Eluting phase, oil gel bead preparation and preparation method thereof

Through oil-coagulation bead preparation and microcapsule granulator technology that does not wrap the wall material, the problem of uneven distribution of oil-coagulation beads in cosmetics is solved, and the regular shape, uniform size distribution and high aesthetics of oil-coagulation beads are achieved, which improves the sense of use and aesthetics of the product.

CN119523847APending Publication Date: 2025-02-28YUNNAN BOTANEE BIO TECH GRP CO LTD +1

Patent Information

Application Number
CN202411767390.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-04
Publication Date
2025-02-28

AI Technical Summary

Technical Problem

It is difficult to directly add fat-soluble raw materials or active substances to existing cosmetic water agent products, and traditional emulsification, solubilization and suspension technologies are difficult to form oil-coagulated beads with regular shapes and uniform size distribution, affecting the aesthetics and sense of use of the product.

Method used

Using an oil-coagulant bead preparation that does not wrap the wall material, the uniform molding and coating of the oil-coagulant beads are achieved through the technology of microcapsule granulator through the composition of isononononanoate, trimethylsilanooxyphenyldimethylsiloxane, stearyl alcohol, behenol, dextrin palmitate and maurime fruit oil, combined with the design of the elution phase and the collection solution.

Benefits of technology

The oil-condensing beads are achieved in a regular form, uniform size distribution, melt-in-applied and high aesthetics, and the "mud rub" phenomenon caused by wall coating is avoided, which improves the use and aesthetics of the product.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to an elution phase, an oil gel bead preparation and a preparation method of the oil gel bead preparation, the surface of the oil gel bead preparation does not wrap a wall material, and the oil gel bead preparation is prepared from 50-80 parts by weight of isononyl isononanoate, 10-20 parts by weight of trimethylsiloxyphenyl polydimethylsiloxane, 0-20 parts by weight of stearyl alcohol and / or 0-15 parts by weight of behenyl alcohol, 1-10 parts by weight of dextrin palmitate and 0-10 parts by weight of rosa palmifolia fruit oil according to 100 parts by weight. The obtained oil gel bead preparation is good in forming effect and more uniform in surface and size distribution, so that the oil gel bead preparation is more attractive, the oil gel bead preparation is melted once being smeared, and the phenomenon of mud rubbing is avoided. Besides, the oil gel bead preparation can be used for embedding fat-soluble active matters, the components are simpler, and the particle size of the oil gel bead preparation can be controlled, so that the oil gel bead preparations with different particle sizes can be obtained and can be applied to different types of cosmetics.
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Description

Technical Field

[0001] The present disclosure relates to the technical field of daily chemical products, and in particular to an elution phase, an oil gel bead preparation and a preparation method thereof. Background Art

[0002] At present, it is not possible to directly add fat-soluble raw materials or active ingredients to aqueous cosmetic products. Fat-soluble raw materials can only be added to aqueous products through emulsification, solubilization, suspension and other technical means, or various oily particles can be added to aqueous products to broaden the efficacy, skin feel and aesthetics of such products.

[0003] However, the above technical means all have some defects. Emulsification and solubilization technology cannot form visible particles, stirring suspension technology is difficult to form well-spherical solid oily particles, and other types of added particles are hard or difficult to spread, which affects the skin feel of the product. For example, CN115553463A discloses a method for preparing β-carotene microcapsules using a microcapsule granulator. The microcapsule is prepared by a microcapsule granulator, the oil phase is selected as the core material, and sodium alginate is prepared by Ca 2+ After solidification, a wall shell is formed. The microcapsule particles have good spherical characteristics and a smooth surface. When applied as a cosmetic, the sodium alginate shell is broken first and then the oil phase is allowed to overflow. However, it has a granular feel when used, and the large molecular compounds of sodium alginate will slow down absorption and even easily produce mud rubbing.

[0004] CN116473857A discloses an oil core condensed bead, a preparation method and a cosmetic, and the preparation principle is also to drain the internal phase oily raw material and the external phase raw material liquid containing sodium alginate into a calcium chloride solution at the same time, and solidify to form a microcapsule wrapped with sodium alginate. In addition, the skin care essence containing micro oil beads disclosed in CN111700856A, the high-stability skin care moisturizing particle essence disclosed in CN113876638A and its preparation method, and the cosmetics containing suspended particles disclosed in CN110585070A and its preparation method, etc., in principle, the oil phase raw material is heated and dissolved and then slowly added to the water phase, and the oil droplets are suspended by stirring. This method is difficult to control the size distribution of the oil droplets due to the uneven shear force inside and outside the stirring paddle, and it is difficult to solidify into a good spherical shape by cooling. Summary of the invention

[0005] The purpose of the present invention is to provide an oil gel bead preparation which has a regular shape, uniform size distribution, melts immediately after application, and has high aesthetics.

