A microbead system and a method for preparing the same

Abstract

The present disclosure provides a microbead system, characterized by comprising: microbeads configured in an aqueous phase; further comprising a first emollient, an emulsifier. The microbeads provided by the present disclosure have good compatibility with the matrix, high centrifugal stability, good high and low temperature stability, and low process loss. The preparation method of the microbeads provided by the present disclosure is particularly suitable for forming microbeads in a high-viscosity formula system.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and more specifically, to a microbead system and its preparation method. Background Technology

[0002] Traditional, homogeneous formulations applied to the skin often suffer from unstable active ingredients due to environmental factors, leading to inactivation. One solution is to develop product systems with controlled-release capabilities. Controlled-release systems allow for stable storage of active ingredients while achieving a slow release, which is beneficial for skin absorption.

[0003] The patent application “A microbead product, preparation method and application thereof” discloses a method for preparing a microbead product. Implementing this preparation method enables microbeads to be formed during the emulsification process and naturally precipitated during the cooling process, resulting in good compatibility between the microbeads and the matrix in the formulation, high centrifugal stability, good high and low temperature stability, and reduced process losses.

[0004] However, the bead yield during the emulsification and cooling process of this method is still not high enough, and microbeads cannot be stably formed. Summary of the Invention

[0005] The technical problem to be solved by this invention:

[0006] How can we improve the existing methods for preparing microbead systems to achieve a satisfactory microbead yield?

[0007] Technical means to solve technical problems:

[0008] Through extensive research, the inventors discovered that by improving the preparation process of microbeads—specifically, by mixing and homogenizing the aqueous and oil phases, then maintaining the mixture at a specific temperature for a certain time, followed by cooling and stirring—the emulsifying ability of the emulsifier in the microbead system can be reduced, the range of emulsifiable components can be narrowed, and the types of encapsulated substances become more homogeneous. This reduces the emulsification of components such as vegetable oils, fatty acids, and fatty alcohols, ultimately resulting in a larger number of microbeads of uniform size. Compared to existing technologies, the yield of microbeads is significantly improved, and the size and shape uniformity of the microbeads are also better.

[0009] This invention provides a microbead system and its preparation method, including the following aspects:

[0010] In a first aspect, the present invention provides a microbead system having microbeads disposed in an aqueous phase;

[0011] First emollient, emulsifier;

[0012] The first emollient is configured to include silicone oil or modified silicone oil; the HLB value of the emulsifier is configured to be in the range of 3 to 10.

[0013] In some embodiments, the weight percentage of the first emollient is configured to be 0.06 to 15 wt%, and the weight percentage of the emulsifier is configured to be 0.02 to 5 wt%.

[0014] In some implementations, the microbead system also includes a thickener at a weight percentage of 0.2 to 5 wt%.

[0015] In some embodiments, a second emollient is also included in the form of 0.01 to 10 wt% by weight.

[0016] In some embodiments, the first emollient is configured as at least one of polydimethylsiloxane, cyclopentadimethylsiloxane, and trimethylpentaphenyltrisiloxane.

[0017] A second aspect of the present invention provides a method for preparing a microbead system, comprising:

[0018] The thickener was mixed with deionized water and heated to obtain an aqueous phase.

[0019] The mixture of the first emollient and the emulsifier, and the second emollient are heated separately, and then the mixture of the first emollient and the emulsifier is mixed with the second emollient to obtain the oil phase; the aqueous phase and the oil phase are mixed and homogenized, and then cooled and stirred to obtain the microbead system; wherein, after the aqueous phase and the oil phase are mixed and homogenized, they are first kept at a high temperature for 10 to 20 minutes and then cooled and stirred.

[0020] In some implementations, the thickener is configured to be 0.2–5 wt% by weight. During the heating process, the thickener is mixed with deionized water and then heated to 70–90°C.

[0021] In some embodiments, when the weight percentage of the first emollient is configured to be 0.06 to 15 wt% and the weight percentage of the emulsifier is configured to be 0.02 to 5 wt%, the mixture of the first emollient and the emulsifier is heated to 50 to 70°C during the heating treatment.

