Preparation method of blocky powder cosmetic and blocky powder cosmetic

Abstract

The invention provides a preparation method of a blocky powder cosmetic and the blocky powder cosmetic. The preparation method of the blocky powder cosmetic comprises the following steps: material mixing: providing raw materials for preparing the blocky powder cosmetic, and mixing the raw materials to obtain a material body; filling and pre-curing: filling the material body into a mold according to a preset amount through an air pressure feeding device, and extruding and drying the material body to obtain a powder master product which is pre-cured and formed in the mold; freezing: freezing the pre-cured and molded powder mother product at a low temperature; demolding and drying: separating the frozen powder mother product from the mold, and drying to obtain the blocky powder cosmetics; or the frozen powder mother product is dried and separated from the mold, and the blocky powder cosmetics are obtained. According to the preparation method disclosed by the invention, the problems of shrinkage deformation, poor drop resistance of a finished product, cracking, air hole appearance, softness and the like in the preparation process can be improved, and the inactivation of high-temperature sensitive active matters in the preparation process is not caused.

Description

Technical Field

[0001] The present application belongs to the technical field of cosmetics, and in particular relates to a preparation method of block powder cosmetics and block powder cosmetics. Background Art

[0002] The preparation of bulk powder cosmetics usually includes the steps of mixing, filling, demoulding, and solvent removal. In the filling step, in order to obtain good filling efficiency and effect, the composition needs to have good fluidity. Therefore, the composition system to be filled must contain a certain amount of solvent (usually water, or a mixture of water and one or more organic solvents, and the amount of solvent added is generally higher than 50%), and the composition to be filled must be preheated at high temperature (usually 70-90 degrees Celsius). Since the powder particle content in the bulk powder cosmetic raw materials is high, and the improvement of the material fluidity is limited, even if the solvent is added and heated for filling, pores are still very likely to appear in the sharp angle parts of some fine reliefs.

[0003] After the filling step, a solvent removal step is also required, such as heating, baking, freeze drying and other process steps to remove the solvent from the powder cosmetics. The solvent content in the final powder cosmetics generally needs to be controlled below 5%. However, the solvent removal process is not easy to control, which may cause shrinkage and deformation during the preparation process, resulting in poor drop resistance, cracking, pores, softness and other problems in the finished product.

[0004] In addition, adding functional ingredients to cosmetic powder products is the product demand trend. The heating operation in the filling step can easily lead to the inactivation of functional ingredients, resulting in some active ingredients that are sensitive to high temperatures being unable to be used in cosmetic powder products. Summary of the invention

[0005] The embodiments of the present application provide a method for preparing block powder cosmetics and block powder cosmetics to improve the shrinkage and deformation during the preparation process, as well as the problems of poor drop resistance, cracking, pores, and softness of the finished product, and will not cause the inactivation of high-temperature sensitive active substances during the preparation process.

[0006] In a first aspect, an embodiment of the present application provides a method for preparing block powder cosmetics, comprising the following steps: mixing: providing raw materials for preparing block powder cosmetics, mixing the raw materials to obtain a material body; filling and pre-curing: filling the material body into a mold according to a preset amount via an air pressure feeding device, extruding and drying the material body to obtain a powder master product pre-cured in the mold; freezing: freezing the pre-cured powder master product at low temperature; demolding and drying: separating the frozen powder master product from the mold, drying, and obtaining a block powder cosmetic; or drying the frozen powder master product, separating it from the mold, and obtaining a block powder cosmetic.

[0007] According to an embodiment of the first aspect of the present application, the step of filling the material body into the mold according to a preset amount via a pneumatic feeding device includes: pressing or sucking the material body into the mold by the action of air pressure.

[0008] According to the embodiment of the first aspect of the present application, the viscosity of the material is below 30000 cP, preferably 10000 cP to 25000 cP; the pressure in the air pressure feeding device is: 0.02 to 0.1 MPa, preferably 0.04 to 0.08 MPa.

[0009] According to an embodiment of the first aspect of the present application, the extrusion drying includes performing filter pressing on the material body in the mold to allow at least part of the solvent to dialyze out of the material body, and transferring the dialyzed solvent simultaneously with or after the filter pressing.

[0010] According to an embodiment of the first aspect of the present application, the extrusion drying includes applying filter pressing and negative pressure suction to the material body in the mold; the pressure parameter of the filter pressing is: 0.05-3Mpa, preferably 0.2-1.5Mpa. The pressure parameter of the negative pressure suction is: 0.02-0.1Mpa, preferably 0.05-0.08Mpa.

[0011] According to an embodiment of the first aspect of the present application, in the step of simultaneously performing filter pressing and negative pressure suction on the material body in the mold, the solvent content in the material body is reduced to 30-80%, preferably 30-50%, of the original solvent content in the material body before filter pressing and negative pressure suction, to obtain a powder masterbatch pre-cured in the mold.

[0012] According to the embodiment of the first aspect of the present application, the solvent content in the prepared block powder cosmetics is less than 5%, preferably within 1%.

[0013] According to an embodiment of the first aspect of the present application, the step of freezing the pre-cured powder masterbatch at low temperature is carried out in a liquid nitrogen quick-freezing device.

[0014] 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 temperature inside the liquid nitrogen tunnel is -120 to -70°C, preferably -95 to -80°C; the powdered mother product passes through the liquid nitrogen tunnel on a conveyor belt in the liquid nitrogen tunnel at a speed of 0.4 to 1.2 m / min, preferably 0.6 to 1 m / min, and the passage time of the powdered mother product in the liquid nitrogen tunnel is 5 to 15 minutes, preferably 6 to 10 minutes.

[0015] According to an embodiment of the first aspect of the present application, drying includes one or any combination of heating drying, vacuum drying, freeze drying, microwave drying and supercritical fluid drying.

[0016] According to an embodiment of the first aspect of the present application, drying includes freeze drying and a combination of one or more of the following drying methods: heating drying, vacuum drying, microwave drying or supercritical fluid drying.

[0017] According to an embodiment of the first aspect of the present application, the temperature of the drying step is lower than 40°C.

[0018] According to the embodiment of the first aspect of the present application, the raw materials for preparing block powder cosmetics include powder phase components, oil phase components and water phase components; 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.

