Preparation method of powder cosmetic with gradient color effect and powder cosmetic

Abstract

The invention provides a preparation method of a powder cosmetic with a gradient color effect and the powder cosmetic. The preparation method comprises the following steps: mixing materials; color distribution: providing a mold, wherein the mold is provided with at least one cavity with an upward opening; respectively diluting at least one water-soluble pigment to obtain at least one pigment solution, and respectively dispensing the at least one pigment solution on at least one preset position at the bottom of the chamber; performing filling; freezing: freezing the material body in the mold at low temperature to obtain a powder mother product; demolding: separating the powder master product from the mold; drying: drying the demolded powder master product to obtain the powder cosmetic with a gradient color effect; the mass percent concentration of the pigment solution is 0.1-10%; and the viscosity of the mixed material body at the temperature of 25 DEG C is 1000-15000 cP. The powder cosmetic prepared by the preparation method provided by the invention can realize natural shading and gradient color effects.

Description

Technical Field

[0001] The present application belongs to the technical field of daily cosmetics, and specifically relates to a preparation method of powder cosmetics with gradient color effects and powder cosmetics. Background Art

[0002] Powder cosmetics can modify facial features and increase the glossiness of makeup. For example, highlighter powder can brighten areas and enhance facial contours, making the base makeup more radiant and eliminating dullness. It can also create a visual contrast between light and shadow, thereby increasing the three-dimensional effect of the facial features.

[0003] The mixed color powder cosmetics currently on the market are mostly compressed powders, which have complex production processes, low production efficiency, and irregular surface colors or obvious splicing effects. Summary of the invention

[0004] In view of this, the present application provides a method for preparing a powder cosmetic with a gradient color effect and a powder cosmetic with a natural gradient blending effect.

[0005] In the first aspect, the embodiment of the present application provides a method for preparing a powder cosmetic with a gradient color effect, comprising the following steps: mixing: providing raw materials for preparing powder cosmetics, mixing, and obtaining a mixed material body; coloring: providing a mold, the mold having at least one cavity opening upward; taking at least one water-soluble pigment, diluting them separately, obtaining at least one pigment solution, and applying the at least one pigment solution to at least one preset position at the bottom of the cavity; filling: filling the mixed material body into the mold after coloring according to a preset amount, and the water-soluble pigment diffuses directionally in the mixed material body under the action of the concentration gradient; freezing: freezing the material body in the mold at low temperature to obtain a powder master product; demolding: separating the powder master product from the mold; drying: drying the demolded powder master product to obtain a powder cosmetic with a gradient color effect; the mass percentage concentration of the pigment solution is 0.1% to 10%, preferably 0.5 to 5%; the viscosity of the mixed material body at 25°C is 1000 to 15000 cP, preferably 2000 to 5000 cP.

[0006] According to an embodiment of the first aspect of the present application, the mold is made of TPR, TPE, silicone, silicone rubber, rubber or metal; the bottom of the cavity of the mold has or does not have a three-dimensional pattern.

[0007] According to the embodiment of the first aspect of the present application, the gradient color effect is formed on the contact surface between the powder cosmetics and the bottom of the chamber, and extends toward the interior of the powder cosmetics.

[0008] According to an embodiment of the first aspect of the present application, in the filling step, the mixed material body is filled into the mold from different directions to achieve control of the diffusion direction of the water-soluble pigment.

[0009] According to an embodiment of the first aspect of the present application, after the filling step, an auxiliary diffusion step is also included, and the auxiliary diffusion step includes: baking or microwave heating the mixed material body in the mold.

[0010] According to an embodiment of the first aspect of the present application, the baking temperature is 30-70°C, and the baking time is 5min-1h; preferably, during the baking, the baking temperature increases gradually from the edge area to the center area of ​​the mixture body; more preferably, the baking temperature of the edge area of ​​the mixture body is 30-40°C, and the baking temperature of the center area of ​​the mixture body is 60-70°C.

[0011] According to an embodiment of the first aspect of the present application, the power of the microwave heating is 0.2 to 1 GHz, preferably 0.3 to 0.5 GHz; the microwave heating time is 20 s to 5 min, preferably 2 to 3 min.

[0012] According to an embodiment of the first aspect of the present application, the step of freezing the material in the mold at low temperature is carried out in a liquid nitrogen quick-freezing device; preferably, the temperature inside the liquid nitrogen quick-freezing device is -120 to -70°C, preferably -95 to -80°C.

[0013] According to an embodiment of the first aspect of the present application, the liquid nitrogen quick-freezing device is a liquid nitrogen tunnel, and the material body passes through the liquid nitrogen tunnel on a conveyor belt in the liquid nitrogen tunnel at a speed of 0.6 to 1 m / min, and the powdered mother product passes through the liquid nitrogen tunnel for 6 to 10 minutes.

[0014] According to an embodiment of the first aspect of the present application, drying includes any combination of one or more of vacuum drying, freeze drying, microwave drying and supercritical fluid drying; preferably, drying is vacuum freeze drying.

[0015] According to an embodiment of the first aspect of the present application, the raw materials for preparing powder cosmetics include a powder phase component, an oil phase component and a water phase component, and the raw materials form an oil-in-water emulsified system, wherein:

[0016] The powder phase components include: one or more of fillers and colorants;

[0017] The oil phase components include: one or more of emollients, antioxidants, and sunscreens;

[0018] The aqueous phase components include: one or more of solvents, thickeners, film formers, emollients, emulsifiers, preservatives, and active ingredients.

[0019] In a second aspect, an embodiment of the present application provides a powder cosmetic with a gradient color effect, characterized in that it is prepared by any of the above methods; optionally, the powder cosmetic is selected from pressed powder, blush, eye shadow or highlighter powder.

