients, losing viscosity and support capacity, thus limiting its compatibility with formulations. Xanthan gum and gellan gum have limited support capacity and often need to be used in combination. Furthermore, they have a relatively sticky feel on the skin, requiring the addition of ethanol to correct this. However, some consumers have a resistance to ethanol. Additionally, dissolving gellan gum requires a heating step, resulting in numerous process control points. The market currently lacks a water-oil two-phase system with more stable support capacity, a refreshing feel, high transparency, a crystal-bubble effect, and a simple manufacturing process. Summary of the Invention

[0004] To partially solve the above-mentioned technical problems, the present invention provides a water-oil microsphere biphase system containing microfibrillated cellulose and its preparation and application.

[0005] This invention provides a water-oil two-phase system with a viscosity not less than 90 mPa·s; the water-oil two-phase system comprises components with a density of 0.95~1.10 g / cm³. 3 The oil phase is suspended in the form of microbeads in the aqueous phase containing microfibrillated cellulose; the mass content of the microfibrillated cellulose in the water-oil biphase system is 0.03~0.075%.

[0006] Microfibrillated cellulose possesses advantages such as high mechanical strength, excellent water retention, perfect biocompatibility, and complete biodegradability. This invention utilizes the supporting capacity of microfibrillated cellulose in the aforementioned water-oil two-phase system. Research has found that the content of microfibrillated cellulose and the density of the oil phase directly affect the transparency, layering state, oil phase structure, and distribution of the water-oil two-phase system. Specifically, excessively high microfibrillated cellulose content not only affects transparency but also hinders the uniform dispersion of the oil phase in the system, leading to oil droplet aggregation and water-oil layering. Conversely, lower microfibrillated cellulose content fails to support the oil droplets. Only when the density of the oil phase falls within the aforementioned range can it achieve overall equilibrium with the water phase, enabling oil droplet dispersion. Excessively high oil phase content not only results in overly dense oil droplets, which is aesthetically unappealing, but also easily causes aggregation and layering. This invention provides a two-phase system with excellent stability, a refreshing skin feel, and high visual transparency.

[0007] To ensure a refreshing feel, preferably, the viscosity of the water-oil two-phase system is not higher than 3000 mPa·s.

[0008] According to the water-oil dual-phase system provided by the present invention, the particle size of the microspheres is not less than 50 micrometers.

[0009] According to the water-oil two-phase system provided by the present invention, the mass content of the oil phase is not higher than 5%, for example, it can be any value or a numerical range composed of 1%, 2%, 3%, 4%, and 5%.

[0010] According to the water-oil two-phase system provided by the present invention, the oil phase includes a base oil, optional oil-soluble functional components, and optional oil-soluble pigments, the main purpose of which is to maintain the overall density of the oil phase at 0.95~1.10 g / cm³. 3 The overall density of the oil phase can be any value or a range of values, such as 0.95%, 1.05%, or 1.1%.

[0011] Preferably, the base oil is selected from one or more of the following: diphenylsiloxyphenyl polytrimethylsiloxane, trimethylpentaphenyltrisiloxane, diphenylsiloxyphenyl polytrimethylsiloxane, diphenylsiloxyphenyl polytrimethylsiloxane, squalane, caprylic / capric triglyceride, hydrogenated polydecene, isopropyl myristate, caprylic / capric / succinic acid triglyceride, meadowfoam (LIMNANTHES ALBA) seed oil, European hazelnut (CORYLUS AVELLANA) seed oil, camellia (CAMELLIA JAPONICA) seed oil, and olive (OLEA EUROPAEA) fruit oil.

[0012] Preferably, the oil-soluble functional ingredient is selected from one or more of grape seed oil, vitamin E, and polyunsaturated fatty acid esters.

[0013] Preferably, the oil-soluble pigment is selected from carotenoids, synthetic oil-soluble pigments, etc.

[0014] According to the water-oil biphase system provided by the present invention, the aqueous phase includes water, a component containing microfibrillated cellulose, an optional polyol, an optional rheology modifier, an optional water-soluble pigment, an optional preservative, an optional complexing agent, an optional pH adjuster, and an optional water-soluble active ingredient.

[0015] Preferably, the polyol is selected from one or more combinations of glycerin, propylene glycol, pentylene glycol, butylene glycol, erythritol, and mannitol. These polyols primarily function to moisturize and improve skin feel.