[0019] According to an embodiment of the first aspect of the present application, the thickener and the film-forming agent are selected from natural water-soluble polymers or derivatives thereof, synthetic water-based polymers or water-based inorganic thickeners; the natural water-soluble polymers or derivatives thereof are 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, arabogalactan, wheat protein, soy protein, gelatin, casein, chitosan, curdlan, cyclodextrin, hyaluronic acid, konjac gum, tremella polysaccharide, codyl gum, microcrystalline cellulose, methylcellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch phosphate, starch, sodium hydroxymethyl starch, sodium polyacrylate grafted starch, and hydroxypropyl guar gum;

[0020] 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;

[0021] 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;

[0022] Based on the prepared block powder cosmetics, the mass percentage of the aqueous inorganic thickener and / or film former is 0.02-15%, preferably 0.05-5%.

[0023] According to an embodiment of the first aspect of the present application, the emollient is selected from at least one of alcohols, silicone oil, mineral oil, synthetic oil, animal and plant oils or their derivatives;

[0024] 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;

[0025] Based on the prepared block powder cosmetics, the mass percentage of the emollient and moisturizing agent is 0.1-40%, preferably 0.5-30%.

[0026] According to an embodiment of the first aspect of the present application, 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;

[0027] The colorant is selected from at least one of iron oxide (CI 77499, CI 77491, CI 77492), titanium dioxide (CI 77891), iron blue (CI 77510), ultramarine (CI 77007), manganese violet (CI 77742), chromium oxide green (CI 77288), chromium hydroxide green, carmine (CI 75470), carbon black (CI 77266), CI 15850, CI 19140, CI 45410, CI 16035, CI 45380, CI17200, CI 73360, CI 42090, and CI 47005;

[0028] Based on the prepared block powder cosmetics, the total mass percentage of the filler and the colorant is 50-99%, preferably 70-95%.

[0029] According to an embodiment of the first aspect of the present application, the preservative is selected from at least one of phenoxyethanol, parabens, chlorphenesin, potassium sorbate, sodium benzoate or a preservative synergist;

[0030] 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;

[0031] Based on the prepared block powder cosmetics, the total mass percentage content of the preservative and the preservative synergist is 0.01-5%, preferably 0.5-1%.

[0032] According to an embodiment of the first aspect of the present application, the active ingredient is selected from a high temperature sensitive active ingredient or a high temperature insensitive active ingredient.

[0033] According to an embodiment of the first aspect of the present application, the active ingredient is selected from high temperature sensitive active ingredients, and the high temperature sensitive active ingredient is selected from at least one of polypeptide active ingredients, astaxanthin, vitamin A alcohol or its derivatives, vitamin C or its derivatives, and arbutin.

[0034] According to an embodiment of the first aspect of the present application, the solvent is water or a mixture of water and an organic solvent.

[0035] According to an embodiment of the first aspect of the present application, the thickener is an inorganic thickener; preferably, the inorganic thickener is at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, lithium magnesium silicate, sodium magnesium silicate, montmorillonite or its derivatives.

[0036] In a second aspect, an embodiment of the present application provides a block powder cosmetic, which is prepared by the method of an embodiment of the first aspect of the present application.

[0037] According to an embodiment of the second aspect of the present application, the block powder cosmetics are selected from pressed powder, blush, eye shadow or highlighter powder.

[0038] Compared with the prior art, the embodiments of the present application have at least the following beneficial effects:

[0039] First, block powder cosmetics are close to solvent-free, but in the preparation process, solvents are necessary for the mixing and transportation of raw materials. The addition and removal of solvents not only affect the production energy efficiency, but also have an adverse effect on the performance of the final product. In this application, the material is quantitatively filled into the mold via an air pressure feeding device, which reduces the requirements for the fluidity of the material and does not require the addition of too much solvent; and extrusion drying is implemented in the filling step, the content of solvent in the material is greatly reduced, and the subsequent drying time is shortened from 12 to 24 hours to 6 to 10 hours, which improves production efficiency and effectively reduces the problems of shrinkage deformation, cracking, and poor drop resistance of the final product.

[0040] Second, for block powder cosmetics that form fine relief, the material is quantitatively filled into the mold through an air pressure feeding device, and the material in the mold is simultaneously filtered and vacuum-sucked. The pressure assists the material to be filled into the sharp corners of the fine relief. Even if the viscosity of the material is high, it can still be well filled into the sharp corners of the fine relief and achieve a good density, thus solving the problems of pores and looseness in the finished product.

[0041] Third, for block powder cosmetics with added functional active ingredients, the preparation process of the present application does not include any high-temperature process, the filling step can be performed at low temperature or room temperature, and high-temperature sensitive active ingredients can be added to the material.

[0042] In summary, the present application provides a method for preparing block powder cosmetics, which can effectively avoid shrinkage and deformation during the desolvation process of the product, as well as cracking, poor drop resistance, pores, and softness of the finished product. It can present an excellent fine embossed surface and can add high-temperature sensitive active substances, while improving production efficiency and reducing energy consumption. DETAILED DESCRIPTION

[0043] The features and exemplary embodiments of various aspects of the present application will be described in detail below. In order to make the purpose, technical solutions and advantages of the present application clearer, the present application will be further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only intended to explain the present application, rather than to limit the present application. For those skilled in the art, the present application can be implemented without the need for some of these specific details. The following description of the embodiments is only to provide a better understanding of the present application by illustrating the examples of the present application.

[0044] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the statement "include..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0045] In the prior art, in the preparation of bulk powder cosmetics, a sufficient amount of solvent is added and the material is heated to improve the fluidity of the material to meet the filling and transfer requirements. After the filling step, a solvent removal step is also performed, such as removing the solvent from the bulk powder cosmetics through heating, baking, freeze drying and other process steps, and the solvent content in the final bulk powder cosmetics product generally needs to be controlled below 5%. The inventor of the present application has noticed that the process of solvent removal is not easy to control, so that the product may shrink and deform during the solvent removal process, and increase the occurrence of problems such as cracking, poor drop resistance, pores, and softness in the finished product. In addition, due to the high content of powder particles in the bulk powder cosmetic raw materials, the improvement of the fluidity of the material is limited. Even if the solvent is added and heated for filling, pores are still very likely to appear in the sharp angle parts of some fine reliefs, and the heating and filling operation will also cause the high temperature sensitive active substances added to the product to be inactivated or partially inactivated.