[0020] Compared with the prior art, this application has at least the following beneficial effects:

[0021] In the method provided in the present application, water is used as a solvent, and water-soluble pigments are dissolved into it to form a pigment solution with good fluidity. The pigment solution is first applied to the bottom of the mold cavity, and then the material is filled. Under the action of the concentration gradient, the pigment naturally diffuses from the high-concentration area to the low-concentration area, forming a soft transition gradient color effect; when two or more water-soluble pigments are used, pigments of different colors naturally merge during the diffusion process, forming multi-color blending and gradient, and by adjusting the initial concentration of the pigment solution and the viscosity of the mixed material, the prepared powder cosmetics have a natural gradient blending effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Other features, objects and advantages of the present application will become more apparent by reading the following detailed description of non-limiting embodiments with reference to the accompanying drawings, in which the same or similar reference numerals represent the same or similar features.

[0023] Figure 1 This is a product schematic diagram of Example 15 provided in the embodiments of the present application;

[0024] Figure 2 This is a product schematic diagram of Example 16 provided in the examples of the present application. DETAILED DESCRIPTION

[0025] In order to make the application purpose, technical solution and beneficial technical effect of the present application clearer, the present application is further described in detail in conjunction with the embodiments below. It should be understood that the embodiments described in this specification are only for explaining the present application, not for limiting the present application.

[0026] For simplicity, this application only explicitly discloses some numerical ranges. However, any lower limit can be combined with any upper limit to form an unclearly recorded range; and any lower limit can be combined with other lower limits to form an unclearly recorded range, and any upper limit can be combined with any other upper limit to form an unclearly recorded range. In addition, although not clearly recorded, each point or single value between the range endpoints is included in the range. Thus, each point or single value can be combined with any other point or single value as its own lower limit or upper limit or with other lower limits or upper limits to form an unclearly recorded range.

[0027] In the description of the present application, it should be noted that, unless otherwise specified, “above” and “below” are inclusive of the number, and the “multiple” in “one or more” means two or more than two.

[0028] The above application content of the present application is not intended to describe each disclosed embodiment or each implementation in the present application. The following description more specifically illustrates exemplary embodiments. In many places throughout the application, guidance is provided by a series of examples, which can be used in various combinations. In each example, enumeration is only used as a representative group and should not be interpreted as exhaustive.

[0029] The mixed color and gradient powder cosmetics currently on the market are mostly pressed powders, which have complex production processes, low production efficiency, and cannot form a natural gradient blending effect on the surface.

[0030] In view of the above problems, the present application provides a method for preparing powder cosmetics with gradient color effects and powder cosmetics with gradient color effects, which have a natural gradient blending effect, can be mass-produced, and improve production efficiency.

[0031] Preparation of powder cosmetics with gradient color effect

[0032] In the first aspect, the embodiment of the present application provides a method for preparing a powder cosmetic with a gradient color effect, comprising the following steps: mixing: providing raw materials for preparing powder cosmetics, mixing, and obtaining a mixed material body; coloring: providing a mold, the mold having at least one cavity opening upward; taking at least one water-soluble pigment, diluting them separately, obtaining at least one pigment solution, and applying the at least one pigment solution to at least one preset position at the bottom of the cavity; filling: filling the mixed material body into the mold after coloring according to a preset amount, and the water-soluble pigment diffuses directionally in the mixed material body under the action of the concentration gradient; freezing: freezing the material body in the mold at low temperature to obtain a powder master product; demolding: separating the powder master product from the mold; drying: drying the demolded powder master product to obtain a powder cosmetic with a gradient color effect; the mass percentage concentration of the pigment solution is 0.1% to 10%, preferably 0.5 to 5%; the viscosity of the mixed material body at 25°C is 1000 to 15000 cP, preferably 2000 to 5000 cP.

[0033] Among them, in the mixing step, the raw materials for preparing the powder cosmetics with gradient color effects can be purchased commercially or homemade. It can be understood that the raw materials for preparing the powder cosmetics with gradient color effects generally include powder phase components, oil phase components and water phase components. The raw materials can be mixed in various ways commonly used in the prior art to add the raw materials step by step and mix them evenly, such as mechanical stirring, etc., and homogenization, defoaming and other operations can be added during the mixing process. Different mixing methods and steps can be used according to different raw materials, and the present application is not limited thereto.

[0034] The preparation method provided in the embodiment of the present application is to pre-apply pigments to the mold, which requires providing a mold and preparing a water-soluble pigment solution. The mold needs to have at least one upwardly open chamber, which is used to accommodate the pigments and mixed materials to be applied; when preparing the water-soluble pigment solution, one or several water-soluble pigments are taken, dissolved and diluted respectively, to obtain one or several pigment solutions, and the one or several pigment solutions are applied to at least one preset position at the bottom of the chamber.

[0035] In the embodiment of the present application, when preparing the pigment solution, the same pigment can be selected and diluted into solutions of multiple concentrations to form a concentration gradient; two or more pigments can be selected and diluted into solutions of different concentrations or diluted into solutions of multiple concentrations to form a concentration gradient; two or more pigments can also be selected and mixed to obtain a pigment of a new color, which is then diluted and applied. There is no limitation on the use of various soluble pigments in the prior art, and they can be selected according to the needs of gradient color effects.

[0036] The embodiments of the present application do not limit the specific color of the water-soluble pigment. For example, the water-soluble pigment can be a commercially available water-soluble pigment product of the following brands: Red 4 (CI 14700), Red 22 (CI 45380), Red 28 (CI 45410), Red 33 (CI17200), Red 40 (CI 16035), Carmine (CI 75470), Blue 1 (CI 42090), Yellow 5 (CI 19140), Yellow 6 (CI15985), Yellow 7 (CI 10316), Yellow 8 (CI 45350), Yellow 10 (CI 47005), Violet 2 (CI 60730), Orange 4 (CI15510), Green 3 (CI 42053), Green 5 (CI 61570), Green 8 (CI 59040) and the like, or a combination of several thereof.

[0037] In the embodiment of the present application, the specific location and number of the preset positions are not limited and can be selected according to the design. For example, the preset positions are evenly distributed in an outer ring at the bottom of the chamber, or evenly distributed on a certain side of the bottom of the chamber, or at a fixed point at the bottom of the chamber.

