Method for preparing compact powder cosmetics, and compact powder cosmetic

Abstract

Provided in the present application are a method for preparing compact powder cosmetics, and a compact powder cosmetic. The method for preparing compact powder cosmetics comprises the following steps: mixing, involving: providing raw materials used for preparing a compact powder cosmetic, and mixing the raw materials to obtain a material body; filling and pre-curing, involving: filling a mold with a predetermined amount of the material body by means of a pneumatic feeding device, and squeezing and drying the material body to obtain a powder preform that is pre-cured and molded in the mold; freezing, involving: freezing the pre-cured and molded powder preform at a low temperature; and demolding and drying, involving: separating the frozen powder preform from the mold, and drying same to obtain a compact powder cosmetic; alternatively, drying the frozen powder preform, and separating same from the mold to obtain a compact powder cosmetic. The preparation method of the present application can ameliorate the problems of shrinkage and deformation during the preparation process of compact powder cosmetics and the problems of poor drop resistance, cracking, air pockets, sponginess, etc., of a finished product; moreover, the preparation method does not cause the inactivation of high-temperature-sensitive active substances during the preparation process.

Description

Method for preparing blocky powder cosmetic and blocky powder cosmetic

[0001] Cross-reference to related applications

[0002] This application claims priority to Chinese Patent Application No. 202411395586.6, filed on September 30, 2024, entitled “Method for preparing blocky powder cosmetic and blocky powder cosmetic”, the entire contents of which are incorporated herein by reference. TECHNICAL FIELD

[0003] The present application belongs to the technical field of cosmetics, and in particular relates to a method for preparing a blocky powder cosmetic and a blocky powder cosmetic. BACKGROUND

[0004] The preparation of blocky powder cosmetics generally includes the steps of mixing, filling, demolding, and removing solvent. In the filling step, in order to obtain good filling efficiency and effect, the composition needs to have good flowability, so a certain amount of solvent (usually water, or a mixture of water and one or more organic solvents, and the addition amount of solvent is generally higher than 50%) needs to be included in the composition system to be filled, and the composition to be filled needs to be preheated at a high temperature (usually 70-90 degrees Celsius). Due to the high content of powder particles in the raw materials of blocky powder cosmetics, the flowability of the material body is limited in the range of improvement, and even if solvent is added and heated for filling, air holes are still prone to occur in some fine relief sharp corner parts.

[0005] After the filling step, a step of removing solvent is also needed, such as through the process steps of heating and baking, freeze-drying, etc., to remove the solvent from the powder cosmetic, and the final solvent content in the shaped powder cosmetic needs to be controlled to be below 5%. However, the process of removing solvent is not easy to control, and can cause shrinkage deformation in the preparation process, resulting in poor drop resistance of the finished product, cracking, air holes, softness, and other problems.

[0006] In addition, the addition of functional ingredients in cosmetic powder products is a product demand trend, and the heating operation in the filling step can easily cause the inactivation of functional ingredients, resulting in the inability to use some high-temperature sensitive active substances in cosmetic powder products.

[0007] SUMMARY

[0008] The present application provides a method for preparing a blocky powder cosmetic and a blocky powder cosmetic to improve shrinkage deformation in the preparation process and problems such as poor drop resistance of the finished product, cracking, air holes, softness, etc., and without causing the inactivation of high-temperature sensitive active substances in the preparation process.

[0009] In a first aspect, the embodiments of the present application provide a preparation method of blocky powder cosmetic, comprising the following steps: mixing: providing raw materials for preparing the blocky powder cosmetic, mixing the raw materials to obtain a material body; filling and pre-solidifying: filling the material body into a mold in a preset amount through a pneumatic feeding device, and extruding and drying the material body to obtain a pre-solidified and formed powder material product in the mold; freezing: freezing the pre-solidified and formed powder material product at low temperature; demolding and drying: separating the frozen powder material product from the mold and drying to obtain the blocky powder cosmetic; or drying the frozen powder material product and separating it from the mold to obtain the blocky powder cosmetic.

[0010] According to the embodiments of the first aspect of the present application, the step of filling the material body into the mold in a preset amount through the pneumatic feeding device comprises: pressing or sucking the material body into the mold by the action of air pressure.

[0011] According to the embodiments of the first aspect of the present application, the viscosity of the material body is below 30,000 cP, preferably 10,000 cP-25,000 cP; the pressure in the pneumatic feeding device is 0.02-0.1 MPa, preferably 0.04-0.08 MPa.

[0012] According to the embodiments of the first aspect of the present application, the extrusion drying comprises performing pressure filtration on the material body in the mold to dialyze at least part of the solvent from the material body, and transferring the dialyzed solvent at the same time or after the pressure filtration.

[0013] According to the embodiments of the first aspect of the present application, the extrusion drying comprises performing pressure filtration and negative pressure suction on the material body in the mold; the pressure parameter of the pressure filtration is 0.05-3 MPa, preferably 0.2-1.5 MPa; the pressure parameter of the negative pressure suction is 0.02-0.1 MPa, preferably 0.05-0.08 MPa.

[0014] According to the embodiments of the first aspect of the present application, in the step of simultaneously performing pressure filtration and negative pressure suction on the material body in the mold, the content of the solvent in the material body is reduced to 30-80%, preferably 30-50%, of the original solvent content in the material body before the pressure filtration and the negative pressure suction, to obtain the pre-solidified and formed powder material product in the mold.

[0015] According to the embodiments of the first aspect of the present application, the content of the solvent in the blocky powder cosmetic prepared is below 5%, preferably within 1%.

[0016] According to the embodiments of the first aspect of the present application, the step of freezing the pre-solidified and formed powder material product at low temperature is performed in a liquid nitrogen quick-freezing device.

[0017] According to an embodiment of the first aspect of the present application, the liquid nitrogen quick-freezing device is a liquid nitrogen tunnel, the temperature inside the liquid nitrogen tunnel is -120 to -70℃, preferably -95 to -80℃; the powder mother product passes through the liquid nitrogen tunnel at a speed of 0.4 to 1.2 meters per minute, preferably 0.6 to 1 meter per minute on the conveying belt inside the liquid nitrogen tunnel, and the passing time of the powder mother product inside the liquid nitrogen tunnel is 5 to 15 minutes, preferably 6 to 10 minutes.

[0018] According to an embodiment of the first aspect of the present application, the drying includes any combination of one or more of the following: heating drying, vacuum drying, freeze drying, microwave drying, and supercritical fluid drying.

[0019] According to an embodiment of the first aspect of the present application, the drying includes freeze drying and a combination of one or more of the following: heating drying, vacuum drying, microwave drying, or supercritical fluid drying.

[0020] According to an embodiment of the first aspect of the present application, the temperature of the drying step is lower than 40℃.

[0021] According to an embodiment of the first aspect of the present application, the raw material for preparing the block-shaped powder cosmetic includes a powder phase component, an oil phase component, and a water phase component; the powder phase component includes one or more of the following: a filler, a coloring agent; the oil phase component includes one or more of the following: an emollient moisturizer, an antioxidant, a sunscreen agent; the water phase component includes one or more of the following: a solvent, a thickening agent, a film-forming agent, an emollient moisturizer, an emulsifier, a preservative, an active substance.