[0046] In order to solve the above problems, the inventor of the present application provides a block powder cosmetic and a preparation method thereof.

[0047] In the first aspect, the embodiments of the present application provide a method for preparing block powder cosmetics, comprising the following steps: mixing: providing raw materials for preparing block powder cosmetics, mixing the raw materials to obtain a material body; filling and pre-curing: filling the material body into a mold according to a preset amount via an air pressure feeding device, extruding and drying the material body to obtain a powder master product pre-cured in the mold; freezing: freezing the pre-cured powder master product at low temperature; demolding and drying: separating the frozen powder master product from the mold, drying, and obtaining a block powder cosmetic; or drying the frozen powder master product, separating it from the mold, and obtaining a block powder cosmetic.

[0048] Among them, in the mixing step, the raw materials for preparing the block powder cosmetics can be purchased or homemade. It can be understood that the raw materials for preparing the block powder cosmetics usually 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.

[0049] In the filling step, the preset amount can be set according to the volume of the block powder cosmetics, the mold capacity or the filling needs, and the preset amount of each filling can be the same or different. The pneumatic feeding device in the present application 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.

[0050] After the filling step, the material body is subjected to an extrusion drying operation, and a mechanical physical drying method is adopted to remove part of the solvent in the material body, so that before entering the subsequent freezing, demoulding and drying steps, a powder masterbatch pre-cured in the mold is obtained.

[0051] The pre-cured powder masterbatch still contains solvent. In the embodiment of the present application, after filling and pre-curing, the powder masterbatch is frozen through a freezing step, and the liquid (such as water, emulsion, etc.) in the powder masterbatch is frozen into ice.

[0052] The order of demoulding and drying steps can be adjusted. For example, after the frozen powdered masterbatch is separated from the mold, it is dried to obtain a block-shaped powdered cosmetic; or after the frozen powdered masterbatch is dried, it is separated from the mold to obtain a block-shaped powdered cosmetic.

[0053] Block powder cosmetics are close to solvent-free, but in the prior art, it is necessary to introduce solvents in the preparation process for the purpose of mixing and transporting raw materials. The addition of solvents and the drying and desolventizing process not only affect the production energy efficiency, but also have an adverse effect on the performance of the final product. In the preparation method of block powder cosmetics provided in the embodiment of the present application, the material body is quantitatively filled into the mold via an air pressure feeding device, which reduces the requirements for the fluidity of the material body and reduces the amount of solvent added; and extrusion drying is implemented in the filling step. Before entering the drying step, the content of solvent in the pre-cured material body has been significantly reduced, reducing the amount of solvent removed in the subsequent drying step and shortening the drying time, thereby effectively reducing the problems of shrinkage deformation, cracking, and poor drop resistance in the final product. In some embodiments, the subsequent drying time is shortened from 12 to 24 hours to 6 to 10 hours.

[0054] For block powder cosmetics that form fine relief, the material is filled into the mold according to a preset amount through an air pressure feeding device, and in the process of squeezing and drying the material in the mold, pressure assists the material to be filled into the sharp corners of the fine relief. Even if the viscosity of the material is high, it can still be well filled into the sharp corners of the fine relief and achieve a good density, thus solving the problems of pores and softness in the finished product.

[0055] For block powder cosmetics with added functional active ingredients, the preparation process of the present application does not include any high-temperature process, the filling step can be performed at low temperature or room temperature, and high-temperature sensitive active ingredients can be added to the material without worrying about the active ingredients becoming ineffective due to high temperature.

[0056] Therefore, the preparation method provided in the embodiment of the present application can effectively avoid shrinkage and deformation during the desolvation process of the product, as well as cracking, poor drop resistance, pores, softness and other problems in the finished product, and can add high-temperature sensitive active substances while improving production efficiency.

[0057] In some embodiments, the step of filling the material body into the mold according to a preset amount via the air pressure feeding device includes: pressing or sucking the material body into the mold by the action of air pressure.

[0058] The present application does not limit the specific method of filling the material into the mold according to the preset amount. The 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. 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.

[0059] Whether the material is pressed into or sucked into the mold, the fluidity of the material is required to be low, and there is no need to add too much solvent, which greatly shortens the subsequent drying time.

[0060] In some embodiments, the viscosity of the material is below 30000 cP, preferably 10000 cP to 25000 cP; the pressure in the air pressure feeding device is: 0.02 to 0.1 MPa, preferably 0.04 to 0.08 MPa.

[0061] In some embodiments, extrusion drying includes performing filter pressing on the material body in the mold to allow at least part of the solvent to be dialyzed out of the material body, and transferring the dialyzed solvent during or after the filter pressing. It is understandable that the transfer of the dialyzed solvent can be achieved in various specific ways, including but not limited to: suction, absorption, drainage, etc.

[0062] In some embodiments, the extrusion drying operation includes applying filter pressing and negative pressure suction to the material in the mold; the pressure parameter of the filter pressing is: 0.05-3Mpa, preferably: 0.2-1.5Mpa. The pressure parameter of the negative pressure suction is: 0.02-0.1Mpa, preferably: 0.05-0.08Mpa.

[0063] The term "filter pressing" in the present application refers to an operation in which a certain pressure is applied to a material body in the presence of a filter medium, so that at least part of the solvent is dialyzed out of the material body through the filter medium.

[0064] The "negative pressure suction" in this application refers to the operation of sucking and transferring the dialyzed solvent through negative pressure difference by using the negative pressure vacuum suction principle.

[0065] Exemplarily, the device for achieving pressure filtration may be a filter press, and the device for achieving negative pressure suction may be a vacuum suction pump. The present application does not limit the specific composition and structure of the device.