[0038] In the filling step, the preset amount can be set according to the volume of the powder cosmetics, the mold capacity or the filling needs, and the preset amount filled each time can be the same or different. After the mixed material body is filled into the color-coated mold according to the preset amount, the water-soluble pigment will diffuse directionally in the mixed material body under the action of the concentration gradient.

[0039] In the embodiments of the present application, during filling, a common filling machine can be used for filling, or a pneumatic feeding device can be used for filling. The pneumatic feeding device refers to a device that fills the material into the mold by pneumatic conveying. Exemplarily, the pneumatic feeding device may include an air pump and a pipeline connected to the air pump, the air pump is used to provide the air pressure required for conveying, and the pipeline is used to fill the material into the mold, but the present application is not limited thereto. When using a common filling machine, the material is filled under the action of gravity. When the fluidity of the material meets the requirements, the filling can be carried out at room temperature; when it is desired to improve the fluidity of the material, the material can be appropriately heated.

[0040] For powder cosmetics with gradient color effects that form fine relief, filling with the help of air pressure feeding device is a better way. The material body is filled into the mold according to the preset amount through the air pressure feeding device, and the pressure assists the material body to fill into the sharp corners of the fine relief. Even if the viscosity of the material body is high, it can still be well filled into the sharp corners of the fine relief and achieve a good density, solving the problem of pores and softness in the finished product.

[0041] Specifically, the mixed material body can be pressed into the mold by the action of air pressure, for example, the air pressure feeding device includes a feeding pipe, an air pump and a discharging pipe, and the air pump provides conveying air pressure to suck the material body from the feeding pipe into the air pressure feeding device and then press it into the mold through the discharging pipe; the material body can also be sucked into the mold by the action of air pressure, for example, the air pressure feeding device is connected to the mold, and the air pressure feeding device provides conveying air pressure to suck the material body into the mold. In some embodiments, the pressure in the air pressure feeding device is: 0.01-0.06MPa, and can also be 0.02-0.04MPa.

[0042] After the filling step, a solvent removal step is also required. The solvent is removed from the powder cosmetics through freeze-drying and other process steps. The solvent content in the final powder cosmetics generally needs to be controlled below 5%.

[0043] In the method provided in the present application, water is used as a solvent, and water-soluble pigments are dissolved into it to form a pigment solution with good fluidity. The pigment solution is first applied to the bottom of the mold cavity, and then the material is filled. Under the action of the concentration gradient, the pigment naturally diffuses from the high-concentration area to the low-concentration area, forming a soft transition gradient color effect; when two or more water-soluble pigments are used, pigments of different colors naturally merge during the diffusion process, forming multi-color shading and gradient.

[0044] The present application utilizes the diffusion of water-soluble pigments in the material body to achieve natural blending and gradient color effects, and the initial concentration of the pigment solution and the viscosity of the mixed material body are key parameters. On the one hand, the mixed material body needs to have an appropriate viscosity suitable for the diffusion of water-soluble pigments. If the viscosity is too large, the diffusion of the pigment is hindered, and the gradient rendering effect is not obvious; if the viscosity is too small, the pigment diffuses excessively in the material body, and a natural gradient blending effect cannot be formed. On the other hand, the pigment solution needs to have an initial concentration suitable for diffusion in the mixed material body. If the initial concentration of the pigment solution is too low, the diffusion effect is not obvious and the blending effect cannot be achieved; if the initial concentration of the pigment solution is too high, pigment accumulation occurs locally in the material body, and the surface is uneven after drying.

[0045] In the embodiment of the present application, the initial concentration of the pigment solution and the viscosity of the mixed material are controlled within a certain range so that the prepared powder cosmetics have a natural gradient blurring effect. The embodiment of the present application is suitable for preparing water-in-oil system powder cosmetics.

[0046] Exemplarily, the viscosity of the mixture at 25° C. is 1000 cP, 2000 cP, 3000 cP, 4000 cP, 5000 cP, 6000 cP, 7000 cP, 8000 cP, 9000 cP, 10000 cP, 11000 cP, 12000 cP, 13000 cP, 14000 cP, 15000 cP or an interval range consisting of any two of the above values.

[0047] Exemplarily, the mass percentage concentration of the pigment solution is 0.1%, 0.2%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 7%, 8%, 9%, 10% or an interval range consisting of any two of the above values.

[0048] The preparation method provided in the embodiment of the present application has a simple manufacturing process, gets rid of the complexity of the traditional color mixing and powder pressing process, can realize mass production, and improve production efficiency.

[0049] In some embodiments, the mold is made of TPR, TPE, silicone, silicone rubber, rubber or metal; the bottom of the cavity of the mold has or does not have a three-dimensional pattern.

[0050] The preparation method in the embodiment of the present application can use the molds made of the above-mentioned TPR, TPE, silicone, silicone rubber, rubber or metal, and can prepare powder cosmetics with natural gradient color effects.

[0051] The bottom of the cavity of the selected mold can be flat and not have a three-dimensional pattern; or the bottom of the cavity of the mold can have a three-dimensional pattern, wherein the three-dimensional pattern can be diverse. For example, the three-dimensional pattern is a deer shape or a wavy shape, but the embodiments of the present application are not limited to this.

[0052] In some embodiments, the gradient color effect is formed on the contact surface between the powder cosmetics and the bottom of the chamber, and extends toward the inside of the powder cosmetics.

[0053] The pigment solution is dotted on the bottom of the chamber, and the gradient color effect is formed on the contact surface between the powder cosmetics and the bottom of the chamber. Under the action of the concentration gradient, the pigment solution diffuses in the thickness direction of the powder cosmetics, and the gradient color effect extends from the contact surface with the bottom of the chamber to the direction away from the contact surface, that is, extends to the inside of the powder cosmetics.

[0054] In some embodiments, during the filling step, the mixed material body is filled into the mold from different directions to achieve control of the diffusion direction of the water-soluble pigment.