[0022] In some embodiments, the second emollient is configured to be 0.01 to 10 wt% by weight, and the second emollient is heated to 60 to 80°C during the heating treatment.

[0023] In a third aspect, the present invention provides a microbead system obtained by implementing the aforementioned method for preparing a microbead system.

[0024] Beneficial effects:

[0025] The inventors, after mixing and homogenizing the aqueous and oil phases, first kept them at a specific temperature for a certain time, and then cooled and stirred them, which resulted in the formation of a large number of uniformly sized microspheres. Compared with existing technologies, the yield of microspheres has been significantly improved, and the size and shape of the microspheres are more uniform.

[0026] The microbeads provided by this invention are formed during the emulsification process and naturally precipitate during the cooling process. The preparation process is simple and energy-efficient, saving process costs.

[0027] The microbeads provided by this invention are formed during the emulsification process and naturally precipitate during the cooling process, avoiding problems encountered by microbeads in other processing steps, such as breakage of microbeads due to mechanical external forces and centrifugal stability caused by the potential suspension of the system.

[0028] The microbead system provided by this invention has good compatibility with the matrix, high centrifugal stability, good high and low temperature stability, and reduces process losses.

[0029] The method for preparing the microbead system provided by this invention is particularly suitable for formulation systems with high viscosity to form microbeads. Attached Figure Description

[0030] This disclosure also provides accompanying drawings in connection with the technical solutions provided herein to illustrate the technical solutions. The drawings and descriptions are intended only to describe this disclosure more clearly and should not be construed as limiting the scope of protection claimed in this disclosure.

[0031] Figure 1 An external view of a microbead system according to one embodiment of the present invention is shown. Detailed Implementation

[0032] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are not all the embodiments.

[0033] The elements and features described in one embodiment of the invention may be combined with elements and features shown in one or more other embodiments. It should be noted that, for clarity, representations and descriptions of components and processes unrelated to the invention and known to those skilled in the art have been omitted from the description.

[0034] wt%: refers to the percentage (%) of the weight of a certain component in this invention compared to the total weight of all components in the formulation.

[0035] HLB value: refers to the hydrophilic-lipophilic balance value of a surfactant (emulsifier).

[0036] This invention

[0037] This invention provides a microbead system, comprising:

[0038] First moisturizer

[0039] In some embodiments, the first emollient is preferably specifically configured to include silicone oil or modified silicone oil.

[0040] When the first emollient is formulated as silicone oil, due to the poor compatibility between silicone oil and plant oils, fatty alcohols, and fatty acids, the added emulsifier emulsifies the silicone oil to form a water-in-oil system, which in turn forms microbeads. The oil-soluble active ingredients, oil components, fatty acids, and fatty alcohol components are encapsulated in the microbeads.

[0041] In some embodiments, the first emollient is preferably configured as at least one of polydimethylsiloxane, cyclopentadimethylsiloxane, and trimethylpentaphenyltrisiloxane.

[0042] In some embodiments, the weight percentage of the first emollient is preferably configured to be 0.06 to 15 wt%.

[0043] emulsifier

[0044] In some embodiments, the emulsifier is preferably configured as an emulsifier with an HLB value of 3 to 10.

[0045] In some embodiments, the emulsifier is preferably configured as an organosilicon or a modified organosilicon.

[0046] In some embodiments, the emulsifier is specifically preferably configured as at least one of polyoxyethylene group-modified silicone and polyglycerol-modified silicone.

[0047] In some embodiments, the emulsifier is preferably configured as at least one of silicone elastomer emulsifier KSG-210, silicone emulsifier KF-6038, silicone elastomer emulsifier SSG-210SP, silicone emulsifier KF-6017, silicone emulsifier KF-6028, and silicone emulsifier KF6100.

[0048] In some embodiments, the weight percentage of the emulsifier is preferably configured to be 0.02 to 5 wt%.

[0049] Thickener

[0050] In some embodiments, the thickener is preferably formulated as at least one of xanthan gum, sodium carbomer, sodium polyacrylate grafted starch, carbomer, acrylate / C10-30 alkanol acrylate crosspolymer, ammonium acryloyl dimethyl taurate / behenol polyether-25 methacrylate crosspolymer, and sodium acrylate copolymer.