[0066] During the operation of air pressure feeding and extrusion drying, the viscosity of the material is closely related to characteristics such as fluidity and surface tension. In the prior art, the viscosity of the filling material is generally less than 5000cP due to fluidity requirements; since the present application adopts air pressure feeding and extrusion drying, the viscosity of the material only needs to be less than 30000cP, and the preferred viscosity range is 10000cP to 25000cP. Corresponding to the viscosity range of the material, the pressure in the feeding and extrusion drying process implemented by the present invention needs to reach a certain threshold to meet the requirements of assisting the material to fill the sharp corners of the fine relief of the powder, and to achieve a good density, and solve the problems of pores and looseness in the finished product; at the same time, the pressure in the feeding and extrusion drying process is not the greater the better. Excessive pressure is not conducive to the stability of the material, and may even cause boiling of some components in the material, which in turn affects the filling effect of the material on the mold. The present application proposes that when the pressure in the air pressure feeding device, the pressure parameters of the filter press, and the pressure parameters of the negative pressure suction are within a certain range, the pressure parameters of the material body and the air pressure feeding and pressurized drying process meet the optimal adaptation, so that the present application can achieve the best performance in improving the porosity, softness, shrinkage deformation and drop resistance of the final product.

[0067] Exemplarily, the viscosity of the material may be 10000 cP, 11000 cP, 12000 cP, 13000 cP, 14000 cP, 15000 cP, 16000 cP, 17000 cP, 18000 cP, 19000 cP, 20000 cP, 21000 cP, 22000 cP, 23000 cP, 24000 cP, 25000 cP, 26000 cP, 27000 cP, 28000 cP, 29000 cP, 30000 cP or a range consisting of any two of the above values.

[0068] Illustratively, the pressure in the pneumatic feeding device can be 0.02 MPa, 0.03 MPa, 0.04 MPa, 0.05 MPa, 0.06 MPa, 0.07 MPa, 0.08 MPa, 0.09 MPa, 0.1 MPa or a range consisting of any two of the above values.

[0069] Illustratively, the pressure of the filter press can be: 0.05MPa, 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, 0.9MPa, 1.0MPa, 1.1MPa, 1.2MPa, 1.3MPa, 1.4MPa, 1.5MPa, 1.6MPa, 1.7MPa, 1.8MPa, 1.9MPa, 2.0MPa, 2.1MPa, 2.2MPa, 2.3MPa, 2.4MPa, 2.5MPa, 2.6MPa, 2.7MPa, 2.8MPa, 2.9MPa, 3.0MPa or a range consisting of any two of the above values.

[0070] Exemplarily, the pressure parameter of negative pressure suction is: 0.02 MPa, 0.03 MPa, 0.04 MPa, 0.05 MPa, 0.06 MPa, 0.07 MPa, 0.08 MPa, 0.09 MPa, 0.1 MPa or a range consisting of any two of the above values.

[0071] In some embodiments, the material body in the mold is simultaneously subjected to the steps of filter pressing and negative pressure suction, and the solvent content in the material body is reduced to 30-80%, preferably 30-50%, of the original solvent content in the material body before filter pressing and negative pressure suction, to obtain a powder masterbatch pre-cured in the mold.

[0072] In some embodiments, the solvent content in the prepared block powder cosmetics is less than 5%, preferably within 1%.

[0073] In some embodiments, the step of solidifying the powder masterbatch at low temperature is performed in a liquid nitrogen quick-freezing device. For example, the liquid nitrogen quick-freezing device can be a liquid nitrogen tunnel, a liquid nitrogen freezer, an ultra-low temperature refrigerator, etc. These devices can be commercially available, and the present application is not limited thereto.

[0074] After the filling step is completed, the present application has obtained a powder master product pre-cured and formed in the mold. Subsequently, the present application uses a liquid nitrogen quick-freezing device to perform ultra-low temperature solidification on the powder master product. The raw material components in the powder master product undergo molecular quick freezing in an extremely low temperature environment in the liquid nitrogen quick-freezing device. The cosmetic 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, the powder master product quickly passes through the maximum ice crystal formation zone during the molecular quick freezing process completed in the liquid nitrogen tunnel in the present application. The distribution of ice crystals in the powder master product is more uniform and dense, 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 anti-drop ability is better.

[0075] Furthermore, the present application also proposes the optimal liquid nitrogen quick-freezing condition parameters suitable for the preparation of block powder cosmetics of the present application through the study of the freezing curve of powder cosmetic materials and the energy transfer characteristics in the liquid nitrogen quick-freezing device. By completing the liquid nitrogen quick-freezing of the powder masterbatch under the above-mentioned condition parameters, the final prepared block powder cosmetics can have a uniform and dense texture, the best skin feel, and the stability of the product structure and the anti-drop ability are optimized.

[0076] In some embodiments, the liquid nitrogen quick-freezing device is a liquid nitrogen tunnel, and the temperature inside the liquid nitrogen tunnel is -120 to -70°C, preferably -95 to -80°C. The liquid nitrogen tunnel is also called a liquid nitrogen tunnel quick-freezer, which is a device that uses liquid nitrogen as a cold source and adopts a continuous production method to deliver materials into the quick-freezing tunnel through a conveyor belt to achieve continuous entry and exit and rapid freezing of materials. The powdered mother product passes through the liquid nitrogen tunnel on the conveyor belt in the liquid nitrogen tunnel at a speed of 0.4 to 1.2 m / min, preferably 0.6 to 1 m / min. The passing time of the powdered mother product in the liquid nitrogen tunnel is 5 to 15 minutes, preferably 6 to 10 minutes.

[0077] In some embodiments, drying comprises one or any combination of heat drying, vacuum drying, freeze drying, microwave drying and supercritical fluid drying.

[0078] In some embodiments, drying includes freeze drying. Freeze drying is a drying method in which a water-containing material is frozen below the freezing point, the water is converted into ice, and then the ice is converted into vapor under a relatively high vacuum and removed. In the freeze drying step, the small and evenly distributed ice crystals in the material body are sublimated into water vapor under high vacuum conditions and removed, which greatly retains the composition, color and aroma of the raw materials, further enhancing the improvement brought by the liquid nitrogen quick freezing step to the performance of block powder cosmetics; the small and evenly distributed ice crystals are easier to remove, and ice residues are not easily generated during the removal process, and the freeze drying efficiency is also improved.

[0079] In some embodiments, drying comprises freeze drying and a combination of one or more of the following drying methods: heating drying, vacuum drying, microwave drying or supercritical fluid drying.