[0055] The mixed material body has an impact when filling, which will drive the diffusion of the water-soluble pigment, thereby controlling the diffusion direction of the water-soluble pigment. When the mixed material body is filled into the mold from different directions, the water-soluble pigment will diffuse in different directions, which is conducive to forming a natural gradient blending effect.

[0056] In the embodiment of the present application, when filling the mixture body, the mixture body is filled into the mold from different directions. For example, the mixture body is filled along different directions at preset angles to the plane where the bottom of the mold is located. Preferably, the preset angle is 30° to 90°. Exemplarily, the preset angle is 30°, 40°, 45°, 50°, 60°, 70°, 80°, 90° or an interval range consisting of any two of the above values.

[0057] For example, when the preset angle is 90°, the mixture body is filled in a direction perpendicular to the plane where the bottom of the mold is located, and when the preset angle is 60°, the mixture body is filled in a direction inclined to the plane where the bottom of the mold is located.

[0058] In some embodiments, after the filling step, an auxiliary diffusion step is further included, and the auxiliary diffusion step may include baking the mixed material body in the mold or performing microwave heating on the mixed material body in the mold.

[0059] The embodiment of the present application adds an auxiliary diffusion step including baking or microwave heating after the filling step. On the one hand, baking or microwave heating can remove part of the water in the mixture body. On the other hand, baking or microwave heating can also promote the formation of a gradient color effect. After the filling is completed, the mixture body is in a steady state. During the baking or microwave heating process, the temperature of the mixture body rises, which helps the water-soluble pigment to continue to diffuse in the steady-state mixture body, making the gradient effect more natural; at the same time, the water-soluble pigment is also better adsorbed on the powder surface in the mixture body, making the gradient color effect more stable. The embodiment of the present application can promote a more natural gradient effect by adding an auxiliary diffusion step after the filling step.

[0060] The baking temperature and baking time are not limited in the present embodiment and can be set as required. Preferably, the baking temperature is 30-70° C. and the baking time is 5 min-1 h.

[0061] The baking temperature is in the range of 30-70°C, which makes the baking process gentler, can slowly evaporate water, help improve the uniformity of powder cosmetics, and can also make the water-soluble pigments diffuse evenly in the steady-state mixture. Exemplarily, the baking temperature is 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C or an interval range consisting of any two of the above values.

[0062] The baking time is within the range of 5 minutes to 1 hour. On the one hand, part of the water in the mixed material will not evaporate excessively, and on the other hand, the baking efficiency is high, saving production time. Exemplarily, the baking time is 5 minutes, 10 minutes, 15 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes, 1 hour, or an interval consisting of any two of the above values.

[0063] Furthermore, in the present application, during the directional diffusion of water-soluble pigments in the mixed material under the action of concentration gradient, the diffusion rate of pigment molecules in the edge area of ​​the material may be faster than that in the central area. The reason for this may be that the probability of pigment molecules in the edge area of ​​the material colliding with each other is low, and the diffusion rate is fast, while the probability of pigment molecules in the central area of ​​the material colliding with each other is high, and the diffusion rate is slow.

[0064] In this regard, in some embodiments, baking is used to assist diffusion, and the baking temperature is increased gradually from the edge area to the center area of ​​the mixed material body. Exemplarily, the baking temperature of the edge area of ​​the mixed material body is 30-40°C, and the baking temperature of the center area of ​​the mixed material body is 60-70°C, so that the assisted diffusion effect on the material body in the center area is greater than the assisted diffusion effect on the pigment molecules in the edge area of ​​the material body, reducing the difference in diffusion speed between the edge area and the center area when the pigment molecules diffuse in the material body.

[0065] In other embodiments, microwave heating is used to assist diffusion. For example, the power of microwave heating is 0.2 to 1 GHz, preferably 0.3 to 0.5 GHz, and the microwave heating time is 20 s to 5 min, preferably 2 to 3 minutes. For example, the power of microwave heating can be 0.2 GHz, 0.3 GHz, 0.4 GHz, 0.5 GHz, 0.6 GHz, 0.7 GHz, 0.8 GHz, 0.9 GHz, 1.0 GHz, or an interval range consisting of any two of the above values. For example, the time of microwave heating can be 20 s, 30 s, 40 s, 50 s, 1 min, 1.2 min, 1.4 min, 1.5 min, 1.6 min, 1.8 min, 2 min, 2.5 min, 3 min, 3.5 min, 4 min, 4.5 min, 5 min, or an interval range consisting of any two of the above values.

[0066] Microwave heating has a central effect, that is, microwaves are reflected in the furnace cavity, and the central position is in the overlapping area of ​​the microwave field. The microwave energy density is high, and the microwave energy decreases toward the edge area. Therefore, the present application uses relatively small-power microwave heating to make the central area of ​​the mixed material body first receive microwave radiation without drying immediately, causing the molecular motion to accelerate, and the auxiliary effect on diffusion is higher than that of the edge area. Due to the above-mentioned characteristics of microwave heating, not only can auxiliary diffusion be achieved in a relatively short time, but also the situation in which the diffusion speed of the edge area is greater than the diffusion speed of the central area when the pigment molecules diffuse in the material body can be solved, so that the interference factors of the gradient color effect are minimized, and the gradient is more natural and soft.

[0067] In some embodiments, the step of freezing the material in the mold at low temperature is performed in a liquid nitrogen quick-freezing device; preferably, the temperature inside the liquid nitrogen quick-freezing device is -120 to -70°C, preferably -95 to -80°C.

[0068] Exemplarily, the liquid nitrogen quick-freezing device may be a liquid nitrogen tunnel, a liquid nitrogen freezer, an ultra-low temperature refrigerator, etc. These devices are commercially available, and the present application is not limited thereto.