[0006] To achieve the above objectives, the present disclosure adopts the following technical solutions:

[0007] Provided is an oil condensation bead preparation, wherein the surface of the oil condensation bead preparation is not covered with a wall material; based on 100 parts by weight, the oil condensation bead preparation comprises:

[0008] 50-80 parts of isononyl isononanoate, 10-20 parts of trimethylsiloxyphenyl dimethicone, 0-20 parts of stearyl alcohol and / or 0-15 parts of behenyl alcohol, 1-10 parts of dextrin palmitate, and 0-10 parts of lily palm fruit oil.

[0009] Preferably, based on 100 parts by weight, the oil gel bead preparation comprises:

[0010] 60-80 parts of isononyl isononanoate, 10-20 parts of trimethylsiloxyphenyl dimethicone, 0-10 parts of stearyl alcohol and / or 0-10 parts of behenyl alcohol, 5-10 parts of dextrin palmitate, and 0-1 part of lily palm fruit oil.

[0011] More preferably, the particle size of the oil bead preparation is 0.5 to 6 mm.

[0012] To achieve the above objectives, the present disclosure adopts the following technical solutions:

[0013] Provide an elution phase, which, during the solidification and molding process of the oil-gelling bead preparation described in any one of the above items, wraps the droplets formed by the oil-gelling bead phase material to prevent the oil-gelling bead phase material from breaking;

[0014] Counting by weight 100 parts, the elution phase includes: 0.05-0.2 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 5-20 parts of pentanediol, 0.05-0.2 parts of aminomethyl propanol, and the balance of purified water.

[0015] Preferably, based on 100 parts by weight, the elution phase comprises: 0.1 parts of acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, 10 parts of pentanediol, 0.1 parts of aminomethyl propanol, and the balance of purified water.

[0016] To achieve the above objectives, the present disclosure also adopts the following technical solutions:

[0017] Provided is a method for preparing any of the above-mentioned oil gel bead preparations, comprising the following steps:

[0018] S1. mixing the oil-gel phase material and the elution phase material and dispersing the resulting mixture to form oil droplets of the oil-gel phase material encapsulated by the elution phase material;

[0019] S2. The oil droplets fall into the collecting liquid, the oil condensation phase material in the core of the oil droplets solidifies in the collecting liquid, and the elution phase material on the surface of the oil droplets dissolves in the collecting liquid;

[0020] S3. Enrich the solidified oil bead phase material to obtain an oil bead preparation.

[0021] Preferably, based on 100 parts by weight, the elution phase material comprises: 0.05-0.2 parts of acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, 5-20 parts of pentanediol, 0.05-0.2 parts of aminomethyl propanol, and the balance of purified water;

[0022] Based on 100 parts by weight, the collected solution includes 10 parts of pentanediol and the balance of water.

[0023] Preferably, before performing step S1, the temperature of the oil bead phase material and the elution phase material is maintained at 55°C to 75°C.

[0024] Preferably, in step S1, the oil condensate phase material and the elution phase material are respectively introduced into the core material nozzle and the wall material nozzle of the microcapsule granulator, and the oil condensate phase material and the elution phase material are sucked into the granulation unit to form the oil droplets after mixing and dispersion.

[0025] More preferably, the pressure of the core material nozzle and the wall material nozzle is 300-600 mbar, and the suction flow rate ratio of the oil-gelled bead phase material and the elution phase material is 1:3;

[0026] The oil bead phase material and the elution phase material are sucked into the granulation unit for mixing, and then dispersed through vibration and electrostatic action of the electrode sheet to form the oil bead droplets.

[0027] The technical solution claimed in the present disclosure has achieved the following beneficial effects:

[0028] 1) Existing oil-gel beads usually use a harder wall material to wrap the core of the oil-gel bead material, while the oil-gel bead preparation provided by the present invention does not contain a wall material. Therefore, compared with traditional oil-gel bead preparations, it can be applied and dissolved immediately, is easier to absorb, is not easy to "rub into mud", and has a better skin feel when used.

[0029] 2) The addition of dextrin palmitate, stearyl alcohol and behenyl alcohol in the raw materials of the oil bead preparation also makes the oil bead phase easier to form and less likely to disperse.

[0030] 3) During the preparation of the oil bead preparation, the elution phase is first used to wrap the oil bead phase particles to prevent them from dispersing and deforming. At the same time, the elution phase also plays a buffering role on the oil bead phase material during dripping into the collecting liquid, further preventing it from breaking, thereby making the solidification rate of the oil bead phase higher. Since the elution phase is dissolved in the collecting liquid, not only can an oil bead preparation with a more uniform and beautiful surface be obtained, but also the coating of the surface wall material can be avoided.