[0080] Heating drying is one of the most common drying methods, which achieves drying by heating the material. Vacuum drying is a drying method in which the material is placed under negative pressure conditions and appropriately heated to the boiling point under negative pressure or cooled to solidify the material and then dried. Microwave drying is a drying method that uses electromagnetic waves as a heating source and the dried material itself as a heating element. Supercritical fluid drying is a method of drying that uses the high solubility of supercritical solvents to remove solvents contained in porous solids. The present application can select one or more drying methods based on the characteristics of the material.

[0081] When a high temperature sensitive active substance is added to the material, the drying step in the embodiment of the present application is not performed at a temperature higher than 40° C. to ensure that the high temperature sensitive active substance is not inactivated or partially inactivated during the drying step.

[0082] In some embodiments, the raw materials for preparing block powder cosmetics include a powder phase component, an oil phase component, and a water phase component;

[0083] The powder phase components include: one or more of fillers and colorants;

[0084] The oil phase components include: one or more of emollients, antioxidants, and sunscreens;

[0085] The aqueous phase components include: one or more of solvents, thickeners, film formers, emollients, emulsifiers, preservatives, and active ingredients.

[0086] 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;

[0087] 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;

[0088] 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;

[0089] 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;

[0090] Based on the prepared block powder cosmetics, the mass percentage of the aqueous inorganic thickener and / or film former is 0.02-15%, preferably 0.05-5%.

[0091] 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;

[0092] 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;

[0093] Based on the prepared block powder cosmetics, the mass percentage of the emollient and moisturizing agent is 0.1-40%, preferably 0.5-30%.

[0094] 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;

[0095] The colorant is selected from at least one of iron oxide (CI 77499, CI 77491, CI 77492), titanium dioxide (CI 77891), iron blue (CI 77510), ultramarine (CI 77007), manganese violet (CI 77742), chromium oxide green (CI 77288), chromium hydroxide green, carmine (CI 75470), carbon black (CI 77266), CI 15850, CI 19140, CI 45410, CI 16035, CI 45380, CI17200, CI 73360, CI 42090, and CI 47005;

[0096] Based on the prepared block powder cosmetics, the total mass percentage of the filler and the colorant is 50-99%, preferably 70-95%.

[0097] In some embodiments, the preservative is selected from at least one of phenoxyethanol, parabens, chlorphenesin, potassium sorbate, sodium benzoate or preservative enhancers;

[0098] 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;

[0099] Based on the prepared block powder cosmetics, the total mass percentage content of the preservative and the preservative synergist is 0.01-5%, preferably 0.5-1%.

[0100] In some embodiments, the active can be selected from high temperature sensitive actives or high temperature insensitive actives.

[0101] In some embodiments, the high temperature sensitive active substance is unstable, has reduced activity or loses activity in an environment above 40° C. For example, the high temperature sensitive active substance can be selected from at least one of polypeptide active substances, astaxanthin, vitamin A alcohol or its derivatives, vitamin C or its derivatives, and arbutin.

[0102] In the existing powder preparation technology, the material is usually heated before filling to increase the fluidity of the material and facilitate filling and transportation. The heating operation determines that active substances that are sensitive to high temperatures cannot be used in the powder raw materials. For example, active substances such as polypeptide active substances, astaxanthin, vitamin A alcohol, vitamin C or its derivatives, arbutin, etc. cannot be added as raw materials, or even if added, some or all of their activity will be lost due to the heating step. The preparation process of the present application does not include any high-temperature process, the filling step can be operated at low temperature or room temperature, and high-temperature sensitive active substances can be added to the material.

[0103] In some embodiments, the solvent is water or a mixture of water and an organic solvent.

[0104] In some embodiments, the thickener is an inorganic thickener; preferably, the inorganic thickener is at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, lithium magnesium silicate, sodium magnesium silicate, montmorillonite or a derivative thereof.

[0105] In the prior art, natural polysaccharides are often used as thickeners for powder products because of their good thickening and bonding effects. Inorganic thickeners are not as good as natural polysaccharides in bonding effects. If they are used alone as thickeners, the products will crack and have poor drop resistance. However, natural polysaccharides also increase the microbial risk of powder products, which is not conducive to the long-term storage of powder products. In the embodiments of the present application, in the air pressure feeding and extrusion drying operations, external forces are used to increase the density of the material body, and due to the reduction in the amount of solvent, the adverse effect of the solvent removal step on the internal bonding stability of the material body is also reduced. Therefore, even if an inorganic thickener whose bonding effect is not as good as that of natural polysaccharides is used, the powder product finally prepared will not crack or have poor drop resistance. And the use of inorganic thickeners instead of natural polysaccharides can reduce microbial risks and increase the long-term storage stability of powder products.

[0106] In the second aspect, the embodiment of the present application provides a block powder cosmetic, which is prepared by the method of the embodiment of the first aspect of the present application. The block powder cosmetic provided by the present application is prepared by using a pneumatic feeding device to fill the mold according to a preset amount, and extruding and drying the material body in the mold, which can effectively avoid the occurrence of ice residue, shrinkage deformation during the desolvation process of the product, and cracking, poor drop resistance, pores, and softness of the finished product. The fine relief presentation effect of the powder surface is good, and high-temperature sensitive active substances can be added.

[0107] In some embodiments, the block powder cosmetics are selected from pressed powder, blush, eye shadow or highlighter powder. The block powder cosmetics may also include products with other functions.

[0108] Example

[0109] 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.

[0110] Recipe 1-4

[0111] Illustratively, the present application provides four preparation raw material compositions, proportions and mixing methods for block powder cosmetics.