[0069] The raw material components in the mixed material body undergo molecular quick freezing in an extremely low temperature environment in a liquid nitrogen quick freezing device. The mixed material body contains components such as oils and emulsions. During its freezing and shaping process, it will experience a maximum ice crystal formation zone, which is approximately in the temperature range of -10 to 0°C, and about 80% of the liquid (water, emulsion, etc.) will turn into ice. Unlike the ordinary freezing implemented before demolding in the prior art, in the molecular quick freezing process completed in the liquid nitrogen tunnel of the present application, the powder master product quickly passes through the maximum ice crystal formation zone. The distribution of ice crystals in the powder master product is smaller, more uniform and dense. In the subsequent drying process, the removal of small and uniform ice crystals will not affect the gradient color effect that has been formed, ensuring a natural, soft and continuous gradient, and making the skin feel of the freeze-dried product softer, the product size variable is smaller and easier to control, the product structure is more stable, and the drop resistance is better.

[0070] In some embodiments, the liquid nitrogen quick-freezing device is a liquid nitrogen tunnel, and the material body passes through the liquid nitrogen tunnel on a conveyor belt in the liquid nitrogen tunnel at a speed of 0.6 to 1 m / min, and the powdered mother product passes through the liquid nitrogen tunnel for 6 to 10 minutes.

[0071] Liquid nitrogen tunnel, also known as liquid nitrogen tunnel quick freezer, is a device that uses liquid nitrogen as a cold source and adopts a continuous production method. It delivers materials into the quick freezing tunnel through a conveyor belt to achieve continuous entry and exit and rapid freezing of materials.

[0072] The present application also proposes the optimal liquid nitrogen quick-freezing condition parameters suitable for the preparation of powder cosmetics of the present application through the study of the freezing curve of the powder cosmetic mixture and the energy transfer characteristics in the liquid nitrogen quick-freezing device. The liquid nitrogen quick-freezing of the powder master product under the above condition parameters can make the powder cosmetics finally prepared have a uniform and dense texture, the best skin feel, and the stability and anti-drop ability of the product structure are optimal. The powder master product passes through the liquid nitrogen tunnel at a speed of 0.6 to 1 m / min on the conveyor belt in the liquid nitrogen tunnel, and the passing time of the powder master product in the liquid nitrogen tunnel is 6 to 10 minutes.

[0073] In some embodiments, drying comprises one or any combination of vacuum drying, freeze drying, microwave drying and supercritical fluid drying; preferably, drying is vacuum freeze drying.

[0074] In the embodiment of the present application, the powder masterbatch after demolding is dried by vacuum freeze-drying technology. Freeze-drying is to freeze the water-containing material below the freezing point to convert water into ice. In a vacuum environment or under higher vacuum conditions, the fine and evenly distributed ice crystals in the powder masterbatch are sublimated into water vapor and removed, thereby retaining the composition, color and aroma of the raw materials to the greatest extent. The pigment is naturally adsorbed on the surface of the powder and will not be transferred with the liquid water, thereby ensuring the stable maintenance of the rendering effect during the entire drying process.

[0075] The embodiments of the present application may also be dried by vacuum drying, freeze drying, microwave drying, supercritical fluid drying, or by superimposing a plurality of the above drying methods.

[0076] In some embodiments, the raw materials for preparing powder cosmetics include a powder phase component, an oil phase component and a water phase component, and the raw materials form an oil-in-water emulsion system, wherein:

[0077] The powder phase components include: one or more of fillers and colorants;

[0078] The oil phase components include: one or more of emollients, antioxidants, and sunscreens;

[0079] The aqueous phase components include: one or more of solvents, thickeners, film formers, emollients, emulsifiers, preservatives, and active ingredients.

[0080] In the embodiment of the present application, the raw materials form an oil-in-water emulsion system, and the oil-in-water emulsion system uses water as a continuous phase, which can make the water-soluble pigment flow better and the gradient effect more natural.

[0081] In some embodiments, the thickener and film former are selected from natural water-soluble polymers or their derivatives, synthetic water-based polymers or water-based inorganic thickeners;

[0082] The natural water-soluble polymer or its derivative is selected from at least one of alginic acid, agar, carrageenan, xanthan gum, gellan gum, crispy chondrus crispus, xanthan gum, guar gum, tamarind gum, tara gum, gum arabic, tragacanth gum, tara gum, pectin, arabinogalactan, wheat protein, soy protein, gelatin, casein, chitosan, curdlan, cyclodextrin, hyaluronic acid, konjac gum, tremella polysaccharide, codyl gelatin, microcrystalline cellulose, methylcellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch phosphate, starch, sodium hydroxymethyl starch, sodium polyacrylate grafted starch, and hydroxypropyl guar gum;

[0083] The synthetic water-based polymer is selected from at least one of acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, carbomer, acrylic acid (esters) / octylacrylamide copolymer, acrylic acid (esters) / ethylhexyl acrylate copolymer, sodium acrylate / sodium acryloyldimethyl taurate copolymer, acrylic acid (esters) / octylacrylamide copolymer, styrene / acrylic acid (esters) copolymer, acrylic acid (esters) copolymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyacrylate crosspolymer-6, acrylic acid (esters) / stearyl alcohol polyether-20 methacrylate copolymer, ammonium acryloyldimethyl taurate / behenyl alcohol polyether-25 methacrylate crosspolymer, acrylic acid (esters) copolymer ammonium, sodium polyacrylate, sodium polyacryloyldimethyl taurate, polyacrylamide, polyvinyl pyrrolidone, polyvinyl alcohol, VP / VA copolymer, polyurethane-1, and polyurethane-35;

[0084] The aqueous inorganic thickener is selected from at least one of aluminum magnesium silicate, sodium magnesium lithium silicate, lithium magnesium silicate, sodium magnesium silicate, montmorillonite or its derivatives;

[0085] In some embodiments, the emollient is selected from at least one of alcohols, silicone oils, mineral oils, synthetic oils, animal and plant oils, or their derivatives;