[0022] According to an embodiment of the first aspect of the present application, the thickening agent and the film-forming agent are selected from at least one of the following: a natural water-soluble polymer or a derivative thereof, a synthetic water-soluble polymer, or a water-soluble inorganic thickening agent; the natural water-soluble polymer or the derivative thereof is selected from at least one of the following: alginic acid, agar, carrageenan, ghatti gum, gellan gum, crispus, xanthan gum, guar gum, tamarind gum, tara gum, gum arabic, tragacanth gum, quince seed gum, pectin, arabinogalactan, wheat protein, soy protein, gelatin, casein, chitosan, curdlan, cyclodextrin, hyaluronic acid, konjac gum, tremella polysaccharide, acacia gum, microcrystalline cellulose, methyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch phosphate, starch, sodium hydroxymethyl starch, sodium polyacrylate grafted starch, and hydroxypropyl guar gum.

[0023] The synthetic water-soluble polymer is selected from at least one of acrylic acid (ester) / C10-30 alkyl acrylate crosspolymer, carbomer, acrylic acid (ester) / octyl acrylamide copolymer, acrylic acid (ester) / ethylhexyl acrylate copolymer, sodium acrylate / sodium acryloyldimethyl taurate copolymer, acrylic acid (ester) / octyl acrylamide copolymer, styrene / acrylic acid (ester) copolymer, acrylic acid (ester) copolymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyacrylate crosspolymer-6, acrylic acid (ester) / steareth-20 methacrylate copolymer, ammonium acryloyldimethyltaurate / beheneth-25 methacrylate crosspolymer, acrylic acid (ester) copolymer ammonium, sodium polyacrylate, sodium polyacryloyldimethyl taurate, polyacrylamide, polyvinylpyrrolidone, polyvinyl alcohol, VP / VA copolymer, polyurethane-1, polyurethane-35;

[0024] The water-soluble inorganic thickening agent is selected from at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, magnesium lithium silicate, magnesium sodium silicate, montmorillonite or its derivatives;

[0025] The mass percentage of the water-soluble inorganic thickening agent and / or the film-forming agent is 0.02-15%, preferably 0.05-5%, based on the prepared block powder cosmetic.

[0026] According to the embodiment of the first aspect of the present application, the emollient moisturizer is selected from at least one of alcohol, silicone oil, mineral oil, synthetic oil, animal and plant oil or its derivatives;

[0027] The animal and plant oil or its derivatives is selected from at least one of glycerin, propylene glycol, dipropylene glycol, pentylene glycol, butylene glycol, ethylene glycol, hexylene glycol, sorbitol, xylitol, polyethylene glycol, dimethicone, octyl dimethicone, phenyl trimethicone, cetyl dimethicone, C30-45 alkyl dimethiconyl propyl trisiloxane, bis-PEG-18 methyl ether dimethyl silane, white mineral oil, petrolatum, hydrogenated polyisobutene, lanolin esters and its derivatives, octyldodecanol, caprylic / capric triglyceride, ethylhexyl palmitate, bis-diglyceryl polyacyladipate-2, isononyl isononanoate, jojoba seed oil, coconut oil, hydrogenated coco-glycerides, white pool seed oil, olive oil, squalane C9-12 alkane, coceth- octanoate / decanoate, tocopheryl acetate, methyl gluceth-10;

[0028] The mass percentage of the emollient moisturizer is 0.1-40%, preferably 0.5-30%, based on the prepared block powder cosmetic.

[0029] 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 mononitride, bismuth oxychloride, silica, potassium sodium aluminosilicate, lauroyl lysine, magnesium stearate, magnesium myristate, calcium boron aluminosilicate, tin oxide, sodium calcium borosilicate, aluminum hydroxide, zinc stearate starch and derivatives thereof, plastic microbeads;

[0030] 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, CI 17200, CI 73360, CI 42090, CI 47005;

[0031] The total mass percentage content of the filler and the colorant is 50-99%, preferably 70-95%, based on the prepared block-shaped powder cosmetic.

[0032] 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 preservative synergists;

[0033] The preservative synergist is selected from at least one of octisalate, p-hydroxyacetophenone, ethylhexylglycerin, 1,2-hexanediol, caprylhydroxamic acid, 1,2-pentanediol, glyceryl caprylate, umbelliferone.

[0034] The total mass percentage content of the preservative and the preservative synergist is 0.01-5%, preferably 0.5-1%, based on the prepared block-shaped powder cosmetic.

[0035] According to an embodiment of the first aspect of the present application, the active is selected from a high-temperature sensitive active or a high-temperature insensitive active.

[0036] According to an embodiment of the first aspect of the present application, the active is selected from a high-temperature sensitive active, which is selected from at least one of polypeptide active, astaxanthin, vitamin A alcohol or derivatives thereof, vitamin C or derivatives thereof, arbutin.

[0037] 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.

[0038] According to the embodiment of the first aspect of the present application, the thickening agent is an inorganic thickening agent; preferably, the inorganic thickening agent is at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, magnesium lithium silicate, magnesium sodium silicate, montmorillonite or a derivative thereof.

[0039] According to the embodiment of the second aspect of the present application, the blocky powder cosmetic is selected from a powder compact, a blush, an eye shadow or a highlighter.

[0040] According to the embodiment of the second aspect of the present application, the blocky powder cosmetic is selected from a powder compact, a blush, an eye shadow or a highlighter.

[0041] Compared with the prior art, the embodiment of the present application has at least the following beneficial effects:

[0042] Firstly, the blocky powder cosmetic is close to a solvent-free state, but in order to mix and transport the raw materials during the preparation process, it is necessary to introduce a solvent, and the addition and removal of the solvent not only affect the production efficiency, but also adversely affect the performance of the final product. In the present application, the material body is quantitatively filled into the mold through the air pressure feeding device, which reduces the requirement for the flowability of the material body, and does not need to add too much solvent; and in the filling step, extrusion drying is implemented, the content of the solvent in the material body is greatly reduced, the subsequent drying time is reduced from 12-24 hours to 6-10 hours, the production efficiency is improved, and the problems of shrinkage deformation, cracking, poor drop resistance of the final product are effectively reduced.

[0043] Secondly, for the blocky powder cosmetic forming a fine relief, the material body is quantitatively filled into the mold through the air pressure feeding device, and the process of simultaneously performing pressure filtration and negative pressure suction on the material body in the mold, the pressure assists the material body to fill into the sharp corner part of the fine relief, even if the viscosity of the material body is high, it can still be better filled into the sharp corner part of the fine relief, and a good density is achieved, solving the problems of air holes and softness in the finished product.

[0044] Thirdly, for the blocky powder cosmetic added with active substances, 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 body.

[0045] In summary, the present application provides a preparation method of a blocky powder cosmetic, which can effectively avoid the problems of shrinkage deformation during the desolventization process of the product, cracking, poor drop resistance, air holes, softness and other problems in the finished product, can present an excellent fine relief surface, can add high-temperature sensitive active substances, and at the same time, can improve the production efficiency and reduce the energy consumption. DETAILED DESCRIPTION

[0046] The features and exemplary embodiments of various aspects of this application will be described in detail below. To make the objectives, technical solutions, and advantages of this application clearer, the application will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are only intended to explain this application and not to limit it. For those skilled in the art, this application can be implemented without some of these specific details. The following description of the embodiments is merely to provide a better understanding of this application by illustrating examples.