[0051] In some implementations, the weight percentage of the thickener used is preferably configured to be 0.2 to 5 wt%.

[0052] Skin feel modifier

[0053] In some embodiments, the skin feel modifier is preferably configured as at least one of silicone powder, silicone elastomer, silicone, starch, modified starch, and silica.

[0054] In some embodiments, the skin feel modifier is preferably configured as at least one of vinyl polydimethylsiloxane / polymethylsiloxane-silsesquioxane crosslinked polymer, diphenyl polydimethylsiloxane / vinyl diphenyl polydimethylsiloxane / silsesquioxane crosslinked polymer, and polymethylsilsesquioxane.

[0055] In some embodiments, the skin feel modifier is preferably configured to a weight percentage of 0–5 wt%.

[0056] Second moisturizer

[0057] In some embodiments, the second emollient is preferably formulated as at least one of a solid alcohol, fatty acid, beeswax, stearic acid, palmitic acid, behenol, stearyl alcohol, and behenic acid.

[0058] In some embodiments, when the second emollient is specifically configured to include at least one of solid alcohol, fatty acid, and beeswax, the second emollient is also preferably configured to include at least one of alkane, synthetic ester, and vegetable oil.

[0059] In some embodiments, the weight percentage of the second emollient is preferably configured to be 0.01 to 10 wt%.

[0060] pH adjuster

[0061] In some implementations, after heating the thickener, a pH adjuster is preferably added, and then the mixture is stirred until a homogeneous aqueous phase is obtained.

[0062] In some embodiments, the pH adjuster is preferably formulated as at least one of arginine, sodium hydroxide, potassium hydroxide, and aminomethylpropanol.

[0063] In some implementations, the added pH adjuster is preferably 0-6 wt% by weight.

[0064] II. The mixture of the first emollient and the emulsifier, and the second emollient are heated separately and then mixed together. The oil-soluble first skin conditioning agent is added and stirred until the mixture is uniform to obtain the oil phase.

[0065] First Skin Conditioner

[0066] In some implementations, the first skin conditioning agent is formulated to be oil-soluble.

[0067] In some embodiments, the first skin conditioning agent is preferably formulated to include at least one of tocopherol, tocopheryl acetate, ubiquinone, hydroxystearic acid, dipalmitoyl hydroxyproline, retinyl palmitate, and phenylethyl resorcinol.

[0068] In some embodiments, the weight percentage of the first skin conditioning agent is preferably configured to be 0.001 to 5 wt%.

[0069] Chelating agents

[0070] In some embodiments, when a chelating agent is added, the weight percentage of the added chelating agent is preferably 0 to 0.1 wt%.

[0071] This invention does not impose any particular limitation on the type of thickener; those skilled in the art can choose conventionally.

[0072] Moisturizer

[0073] In some implementations, when a humectant is added, the weight percentage of the humectant added is preferably 0 to 15 wt%.

[0074] This invention does not impose any particular limitation on the type of moisturizer; those skilled in the art can choose conventionally.

[0075] Second skin conditioning agent

[0076] In some embodiments, when a second skin conditioning agent is added, the weight percentage of the added skin conditioning agent is preferably 0 to 10 wt%.

[0077] This invention does not impose any particular limitation on the types of skin conditioning agents; those skilled in the art can choose conventionally.

[0078] preservative

[0079] In some implementations, when a preservative is added, the weight percentage of the preservative added is preferably 0 to 6 wt%.

[0080] This invention does not impose any particular limitation on the type of preservative; those skilled in the art can choose conventionally.

[0081] Deionized water

[0082] In some implementations, the aqueous phase is preferably configured to include deionized water.

[0083] In some implementations, the aqueous phase is preferably configured to include a second skin conditioning agent and deionized water.

[0084] In some embodiments, the second skin conditioning agent is preferably formulated as at least one of tetrahydromethylpyrimidine carboxylic acid, ectoine, snow lotus extract, and palmitoyl tripeptide-5.

[0085] This invention also provides a method for preparing a microbead system, comprising:

[0086] I. The thickener was mixed with deionized water and heated to obtain an aqueous phase.