[0112] The raw material components of the block powder cosmetic formula 1 are shown in Table 1:

[0113] Table 1

[0114]

[0115] Mixing: (1) Heat phase A and disperse it evenly, the temperature is 75±5℃; (2) Add phase B to phase A and homogenize and emulsify it, the temperature is 75±5℃; (3) Add phase C to (2) and mix evenly, the temperature is 75±5℃; (4) Cool the material to 50±5℃; (5) Add D (needs to be pre-dissolved), E, ​​and F to (4) and mix evenly, and vacuum degas at 50±5℃ to obtain the material;

[0116] The raw material components of block powder cosmetic formula 2 are shown in Table 2:

[0117] Table 2

[0118]

[0119]

[0120] Mixing: (1) Heat phase A and disperse it evenly, the temperature is 75±5℃; (2) Add phase B to phase A and emulsify it, the temperature is 75±5℃; (3) Add phase C to (2) and mix evenly, the temperature is 75±5℃; (4) Cool the material to 50±5℃; (5) Add D (needs to be pre-dissolved) and E to (4), mix evenly, and vacuum degas at 50±5℃ to obtain the material;

[0121] The raw material components of the block powder cosmetic formula 3 are shown in Table 3:

[0122] Table 3

[0123]

[0124] Mixing: (1) Heat phase A and disperse it evenly, the temperature is 75±5℃; (2) Add phase B to phase A and emulsify it, the temperature is 75±5℃; (3) Add phase C to (2) and mix evenly, the temperature is 75±5℃; (4) Cool the material to 50±5℃; (5) Add D (needs to be pre-dissolved) and E to (4), mix evenly, and vacuum degas at 50±5℃ to obtain the material;

[0125] The raw material components of block powder cosmetic formula 4 are shown in Table 4:

[0126] Table 4

[0127]

[0128] Mixing: (1) Heat phase A and disperse it evenly, the temperature is 75±5℃; (2) Add phase B to phase A and emulsify it homogenously, the temperature is 75±5℃; (3) Add phase C to (2) and mix evenly, the temperature is 75±5℃; (4) Cool the material to 50±5℃; (5) Add D (needs to be pre-dissolved) and E to (4), mix evenly, and vacuum degas at 50±5℃ to obtain the material.

[0129] Examples 1 to 12

[0130] The block powder cosmetics are prepared as follows:

[0131] Mixing: providing raw materials according to the raw material components of the bulk powder cosmetic formula, mixing the raw materials according to the mixing steps to obtain a material body;

[0132] Filling and pre-curing: the material body is filled into the mold according to a preset amount through the air pressure feeding device, and the material body is subjected to pressure filtration and negative pressure suction to reduce the solvent content in the material body to 30-50% of the original solvent content in the material body before pressure filtration and negative pressure suction, so as to obtain a powder masterbatch pre-cured in the mold;

[0133] Freezing: Freeze the pre-cured powder masterbatch at low temperature, and the freezing step is carried out in a liquid nitrogen tunnel;

[0134] Demolding and drying: separating the frozen powdered master product from the mold and drying it to obtain a block-shaped powdered cosmetic; or drying the frozen powdered master product and separating it from the mold to obtain a block-shaped powdered cosmetic, wherein the solvent content in the block-shaped powdered cosmetic is less than 5%.

[0135] Among them, the material viscosity, the pressure in the air pressure feeding device, the pressure of the material pressure filtration and negative pressure suction, the temperature inside the liquid nitrogen tunnel in the step of solidifying and freezing the powder master product at low temperature, the speed of the powder master product in the liquid nitrogen tunnel, the passing time, the drying method and other parameters involved in Examples 1 to 12 are shown in Table 5.

[0136] Comparative Examples 1 to 5

[0137] The difference between Comparative Example 1 and Example 4 is that the feeding is not carried out by a pneumatic feeding device, but gravity filling is carried out at room temperature of 25° C., and the material body is not subjected to pressure filtration and negative pressure suction.

[0138] The difference between Comparative Example 2 and Example 4 is that the pneumatic feeding device is not used for feeding, but the material body is heated to 50° C. and then gravity filling is performed, and the material body is not subjected to pressure filtration and negative pressure suction.

[0139] The difference between Comparative Example 3 and Example 4 is that the pneumatic feeding device is not used for feeding, but the material body is heated to 90° C. and then gravity filling is performed, and the material body is not subjected to pressure filtration and negative pressure suction.

[0140] The difference between Comparative Example 4 and Example 4 is that solvent water is added to the raw material components of Formula 4 to reduce the viscosity of the mixed material to 5000 cP, and then the material is not fed by a pneumatic feeding device, but is heated to 50°C and then gravity filled, and the material is not filtered or vacuum-pumped.

[0141] The difference between Comparative Example 5 and Example 1 is that solvent water is added to the raw material components of Formula 1 to reduce the viscosity of the mixed material to 3000 cP, and then the material is not fed by a pneumatic feeding device, but is gravity filled after being heated to 50°C, and the material is not filtered or vacuum-pumped.

[0142] Among them, the material viscosity, the pressure in the air pressure feeding device, the pressure of the material pressure filter and negative pressure suction, the temperature inside the liquid nitrogen tunnel in the step of solidifying and freezing the powder master product at low temperature, the speed of the powder master product in the liquid nitrogen tunnel, the passing time, the drying method and other parameters involved in Comparative Examples 1 to 5 are shown in Table 5.

[0143] Table 5 Process parameters of Examples 1 to 12 and Comparative Examples 1 to 5

[0144]

[0145]

[0146] Test Section

[0147] Powder cakes were prepared according to the methods of Examples 1 to 12 and Comparative Examples 1 to 5, and 100 powder cakes were prepared for each Example or Comparative Example. Appearance observation, diameter shrinkage rate test, and drop test were performed, and the presence of microbial risks caused by natural polysaccharides and the possibility of inactivation or partial inactivation of high-temperature sensitive active substances were recorded.

[0148] 1) Appearance observation

[0149] Observe the appearance of the powder cake with the naked eye or with the help of a microscope, including the surface relief effect. Pay special attention to whether the sharp corners of the fine relief on the surface of the powder cake are filled completely, whether there are bubbles, whether the bottom of the powder cake is flat, and whether the powder texture is uniform and dense.

[0150] The appearance recorded is based on the observation of more than 90% of the 100 pressed powders.

[0151] 2) Diameter shrinkage

[0152] The diameter D of the mold and the diameter d of the prepared powder cake were measured with a vernier caliper. Since the present application implements air pressure feeding, filter pressing and negative pressure suction, it can be considered that when the filling and pre-curing steps are completed, the material body is fully filled in the mold, so the diameter of the filling mold is taken as the diameter of the powder master product before freezing, demoulding and drying.

[0153] The diameter shrinkage is calculated by the following formula:

[0154] Diameter shrinkage = [(Dd)\D]*100%

[0155] Wherein, D is the diameter of the filling mold, and d is the diameter of the prepared powder cake.

