A method of emulsifying wax

Abstract

The application provides a wax-based emulsification method, comprising the following steps: S1, raw material preparation and pretreatment: weighing, by weight parts, 8-20 parts of wax-based raw materials, 15-35 parts of liquid oil, 2-8 parts of non-ionic emulsifier, 0.5-3 parts of auxiliary agent, 5-15 parts of polyhydric alcohol, 20-30 parts of deionized water; the wax-based raw materials, the liquid oil, the non-ionic emulsifier and the auxiliary agent are added into an oil phase pot, heated to 80-85 DEG C, and stirred until completely melted to obtain an oil phase; then the polyhydric alcohol and the deionized water are added into a water phase pot, heated to 78-83 DEG C, and stirred uniformly to obtain a water phase, S2, initial mixing of oil and water: the temperature difference between the oil phase and the water phase is controlled to be within 2 DEG C, the water phase is added into the oil phase under stirring to form a water-in-oil type initial emulsion; the existing powder group preparation method has inherent defects in the aspects of interfacial bonding strength and powder compactness, which leads to poor product stability and high rate of defective products.

Description

Technical Field

[0001] This invention relates to the field of cosmetic preparation, specifically a wax-based emulsification method. Background Technology

[0002] Wax-based products, such as creams, lipsticks, and eyeshadow bases, are highly favored in the market due to their unique texture and setting effect. However, wax-based formulas typically contain a high proportion of solid oils and waxes, which can easily lead to uneven dispersion, a grainy texture, and a coarse consistency during emulsification.

[0003] Traditional wax-based emulsification processes often use single-melting-point waxes as raw materials, which frequently leads to the following problems: First, a single wax makes it difficult to balance the product's hardness and flexibility. An excessively high proportion of high-melting-point waxes can cause the paste to become dry and hard, resulting in stretching during application. Conversely, an excessively high proportion of low-melting-point waxes can lead to a soft paste, deformation at high temperatures, and oil seepage / sweating. Second, conventional emulsification steps rely solely on simple stirring and mixing, resulting in uneven emulsion particle size distribution, which can easily lead to stratification and flocculation. During storage, wax crystals tend to agglomerate, resulting in a rough product texture and decreased stability. Third, the cooling and crystallization stage often uses natural cooling or rapid cooling methods, which cannot precisely control the wax crystallization rate and crystal morphology, easily forming large, irregular crystals that affect the paste's smoothness and application performance.

[0004] Therefore, to solve the above problems, it is necessary to develop a new wax-based emulsification method. Summary of the Invention

[0005] This invention provides a wax-based emulsification method that solves the inherent defects in the interfacial bonding strength and compaction of existing powder packaging preparation methods, which lead to poor product stability and high defect rate.

[0006] This invention is achieved as follows: a wax-based emulsification method, comprising the following steps: S1 Raw Material Preparation and Pretreatment: Weigh out 8-20 parts by weight of wax-based raw material, 15-35 parts of liquid oil, 2-8 parts of nonionic emulsifier, 0.5-3 parts of additives, 5-15 parts of polyol, and 20-30 parts of deionized water. Wax-based raw materials, liquid oils, nonionic emulsifiers, and additives are added to an oil phase pot, heated to 80℃-85℃, and stirred until completely melted to obtain the oil phase; then polyols and deionized water are added to an aqueous phase pot, heated to 78℃-83℃, and stirred evenly to obtain the aqueous phase; S2 Oil-Water Initial Mixing: Control the temperature difference between the oil phase and the water phase to within 2℃, and add the water phase to the oil phase under stirring conditions to form a water-in-oil type primary emulsion; S3 Homogenization and Refinement: Pour the above water-in-oil pre-emulsion into a homogenizer and perform high-speed shearing on the obtained water-in-oil pre-emulsion at a speed of 2500rpm-3500rpm for 5min-10min to obtain a fine homogenized emulsion. S4 Cooling and Stirring and Wax Crystal Formation: The homogenized emulsion obtained above is transferred into a cooling reaction vessel equipped with a wall-scraping stirring device. It is stirred at low speed and slowly cooled to 58℃-62℃ at a rate of 0.5℃ / min-2℃ / min. Heat-sensitive ingredients, preservatives and fragrances are added, and stirring is maintained within this temperature range for 8min-15min to allow the wax to crystallize and precipitate, forming a semi-paste structure. S5 Filling and Cooling: Continue cooling at a rate of 0.5℃ / min-1℃ / min to 43℃-47℃, then perform vacuum degassing, and fill at 40℃-45℃. Cool to room temperature to obtain the wax-based emulsified product.