[0016] Preferably, the rheology modifier includes one or more combinations of hydroxyethyl cellulose, hydroxypropyl methyl cellulose, sodium carboxymethyl cellulose, xanthan gum, carbomer, guar gum, gellan gum, pectin, sodium alginate, sodium polyacrylate, ammonium polyacrylate, PEG-150 distearate, cocoamide DEA, sodium hyaluronate, etc., with the main purpose of selection being to provide a suitable viscosity for the two-phase system.

[0017] Preferably, water-soluble pigments include natural coloring substances such as beetroot extract, turmeric, gardenia yellow, and anthocyanins, and may also include synthetic pigments such as CI 19140 tartrazine and CI 15985 sunset yellow, without any special limitation.

[0018] Preferably, the preservative is selected from one or more of the following: capryloyl hydroxamic acid, caprylyl glycol, butylene glycol, 1,2-hexanediol, pentanediol, phenoxyethanol, and ethylhexylglycerin.

[0019] Preferably, the chelating agent may include commonly used ingredients in the skin care field such as disodium EDTA, tetrasodium EDTA, trisodium HEDTA, and sodium gluconate, without any special limitations.

[0020] Preferably, pH adjusters may include commonly used ingredients in the skin care field such as citric acid, lactic acid, malic acid, tartaric acid, sodium hydroxide, potassium hydroxide, triethanolamine, and arginine, without any special limitations.

[0021] Preferably, the water-soluble active ingredients are selected from common functional ingredients in the skin care field such as hyaluronic acid, sialic acid, vitamin C, niacinamide, arbutin, and tranexamic acid, and no special limitations are made here.

[0022] In some specific implementations, certain raw materials may be selected repeatedly. For example, in some implementations, preservatives and polyols may be selected repeatedly, such as hexanediol, propylene glycol, and butylene glycol, which can both enhance the skin feel and moisturize, and also serve as preservatives. For example, sodium hyaluronate can be added as a rheology modifier or as a water-soluble functional ingredient.

[0023] In the water-oil biphase system provided by the present invention, the microfibrillated cellulose is selected from bacterial microfibrillated cellulose.

[0024] According to the water-oil two-phase system provided by the present invention, based on a total mass fraction of 100% for the components containing microfibrillated cellulose, the components containing microfibrillated cellulose include: Glycerin 10-18%; Microfibrillary cellulose: 0.6-0.8%; Sodium benzoate 0.2~0.5%; Citric acid 0.1~0.3%; Water balance.

[0025] According to the water-oil biphase system provided by the present invention, the yield value of the component containing microfibrillated cellulose is 5 Pa or higher.

[0026] According to the water-oil two-phase system provided by the present invention, the raw materials of the water-oil two-phase system further include, by mass percentage: Polyols 0.1-7%; Rheology modifier 0.01~0.5%; Preservatives: 0.001~1.0%; Complexing agent 0~0.1%; pH adjuster 0~2.5%; Water-soluble functional ingredients: 0-10%; Water-soluble pigments: 0-1%; 0-5% base oil; Oil-soluble functional ingredients: 0-5%; Oil-soluble pigments 0-1%; The base oil, the oil-soluble functional component, and the oil-soluble pigment are not all simultaneously zero.

[0027] According to the water-oil two-phase system provided by the present invention, the raw materials of the water-oil two-phase system, by mass percentage, include: Complexing agent 0~0.1%; Glycerin 0~7%; Xanthan gum 0~0.3%; Hyaluronic acid 0~0.1%; Microfibrillary cellulose: 0.03–0.075%; pH adjuster 0~2.5%; Preservatives: 0.001~1.0%; Diphenylsiloxyphenyl polytrimethylsiloxane 0~5%; Trimethylpentaphenyltrisiloxane 0~5%; Squalane 0~3%; Isopropyl myristate 0-3%; Camellia seed oil 0-3%; Methylphenylcyclotrisiloxane 0~4.8%; Water balance; Among them, diphenylsiloxyphenyl polytrimethylsiloxane, trimethylpentaphenyltrisiloxane, squalane and isopropyl myristate are not simultaneously 0; glycerol, xanthan gum and sodium hyaluronate are not simultaneously 0.