[0156] The diameter shrinkage rate recorded is the average value of the test values ​​of 100 pressed powders.

[0157] 3) Drop detection

[0158] 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.

[0159] 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.

[0160] 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. The first breakage rate, the second breakage rate, and the third breakage rate of Examples 1 to 12 and Comparative Examples 1 to 5 are recorded respectively.

[0161] 4) Microbial risks caused by natural polysaccharides

[0162] If the raw materials of powder cake do not contain natural polysaccharide components, it is considered that the powder cake does not have the microbial risk caused by natural polysaccharides; if the raw materials of powder cake contain natural polysaccharide components, it is considered that the powder cake has the possibility of microbial risk caused by natural polysaccharides.

[0163] 5) Activity of high temperature sensitive active ingredients

[0164] If the preparation process of the pressed powder includes a step at a temperature exceeding 40°C, it is considered that the high temperature sensitive active substance may be inactivated or partially inactivated. If the preparation process of the pressed powder does not include a step at a temperature exceeding 40°C, it is considered that the high temperature sensitive active substance is active.

[0165] The above test results of Examples 1 to 12 and Comparative Examples 1 to 5 are recorded in Table 6.

[0166] Table 6 Test results of Examples 1 to 12 and Comparative Examples 1 to 5

[0167]

[0168]

[0169] As shown in the test results in Table 6, Examples 1 to 12 adopt the preparation method of block powder cosmetics provided by the present application, the material body is quantitatively filled into the mold via a pneumatic feeding device, and a part of the solvent in the material body is removed by extrusion drying to achieve pre-curing, and then frozen, dried and demolded to obtain block powder cosmetics. Compared with Comparative Examples 1 to 5 that do not adopt the preparation method of the present application, Examples 1 to 12 have obvious improvements in filling efficiency, filling effect on mold relief, appearance, texture and skin feel of the obtained block powder cosmetics, and also have significant effects in improving the diameter shrinkage rate in the preparation process, reducing the cracking rate of the powder drop detection, etc., and provide a feasible solution for avoiding microbial risks caused by natural polysaccharides and using high temperature sensitive active substances in powder products.

[0170] The average diameter shrinkage rate of the powder cakes in Examples 1 to 12 during the preparation process was less than 1%, and the sum of the rupture rates of three drop tests did not exceed 15%, and the presentation effect of fine relief on the surface of the powder cakes was significantly better than that of Comparative Examples 1 to 5. However, since Comparative Examples 1 to 5 did not adopt the preparation method of the present application, they could not be effectively filled and produced at all under the condition of using less solvent in the filling material body and high material viscosity; even if the material body was heated before filling or the solvent was added to reduce the viscosity of the material body, the performance data of the block powder cosmetics prepared therefrom in terms of diameter shrinkage rate, drop test rupture rate, etc. were still significantly inferior to those of Examples 1 to 12 of the present application.

[0171] Furthermore, in the method for preparing bulk powder cosmetics provided by the present application, the pressure of the air pressure feeding device to assist in feeding, the pressure of the material body for pressure filtration and negative pressure suction, the temperature and time control for curing the powder master product at low temperature, and other parameters also have an impact on the technical effect of the present application. The present application also provides a preferred range for the above process parameters to further optimize the various properties of the bulk powder cosmetics prepared by the method provided by the present application. For example, in Examples 1 to 4, when the viscosity of the material is between 10000 and 30000 cP and the feed pressure in the air pressure feed device is between 0.02 and 0.1 MPa, the pressure parameter of the pressure filtration in the extrusion drying is between 0.05 and 3 MPa, the pressure parameter of the negative pressure suction is between 0.02 and 0.1 MPa, the temperature inside the liquid nitrogen tunnel is between -120 and -70°C, and the powder masterbatch passes through the liquid nitrogen tunnel on the conveyor belt in the liquid nitrogen tunnel at a speed of 0.4 to 1.2 m / min, and the passing time is 5 to 15 minutes. Finally, the sharp corners of the surface relief of the block powder cosmetics are filled completely without bubbles, the bottom is flat, the powder texture is uniform and dense, the drop resistance is excellent, and the average diameter shrinkage rate is less than 0.2%.

[0172] The preparation method of block powder cosmetics provided in the present application successfully solves technical problems such as shrinkage and deformation of powder products during the preparation and desolvation process, cracking of the prepared powder products, poor drop resistance, pores and softness. At the same time, it also enables block powder cosmetics to avoid microbial risks caused by natural polysaccharides and the addition of high-temperature sensitive active ingredients, providing better prospects for the development and application of block powder cosmetics.

[0173] The above is only a specific implementation method of the present application. Those skilled in the art can clearly understand that for the convenience and simplicity of description, the specific working process described above can refer to the corresponding process in the aforementioned method embodiment, and will not be repeated here. It should be understood that the protection scope of the present application is not limited to this. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed in this application, and these modifications or replacements should be included in the protection scope of the present application.

Claims

1. A method for preparing block powder cosmetics, characterized in that: The steps include: Mixing: providing raw materials for preparing block powder cosmetics, mixing the raw materials to obtain a material body; Filling and pre-curing: filling the material into the mold according to a preset amount through an air pressure feeding device, extruding and drying the material to obtain a powder masterbatch pre-cured in the mold; Freezing: freezing the pre-cured powder masterbatch at low temperature; Demolding and drying: separating the frozen powdered master product from the mold and drying it to obtain a block-shaped powdered cosmetic; or drying the frozen powdered master product and separating it from the mold to obtain a block-shaped powdered cosmetic.

2. The method for preparing block powder cosmetics according to claim 1, characterized in that: The step of filling the material body into the mold according to a preset amount via the air pressure feeding device includes: pressing or sucking the material body into the mold by the action of air pressure.

3. The method for preparing block powder cosmetics according to claim 2, characterized in that: The viscosity of the material is below 30000 cP, preferably 10000 cP to 25000 cP; the pressure in the air pressure feeding device is: 0.02 to 0.1 MPa, preferably 0.04 to 0.08 MPa.

4. The method for preparing block powder cosmetics according to claim 1, characterized in that: The extrusion drying comprises performing filter pressing on the material body in the mold to make at least part of the solvent dialyze out of the material body, and transferring the dialyzed solvent at the same time or after the filter pressing.