[0047] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Unless otherwise specified, an element defined by the phrase "comprising..." does not exclude the presence of additional identical elements in the process, method, article, or apparatus that includes the element.

[0048] In existing technologies, the preparation of block-shaped powder cosmetics involves adding a sufficient amount of solvent and heating the material to improve its fluidity, thus meeting the requirements for filling and transfer. After the filling step, a solvent removal step is required, such as through heating, baking, or freeze-drying, to remove the solvent from the block-shaped powder cosmetic. The solvent content in the final block-shaped powder cosmetic product generally needs to be controlled below 5%. The inventors of this application have noted that the solvent removal process is difficult to control, which may cause the product to shrink and deform during the solvent removal process, increasing the likelihood of cracking, poor drop resistance, porosity, and softness in the finished product. In addition, because the raw materials of block-shaped powder cosmetics have a high content of powder particles, and the improvement in material fluidity is limited, even with the addition of solvent and heating during filling, porosity is still very likely to occur in some sharp corners of fine reliefs. Furthermore, the heating filling operation can also cause the inactivation or partial inactivation of high-temperature sensitive active ingredients added to the product.

[0049] To address the aforementioned problems, the inventors of this application provide a block-shaped powder cosmetic and a method for preparing the same.

[0050] In a first aspect, the embodiments of the present application provide a preparation method of blocky powder cosmetic, comprising the following steps: mixing: providing raw materials for preparing the blocky powder cosmetic, mixing the raw materials to obtain a material body; filling and pre-solidifying: filling the material body into a mold by a gas pressure feeding device according to a preset amount, and performing extrusion drying on the material body to obtain a powder material master product pre-solidified and formed in the mold; freezing: freezing the powder material master product pre-solidified and formed at a low temperature; demolding and drying: separating the frozen powder material master product from the mold and drying to obtain the blocky powder cosmetic; or drying the frozen powder material master product and separating it from the mold to obtain the blocky powder cosmetic.

[0051] In the mixing step, the raw materials for preparing the blocky powder cosmetic can be commercially available or self-made. It can be understood that the raw materials for preparing the blocky powder cosmetic generally include a powder phase component, an oil phase component, and a water phase component. The raw materials can be added step by step and mixed uniformly in various ways commonly used in the prior art, such as mechanical stirring, and homogenization, defoaming, and the like 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.

[0052] In the filling step, the preset amount can be set according to the volume of the blocky powder cosmetic, the capacity of the mold, or the filling requirement. The preset amount filled each time can be the same or different. In the present application, the gas pressure feeding device refers to a device for filling the material body into the mold by gas pressure delivery. Illustratively, the gas pressure feeding device can include a gas pump and a pipeline connected to the gas pump, the gas pump being used to provide the gas pressure required for delivery, and the pipeline being used to fill the material body into the mold. The present application is not limited thereto.

[0053] After the filling step, the extrusion drying operation is performed on the material body, and a mechanical physical drying method is used to remove part of the solvent in the material body, so that the powder material master product pre-solidified and formed in the mold is obtained before the subsequent freezing, demolding, and drying steps.

[0054] The pre-solidified and formed powder material master product still contains solvent. After the filling and pre-solidifying steps, the powder material master product is frozen by the freezing step, and the liquid (such as water, emulsion, etc.) in the powder material master product is frozen into ice.

[0055] The sequence of the demolding and drying steps can be adjusted. For example, after the frozen powder material master product is separated from the mold, drying is performed to obtain the blocky powder cosmetic; or after the frozen powder material master product is dried, it is separated from the mold to obtain the blocky powder cosmetic.

[0056] The blocky powder cosmetic is close to a solvent-free state, but the prior art necessarily introduces a solvent in the preparation process for the need of raw material mixing and transportation. The addition of the solvent and the solvent removal process not only affects the production efficiency, but also adversely affects the performance of the final product. In the preparation method of the blocky powder cosmetic provided in the embodiments of the present application, the material body is quantitatively filled into the mold through the air pressure feeding device, which reduces the requirement for the flowability of the material body and reduces the amount of solvent added. In the filling step, extrusion drying is implemented. Before entering the drying step, the content of the solvent in the pre-solidified and formed 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, poor drop resistance of the final product. In some embodiments, the subsequent drying time is reduced from 12-24 hours to 6-10 hours.

[0057] For the blocky powder cosmetic forming a fine relief, in the process of filling the material body into the mold through the air pressure feeding device according to the preset amount and extruding and drying the material body in the mold, the pressure assists the material body to fill into the sharp corner part of the fine relief. Even if the viscosity of the material body is high, the material body can still be well filled into the sharp corner part of the fine relief and achieve good density, solving the problems of air holes and softness in the finished product.

[0058] For the blocky powder cosmetic added with active substances, 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 without worrying about the failure of the active substances due to high temperature.

[0059] Therefore, the preparation method provided in the embodiments of the present application can effectively avoid the problems of shrinkage deformation, cracking, poor drop resistance, air holes, softness and the like in the product desolventization process, and can add high-temperature sensitive active substances, while improving the production efficiency.

[0060] In some embodiments, the step of filling the material body into the mold through the air pressure feeding device according to the preset amount includes: pressing or sucking the material body into the mold by the action of air pressure.

[0061] The present application does not limit the specific way of filling the material body 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, a gas pump and a discharge pipe. The material body is sucked into the air pressure feeding device from the feeding pipe by the gas pump providing conveying air pressure, and then pressed into the mold through the discharge 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 with the mold. The material body is sucked into the mold by the air pressure feeding device providing conveying air pressure.

[0062] Whether the material body is pressed or sucked into the mold, the flowability requirement of the material body is low, and too much solvent does not need to be added, which greatly shortens the subsequent drying time.

[0063] In some embodiments, the viscosity of the material is below 30000 cP, preferably 10000 cP-25000 cP; the pressure in the air pressure feeding device is 0.02-0.1 MPa, preferably 0.04-0.08 MPa.

[0064] In some embodiments, the extrusion drying comprises performing pressure filtration on the material in the mold to cause at least part of the solvent to be dialyzed out of the material, and transferring the dialyzed solvent at the same time or after the pressure filtration. It is understood that the transferring of the dialyzed solvent can be achieved in various specific ways, including but not limited to suction, pumping, drainage, etc.

[0065] In some embodiments, the extrusion drying operation comprises performing pressure filtration and negative pressure suction on the material in the mold; the pressure parameter for the pressure filtration is 0.05-3 MPa, preferably 0.2-1.5 MPa; the pressure parameter for the negative pressure suction is 0.02-0.1 MPa, preferably 0.05-0.08 MPa.

[0066] In the present application, "pressure filtration" refers to an operation of applying a certain pressure to the material in the presence of a filter medium, so that at least part of the solvent is dialyzed out of the material through the filter medium.

[0067] In the present application, "negative pressure suction" refers to an operation of using the principle of negative pressure vacuum suction to suction and transfer the dialyzed solvent through a negative pressure differential.

[0068] Exemplarily, the device for achieving pressure filtration can be a filter press, and the device for achieving negative pressure suction can be a vacuum suction pump, and the present application does not limit the specific composition and structure of the device.