[0028] Using the above-mentioned raw material formula, a water-oil two-phase system with better performance can be achieved at low cost. In some specific embodiments, more functional ingredients, pigments and aromatherapy ingredients can be added according to the end-user requirements.

[0029] The present invention also provides a method for preparing the water-oil two-phase system as described above, comprising: preparing a water-oil two-phase system with a density of 0.95~1.10 g / cm³. 3 The oil phase is suspended in the form of microbeads in an aqueous phase containing microfibrillated cellulose.

[0030] The method for preparing the water-oil biphase system provided by the present invention includes: heating and dissolving phase A until it becomes transparent, then adding phase B and mixing evenly, then adding phase C and mixing evenly, and finally adding phase D and mixing evenly. Phase A includes one or more of the following: rheology modifier, complexing agent, polyol, complexing agent, water-soluble pigment, and water-soluble functional component; Phase B includes a component containing microfibrillated cellulose, an optional preservative, an optional polyol, and an optional pH adjuster; The C phase includes preservatives and / or polyols; The D phase includes a base oil, optional oil-soluble functional components, and optional oil-soluble pigments.

[0031] The present invention also provides a cosmetic product comprising the water-oil biphase system as described above, or the water-oil biphase system prepared by the method described above.

[0032] The present invention provides a water-oil microsphere biphase system containing microfibrillated cellulose, its preparation and application. By optimizing the amount of microfibrillated cellulose, its supporting capacity in the water-oil biphase system of the present invention is fully utilized. Combined with the synergistic control of the density of the oil phase and the viscosity of the system, a water-oil biphase system with high transparency, uniform dispersion of the oil phase, avoidance of water-oil separation, aesthetics and system stability is achieved. Detailed Implementation

[0033] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this invention, not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0034] Where specific techniques or conditions are not specified in the examples, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.

[0035] The method for testing the yield value of the component containing microfibrillated cellulose in this invention is as follows: using a NETZSCH Kinexus Pro+ rotational rheometer, with a plate size of 40 mm and an angle of 25 degrees, the yield value is obtained by fitting the viscosity curve using the HB model.

[0036] Preparation Example 1: Components containing microfibrillary cellulose A component containing microfibrillated cellulose, by mass percentage, comprises: Glycerin 15%; Microfibrillary cellulose 0.7%; Sodium benzoate 0.4%; Citric acid 0.1%; Water balance.

[0037] The yield value of the component containing microfibrillated cellulose is 10.45 Pa.

[0038] Preparation Example 2: Components containing microfibrillary cellulose A component containing microfibrillated cellulose, by mass percentage, comprises: Glycerin 15%; Microfibrillary cellulose 0.6%; Sodium benzoate 0.4%; Citric acid 0.1%; Water balance.

[0039] The yield value of the component containing microfibrillated cellulose is 7.34 Pa.

[0040] Examples 1-10: Water-Oil Two-Phase Systems A water-oil two-phase system is prepared by the following method: Phase A was heated to 80°C and dissolved completely until transparent, then the temperature was lowered. Phase B, which was uniformly dispersed, was added and stirred until homogeneous. Phase C, a preservative (Spectrastat™ PHL, composed of 1,2-hexanediol, 1,3-propanediol, and octanoyl hydroxamic acid), was added and stirred until homogeneous. The compositions of phases A, B, C, and D are shown in Tables 1 and 2 below.

[0041] Table 1

[0042] Table 2

[0043] Examples 11-12 The difference from Example 1 is that the composition of phase A, phase B, phase C and phase D is shown in Table 3 below.

[0044] Table 3

[0045] Test Example 1 Viscosity The viscosity of the above water-oil two-phase system was tested using the following method: The IKA ROTAVISC viscosity meter was used at 25°C and 20 rpm. The test results are shown in Table 4.

[0046] Test Example 2: Oil Phase Density The density of the oil phase obtained in each embodiment was tested, and the test results are shown in Table 4.

[0047] Test Example 3: Appearance In the water-oil two-phase systems obtained in each embodiment, the oil phase can be suspended in the aqueous phase containing microfibrillated cellulose in the form of microbeads. The oil beads are transparent in appearance and uniformly dispersed throughout the system. The particle size range of the microbeads is not less than 50 μm. The suspension stability was then investigated by placing them in a constant temperature and humidity chamber at 45℃ and room temperature. The system parameters and suspension stability observations are shown in Table 4 below. Normal indicates that the oil beads have good suspension properties and can be uniformly dispersed throughout the system without floating, settling, or agglomeration.