[0007] In one embodiment of the present invention, in step S1: the wax base material is composed of high melting point wax and low melting point wax, the high melting point wax is one or two of carnauba wax and candelilla wax, and the low melting point wax is beeswax or microcrystalline wax.

[0008] In one embodiment of the present invention, in step S1: the additive is cetearyl alcohol or behenyl alcohol.

[0009] In one embodiment of the present invention, in step S1: the HLB value of the nonionic emulsifier is between 8 and 12, and the nonionic emulsifier is one or more of cetearyl oleate, sorbitan oleate, and glyceryl stearate; the liquid oil is one or more of isononyl isononanoate, caprylic / capric triglyceride, and jojoba seed oil.

[0010] In one embodiment of the present invention, in step S1, the polyol is one or more of glycerol, butanediol, 1,3-propanediol, and panthenol.

[0011] In one embodiment of the present invention, in step S1: the heat-sensitive component is one or more of acetyl hexapeptide-8, sodium hyaluronate, nicotinamide, and plant extracts.

[0012] In one embodiment of the present invention, the stirring speed in step S2 is 300 rpm to 800 rpm; the time for adding the aqueous phase to the oil phase is controlled at 2 min to 5 min to maintain uniform mixing.

[0013] In one embodiment of the present invention, in step S3: the homogenizer is maintained at a temperature of 80°C-85°C.

[0014] In one embodiment of the present invention, the stirring speed in step S4 is 250 rpm to 400 rpm, and the stirring temperature is maintained between 58°C and 62°C to stably control the crystallization rate and crystal morphology of the wax.

[0015] In one embodiment of the present invention, the vacuum degree of vacuum degassing in step S5 is -0.06MPa to -0.9MPa, and the processing time is 2min to 5min, to remove air bubbles from the paste.

[0016] The beneficial effects of this invention are: 1. By controlling the mixing temperature difference between the oil phase and the water phase and the homogenization and refinement parameters, the emulsion droplet distribution becomes more uniform. This not only solves the problem that existing wax-based products are prone to oil phase precipitation, stratification and deformation under high temperature or alternating hot and cold environments, but also improves the centrifugal stability and weather resistance of the product. 2. By stably controlling the cooling rate and stirring speed, this invention effectively avoids the coarsening and agglomeration of wax grains during the cooling process, promoting the formation of a fine and uniform crystalline network structure of wax crystals. This reduces the frictional resistance of the paste, not only avoiding the grainy feeling and skin-pulling sensation produced when applying products prepared by traditional processes, but also significantly improving the smoothness, delicacy and gloss of the product while maintaining the hardness of the paste. Attached Figure Description

[0017] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention, making other features, objects, and characteristics of the invention more apparent. The illustrative embodiments of the invention, along with their descriptions, are used to explain the invention and do not constitute an undue limitation of the invention.

[0018] Figure 1 This is a schematic diagram of the overall preparation process of the present invention; Figure 2 This is a graph showing the experimental comparison results of the embodiments and comparative examples of the present invention. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0020] like Figures 1-2 As shown, the present invention provides a wax-based emulsification method, comprising the following steps: S1 Raw Material Preparation and Pretreatment: Weigh out 8-20 parts by weight of wax base raw material, 15-35 parts of liquid oil, 2-8 parts of nonionic emulsifier, 0.5-3 parts of additives, 5-15 parts of polyol, and 20-30 parts of deionized water; the wax base raw material is composed of high melting point wax and low melting point wax. The high melting point wax is one or two of carnauba wax and candelilla wax, and the low melting point wax is beeswax or microcrystalline wax.