[0069] In the operation process of the pneumatic feeding and extrusion drying, the viscosity of the material body is closely related to the flowability and surface tension and other characteristics. In the prior art, the viscosity of the filling material body is generally less than 5000 cP due to the need for flowability; in the present application, the viscosity of the material body can be less than 30000 cP due to the use of pneumatic feeding and extrusion drying, and the preferred viscosity range is 10000 cP to 25000 cP. Corresponding to the viscosity range of the material body, the pressure in the feeding and extrusion drying process of the present application needs to reach a certain threshold value to meet the requirements of filling the auxiliary material body to the sharp corner part of the fine relief of the powder and achieving better density, solving the problems of air holes, loose and other problems in the finished product; at the same time, the pressure in the feeding and extrusion drying process is not the higher the better, and excessive pressure is not conducive to the stability of the material body, and may even cause part of the components in the material body to boil, which will affect the filling effect of the material body on the mold. The present application proposes that when the pressure in the pneumatic feeding device, the pressure parameters of pressure filtration and negative pressure suction are within a certain range, the pressure parameters of the material body and the pneumatic feeding and pressure drying process meet the optimal adaptation, so that the performance of the present application in improving the air holes, softness, shrinkage deformation and drop resistance of the final product is optimal.

[0070] Exemplarily, the viscosity of the material body can 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 composed of any two of the above values.

[0071] Exemplarily, 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 composed of any two of the above values.

[0072] Exemplarily, the pressure of the pressure filtration can be 0.05 MPa, 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa, 0.5 MPa, 0.6 MPa, 0.7 MPa, 0.8 MPa, 0.9 MPa, 1.0 MPa, 1.1 MPa, 1.2 MPa, 1.3 MPa, 1.4 MPa, 1.5 MPa, 1.6 MPa, 1.7 MPa, 1.8 MPa, 1.9 MPa, 2.0 MPa, 2.1 MPa, 2.2 MPa, 2.3 MPa, 2.4 MPa, 2.5 MPa, 2.6 MPa, 2.7 MPa, 2.8 MPa, 2.9 MPa, 3.0 MPa, or a range formed by any two of the above values.

[0073] Exemplarily, the pressure parameter of the negative pressure suction 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 formed by any two of the above values.

[0074] In some embodiments, the steps of pressure filtration and negative pressure suction are simultaneously performed on the material in the mold, and the content of the solvent in the material is reduced to 30-80%, preferably 30-50%, of the original solvent content in the material before the pressure filtration and negative pressure suction, to obtain a pre-solidified and formed powder master product in the mold.

[0075] In some embodiments, the solvent content in the obtained block-shaped powder cosmetic is less than 5%, preferably within 1%.

[0076] In some embodiments, the step of solidifying the powder master product at low temperature is performed in a liquid nitrogen quick-freezing device. Exemplarily, the liquid nitrogen quick-freezing device can be a liquid nitrogen tunnel, a liquid nitrogen freezer, an ultra-low temperature refrigerator, etc., which can be commercially available, and the present application is not limited thereto.

[0077] After the filling step is completed, the present application has obtained a pre-solidified and formed powder master product in the mold, and then the present application uses a liquid nitrogen quick-freezing device to perform extremely low-temperature solidification on the powder master product, and the raw material components in the powder master product undergo molecular quick-freezing in the extremely low-temperature environment in the liquid nitrogen quick-freezing device. The cosmetic material contains components such as oil and emulsion, which will undergo a maximum ice crystal generation zone of about -10-0°C during the freezing and setting process, and about 80% of the liquid (water, emulsion, etc.) will become ice. Unlike the ordinary freezing performed before demolding in the prior art, the powder master product quickly passes through the maximum ice crystal generation zone in the molecular quick-freezing process completed in the liquid nitrogen tunnel. The distribution of ice crystals in the powder master product is more uniform and dense, the skin feel of the product after freeze-drying is more soft and tender, the product size variation is smaller and easier to control, the product structure is more stable, and the anti-falling ability is better.

[0078] Further, the present application also proposes the optimal liquid nitrogen quick-freezing condition parameters suitable for the preparation of the block-shaped powder cosmetic by studying the freezing curve of the powder cosmetic material and the energy transfer characteristics of the liquid nitrogen quick-freezing device. The liquid nitrogen quick-freezing of the powder material masterbatch under the above condition parameters can make the finally prepared block-shaped powder cosmetic have a uniform and dense texture, the best skin feel, and the best stability and anti-falling ability of the product structure.

[0079] 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℃, preferably -95 to -80℃. The liquid nitrogen tunnel is also called a liquid nitrogen tunnel type quick-freezing machine, which is a device that uses liquid nitrogen as a cold source and realizes the continuous entry and quick freezing of materials by conveying the materials into the quick-freezing tunnel through a conveying belt in a continuous production mode. The powder material masterbatch passes through the liquid nitrogen tunnel at a speed of 0.4 to 1.2 meters / minute, preferably 0.6 to 1 meter / minute, and the passing time of the powder material masterbatch in the liquid nitrogen tunnel is 5 to 15 minutes, preferably 6 to 10 minutes.

[0080] In some embodiments, the drying includes any combination of one or more of heating drying, vacuum drying, freeze drying, microwave drying, and supercritical fluid drying.

[0081] In some embodiments, the drying includes freeze drying. Freeze drying is a drying method that freezes the water-containing material below the freezing point to convert the water into ice, and then removes the ice by converting it into vapor under a high vacuum. In the freeze drying step, the fine and uniformly distributed ice crystals in the material are sublimated into water vapor under high vacuum conditions to remove them, greatly preserving the ingredients, color, and aroma of the original material, and further enhancing the performance improvement of the block-shaped powder cosmetic brought by the liquid nitrogen quick-freezing step; the fine and uniformly distributed ice crystals are easier to remove, and ice residues are less likely to be produced during the removal process, and the freeze drying efficiency is also improved.

[0082] In some embodiments, the 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.

[0083] Heating drying is the most common drying method, which realizes drying by heating the material. Vacuum drying is a drying method that places the material under negative pressure conditions and appropriately heats it to the boiling point under negative pressure or coagulates the material by cooling to dry the material. Microwave drying is a drying method that uses electromagnetic waves as a heating source and the material itself as a heating body. Supercritical fluid drying is a drying method that uses the high solubility of supercritical solvents to remove the solvents contained in porous solids. The present application can select one or more drying methods according to the characteristics of the material.

[0084] When a high-temperature sensitive active is added to the material, the drying step in the embodiments of the present application is not performed at a temperature higher than 40℃ to ensure that the high-temperature sensitive active is not inactivated or partially inactivated during the drying step.

[0085] In some embodiments, the raw materials for preparing the block-shaped powder cosmetic include a powder phase component, an oil phase component, and a water phase component;

[0086] The powder phase component includes one or more of a filler, a coloring agent;

[0087] The oil phase component includes one or more of an emollient moisturizer, an antioxidant, a sunscreen agent;

[0088] The water phase component includes one or more of a solvent, a thickening agent, a film-forming agent, an emollient moisturizer, an emulsifier, a preservative, an active.