[0048] Table 4

[0049] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A water-oil two-phase system, characterized in that, Its viscosity is not less than 90 mPa·s; the water-oil two-phase system comprises components with a density of 0.95~1.10 g / cm³. 3 The oil phase is suspended in the form of microbeads in the aqueous phase containing microfibrillated cellulose; the mass content of the microfibrillated cellulose in the water-oil biphase system is 0.03~0.075%.

2. The water-oil dual-phase system according to claim 1, characterized in that, The particle size of the microspheres is not less than 50 micrometers.

3. The water-oil dual-phase system according to claim 1 or 2, characterized in that, The mass content of the oil phase is no higher than 5%.

4. The water-oil dual-phase system according to any one of claims 1 to 3, characterized in that, The oil phase includes a base oil, optional oil-soluble functional components, and optional oil-soluble pigments; And / or, the aqueous phase includes water, a component containing microfibrillated cellulose, optional polyols, optional rheology modifiers, optional water-soluble pigments, optional preservatives, optional complexing agents, optional pH adjusters, and optional water-soluble active ingredients. Preferably, the microfibrillated cellulose is selected from bacterial microfibrillated cellulose.

5. The water-oil two-phase system according to any one of claims 1 to 4, characterized in that, The yield value of the component containing microfibrillated cellulose is 5 Pa or higher.

6. The water-oil two-phase system according to any one of claims 1 to 5, characterized in that, The raw materials for the water-oil two-phase system, by mass percentage, include: Polyols 0.1-7%; Rheology modifier 0.01~0.5%; Preservatives: 0.001~1.0%; Complexing agent 0~0.1%; pH adjuster 0~2.5%; Water-soluble functional ingredients: 0-10%; Water-soluble pigments: 0-1%; 0-5% base oil; Oil-soluble functional ingredients: 0-5%; Oil-soluble pigments 0-1%; The base oil, the oil-soluble functional component, and the oil-soluble pigment are not all simultaneously zero.

7. The water-oil dual-phase system according to any one of claims 1 to 6, characterized in that, The raw materials for the water-oil two-phase system, by mass percentage, include: Complexing agent 0~0.1%; Glycerin 0~7%; Xanthan gum 0~0.3%; Hyaluronic acid 0~0.1%; Microfibrillary cellulose: 0.03–0.075%; pH adjuster 0~2.5%; Preservatives: 0.001~1.0%; Diphenylsiloxyphenyl polytrimethylsiloxane 0~5%; Trimethylpentaphenyltrisiloxane 0~5%; Squalane 0~3%; Isopropyl myristate 0-3%; Camellia seed oil 0-3%; Methylphenylcyclotrisiloxane 0~4.8%; Water balance; Among them, diphenylsiloxyphenyl polytrimethylsiloxane, trimethylpentaphenyltrisiloxane, squalane, and isopropyl myristate are not simultaneously 0; glycerol, xanthan gum, and sodium hyaluronate are not simultaneously 0.

8. The method for preparing the water-oil dual-phase system according to claims 1-7, characterized in that, include: With a density of 0.95~1.10 g / cm³ 3 The oil phase is suspended in the form of microbeads in an aqueous phase containing microfibrillated cellulose.

9. The method for preparing the water-oil dual-phase system according to claim 8, characterized in that, include: After heating and dissolving phase A until it becomes transparent, add phase B and mix thoroughly. Then add phase C and mix thoroughly. Finally, add phase D and mix thoroughly. Phase A includes one or more of the following: rheology modifier, complexing agent, polyol, complexing agent, water-soluble pigment, and water-soluble functional component; Phase B includes a component containing microfibrillated cellulose, an optional preservative, an optional polyol, and an optional pH adjuster; The C phase includes preservatives and / or polyols; The D phase includes a base oil, optional oil-soluble functional components, and optional oil-soluble pigments.

10. A cosmetic product, characterized in that, This includes the water-oil biphase system described in claims 1 to 7, or the water-oil biphase system prepared by the preparation method described in claim 8 or 9.

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