[0021] The additives are cetearyl alcohol or behenyl alcohol.

[0022] The HLB value of the nonionic emulsifier is between 8 and 12. The nonionic emulsifier is one or more of cetearyl oleate, sorbitan oleate, and glyceryl stearate. The liquid oil is one or more of isononyl isononanoate, caprylic / capric triglyceride, and jojoba seed oil.

[0023] The polyol is one or more of glycerol, butanediol, 1,3-propanediol, and panthenol.

[0024] The heat-sensitive ingredients are one or more of acetyl hexapeptide-8, sodium hyaluronate, niacinamide, and plant extracts.

[0025] Wax-based raw materials, liquid oils, nonionic emulsifiers, and additives are added to an oil phase pot, heated to 80℃-85℃, and stirred until completely melted to obtain the oil phase; then polyols and deionized water are added to an aqueous phase pot, heated to 78℃-83℃, and stirred evenly to obtain the aqueous phase; S2 Oil-Water Initial Mixing: Control the temperature difference between the oil phase and the water phase within 2℃. Under stirring conditions, the stirring speed is 300rpm-800rpm. The time for adding the water phase to the oil phase is controlled at 2min-5min to maintain uniform mixing. Add the water phase to the oil phase to form a water-in-oil primary emulsion. S3 Homogenization and Refinement: Pour the above water-in-oil primary emulsion into a homogenizer. Maintain the homogenizer temperature at 80℃-85℃ and perform high-speed shearing on the obtained water-in-oil primary emulsion at a speed of 2500rpm-3500rpm for 5min-10min to obtain a fine homogenized emulsion. S4 Cooling and Stirring with Wax Crystal Formation: The homogenized emulsion obtained above is transferred to a cooling reactor equipped with a wall-scraping stirrer. The mixture is stirred at low speed, and the temperature is slowly reduced to 58℃-62℃ at a rate of 0.5℃ / min-2℃ / min. Heat-sensitive components, preservatives, and fragrances are added, and stirring is maintained within this temperature range for 8-15 minutes at a low stirring speed of 250-400 rpm. Stirring is maintained within the 58℃-62℃ temperature range to stably control the crystallization rate and morphology of the wax. This causes the wax to crystallize and precipitate, forming a semi-paste structure. S5 Filling and Cooling: Continue cooling at a rate of 0.5℃ / min-1℃ / min to 43℃-47℃, followed by vacuum degassing at a vacuum level of -0.06MPa to -0.9MPa for 2-5 minutes to remove air bubbles from the paste. Filling is then performed at 40℃-45℃, followed by cooling to room temperature to obtain the wax-based emulsion product.

[0026] Specific Example 1: This example prepares a high-hardness wax-based emulsion for use in lipstick products. The specific steps are as follows: S1 Raw Material Preparation and Pretreatment: Weigh out 10 parts by weight of carnauba wax, 5 parts of beeswax, 18 parts of isononyl isononanoate, 10 parts of jojoba seed oil, 4 parts of cetearyl oleate, 2 parts of sorbitan oleate, 15 parts of cetearyl alcohol, 8 parts of glycerin, and 25 parts of deionized water.

[0027] Carnauba wax, beeswax, isononyl isononanoate, jojoba seed oil, cetearyl oleate, sorbitan oleate, and cetearyl alcohol are added to an oil phase pot, stirred, and heated to 81°C-83°C. The mixture is kept warm and stirred until all solid components are completely melted, resulting in a homogeneous and transparent oil phase. Glycerin and deionized water are added to an aqueous phase pot, heated to 79°C-81°C, and stirred until homogeneous, resulting in an aqueous phase.