[0031] 4) During the preparation process, the oil-gel phase material and the elution phase material are kept warm, which can make the materials uniform and unified. The vibration and electrostatic effects can further make the oil-gel phase material and the elution phase material uniformly mixed and coated, making the surface and size distribution of the oil-gel bead preparation obtained by granulation more uniform and more beautiful.

[0032] 5) The use of microcapsule granulator can obtain oil bead preparations with different particle sizes by adjusting the nozzle aperture, material flow rate, vibration frequency and the composition of the oil bead phase, which can be used in different types of cosmetics.

[0033] 6) The obtained oil bead preparation can embed fat-soluble active substances, does not contain other ingredients such as emulsifiers and curing agents, has more streamlined ingredients, can be added to various lotions and essence products, and has a wide range of applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings in the following description are merely embodiments of the present disclosure, and a person of ordinary skill in the art can obtain other drawings based on the provided drawings without paying any creative work.

[0035] Figure 1 This is a photograph of the appearance of the oil beads preparation in Example 1.

[0036] Figure 2 This is a photograph of the appearance of the oil beads preparation in Example 2.

[0037] Figure 3 This is a photograph of the appearance of the oil beads preparation in Example 3.

[0038] Figure 4 This is a photograph of the appearance of the oil beads preparation in Comparative Example 1.

[0039] Figure 5 This is a photograph of the appearance of the oil beads preparation in Comparative Example 2.

[0040] Figure 6 The microscopic appearance and size diagram of the sampled particles of the oil bead preparation in Examples 1, 2, and 3.

[0041] Figure 7 The diagram shows the application effect of the oil gel beads preparation in Examples 1, 2, and 3 in essence. DETAILED DESCRIPTION

[0042] In order to make the purpose, technical solution and beneficial effects of the embodiments of the present disclosure clearer, the technical solution in the embodiments of the present disclosure will be clearly and completely described below in conjunction with the drawings in the embodiments of the present disclosure. Obviously, the described embodiments are part of the embodiments of the present disclosure, not all of the embodiments. Based on the embodiments of the present disclosure, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present disclosure.

[0043] Example 1

[0044] This embodiment provides an oil bead preparation, which does not contain a wall material.

[0045] Specifically, the oil gel bead preparation includes 69.9 parts of isononyl isononanoate, 10 parts of trimethylsiloxyphenyl polydimethicone, 10 parts of stearyl alcohol, 0 parts of behenyl alcohol, 10 parts of dextrin palmitate, and 0.1 parts of safflower oil, based on 100 parts by weight. Among them, dextrin palmitate is used as an excipient; stearyl alcohol and behenyl alcohol are used as solidifying agents; safflower oil is used as a toner or efficacy agent. The addition of dextrin palmitate and stearyl alcohol makes the oil gel bead phase easier to form and less likely to disperse, which is beneficial to the subsequent preparation of the oil gel bead preparation.

[0046] The preparation process of the oil beads preparation of this embodiment uses an elution phase, which, based on 100 parts by weight, includes: 0.1 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 10 parts of pentanediol, 0.1 parts of aminomethyl propanol, and the balance of purified water.

[0047] The preparation process of the oil bead preparation of this embodiment also uses a collecting liquid, which includes, by weight, 10 parts of pentanediol and the balance of purified water.

[0048] The preparation method of the oil gel beads preparation in this embodiment is as follows:

[0049] S1. Accurately weigh the components of the oil gel bead preparation, put them into a beaker, stir and dissolve them at 85°C, put the obtained oil gel bead phase material into a pressure bottle, keep it warm in a 75°C water bath to prevent the oil gel bead phase material from solidifying, and set aside.

[0050] S2. Accurately weigh the components of the elution phase, put them into a beaker and stir to mix. After preparing a viscous solution, transfer the elution phase to another pressure-resistant bottle and keep it warm in a 75°C water bath for standby use.

[0051] S3. Accurately weigh the components of the collected liquid, put them into a beaker, stir evenly, and set aside at room temperature.

[0052] S4. Connect the pressure-resistant bottle filled with oil-gelled bead phase material to the core material inlet of the microencapsulation granulator, connect the pressure-resistant bottle filled with elution phase material to the wall material inlet of the microencapsulation granulator, and wrap the material conveying pipeline of the pressure-resistant bottle filled with oil-gelled bead phase material with an electric heating belt to keep it warm at 75°C.