[0087] In some embodiments, the thickener is preferably configured to a weight percentage of 0.2–5 wt%. After mixing the thickener with deionized water, the mixture is preferably heated to 70–90°C.

[0088] In some implementations, at least one of a chelating agent, a moisturizer, a primary skin conditioning agent, and a preservative is also added to the mixture of the thickener and deionized water.

[0089] In some implementations, a pH adjuster is also added when the thickener is mixed with deionized water and heated.

[0090] II. The mixture of the first emollient and the emulsifier, and the second emollient are heated separately, and then the mixture of the first emollient and the emulsifier is mixed with the second emollient to obtain the oil phase.

[0091] In some embodiments, the mixture of the first emollient and the emulsifier preferably comprises 0.06 to 15 wt% by weight and 0.02 to 5 wt% by weight of the first emollient and the emulsifier. The mixture of the first emollient and the emulsifier is preferably heated to 50 to 70°C and then mixed with the second emollient.

[0092] In some embodiments, the second emollient is preferably configured to be 0.01 to 10 wt%. The second emollient is preferably heated to 60 to 80°C and mixed with the mixture of the first emollient and the emulsifier.

[0093] In some embodiments, a skin feel modifier is also added when the second emollient is mixed with the mixture of the first emollient and the emulsifier.

[0094] III. The aqueous phase and oil phase are mixed and homogenized. The mixture is then kept at a high temperature for 10-20 minutes, cooled, and stirred to obtain the microbead system.

[0095] When the heat preservation time is less than 10 minutes, the microbead system cannot be formed.

[0096] When the heat preservation time exceeds 20 minutes, a water-in-oil system cannot be formed. At this time, the emulsifying ability of the emulsifier is greatly destroyed, and a water-in-oil system cannot be formed. The oil components are merely suspended in the thickener, resulting in uneven particles with poor hardness.

[0097] In some implementation schemes, a second skin conditioning agent is added when the microbeads appear after cooling and stirring following a 10-20 minute heat treatment.

[0098] Example

[0099] In Examples 1-15, there are phases A, B, C, D, E, and F. Phase F is configured to include a thickener and deionized water; phase A is configured to include a first emollient and an emulsifier; phase B is configured to include a second emollient; phase C is configured to include a skin feel modifier; phase D is configured to include a second skin conditioning agent and deionized water; phase E is configured to include deionized water and a pH adjuster; and phase F is configured to include a thickener and deionized water.

[0100] The specific raw materials for each phase are shown in Table 1.

[0101] Table 1

[0102]

[0103]

[0104] The preparation methods of Examples 1-5 are as follows:

[0105] Heat phase F to 75°C and stir until dissolved; mix and dissolve phase E and add it to phase F, stir evenly to obtain phase (E+F), which is an aqueous phase.

[0106] Stir phase A until it is uniformly mixed and heat it to 40°C. Heat phase B to 60°C and stir until it is dissolved, then add it to phase A. Add phase C to phase (A+B) and stir until it is uniformly mixed to obtain phase (A+B+C), which is the oil phase.

[0107] Turn on the homogenizer, mix the oil phase and water phase, homogenize until the emulsion is uniform, keep warm for a specific time (the warming time for Examples 1 to 5 is 10 min, 12 min, 15 min, 18 min and 20 min respectively), stir and cool until condensation occurs; add phase D and stir until the mixture is uniform.

[0108] The preparation methods for Examples 6-10 are as follows:

[0109] Heat phase F to 80°C and stir until dissolved; mix and dissolve phase E and add it to phase F, stir evenly to obtain phase (E+F), which is the aqueous phase.

[0110] Stir phase A until it is uniformly mixed and heat it to 60°C. Heat phase B to 70°C and stir until it is dissolved, then add it to phase A. Add phase C to phase (A+B) and stir until it is uniformly mixed to obtain phase (A+B+C), which is the oil phase.

[0111] Turn on the homogenizer, mix the oil phase and water phase, homogenize until the emulsion is uniform, keep warm for a specific time (wherein, the warming time for Examples 6 to 10 is 10 min, 12 min, 15 min, 18 min, and 20 min, respectively), stir and cool until condensation occurs; add the D phase and stir until the mixture is uniform.