[0089] In some embodiments, the thickening agent and the film-forming agent are selected from a natural water-soluble polymer or a derivative thereof, a synthetic water-soluble polymer, or a water-soluble inorganic thickening agent;

[0090] The natural water-soluble polymer or a derivative thereof is selected from at least one of alginic acid, agar, carrageenan, hanseong-gel, gellan gum, crispus, xanthan gum, guar gum, tamarind gum, tara gum, gum arabic, tragacanth gum, quince seed gum, pectin, arabinogalactan, wheat protein, soy protein, gelatin, casein, chitosan, curdlan, cyclodextrin, hyaluronic acid, konjac gum, tremella polysaccharide, acacia gum, microcrystalline cellulose, methyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch phosphate, starch, sodium hydroxymethyl starch, sodium polyacrylate grafted starch, and hydroxypropyl guar gum;

[0091] The synthetic water-soluble polymer is selected from at least one of acrylates / C10-30 alkyl acrylate crosspolymer, carbomer, acrylates / octylacrylamide copolymer, acrylates / ethylhexyl acrylate copolymer, sodium acrylates / acryloyldimethyltaurate copolymer, acrylates / octylacrylamide copolymer, styrene / acrylates copolymer, acrylates copolymer, hydroxyethyl acrylate / acryloyldimethyltaurate copolymer, polyacrylate crosspolymer-6, acrylates / steareth-20 methacrylate copolymer, ammonium acryloyldimethyltaurate / beheneth-25 methacrylate crosspolymer, acrylates copolymer ammonium, sodium polyacrylate, sodium polyacryloyldimethyltaurate, polyacrylamide, polyvinylpyrrolidone, polyvinyl alcohol, VP / VA copolymer, polyurethane-1, and polyurethane-35;

[0092] The aqueous inorganic thickening agent is selected from at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, magnesium lithium silicate, magnesium sodium silicate, montmorillonite or its derivatives;

[0093] The mass percentage content of the aqueous inorganic thickening agent and / or the film forming agent is 0.02-15%, preferably 0.05-5%, based on the prepared block powder type cosmetic.

[0094] In some embodiments, the emollient moisturizer is selected from at least one of an alcohol, a silicone oil, a mineral oil, a synthetic oil, a plant or animal oil or its derivatives;

[0095] The plant or animal oil or its derivatives is selected from at least one of glycerin, propylene glycol, dipropylene glycol, pentylene glycol, butylene glycol, ethylene glycol, hexylene glycol, sorbitol, xylitol, polyethylene glycol, dimethicone, octyl poly-methyl siloxane, phenyl trimethyl siloxane, cetyl dimethicone, C30-45 alkyl dimethicone polypropyl disiloxane, bis-PEG-18 methyl ether dimethyl silane, white mineral oil, petrolatum, hydrogenated polyisobutene, lanolin esters and its derivatives, octyldodecanol, caprylic / capric triglyceride, ethylhexyl palmitate, bis-diglyceryl polyacyladipate-2, isononyl isononanoate, jojoba seed oil, coconut oil, hydrogenated coco-glycerides, rapeseed oil, olive oil, squalane, C9-12 alkane, cocoglycerol caprylate / caprate, tocopheryl acetate, methyl gluceth-10;

[0096] The mass percentage content of the emollient moisturizer is 0.1-40%, preferably 0.5-30%, based on the prepared block powder type cosmetic.

[0097] In some embodiments, the filler is selected from at least one of mica, talc, synthetic fluorphlogopite, kaolin, bentonite, boron mononitride, bismuth oxychloride, silica, potassium sodium aluminum silicate, lauroyl lysine, magnesium stearate, magnesium myristate, calcium aluminum borosilicate, tin oxide, sodium calcium borosilicate, aluminum hydroxide, zinc stearate starch and its derivatives, plastic microbeads;

[0098] 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, CI 17200, CI 73360, CI 42090, CI 47005;

[0099] The total mass percentage of the filler and the colorant is 50-99%, preferably 70-95%, based on the prepared blocky powder cosmetic.

[0100] In some embodiments, the preservative is selected from at least one of phenoxyethanol, parabens, chlorphenesin, potassium sorbate, sodium benzoate, or a preservative synergist.

[0101] The preservative synergist is selected from at least one of octoxyglycerin, p-hydroxyacetophenone, ethylhexylglycerin, 1,2-hexanediol, caprylyl oxyhydroxamic acid, 1,2-pentanediol, glyceryl caprylate, or umbelliferone.

[0102] The total mass percentage of the preservative and the preservative synergist is 0.01-5%, preferably 0.5-1%, based on the prepared blocky powder cosmetic.

[0103] In some embodiments, the active can be selected from a high-temperature sensitive active or a high-temperature insensitive active.

[0104] In some embodiments, the high-temperature sensitive active is unstable, has reduced activity, or loses activity in an environment above 40°C. For example, the high-temperature sensitive active can be selected from at least one of a polypeptide active, astaxanthin, vitamin A alcohol or its derivative, vitamin C or its derivative, or arbutin.

[0105] In existing powder preparation techniques, the material is usually heated before filling to increase the flowability of the material, facilitating filling and transportation. The heating operation determines that high-temperature sensitive active materials, such as polypeptide active, astaxanthin, vitamin A alcohol, vitamin C or its derivative, and arbutin, cannot be used as raw materials. Even if they are added, part or all of the activity will be lost due to the heating step. The preparation process of the present application does not include any high-temperature process, and the filling step can be operated at low temperature or room temperature. High-temperature sensitive active materials can be added to the material.

[0106] In some embodiments, the solvent is water or a mixture of water and an organic solvent.

[0107] In some embodiments, the thickening agent is an inorganic thickening agent; preferably, the inorganic thickening agent is at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, magnesium lithium silicate, magnesium sodium silicate, montmorillonite, or a derivative thereof.

[0108] In the prior art, natural polysaccharides are often used as thickeners for powder products due to their good thickening and adhesive effects. Inorganic thickeners cannot be used as thickeners alone because of their poor adhesive effects, which can cause cracking and poor drop resistance of the product. However, natural polysaccharides increase the microbial risk of powder products and are not conducive to long-term storage of powder products. In the embodiments of the present application, external force is used to increase the compactness of the material during air pressure feeding and extrusion drying. In addition, the use of less solvent reduces the adverse effects of the solvent removal step on the internal bonding stability of the material. Therefore, even if inorganic thickeners with poor adhesive effects are used, the final powder product will not crack or have poor drop resistance. In addition, the use of inorganic thickeners instead of natural polysaccharides can reduce the microbial risk and increase the long-term storage stability of powder products.

[0109] In a second aspect, the embodiments of the present application provide a block-shaped powder cosmetic prepared by the method of the first aspect of the present application. The block-shaped powder cosmetic provided by the present application is prepared by filling the mold with the preset amount of material by the air pressure feeding device and extruding and drying the material in the mold, which can effectively avoid the problems of ice slag, shrinkage deformation, cracking of the finished product, poor drop resistance, air holes, softness, and the like during the desolvation process of the product. The block-shaped powder cosmetic has a good presentation effect of fine surface relief and can add high-temperature sensitive active substances.

[0110] In some embodiments, the block-shaped powder cosmetic is selected from the group consisting of a powder compact, a blush, an eye shadow, and a highlighter. The block-shaped powder cosmetic can also include other functional products.