[0086] The animal and plant oil or its derivative is selected from at least one of glycerin, propylene glycol, dipropylene glycol, pentylene glycol, butylene glycol, ethylene glycol, hexylene glycol, sorbitol, xylitol, polyethylene glycol, polydimethylsiloxane, caprylyl polymethylsiloxane, phenyl trimethicone, cetyl polydimethylsiloxane, C30-45 alkyldimethylsilyl polypropyl silsesquioxane, bis-PEG-18 methyl ether dimethyl silane, white mineral oil, petrolatum, hydrogenated polyisobutene, lanolin and its derivatives, octyldodecanol, caprylic / capric triglyceride, ethylhexyl palmitate, bis-diglyceryl polyacyl adipate-2, isononyl isononanoate, jojoba seed oil, coconut oil, hydrogenated coconut glycerides, white meadowfoam seed oil, olive oil, squalane, C9-12 alkane, coconut alcohol-caprylate / caprate, tocopheryl acetate, and methyl gluceth-10;

[0087] In some embodiments, the filler is selected from at least one of mica, talc, synthetic fluorphlogopite, kaolin, bentonite, boron nitride, bismuth oxychloride, silica, sodium potassium aluminum silicate, lauroyl lysine, magnesium stearate, magnesium myristate, calcium aluminum borosilicate, tin oxide, sodium calcium borosilicate, aluminum hydroxide, zinc stearate starch and its derivatives, and plastic microbeads.

[0088] In some embodiments, the preservative is selected from at least one of phenoxyethanol, parabens, chlorphenesin, potassium sorbate, sodium benzoate or preservative enhancers.

[0089] The preservative synergist is selected from at least one of caprylyl glycol, p-hydroxyacetophenone, ethylhexylglycerin, 1,2-hexanediol, caprylhydroxamic acid, 1,2-pentanediol, glyceryl caprylate, and cymene;

[0090] In a second aspect, an embodiment of the present application provides a powder cosmetic with a gradient color effect, characterized in that it is prepared by any of the above methods; optionally, the powder cosmetic is selected from pressed powder, blush or eye shadow.

[0091] The powder cosmetics prepared in the embodiment of the present application have a natural gradient blurring effect.

[0092] In some embodiments, the powder cosmetics with gradient color effects are selected from pressed powder, blush, eye shadow or highlighter powder. The powder cosmetics with gradient color effects may also include products with other functions.

[0093] Example

[0094] The following examples describe the disclosure of the present application in more detail, and these examples are for illustrative purposes only, as various modifications and variations within the scope of the disclosure of the present application are apparent to those skilled in the art. Unless otherwise stated, all parts, percentages, and ratios reported in the following examples are by mass, and all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the instruments used in the examples are commercially available.

[0095] Example 1

[0096] (1) Mixing: Provide the following raw materials: Phase A: water, binder, potassium chloride solution, emulsifier, oil, VE; Phase B: synthetic fluorphlogopite, silica; Phase C: pearlescent agent; Phase D: preservative. The temperature control range of the mixing process is 60-65°C. Heat phase A, add phase B, phase C, and phase D, and emulsify and homogenize. After emulsification and homogenization, vacuum degassing is performed to obtain a mixed material. The viscosity of the mixed material at 25°C is 5000cP, and it is ready for filling.

[0097] (2) Coloring: A silicone mold is provided, wherein the silicone mold has a cavity opening upward and a 3D embossed pattern at the bottom of the cavity; a water-soluble pigment CI 42090 is diluted with water to form a pigment solution having a mass percentage concentration of 3%, and the pigment solution is applied to the preset positions at the bottom of the cavity of the silicone mold.

[0098] (3) Filling: Fill the mixture into the mold after coloring from the center of the mold according to the preset amount;

[0099] (4) Freezing: placing the mold filled with the mixed material in a freezer at -15°C to freeze the mold to obtain a powdered masterbatch;

[0100] (5) Demolding: Separating the powder masterbatch from the mold;

[0101] (6) Drying: The powdered masterbatch after demoulding is baked to obtain powdered cosmetics.

[0102] Embodiment 2-5

[0103] The difference between Examples 2-5 and Example 1 is that the mass percentage concentration of the pigment solution or the viscosity of the mixed material body is different.

[0104] Embodiment 6-9

[0105] The difference between Example 6-9 and Example 1 is that after the filling step, an auxiliary diffusion step is performed on the material body in the mold.

[0106] The assisted diffusion step of Example 6 is baking, and the mixed material body is baked uniformly at 50°C as a whole.

[0107] The assisted diffusion step of Example 7 is baking, and the baking temperature increases gradually from the edge area to the center area of ​​the mixture body; the baking temperature of the edge area of ​​the mixture body is 30°C, and the baking temperature of the center area of ​​the mixture body is 70°C.

[0108] The assisted diffusion step of Examples 8 and 9 is microwave heating, the microwave frequencies in the microwave cavity are 0.3 GHz and 0.5 GHz, and the microwave heating time is 3 min and 2 min.

[0109] Examples 10-12

[0110] The difference between Examples 10-12 and Example 1 is that the step of freezing the material body in the mold is performed in a liquid nitrogen tunnel.

[0111] Embodiment 13

[0112] The difference between Example 13 and Example 1 is that the drying step adopts vacuum freeze drying. Specifically, vacuum freeze drying includes pre-freezing, sublimation drying and analytical drying. Pre-freezing specifically includes: freezing for 0.5h-2h under -40℃~-50℃. Sublimation drying includes: first heating treatment to -3℃~3℃, the heating treatment includes several first heating stages and several first insulation stages, and the first heating stage is alternately performed with the first insulation stage; the first heating stage is heated at 0.5~1℃ / min for 10~20min, and the first insulation time is 1.5~2h. Analytical drying includes: drying treatment at 20℃~60℃, the drying treatment includes several second heating stages and several second insulation stages, and the second heating stage is alternately performed with the second insulation stage; the second heating stage is heated at 0.5~1℃ / min for 10~20min, and the second insulation time is 1.5h~2h.