[0053] S5. The microcapsule granulator uses a core material nozzle with an aperture of 450μm and a wall material nozzle with an aperture of 900μm. The nozzle temperature is set to 65℃ to prevent the oil-gel phase material from solidifying and clogging the pipeline before dripping. The pressure is set to 350mbar. The flow rate valve is adjusted to control the flow rate ratio of the oil-gel phase material and the elution phase material to be 1:3. The oil-gel phase material and the elution phase material are sucked into the granulation unit and mixed. After the vibration of 750Hz frequency and the electrostatic effect of the electrode sheet, they are dispersed into oil droplets of the elution phase enveloping the oil-gel phase. The oil droplets fall into the collection liquid that moves back and forth. The oil-gel phase in the core of the oil droplet is further solidified and enriched, and the oil-gel preparation is obtained. At the same time, the elution phase on the surface of the oil-gel phase is dissolved in the collection liquid.

[0054] In this embodiment, the size of the oil bead preparation is related to the aperture of the nozzle, the material flow rate, the frequency of vibration, and the composition of the oil bead phase. Among them, the aperture of the nozzle determines an approximate range of the particle size of the oil bead preparation. The pressure value and the flow rate valve can determine the material flow rate, and the flow rate also indirectly affects the size of the oil bead preparation. In addition, some rheological properties of the oil bead phase of different oil components will also be different, and the size of the oil bead formed when passing through the nozzle will be affected by this. Therefore, in practical applications, by adjusting the above parameter conditions, oil bead preparations with different particle sizes can be obtained and used in different types of cosmetics.

[0055] In the prior art, the main function of the collecting liquid is to form a harder shell after a cross-linking reaction with the wall material. However, since the oil-gelled bead particles in this embodiment have no wall material and do not require a cross-linking reaction, the collecting liquid mainly plays the role of protecting the oil-gelled bead particles from solidification and corrosion.

[0056] In the preparation method of this embodiment, the elution phase is firstly wrapped around the oil bead phase to prevent it from dispersing and deforming. At the same time, it also plays a buffering role on the oil bead phase in the process of dripping into the collecting liquid, further preventing it from being broken by gravity and the movement of the collecting liquid, so that the solidification rate of the oil beads is higher. Moreover, since the elution phase is dissolved in the collecting liquid, not only can an oil bead preparation with a more uniform and beautiful surface be obtained, but also the coating of the surface wall material is avoided. When used, it can be applied and dissolved, is easier to absorb, is not easy to "rub mud", and has a better skin feel.

[0057] In addition, the insulation of the oil bead phase material and the elution phase material can make the materials uniform, and the vibration and static electricity can further make the oil bead phase material and the elution phase material uniformly mixed and coated, making the surface and size distribution of the oil bead preparation obtained by granulation more uniform and also making the oil bead preparation more beautiful.

[0058] In addition, the obtained oil gel beads preparation can embed fat-soluble active substances, does not contain other ingredients such as emulsifiers and curing agents, and has more concise ingredients. The obtained oil gel beads preparation can be added to various lotions and essence products and has a wide range of applications.

[0059] Example 2

[0060] This embodiment provides an oil bead preparation, which does not contain a wall material.

[0061] Specifically, the oil gel bead preparation includes 64.95 parts of isononyl isononanoate, 20 parts of trimethylsiloxyphenyl polydimethicone, 10 parts of stearyl alcohol, 0 parts of behenyl alcohol, 5 parts of dextrin palmitate, and 0.05 parts of safflower oil, based on 100 parts by weight. Among them, dextrin palmitate is used as an excipient; stearyl alcohol and behenyl alcohol are used as solidifying agents; safflower oil is used as a toner or efficacy agent. The addition of dextrin palmitate and stearyl alcohol makes the oil gel bead phase easier to form and less likely to disperse, which is beneficial to the subsequent preparation of the oil gel bead preparation.

[0062] The preparation process of the oil beads preparation of this embodiment uses an elution phase, which, based on 100 parts by weight, includes: 0.1 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 10 parts of pentanediol, 0.1 parts of aminomethyl propanol, and the balance of purified water.

[0063] The preparation process of the oil bead preparation of this embodiment also uses a collecting liquid, which, by weight, includes: 10 parts of pentanediol and the balance of purified water.

[0064] The preparation method of the oil gel beads preparation in this embodiment is as follows:

[0065] S1. Accurately weigh the components of the oil gel bead preparation, put them into a beaker, stir and dissolve them at 80°C, put the obtained oil gel bead phase material into a pressure-resistant bottle, keep it warm in a 70°C water bath to prevent the oil gel bead phase material from solidifying, and set aside.

[0066] S2. Accurately weigh the components of the elution phase, put them into a beaker and stir to mix. After preparing a viscous solution, transfer the elution phase to another pressure-resistant bottle and keep it warm in a 70°C water bath for standby use.

[0067] S3. Accurately weigh the components of the collected liquid, put them into a beaker, stir evenly, and set aside at room temperature.