[0111] Embodiments

[0112] The following examples more specifically describe the present disclosure, which are only used for illustrative purposes, because various modifications and changes within the scope of the present disclosure are obvious to those skilled in the art. Unless otherwise stated, all parts, percentages and ratios reported in the following examples are based on 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.

[0113] Formulations 1-4

[0114] Exemplarily, the present application provides the preparation of raw material composition, ratio and mixing method of four block-shaped powder cosmetics.

[0115] The raw material components of the block-shaped powder cosmetic formulation 1 are shown in Table 1:

[0116] Table 1

[0117] Mixing: (1) uniformly disperse A phase under heating, temperature 75±5℃; (2) homogenously emulsify B phase into A, temperature 75±5℃; (3) mix C phase into (2) uniformly, temperature 75±5℃; (4) reduce the material to 50±5℃; (5) mix D (need to be pre-dissolved), E, F into (4) uniformly, and vacuum defoam at 50±5℃; get the material;

[0118] The raw material components of the blocky powder cosmetic formulation 2 are shown in Table 2:

[0119] Table 2

[0120] Mixing: (1) uniformly disperse A phase under heating, temperature 75±5℃; (2) homogenously emulsify B phase into A, temperature 75±5℃; (3) mix C phase into (2) uniformly, temperature 75±5℃; (4) reduce the material to 50±5℃; (5) mix D (need to be pre-dissolved), E into (4) uniformly, and vacuum defoam at 50±5℃; get the material;

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

[0122] Table 3

[0123] Mixing: (1) uniformly disperse A phase under heating, temperature 75±5℃; (2) homogenously emulsify B phase into A, temperature 75±5℃; (3) mix C phase into (2) uniformly, temperature 75±5℃; (4) reduce the material to 50±5℃; (5) mix D (need to be pre-dissolved), E into (4) uniformly, and vacuum defoam at 50±5℃; get the material;

[0124] The raw material components of the blocky powder cosmetic formulation 4 are shown in Table 4:

[0125] Table 4

[0126] Mixing: (1) uniformly disperse A phase under heating, temperature 75±5℃; (2) homogenously emulsify B phase into A, temperature 75±5℃; (3) mix C phase into (2) uniformly, temperature 75±5℃; (4) reduce the material to 50±5℃; (5) mix D (need to be pre-dissolved), E into (4) uniformly, and vacuum defoam at 50±5℃; get the material.

[0127] Examples 1-12

[0128] The preparation of the blocky powder cosmetic is carried out according to the following method:

[0129] Mixing: raw materials are provided according to the raw material components of the blocky powder cosmetic formula, the raw materials are mixed according to the mixing steps, and a material body is obtained;

[0130] Filling and pre-solidification: the material body is filled into a mold by a preset amount via a gas pressure feeding device, the material body is subjected to pressure filtration and negative pressure suction, the content of the solvent in the material body is reduced to 30-50% of the original solvent content in the material body before pressure filtration and negative pressure suction, and a powder material master product pre-solidified and formed in the mold is obtained;

[0131] Freezing: the powder material master product pre-solidified and formed is frozen at low temperature, and the freezing step is carried out in a liquid nitrogen tunnel;

[0132] Demolding and drying: the frozen powder material master product is separated from the mold and dried to obtain a blocky powder cosmetic, or the frozen powder material master product is dried and separated from the mold to obtain a blocky powder cosmetic, and the content of the solvent in the blocky powder cosmetic is less than 5%.

[0133] In the examples 1-12, the viscosity of the material body, the pressure in the gas pressure feeding device, the pressure for pressure filtration and negative pressure suction of the material body, the temperature inside the liquid nitrogen tunnel for solidification and freezing of the powder material master product at low temperature, the speed of the powder material master product in the liquid nitrogen tunnel, the through time, and the drying method are shown in Table 5.

[0134] Comparative examples 1-5

[0135] The difference between comparative example 1 and example 4 is that the gas pressure feeding device is not used for feeding, but gravity filling is carried out at room temperature 25℃, and the material body is not subjected to pressure filtration and negative pressure suction.

[0136] The difference between comparative example 2 and example 4 is that the gas pressure feeding device is not used for feeding, but gravity filling is carried out after the material body is heated to 50℃, and the material body is not subjected to pressure filtration and negative pressure suction.

[0137] The difference between comparative example 3 and example 4 is that the gas pressure feeding device is not used for feeding, but gravity filling is carried out after the material body is heated to 90℃, and the material body is not subjected to pressure filtration and negative pressure suction.

[0138] The difference between comparative example 4 and example 4 is that the solvent water is added to the raw material components of the formula 4, the viscosity of the material body obtained by mixing is reduced to 5000cP, then the gas pressure feeding device is not used for feeding, but gravity filling is carried out after the material body is heated to 50℃, and the material body is not subjected to pressure filtration and negative pressure suction.

[0139] The difference between Comparative Example 5 and Example 1 is that the viscosity of the mixture is reduced to 3000 cP by adding solvent water to the raw material components of Formulation 1, then the mixture is fed by gravity filling after being heated to 50°C instead of using the air pressure feeding device, and the mixture is not subjected to pressure filtration and negative pressure suction.

[0140] The viscosity of the mixture, the pressure in the air pressure feeding device, the pressure at which the mixture is subjected to pressure filtration and negative pressure suction, the temperature inside the liquid nitrogen tunnel during the low-temperature curing and freezing steps, the speed of the powder mother article in the liquid nitrogen tunnel, the through time, and the drying method for Comparative Examples 1-5 are shown in Table 5.

[0141] Table 5 Process parameter table for Examples 1-12 and Comparative Examples 1-5

[0142] Test section

[0143] The powder compacts were prepared according to the methods of Examples 1-12 and Comparative Examples 1-5, with 100 powder compacts prepared for each example or comparative example. The appearance, diameter shrinkage, and drop test were performed, and whether there was a risk of microbial contamination caused by natural polysaccharides and whether there was a possibility of inactivation or partial inactivation of high-temperature sensitive active substances was recorded.

[0144] 1) Appearance observation

[0145] The appearance of the powder compacts was observed by the naked eye or with the aid of a microscope, including the surface relief rendering effect, with a focus on whether the sharp corners of the fine relief on the surface of the powder compact were completely filled, whether there were air bubbles, whether the bottom of the powder compact was flat, and whether the texture of the powder was uniform and dense.

[0146] The recorded appearance was based on the observation of more than 90% of the powder compacts in 100 powder compacts.

[0147] 2) Diameter shrinkage

[0148] The diameter D of the mold and the diameter d of the prepared powder compact were measured by a vernier caliper. Since air pressure feeding, pressure filtration, and negative pressure suction were implemented, it was considered that the mixture was fully filled in the mold when the filling and pre-curing steps were completed, so the diameter of the filling mold was taken as the diameter of the powder mother article before freezing, demolding, and drying.

[0149] The diameter shrinkage was calculated by the following formula:

[0150] Diameter shrinkage = [(D-d) / D] * 100%

[0151] Where D is the diameter of the filling mold, and d is the diameter of the prepared powder compact.

[0152] The recorded diameter shrinkage is the average of the measured values of 100 cakes.

[0153] 3) Drop test

[0154] Adjust the drop test table ground rotating screw, and adjust the flat plate to the 30 cm scale; place the cake with the front face upward in the center of the test height.