[0113] Embodiment 14

[0114] The difference between Example 14 and Example 1 is that after the filling step, the material body in the mold is subjected to microwave-assisted diffusion; the step of freezing the material body in the mold is carried out in a liquid nitrogen tunnel; the drying step adopts vacuum freeze drying, and the specific steps of freeze drying are the same as the freeze drying steps in Example 13.

[0115] Embodiment 15

[0116] The difference between Example 15 and Example 1 is that after the filling step, the material body in the mold is baked; the step of freezing the material body in the mold is carried out in a liquid nitrogen tunnel; the drying step adopts vacuum freeze drying, and the specific steps of freeze drying are the same as the freeze drying steps in Example 13; step (2) is the coloring step, in which water-soluble pigments CI19140 and CI 42090 are premixed to obtain a combination pigment of the desired color, which is then diluted with water in different proportions to obtain several pigment solutions of different concentrations, and the pigment solutions are respectively dotted at preset positions on the bottom periphery of the mold cavity.

[0117] Example 16

[0118] The difference between Example 16 and Example 15 lies in the step (2) of coloring, in which the water-soluble pigment Cl42090 is diluted with water in a certain ratio (blue); the water-soluble pigment CI17200 is diluted with water in a certain ratio (red); the water-soluble pigments CI42090 and CI17200 are mixed in a certain ratio and then diluted with water (purple); the blue and red pigment solutions are respectively applied to the diagonal positions of the bottom of the mold, and the purple pigment solution is applied to the other two diagonal positions.

[0119] Comparative Examples 1 to 6

[0120] The difference between Comparative Example 1 and Example 1 is that, before filling, a syringe is used to inject a pigment solution into the mixed material body, and then the material body is filled.

[0121] The difference between Comparative Example 2 and Example 1 is that after filling, the pigment solution is immediately injected into the bottom of the mold cavity using a syringe.

[0122] The difference between Comparative Examples 3-6 and Example 1 lies in the difference in the concentration of the pigment solution and the viscosity of the mixed material.

[0123] The parameters of mixing, coloring, filling and baking, freezing demoulding and drying of Examples 1-16 and Comparative Examples 1-6 are shown in Table 1.

[0124] Table 1 Process parameters of Examples 1 to 16 and Comparative Examples 1 to 6

[0125]

[0126] Test Section

[0127] Pressed powders were prepared according to the methods of Examples 1 to 16 and Comparative Examples 1 to 6, 100 pressed powders were prepared for each Example or Comparative Example, and appearance observation and drop test were performed.

[0128] 1) Appearance observation

[0129] Observe the appearance of the pressed powder with the naked eye or with the aid of a microscope, including the appearance of the gradient color effect, with a focus on whether the gradient color effect is natural and uniform, and the smoothness of the gradient color surface.

[0130] The appearance recorded is based on the observation of more than 90% of the 100 pressed powders.

[0131] 2) Drop detection

[0132] Adjust the rotating screws on the drop test table and adjust the flat plate to the 30cm scale; place the powder block with the front side facing up in the center of the test height.

[0133] Perform the first drop test: Press the test bench button to let the powder block fall onto the hard board, pick up the powder block that has fallen onto the table, and check whether the powder block surface is cracked or broken. If the powder block is cracked or broken, stop the drop test for this powder block. If the powder block is normal, then perform the second drop test. The operation steps for the second drop test are the same as the first drop test. If the powder block is cracked or broken, then stop the drop test for this powder block; if the powder block is normal, then perform the third drop test. The operation steps for the third drop test are the same as the first drop test.

[0134] The ratio of the number of powder cakes that broke in each drop test to the total number of powder cakes that were dropped in the drop test is the breakage rate of each drop test, and the first breakage rate, the second breakage rate, and the third breakage rate of Examples 1 to 16 and Comparative Examples 1 to 6 are recorded respectively. The drop resistance scoring standard is shown in Table 2:

[0135] Table 2 Drop resistance rating standard

[0136] The sum of three rupture rates Less than 5% 5％～10％ 10％～15％ 15％～20％ 20％～25％ 25％～30％ Drop resistance rating 5 points 4 points 3 points 2 points 1 point 0 points

[0137] The above test results of Examples 1 to 16 and Comparative Examples 1 to 6 are recorded in Table 3.

[0138] Table 3 Test results of Examples 1 to 16 and Comparative Examples 1 to 6

[0139]

[0140]

[0141] From the test results shown in Table 3, it can be seen that Examples 1 to 16 adopt the preparation method of powder cosmetics with gradient color effects provided by the present application, and are filled into the mold after coloring and filling, and then frozen, dried and demolded to obtain block powder cosmetics. Compared with Comparative Examples 1 to 6 that do not adopt the preparation method of the present application, Comparative Examples 1 to 6 cannot form a gradient color effect, or the color and gradient effects are not obvious; Examples 1 to 16 have significantly improved filling efficiency, whether the gradient color effect is natural and uniform, and the smoothness of the gradient color surface, and also have a significant effect in reducing the cracking rate of the powder cake drop detection.

[0142] In the preparation method of powder cosmetics with gradient color effects provided by the present application, the initial concentration of the pigment solution and the viscosity of the mixed material, the temperature and time control of the powder master product solidified at low temperature, and other parameters also have an impact on the technical effect of the present application. The present application also provides a selectable optimal range for the above process parameters, so that the various properties of the powder cosmetics with gradient color effects prepared by the method provided by the present application are further improved. For example, in Examples 6 to 9, assisted diffusion is performed after filling, and the gradient color range that can be formed is larger than that of Examples 1-5. In particular, the assisted diffusion through gradient baking and microwave heating can avoid the phenomenon that the diffusion speed of pigment molecules in the edge area of ​​the material body is faster than that in the central area during the preparation process, and the interference with the gradient effect is reduced, and the gradient is softer and more natural; in Examples 10 to 12, ultra-low temperature pre-freezing is performed in a liquid nitrogen tunnel, which not only forms a gradient color effect, but also the gradient color is more obvious than that of Examples 1-5, and no color loss occurs after drying; Example 13 adopts vacuum freeze drying including pre-freezing, sublimation drying and analytical drying, which not only forms a gradient color effect, but also the gradient color is more obvious than that of Examples 1-5, and no color loss occurs after drying; Examples 14-16 form better gradient color effects by adjusting process parameters, the interference with the gradient effect is reduced, the gradient is soft and natural, the color is obvious, and no color loss occurs after drying. For the product effect of Example 15, please refer to the attached Figure 1 For the product effect of Example 16, please refer to the attached Figure 2 .