[0068] S4. Connect the pressure-resistant bottle filled with oil-gelled bead phase material to the core material inlet of the microencapsulation granulator, connect the pressure-resistant bottle filled with elution phase material to the wall material inlet of the microencapsulation granulator, and wrap the material conveying pipeline of the pressure-resistant bottle filled with oil-gelled bead phase material with an electric heating belt to keep it warm at 70°C.

[0069] S5. The microcapsule granulator uses a core material nozzle with an aperture of 450μm and a wall material nozzle with an aperture of 900μm. The nozzle temperature is set to 65℃ to prevent the oil-gel phase material from solidifying and blocking the pipeline before dripping. The pressure is set to 450mbar. The flow rate valve is adjusted to control the flow rate ratio of the oil-gel phase material and the elution phase material to be 1:3. The oil-gel phase material and the elution phase material are sucked into the granulation unit and mixed. After the vibration of 750Hz frequency and the electrostatic effect of the electrode sheet, they are dispersed into oil droplets of the elution phase enveloping the oil-gel phase. The oil droplets fall into the reciprocating collection liquid. The oil-gel phase in the core of the oil droplets is further solidified and enriched to obtain the oil-gel preparation. At the same time, the elution phase on the surface of the oil-gel phase is dissolved in the collection liquid.

[0070] In this embodiment, the size of the oil bead preparation is related to the aperture of the nozzle, the material flow rate, the frequency of vibration, and the composition of the oil bead phase. Among them, the aperture of the nozzle determines an approximate range of the particle size of the oil bead preparation. The pressure value and the flow rate valve can determine the material flow rate, and the flow rate also indirectly affects the size of the oil bead preparation. In addition, some rheological properties of the oil bead phase of different oil components will also be different, and the size of the oil bead formed when passing through the nozzle will be affected by this. Therefore, in practical applications, by adjusting the above parameter conditions, oil bead preparations with different particle sizes can be obtained and used in different types of cosmetics.

[0071] In the prior art, the main function of the collecting liquid is to form a harder shell after a cross-linking reaction with the wall material. However, since the oil-gelled bead particles in this embodiment have no wall material and do not require a cross-linking reaction, the collecting liquid mainly plays the role of protecting the oil-gelled bead particles from solidification and corrosion.

[0072] In the preparation method of this embodiment, the elution phase is firstly wrapped around the oil bead phase to prevent it from dispersing and deforming. At the same time, it also plays a buffering role on the oil bead phase in the process of dripping into the collecting liquid, further preventing it from being broken by gravity and the movement of the collecting liquid, so that the solidification rate of the oil beads is higher. Moreover, since the elution phase is dissolved in the collecting liquid, not only can an oil bead preparation with a more uniform and beautiful surface be obtained, but also the coating of the surface wall material is avoided. When used, it can be applied and dissolved, is easier to absorb, is not easy to "rub mud", and has a better skin feel.

[0073] In addition, the insulation of the oil bead phase material and the elution phase material can make the materials uniform, and the vibration and static electricity can further make the oil bead phase material and the elution phase material uniformly mixed and coated, making the surface and size distribution of the oil bead preparation obtained by granulation more uniform, and also making the oil bead preparation more beautiful.

[0074] In addition, the obtained oil gel beads preparation can embed fat-soluble active substances, does not contain other ingredients such as emulsifiers and curing agents, and has more concise ingredients. The obtained oil gel beads preparation can be added to various lotions and essence products and has a wide range of applications.

[0075] Example 3

[0076] This embodiment provides an oil bead preparation, which does not contain a wall material.

[0077] Specifically, the oil gel bead preparation includes 77.95 parts of isononyl isononanoate, 10 parts of trimethylsiloxyphenyl dimethicone, 0 parts of stearyl alcohol, 6 parts of behenyl alcohol, 6 parts of dextrin palmitate, and 0.05 parts of safflower oil, based on 100 parts by weight. Among them, dextrin palmitate is used as an excipient; behenyl alcohol and stearyl alcohol are used as solidifying agents; safflower oil is used as a toner or efficacy agent. The addition of dextrin palmitate and behenyl alcohol makes the oil gel bead phase easier to form and less likely to disperse, which is beneficial to the subsequent preparation of the oil gel bead preparation.

[0078] The preparation process of the oil beads preparation of this embodiment uses an elution phase, which, based on 100 parts by weight, includes: 0.1 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 10 parts of pentanediol, 0.1 parts of aminomethyl propanol, and the balance of purified water.

[0079] The preparation process of the oil bead preparation of this embodiment also uses a collecting liquid, which includes, by weight, 10 parts of pentanediol and the balance of purified water.