[0112] The preparation methods of Examples 11-15 are as follows:

[0113] Heat phase F to 85°C and stir until dissolved; mix and dissolve phase E and add it to phase F, stir evenly to obtain phase (E+F), which is an aqueous phase.

[0114] Stir phase A until it is uniformly mixed and heat it to 80°C. Heat phase B to 80°C and stir until it is dissolved, then add it to phase A. Add phase C to phase (A+B) and stir until it is uniformly mixed to obtain phase (A+B+C), which is the oil phase.

[0115] Turn on the homogenizer, mix the oil phase and water phase, homogenize until the emulsion is uniform, keep warm for a specific time (the warming time for Examples 11 to 15 is 10 min, 12 min, 15 min, 18 min, and 20 min, respectively), stir and cool until condensation occurs; add phase D and stir until the mixture is uniform.

[0116] The preparation methods for Comparative Examples 1-4 are as follows:

[0117] Heat phase F to 80°C and stir until dissolved; mix and dissolve phase E and add it to phase F, stir evenly to obtain phase (E+F), which is the aqueous phase.

[0118] Stir phase A until it is uniformly mixed and heat it to 60°C. Heat phase B to 70°C and stir until it is dissolved, then add it to phase A. Add phase C to phase (A+B) and stir until it is uniformly mixed to obtain phase (A+B+C), which is the oil phase.

[0119] Turn on the homogenizer, mix the oil phase and water phase, homogenize until the emulsion is uniform, keep it at a specific time (the keeping time for Comparative Examples 1 to 4 is 0 min, 5 min, 7 min, and 25 min, respectively), stir and cool until condensation occurs; add the D phase and stir until the mixture is uniform.

[0120] The results are shown in Table 2.

[0121] Table 2

[0122]

[0123] From the data in Table 2 and Figure 1 It can be seen that after the oil phase and water phase are mixed and emulsified evenly, the microbeads can be more stably formed by keeping them at a temperature of 10-20 minutes. Moreover, the microbeads formed are uniform in size, which can further increase the proportion of active ingredients encapsulated in the system and improve the preservation activity of the active ingredients.

[0124] Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0125] Those skilled in the art can modify the technical solutions described in the above embodiments or make equivalent substitutions for some of the technical features; however, such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the protection scope of the technical solutions of the embodiments of this disclosure.

Claims

1. A method for preparing a microbead system, characterized in that, include: The thickener is mixed with deionized water and heated to 70-90°C to obtain an aqueous phase. The mixture of the first emulsifier and the emulsifier, and the second emulsifier are heated separately. The mixture of the first emulsifier and the emulsifier is heated to 50-70°C; the second emulsifier is heated to 60-80°C. The mixture of the first emulsifier and the emulsifier is then mixed with the second emulsifier to obtain the oil phase. The aqueous phase and oil phase are mixed and homogenized, and then cooled and stirred to obtain the microbead system. In this process, after the aqueous phase and oil phase are mixed and homogenized, they are first kept at a high temperature for 10 to 20 minutes and then cooled and stirred. The thickener is formulated as at least one of xanthan gum, sodium carbomer, sodium polyacrylate grafted starch, carbomer, acrylate / C10-30 alkanol acrylate crosspolymer, ammonium acryloyl dimethyl taurate / behenol polyether-25 methacrylate crosspolymer, and sodium acrylate copolymer. The first emollient is formulated as at least one of polydimethylsiloxane, cyclopentadimethylsiloxane, and trimethylpentaphenyltrisiloxane; The emulsifier is configured as a combination of silicone elastomer emulsifier KSG-210 and silicone emulsifier KF-6038, or a combination of silicone elastomer emulsifier SSG-210SP and silicone emulsifier KF-6038. The second emollient is specifically formulated as at least one of beeswax, stearic acid, palmitic acid, behenol, stearyl alcohol, and behenic acid; The first emollient is configured to have a weight percentage of 0.06 to 15 wt%, and the emulsifier is configured to have a weight percentage of 0.02 to 5 wt%. The second emollient is configured to have a weight percentage of 0.01 to 10 wt%.

2. The preparation method according to claim 1, characterized in that, The thickener is configured to have a weight percentage of 0.2–5 wt%.

3. A microbead system, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 2.

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