[0143] In Comparative Examples 1 to 6, which do not use the method provided in the present application to implement the preparation steps, powder cosmetics with a gradient color effect cannot be obtained.

[0144] In comparative example 1, the pigment solution is injected into the mixed material body with a syringe before filling, and then filled. The surface has a smudge effect, but a directional and natural gradient smudge effect cannot be formed. After filling in comparative example 2, the pigment solution is immediately injected into the bottom of the mold cavity with a syringe. The pigment can only diffuse locally, and air is introduced into the material body, which destroys the compactness inside the material body. Holes, cracks, and pigment spots appear in the powder product, and the drop resistance is poor. In comparative example 3, the viscosity of the material body is too small, and the pigment diffuses excessively in the material body. If it is a multi-color mixture, it may be mixed together to form a single color, and the viscosity of the material body is too small. After the powder block is formed, it will be too soft and have poor drop resistance. In comparative example 4, the viscosity of the material body is too large, the diffusion of the pigment is hindered, and the rendering effect is not obvious. In comparative example 5, the concentration of the pigment solution is too low, and the smudge effect is not obvious; in comparative example 6, the concentration of the pigment solution is too high: pigment accumulation occurs locally in the material body, and the surface is uneven after drying.

[0145] The above examples 1 to 16 and comparative examples 1 to 6 fully demonstrate that the preparation method provided in the present application has outstanding beneficial effects and can prepare powder cosmetics with natural blooming and gradient color effects.

[0146] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed in the present application, and these modifications or replacements should be included in the protection scope of the present application. Therefore, the protection scope of the present application shall be based on the protection scope of the claims.

Claims

1. A method for preparing powder cosmetics with gradient color effect, characterized in that: The steps include: Mixing: providing raw materials for preparing powder cosmetics, mixing them to obtain a mixed material; Cloth color: providing a mold, the mold having at least one cavity opening upward; Taking at least one water-soluble pigment, diluting it respectively to obtain at least one pigment solution, and applying the at least one pigment solution to at least one preset position on the bottom of the chamber; Filling: Filling the mixture into the color-applied mold according to a preset amount, and the water-soluble pigment diffuses directionally in the mixture under the action of the concentration gradient; Freezing: Freeze the material in the mold at low temperature to obtain a powder masterbatch; Demoulding: Separate the powder masterbatch from the mould; Drying: Dry the powdered masterbatch after demoulding to obtain powdered cosmetics with gradient color effects; The mass percentage concentration of the pigment solution is 0.1% to 10%, preferably 0.5 to 5%; The viscosity of the mixture at 25° C. is 1000 to 15000 cP, preferably 2000 to 5000 cP.

2. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: The mold is made of TPR, TPE, silicone, silicone rubber, rubber or metal; the bottom of the cavity of the mold has or does not have a three-dimensional pattern.

3. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: The gradient color effect is formed on the contact surface between the powder cosmetic and the bottom of the chamber, and extends toward the inside of the powder cosmetic.

4. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: In the filling step, the mixed material body is filled into the mold from different directions to achieve control of the diffusion direction of the water-soluble pigment.

5. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: After the filling step, an auxiliary diffusion step is also included, and the auxiliary diffusion step includes: baking or microwave heating the mixed material body in the mold.

6. The method for preparing powder cosmetics with gradient color effect according to claim 5, characterized in that: The baking temperature is 30-70°C, and the baking time is 5min-1h; preferably, during the baking, the baking temperature increases gradually from the edge area to the center area of ​​the mixture body; more preferably, the baking temperature of the edge area of ​​the mixture body is 30-40°C, and the baking temperature of the center area of ​​the mixture body is 60-70°C.

7. The method for preparing powder cosmetics with gradient color effect according to claim 5, characterized in that: The frequency of the microwave heating is 0.2-1 GHz, preferably 0.3-0.5 GHz; the microwave heating time is 20 s-5 min, preferably 2-3 min.

8. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: The step of freezing the material in the mold at low temperature is carried out in a liquid nitrogen quick freezing device; Preferably, the temperature inside the liquid nitrogen quick-freezing device is -120°C to -70°C, preferably -95°C to -80°C.

9. The method for preparing powder cosmetics with gradient color effect according to claim 8, characterized in that: The liquid nitrogen quick-freezing device is a liquid nitrogen tunnel. The material body passes through the liquid nitrogen tunnel on a conveyor belt in the liquid nitrogen tunnel at a speed of 0.6 to 1 m / min. The powdered mother product passes through the liquid nitrogen tunnel for 6 to 10 minutes.

10. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: The drying includes one or any combination of vacuum drying, freeze drying, microwave drying and supercritical fluid drying; Preferably, the drying is vacuum freeze drying.

11. The method for preparing powder cosmetics with gradient color effect according to claim 1, characterized in that: The raw materials for preparing powder cosmetics include a powder phase component, an oil phase component and a water phase component, and the raw materials form an oil-in-water emulsified system, wherein: The powder phase components include: one or more of fillers and colorants; The oil phase components include: one or more of emollients, antioxidants, and sunscreens; The water phase components include: one or more of solvents, thickeners, film formers, emollients, emulsifiers, preservatives, and active ingredients.

12. A powder cosmetic with a gradient color effect, characterized in that: Prepared by the method according to any one of claims 1 to 11; optionally, the powder cosmetics are selected from pressed powder, blush, eye shadow or highlighter.

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