[0080] The preparation method of the oil gel beads preparation in this embodiment is as follows:

[0081] S1. Accurately weigh the components of the oil gel bead preparation, put them into a beaker, stir and dissolve them at 80°C, put the obtained oil gel bead phase material into a pressure bottle, keep it warm in a 65°C water bath to prevent the oil gel bead phase material from solidifying, and set aside.

[0082] S2. Accurately weigh the components of the elution phase, put them into a beaker and stir to mix. After preparing a viscous solution, transfer the elution phase to another pressure-resistant bottle and keep it warm in a 65°C water bath for standby use.

[0083] S3. Accurately weigh the components of the collected liquid, put them into a beaker, stir evenly, and set aside at room temperature.

[0084] S4. Connect the pressure-resistant bottle filled with oil-gelled bead phase material to the core material inlet of the microencapsulation granulator, connect the pressure-resistant bottle filled with elution phase material to the wall material inlet of the microencapsulation granulator, and wrap the material conveying pipeline of the pressure-resistant bottle filled with oil-gelled bead phase material with an electric heating belt to keep it warm at 65°C.

[0085] S5. The microcapsule granulator uses a core material nozzle with an aperture of 450μm and a wall material nozzle with an aperture of 900μm. The nozzle temperature is set to 65℃ to prevent the oil-gel phase material from solidifying and blocking the pipeline before dripping. The pressure is set to 500mbar. The flow rate valve is adjusted to control the flow rate ratio of the oil-gel phase material and the elution phase material to be 1:3. The oil-gel phase material and the elution phase material are sucked into the granulation unit and mixed. After the vibration of 750Hz frequency and the electrostatic effect of the electrode sheet, they are dispersed into oil droplets of the elution phase enveloping the oil-gel phase. The oil droplets fall into the collection liquid that moves back and forth. The oil-gel phase in the core of the oil droplets is further solidified and enriched, and the oil-gel preparation is obtained. At the same time, the elution phase on the surface of the oil-gel phase is dissolved in the collection liquid.

[0086] In this embodiment, the size of the oil bead preparation is related to the aperture of the nozzle, the material flow rate, the frequency of vibration, and the composition of the oil bead phase. Among them, the aperture of the nozzle determines an approximate range of the particle size of the oil bead preparation. The pressure value and the flow rate valve can determine the material flow rate, and the flow rate also indirectly affects the size of the oil bead preparation. In addition, some rheological properties of the oil bead phase of different oil components will also be different, and the size of the oil bead formed when passing through the nozzle will be affected by this. Therefore, in practical applications, by adjusting the above parameter conditions, oil bead preparations with different particle sizes can be obtained and used in different types of cosmetics.

[0087] In the prior art, the main function of the collecting liquid is to form a harder shell after a cross-linking reaction with the wall material. However, since the oil-gelled bead particles in this embodiment have no wall material and do not require a cross-linking reaction, the collecting liquid mainly plays the role of protecting the oil-gelled bead particles from solidification and corrosion.

[0088] In the preparation method of this embodiment, the elution phase is firstly wrapped around the oil bead phase to prevent it from dispersing and deforming. At the same time, it also plays a buffering role on the oil bead phase in the process of dripping into the collecting liquid, further preventing it from being broken by gravity and the movement of the collecting liquid, so that the solidification rate of the oil beads is higher. Moreover, since the elution phase is dissolved in the collecting liquid, not only can an oil bead preparation with a more uniform and beautiful surface be obtained, but also the coating of the surface wall material is avoided. When used, it can be applied and dissolved, is easier to absorb, is not easy to "rub mud", and has a better skin feel.

[0089] In addition, the insulation of the oil bead phase material and the elution phase material can make the materials uniform, and the vibration and static electricity can further make the oil bead material and the elution phase material uniformly mixed and coated, making the surface and size distribution of the oil bead preparation obtained by granulation more uniform, and also making the oil bead preparation more beautiful.

[0090] In addition, the obtained oil gel beads preparation can embed fat-soluble active substances, does not contain other ingredients such as emulsifiers and curing agents, and has more concise ingredients. The obtained oil gel beads preparation can be added to various lotions and essence products and has a wide range of applications.

[0091] Comparative Example 1

[0092] This comparative example provides an oil gel bead preparation.

[0093] Among them, counting by weight 100 parts, the oil gel bead preparation includes: 77.9 parts of isononyl isononanoate, 10 parts of trimethylsiloxyphenyl polydimethicone, 0 parts of stearyl alcohol, 6 parts of behenyl alcohol, 6 parts of dextrin palmitate, and 0.1 parts of palmitole fruit oil.

[0094] Counted as 100 parts by weight, the collected liquid includes: 10 parts of pentanediol and the balance of purified water.

[0095] This comparative example did not use an elution phase.