5. The method for preparing block powder cosmetics according to claim 4, characterized in that: The extrusion drying includes applying pressure filtration and negative pressure suction to the material in the mold; the pressure parameter of the pressure filtration is: 0.05-3Mpa, preferably 0.2-1.5Mpa; the pressure parameter of the negative pressure suction is: 0.02-0.1Mpa, preferably 0.05-0.08Mpa.

6. The method for preparing block powder cosmetics according to claim 5, characterized in that: In the step of simultaneously performing filter pressing and negative pressure suction on the material body in the mold, the solvent content in the material body is reduced to 30-80%, preferably 30-50%, of the original solvent content in the material body before filter pressing and negative pressure suction, to obtain a powder masterbatch pre-cured in the mold.

7. The method for preparing block powder cosmetics according to claim 1, characterized in that: The solvent content in the prepared block powder cosmetics is less than 5%, preferably within 1%.

8. The method for preparing block powder cosmetics according to claim 1, characterized in that: The step of freezing the pre-cured powder master product at low temperature is carried out in a liquid nitrogen quick-freezing device.

9. The method for preparing block powder cosmetics according to claim 8, characterized in that: The liquid nitrogen quick freezing device is a liquid nitrogen tunnel, and the temperature inside the liquid nitrogen tunnel is -120 to -70°C, preferably -95 to -80°C; The powdered precursor passes through the liquid nitrogen tunnel on the conveyor belt in the liquid nitrogen tunnel at a speed of 0.4 to 1.2 m / min. Preferably, the powdered precursor passes through the liquid nitrogen tunnel on the conveyor belt in the liquid nitrogen tunnel at a speed of 0.6 to 1 m / min. The powder masterbatch passes through the liquid nitrogen tunnel for 5 to 15 minutes, preferably 6 to 10 minutes.

10. The method for preparing block powder cosmetics according to claim 9, characterized in that: The drying comprises one or any combination of heating drying, vacuum drying, freeze drying, microwave drying and supercritical fluid drying; preferably, the temperature of the drying step is lower than 40°C.

11. The method for preparing block powder cosmetics according to claim 10, characterized in that: The drying includes freeze drying and one or a combination of the following drying methods: heating drying, vacuum drying, microwave drying, and supercritical fluid drying.

12. The method for preparing block powder cosmetics according to claim 1, characterized in that: The raw materials used to prepare the block powder cosmetics include a powder phase component, an oil phase component and a water phase component; 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.

13. The method for preparing block powder cosmetics according to claim 12, characterized in that: The thickener and film-forming agent are selected from natural water-soluble polymers or their derivatives, synthetic water-based polymers or water-based inorganic thickeners; 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; The synthetic water-based polymer is selected from at least one of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, carbomer, acrylic acid (ester) / octylacrylamide copolymer, acrylic acid (ester) / ethylhexyl acrylate copolymer, sodium acrylate / sodium acryloyldimethyl taurate copolymer, acrylic acid (ester) / octylacrylamide copolymer, styrene / acrylic acid (ester) copolymer, acrylic acid (ester) copolymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyacrylate cross-linked polymer-6, acrylic acid (ester) / stearyl alcohol polyether-20 methacrylate copolymer, ammonium acryloyldimethyl taurate / behenyl alcohol polyether-25 methacrylate cross-linked polymer, acrylic acid (ester) copolymer ammonium, sodium polyacrylate, sodium polyacryloyldimethyl taurate, polyacrylamide, polyvinyl pyrrolidone, polyvinyl alcohol, VP / VA copolymer, polyurethane-1, and polyurethane-35; 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; Based on the prepared block powder cosmetics, the mass percentage of the aqueous inorganic thickener and / or film-forming agent is 0.02-15%, preferably 0.05-5%.

14. The method for preparing block powder cosmetics according to claim 12, characterized in that: The emollient and moisturizing agent is selected from at least one of alcohols, silicone oil, mineral oil, synthetic oil, animal and plant oils or their derivatives; The animal and plant oil or its derivative is selected from at least one of glycerol, 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; Based on the prepared block powder cosmetics, the mass percentage of the emollient and moisturizing agent is 0.1-40%, preferably 0.5-30%.

15. The method for preparing block powder cosmetics according to claim 12, characterized in that: 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, calcium sodium borosilicate, aluminum hydroxide, zinc stearate starch and its derivatives, and plastic microbeads; The colorant is selected from at least one of iron oxide CI 77499, iron oxide CI 77491, iron oxide CI 77492, titanium dioxide CI77891, iron blue CI 77510, ultramarine CI 77007, manganese violet CI 77742, chromium oxide green CI 77288, chromium hydroxide green, carmine CI 75470, carbon black CI 77266, CI 15850, CI 19140, CI 45410, CI 16035, CI 45380, CI17200, CI 73360, CI 42090, and CI 47005; Based on the prepared block powder cosmetics, the total mass percentage of the filler and the colorant is 50-99%, preferably 70-95%.

16. The method for preparing block powder cosmetics according to claim 12, characterized in that: The preservative is selected from at least one of phenoxyethanol, parabens, chlorphenesin, potassium sorbate, sodium benzoate or preservative synergist; 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; Based on the prepared block powder cosmetics, the total mass percentage content of the preservative and the preservative synergist is 0.01-5%, preferably 0.5-1%.

17. The method for preparing block powder cosmetics according to claim 12, characterized in that: The active substance is selected from a high temperature sensitive active substance or a high temperature insensitive active substance; Preferably, the high temperature sensitive active substance is selected from at least one of polypeptide active substances, astaxanthin, vitamin A alcohol or its derivatives, vitamin C or its derivatives, and arbutin.

18. The method for preparing block powder cosmetics according to claim 12, characterized in that: The solvent is water or a mixture of water and an organic solvent.

19. The method for preparing block powder cosmetics according to claim 12, characterized in that: The thickener is an inorganic thickener; preferably, the inorganic thickener is at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, lithium magnesium silicate, sodium magnesium silicate, montmorillonite or a derivative thereof.

20. A block powder cosmetic, characterized in that: The method is prepared by any one of claims 1 to 19.

21. The block powder cosmetic according to claim 20, characterized in that: The block powder cosmetics are selected from pressed powder, blush, eye shadow or highlighter powder.

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