[0155] Perform the first drop test: press the test table button, and let the cake drop onto the hard plate; pick up the cake dropped on the table, and detect whether the cake surface is cracked or broken; if the cake is cracked or broken, stop the drop test of this cake; if the cake is not abnormal, then perform the second drop test; the operation steps of the second drop test are the same as those of the first drop test; if the cake is cracked or broken, stop the drop test of this cake; if the cake is not abnormal, then perform the third drop test; the operation steps of the third drop test are the same as those of the first drop test.

[0156] The ratio of the number of broken cakes in each drop test to the total number of cakes subjected to the drop test is the breakage rate of each drop test; record the first breakage rate, the second breakage rate, and the third breakage rate of Examples 1 to 12 and Comparative Examples 1 to 5, respectively.

[0157] 4) Microbial risk caused by natural polysaccharides

[0158] If the cake raw material does not contain a natural polysaccharide component, it is considered that the cake does not have a microbial risk caused by natural polysaccharides; if the cake raw material contains a natural polysaccharide component, it is considered that the cake has a possibility of a microbial risk caused by natural polysaccharides.

[0159] 5) Activity of high-temperature sensitive active substances

[0160] If the preparation process of the cake contains a step with a temperature exceeding 40°C, it is considered that the high-temperature sensitive active substances may have been inactivated or partially inactivated; if the preparation process of the cake does not contain a step with a temperature exceeding 40°C, it is considered that the high-temperature sensitive active substances are active.

[0161] Record the above test results of Examples 1 to 12 and Comparative Examples 1 to 5 in Table 6.

[0162] Table 6 Test results of Examples 1 to 12 and Comparative Examples 1 to 5

[0163] From the detection results shown in Table 6, it can be seen that Examples 1-12 adopt the preparation method of blocky powder cosmetic provided by the present application, the material body is quantitatively filled into the mold through the air pressure feeding device, part of the solvent in the material body is removed by extrusion drying to realize pre-solidification, and then the blocky powder cosmetic is obtained through freezing, drying and demolding. Compared with Comparative Examples 1-5 which do not adopt the preparation method of the present application, Examples 1-12 have obvious improvement in filling efficiency, filling effect on mold relief, appearance, texture and skin feel of the prepared blocky powder cosmetic, and also have significant effect in improving the diameter shrinkage rate in the preparation process and reducing the breakage rate in the powder cake drop test, and provide a feasible scheme for avoiding the microbial risk caused by natural polysaccharide and using high-temperature sensitive active substances in powder products.

[0164] The average diameter shrinkage rate in the preparation process of the powder cake of Examples 1-12 is less than 1%, the sum of the breakage rates in three drop tests is not more than 15%, and the presentation effect of the fine relief on the surface of the powder cake is significantly better than that of Comparative Examples 1-5. Since Comparative Examples 1-5 do not adopt the preparation method of the present application, they cannot be effectively filled and produced under the condition of using less solvent in the filling material body and high viscosity of the material body. Even if the measures of heating the material body before filling or increasing the solvent to reduce the viscosity of the material body are taken, the performance data of the blocky powder cosmetic prepared in terms of diameter shrinkage rate, drop test breakage rate and the like are still significantly worse than those of Examples 1-12 of the present application.

[0165] Further, the pressure of the air pressure feeding device for auxiliary feeding, the pressure for pressure filtration and negative pressure suction of the material body, the temperature and time control of the powder material mother product solidification at low temperature and the like parameters in the preparation method of the blocky powder cosmetic provided by the present application also have an influence on the achievement of the technical effect of the present application. The present application also provides a relatively optimal range for selection of the above process parameters, so that the performance of the blocky powder cosmetic prepared according to the method provided by the present application is further improved to the best. For example, in Examples 1-4, when the viscosity of the material body is 10000-30000 cP, the feeding pressure in the air pressure feeding device is 0.02-0.1 Mpa, the pressure filtration pressure parameter in the extrusion drying is 0.05-3 Mpa, the negative pressure suction pressure parameter is 0.02-0.1 Mpa, the temperature inside the liquid nitrogen tunnel is -120 to -70℃, the powder material mother product passes through the liquid nitrogen tunnel at a speed of 0.4-1.2 meters / minute on the conveying belt in the liquid nitrogen tunnel, the passing time is 5-15 minutes, the sharp angle filling of the surface relief of the final blocky powder cosmetic is complete and free of bubbles, the bottom is flat, the powder texture is uniform and dense, and the anti-drop performance is excellent, the average diameter shrinkage rate is less than 0.2%.

[0166] The preparation method of the blocky powder cosmetic provided by the application successfully solves the technical problems of shrinkage and deformation of the powder product during preparation and desolvation, cracking of the prepared powder product, poor anti-falling property, air holes and softness, etc., and also avoids the microbial risk caused by natural polysaccharides and the addition of high-temperature sensitive active substances, thereby providing a better prospect for the development and application of the blocky powder cosmetic.

[0167] The above is only a specific embodiment of the present application, and those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working process described above can refer to the corresponding process in the foregoing method embodiment, which will not be described here. It should be understood that the protection scope of the present application is not limited thereto, and any person skilled in the art can easily think of various equivalent modifications or replacements within the technical scope disclosed by the present application, and these modifications or replacements should be covered within the protection scope of the present application.

Claims

1. A method for preparing a bulk powder cosmetic, wherein, The method comprises the following steps: mixing: providing raw materials for preparing the block-shaped powder cosmetic, mixing the raw materials to obtain a material body; filling and pre-solidification: filling the material body into a mold through a gas pressure feeding device in a preset amount, and performing extrusion drying on the material body to obtain a pre-solidified and formed powder material mother product in the mold; freezing: freezing the pre-solidified and formed powder material mother product at low temperature; demolding and drying: separating the frozen powder material mother product from the mold and drying to obtain the block-shaped powder cosmetic, or drying the frozen powder material mother product and separating it from the mold to obtain the block-shaped powder cosmetic.

2. The method for preparing a bulk powder cosmetic according to claim 1, wherein The step of filling the material body into the mold through the gas pressure feeding device comprises pressing or sucking the material body into the mold by gas pressure.

3. The method for preparing a bulk powder cosmetic according to claim 2, wherein The viscosity of the material body is below 30,000 cP, preferably 10,000 cP to 25,000 cP; the pressure in the gas pressure feeding device is 0.02 to 0.1 MPa, preferably 0.04 to 0.08 MPa.

4. The method of preparing a bulk powder cosmetic according to claim 1, wherein The extrusion drying comprises performing filter pressing on the material body in the mold to dialyze at least part of the solvent from the material body, and transferring the dialyzed solvent at the same time or after the filter pressing.

5. The method for preparing a bulk powder cosmetic according to claim 4, wherein The extrusion drying comprises performing filter pressing and negative pressure suction on the material body in the mold; the pressure parameter of the filter pressing is 0.05 to 3 MPa, preferably 0.2 to 1.5 MPa; the pressure parameter of the negative pressure suction is 0.02 to 0.1 MPa, preferably 0.05 to 0.08 MPa.

6. The method for preparing a bulk powder cosmetic according to claim 5, wherein In the step of simultaneously performing filter pressing and negative pressure suction on the material body in the mold, the content of the solvent in the material body is reduced to 30 to 80%, preferably 30 to 50%, of the original solvent content in the material body before the filter pressing and negative pressure suction, to obtain the pre-solidified and formed powder material mother product in the mold.