[0096] The preparation method of the oil gel beads preparation in this comparative example is as follows:

[0097] S1. Accurately weigh the raw materials of the oil-gel phase, put them into a beaker, stir and dissolve them at 80°C, put the obtained raw materials of the oil-gel phase into a pressure-resistant bottle, keep it warm in a 65°C water bath to prevent the oil-gel phase materials from solidifying, and set aside.

[0098] S3. Accurately weigh the component raw materials of the collected liquid, put them into a beaker, stir evenly, and set aside at room temperature.

[0099] S4. Connect the pressure-resistant bottle containing the oil-gel phase material to the core material inlet of the microencapsulation granulator, and wrap the material conveying pipe of the pressure-resistant bottle with an electric heating belt to keep it warm at 65°C.

[0100] S5. The microcapsule granulator uses a core material nozzle with an aperture of 450μm, the nozzle temperature is set to 65℃, the pressure is set to 500mbar, and the flow rate valve is adjusted. After the oil-gel phase material is sucked into the granulation unit, it is dispersed into oil droplets through 750Hz frequency vibration and electrostatic action of the electrode sheet, and then drips into the collection liquid that moves back and forth, and is further solidified and enriched to obtain the oil-gel preparation.

[0101] Comparative Example 2

[0102] This comparative example provides an oil bead preparation, which does not contain a wall material.

[0103] Among them, counting by weight 100 parts, the oil bead phase includes: 79.9 parts of isononyl isononanoate, 10 parts of trimethylsiloxyphenyl polydimethicone, 10 parts of stearyl alcohol, 0 parts of behenyl alcohol, 0 parts of dextrin palmitate, and 0.1 parts of palmitole fruit oil (the difference between this comparative example and Example 1 is that dextrin palmitate is not added).

[0104] The preparation process of the oil beads preparation of this embodiment uses an elution phase, which, based on 100 parts by weight, includes: 0.1 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 10 parts of pentanediol, 0.1 parts of aminomethyl propanol, and the balance of purified water.

[0105] The preparation process of the oil gel beads preparation of this comparative example also uses a collecting liquid, which, by weight, includes: 10 parts of pentanediol and the balance of purified water.

[0106] The preparation method of the oil gel beads preparation in this comparative example is as follows:

[0107] S1. Accurately weigh the components of the oil gel bead preparation, put them into a beaker, stir and dissolve them at 85°C, then put the oil gel bead phase raw materials into a pressure bottle, keep warm in a 75°C water bath, and set aside.

[0108] S2. Accurately weigh the components of the elution phase, put them into a beaker and stir to mix. After preparing a viscous solution, transfer the elution phase to another pressure-resistant bottle and keep it warm in a 75°C water bath for standby use.

[0109] S3. Accurately weigh the components of the collected liquid, put them into a beaker, stir evenly, and set aside at room temperature.

[0110] S4. Connect the pressure-resistant bottle filled with oil-gelled bead phase material to the core material inlet of the microencapsulation granulator, connect the pressure-resistant bottle filled with elution phase material to the wall material inlet of the microencapsulation granulator, and wrap the material conveying pipeline of the pressure-resistant bottle filled with oil-gelled bead phase material with an electric heating belt to keep it warm at 75°C.

[0111] S5. The microcapsule granulator uses a core material nozzle with a pore size of 450μm and a wall material nozzle with a pore size of 900μm. The nozzle temperature is set to 65℃, the pressure is set to 350mbar, and the flow rate valve is adjusted to control the flow rate ratio of the oil-gel phase material and the elution phase material to be 1:3. The oil-gel phase material and the elution phase material are sucked into the granulation unit for mixing. After the vibration of 750Hz frequency and the electrostatic effect of the electrode sheet, they are dispersed into oil droplets of the elution phase enveloping the oil-gel phase, and drip into the collection liquid that moves back and forth. The oil-gel phase in the core of the oil droplet is further solidified and enriched to obtain the oil-gel preparation. At the same time, the elution phase on the surface of the oil-gel phase is dissolved in the collection liquid.

[0112] The oil bead phase components (weight percentage) and product test results of each embodiment and comparative example are shown in Table 1:

[0113] Table 1

[0114]

[0115] The appearance and performance of each oil gel bead preparation in Table 1 were observed and tested. The oil gel bead preparation obtained in Example 1 has a high content of dextrin palmitate, so tiny wrinkles appear on the surface, but the size distribution is uniform and moderate, and it melts as soon as it is applied. Figure 1 The oil bead preparation obtained in Example 2 has a uniform surface, a uniform size distribution, a moderate size, and melts as soon as it is applied. Figure 2 The oil beads obtained in Example 3 have a uniform surface, uniform size distribution, moderate size, and melt immediately after application. Figure 3 shown.

[0116] Comparative Example 1 does not use an elution phase, and the oil condensate phase cannot be formed in the granulation unit, so it drips into the collection liquid and aggregates into a mass, and its appearance is as follows: Figure 4 As shown in the comparative example 2, dextrin palmitate was not used, and the oil condensate beads dropped into the collection liquid could not form a sphere, and the shape was irregular and the size distribution was uneven. Its appearance was as follows Figure 5 shown. Figure 6 The microscopic appearance and size diagram of the sampled particles of the oil bead preparations of Examples 1, 2, and 3 are shown. It can be seen from the figure that the particle size of the oil bead preparation in Example 1 is about 4.3 mm, the particle size of the oil bead preparation in Example 2 is about 3.4 mm, and the particle size of the oil bead preparation in Example 3 is about 6.7 mm. Figure 7 The results of applying the oil beads preparations of Examples 1, 2, and 3 to cosmetic essences are shown. It can be seen from the figure that each oil beads preparation has good compatibility with the essence material and can exist stably.

[0117] The embodiments and comparative examples described above are merely illustrative descriptions of the present disclosure and are not intended to limit the scope of the present disclosure. Without departing from the design spirit of the present disclosure, various modifications and improvements made to the technical solutions of the present disclosure by ordinary technicians in this field should all fall within the protection scope determined by the present disclosure.

Claims

1. An oil bead preparation, characterized in that: The surface of the oil bead preparation is not covered with wall material; Counted by 100 parts by weight, the oil gel bead preparation comprises: 50-80 parts of isononyl isononanoate, 10-20 parts of trimethylsiloxyphenyl dimethicone, 0-20 parts of stearyl alcohol and / or 0-15 parts of behenyl alcohol, 1-10 parts of dextrin palmitate, and 0-10 parts of lily palm fruit oil.

2. The oil bead preparation according to claim 1, characterized in that Counted by 100 parts by weight, the oil gel bead preparation comprises: 60-80 parts of isononyl isononanoate, 10-20 parts of trimethylsiloxyphenyl dimethicone, 0-10 parts of stearyl alcohol and / or 0-10 parts of behenyl alcohol, 5-10 parts of dextrin palmitate, and 0-1 part of lily palm fruit oil.

3. The oil bead preparation according to claim 1, characterized in that The particle size of the oil bead preparation is 0.5 to 6 mm.

4. An elution phase, characterized in that In the solidification and molding process of the oil gel bead preparation according to any one of claims 1 to 3, the elution phase envelops the droplets formed by the oil gel bead phase material to prevent the oil gel bead phase material from breaking; Counting by weight 100 parts, the elution phase includes: 0.05-0.2 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 5-20 parts of pentanediol, 0.05-0.2 parts of aminomethyl propanol, and the balance of purified water.

5. The elution phase according to claim 4, characterized in that Based on 100 parts by weight, the elution phase includes: 0.1 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 10 parts of pentanediol, 0.1 parts of aminomethyl propanol, and the balance of purified water.

6. A method for preparing the oil bead preparation according to any one of claims 1 to 3, characterized in that: The following steps are involved: S1. mixing the oil-gel phase material and the elution phase material and dispersing the resulting mixture to form oil droplets of the oil-gel phase material encapsulated by the elution phase material; S2. The oil droplets fall into the collecting liquid, the oil condensation phase material at the core of the oil droplets solidifies in the collecting liquid, and the elution phase material on the surface of the oil droplets dissolves in the collecting liquid; S3. Enrich the solidified oil bead phase material to obtain an oil bead preparation.

7. The method according to claim 6, characterized in that The elution phase material comprises, based on 100 parts by weight, 0.05-0.2 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, 5-20 parts of pentanediol, 0.05-0.2 parts of aminomethyl propanol, and the balance of purified water; Based on 100 parts by weight, the collected solution includes 10 parts of pentanediol and the balance of water.

8. The method according to claim 6, characterized in that Before performing step S1, the temperature of the oil-gelled bead phase material and the elution phase material is maintained at 55°C to 75°C.

9. The method according to claim 6, characterized in that In step S1, the oil-gelled bead phase material and the elution phase material are respectively introduced into the core material nozzle and the wall material nozzle of the microcapsule granulator, and the oil-gelled bead phase material and the elution phase material are sucked into the granulation unit, and the oil droplets are formed after mixing and dispersion.

10. The method according to claim 9, characterized in that The pressure of the core material nozzle and the wall material nozzle is 300-600 mbar, and the suction flow rate ratio of the oil condensate phase material and the elution phase material is 1:3; The oil bead phase material and the elution phase material are sucked into the granulation unit for mixing, and then dispersed through vibration and electrostatic action of the electrode sheet to form the oil bead droplets.

Citation Information

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