7. The method of preparing a bulk powder cosmetic according to claim 1, wherein The content of the solvent in the block-shaped powder cosmetic prepared is below 5%, preferably within 1%.

8. The method of preparing a bulk powder cosmetic according to claim 1, wherein The step of freezing the pre-solidified and formed powder material mother product at low temperature is performed in a liquid nitrogen quick-freezing device.

9. The method of preparing a bulk powder cosmetic according to claim 8, wherein 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 powder material mother product passes through the liquid nitrogen tunnel at a speed of 0.4 to 1.2 meters per minute on a conveying belt in the liquid nitrogen tunnel, preferably at a speed of 0.6 to 1 meter per minute on a conveying belt in the liquid nitrogen tunnel; The passing time of the powder material mother product in the liquid nitrogen tunnel is 5 to 15 minutes, preferably 6 to 10 minutes.

10. The method of preparing a bulk powder cosmetic according to claim 9, wherein The drying comprises one or more of any combination of heating drying, vacuum drying, freeze drying, microwave drying and supercritical fluid drying; preferably, the temperature in the drying step is below 40°C.

11. The method of preparing a bulk powder cosmetic according to claim 10, wherein The drying comprises freeze drying and one or more of any combination of heating drying, vacuum drying, microwave drying and supercritical fluid drying.

12. The method of preparing a bulk powder cosmetic according to claim 1, wherein The raw materials for preparing the block-shaped powder cosmetic comprise a powder phase component, an oil phase component and a water phase component; The powder phase component comprises one or more of a filler and a colorant; The oil phase component comprises one or more of emollient moisturizer, antioxidant, sunscreen agent; The water phase component comprises one or more of solvent, thickening agent, film forming agent, emollient moisturizer, emulsifier, preservative, active substance.

13. The method of preparing a bulk powder cosmetic according to claim 12, wherein The thickening agent and film forming agent are selected from at least one of natural water-soluble polymer or its derivative, synthetic water-soluble polymer or water-soluble inorganic thickening agent; The natural water-soluble polymer or its derivative is selected from at least one of alginic acid, agar, carrageenan, rhamsan gum, gellan gum, crispus, xanthan gum, guar gum, tamarind gum, tara gum, gum arabic, tragacanth gum, quince seed gum, pectin, arabinogalactan, wheat protein, soy protein, gelatin, casein, chitosan, curdlan, cyclodextrin, hyaluronic acid, konjac gum, tremella polysaccharide, acacia gum, microcrystalline cellulose, methyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch phosphate, starch, sodium hydroxymethyl starch, polyacrylic acid sodium grafted starch, hydroxypropyl guar gum; The synthetic water-soluble polymer is selected from at least one of acrylate / C10-30 alkyl acrylate crosspolymer, carbomer, acrylate / octylacrylamide copolymer, acrylates / ethylhexyl acrylate copolymer, sodium acrylates / acryloyldimethyltaurate copolymer, acrylate / octylacrylamide copolymer, styrene / acrylate copolymer, acrylate copolymer, hydroxyethyl acrylate / acryloyldimethyltaurate copolymer, polyacrylate crosspolymer-6, acrylate / steareth-20 methacrylate copolymer, ammonium acryloyldimethyltaurate / beheneth-25 methacrylate crosspolymer, acrylate copolymer ammonium, polyacrylate sodium, polyacryloyldimethyltaurate sodium, polyacrylamide, polyvinylpyrrolidone, polyvinyl alcohol, VP / VA copolymer, polyurethane-1, polyurethane-35; The water-soluble inorganic thickening agent is selected from at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, magnesium lithium silicate, magnesium sodium silicate, montmorillonite or its derivative; The mass percentage content of the water-soluble inorganic thickening agent and / or film forming agent is 0.02-15%, preferably 0.05-5%, based on the prepared blocky powder cosmetic. The emollient moisturizer is selected from at least one of alcohol, silicone oil, mineral oil, synthetic oil, animal and plant oil or its derivative; 14. The method of preparing a bulk powder cosmetic according to claim 12, wherein ​ The animal or 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, dimethicone, octyl dimethicone, phenyl trimethicone, cetyl dimethicone, C30-45 alkyl dimethicone polypropylphenyl silsesquioxane, bis-PEG-18 methyl ether dimethicone, white mineral oil, petrolatum, hydrogenated polyisobutene, lanolin esters and their derivatives, octyldodecanol, caprylyl / capryl methicillin, ethylhexyl palmitate, bis-diglyceryl polyacyladipate-2, isononyl isononanoate, jojoba seed oil, coconut oil, hydrogenated coco-glycerides, white pool seed oil, olive oil, squalane, C9-12 alkane, coco-caprylate / caprate, tocopheryl acetate, methyl gluceth-10; The mass percentage content of the emollient moisturizer is 0.1-40%, preferably 0.5-30%, based on the prepared blocky powder cosmetic.

15. The method of preparing a bulk powder cosmetic according to claim 12, wherein The filler is selected from at least one of mica, talc, synthetic fluorphlogopite, kaolin, bentonite, boron mononitride, bismuth oxychloride, silica, potassium sodium aluminum silicate, lauroyl lysine, magnesium stearate, magnesium myristate, boro calcium aluminum silicate, tin oxide, sodium calcium boro silicate, aluminum hydroxide, zinc stearate starch and its derivatives, 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 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, CI 17200, CI 73360, CI 42090, CI 47005; The total mass percentage content of the filler and the colorant is 50-99%, preferably 70-95%, based on the prepared blocky powder cosmetic.

16. The method of preparing a bulk powder cosmetic according to claim 12, wherein The preservative is selected from at least one of phenoxyethanol, parabens, chlorphenesin, potassium sorbate, sodium benzoate or a preservative synergist; The preservative synergist is selected from at least one of octoxyglycerin, p-hydroxyacetophenone, ethylhexylglycerin, 1,2-hexanediol, caprylyl oxyhydroxamic acid, 1,2-pentanediol, glyceryl caprylate, umbelliferone; The total mass percentage content of the preservative and the preservative synergist is 0.01-5%, preferably 0.5-1%, based on the prepared blocky powder cosmetic.

17. The method of preparing a bulk powder cosmetic according to claim 12, wherein The active is selected from a high-temperature sensitive active or a high-temperature insensitive active; Preferably, the high-temperature sensitive active is selected from at least one of a polypeptide active, astaxanthin, vitamin A alcohol or its derivative, vitamin C or its derivative, arbutin.

18. The method of preparing a bulk powder cosmetic according to claim 12, wherein, The solvent is water or a mixture of water and an organic solvent.

19. The method of preparing a bulk powder cosmetic according to claim 12, wherein The thickening agent is an inorganic thickening agent; preferably, the inorganic thickening agent is at least one of magnesium aluminum silicate, sodium magnesium lithium silicate, magnesium lithium silicate, magnesium sodium silicate, montmorillonite, or a derivative thereof.

20. A bulk powder cosmetic, wherein, obtained by the process of any one of claims 1-19.

21. The bulk powder cosmetic according to claim 20, wherein The compact powder cosmetic is selected from the group consisting of a powder foundation, a blush, an eyeshadow, or a highlighter.

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