[0028] S2 Oil-Water Initial Mixing: Maintain the oil phase temperature at 81℃ and the water phase temperature at 80℃, controlling the temperature difference between the two phases within 2℃. The stirring speed of the agitator is 500 rpm. The water phase is added to the oil phase through a dropping device, controlling the addition time to be 3 minutes, forming a preliminary water-in-oil emulsion.

[0029] S3 Homogenization and Refinement: Transfer the colostrum obtained in step S2 to a homogenizer and maintain the temperature at 82℃. Start the homogenizer and set the rotation speed to 3000 rpm to perform high-speed shearing treatment on the colostrum for 8 minutes to obtain a fine homogenized emulsion with uniform particle size distribution.

[0030] S4 Cooling and Stirring with Wax Crystal Formation: Transfer the homogenized emulsion to a cooling reactor equipped with a wall-scraping stirrer, and set the stirring speed to 300 rpm. Slowly cool at a rate of 1℃ / min. When the temperature drops to 60℃, add 0.5 parts of pre-weighed acetyl hexapeptide-8, 0.2 parts of phenoxyethanol, and 0.5 parts of food flavoring. Maintain stirring within the temperature range of 58-62℃ for 10 minutes to promote full crystallization of the wax and form a stable semi-paste structure.

[0031] S5 Filling and Cooling: Continue cooling to 45℃ at a rate of 0.8℃ / min. Connect the cooling reactor and turn on the vacuum pump for degassing treatment, setting the vacuum degree to -0.09MPa and the treatment time to 3min. Then, vacuum filling is performed at 42℃. After filling, the product is naturally cooled to room temperature to obtain a high-hardness wax-based emulsion product.

[0032] Example 2: This example describes the preparation of a moisturizing wax-based emulsion for use in skin creams and lotions. The specific steps are as follows: S1 Raw material preparation and pretreatment: Weigh out 6 parts by weight of candelilla wax, 4 parts by weight of microcrystalline wax, 20 parts by weight of triglyceride decanoate, 10 parts by weight of isononyl isononanoate, 3 parts by weight of glyceryl stearate, 1 part by weight of behenol, 10 parts by weight of 1,3-propanediol, 3 parts by weight of panthenol, and 28 parts by weight of deionized water.

[0033] Candelilla wax, microcrystalline wax, caprylic / capric triglyceride, isononyl isononanoate, glyceryl stearate, and behenol are added to an oil phase pot and heated to 83°C-85°C. The mixture is stirred until completely melted and homogenized to obtain the oil phase. 1,3-propanediol, panthenol, and deionized water are added to an aqueous phase pot and heated to 81°C-83°C. The mixture is stirred until dissolved and homogeneous to obtain the aqueous phase.

[0034] S2 Oil-Water Initial Mixing: Maintain the oil phase temperature at 83℃ and the water phase temperature at 81℃, with the temperature difference controlled within 2℃. The stirring device is set to a stirring speed of 600 rpm. The water phase is added to the oil phase through a dripping device, with the addition time controlled at 4 minutes, to form a water-in-oil primary emulsion.

[0035] S3 Homogenization and Refinement: The obtained water-infused colostrum is introduced into a homogenizer, the temperature is maintained at 84℃, the homogenizer is started, the speed is set to 3000 rpm, and the colostrum is subjected to high-speed shearing treatment for 6 minutes to obtain a fine homogenized emulsion with uniform particle size distribution.

[0036] S4 Cooling and Stirring with Wax Crystal Formation: Transfer the homogenized emulsion to a cooling reactor equipped with a wall-scraping agitator. Turn on the agitator and set the speed to 350 rpm. Cool to 59°C at a rate of 1°C / min. Add 0.5 parts of pre-weighed sodium hyaluronate, 0.2 parts of preservative, and 0.5 parts of fragrance. Continue stirring within the range of 58°C-62°C for 12 minutes to allow the wax to form a fine crystalline structure and a stable semi-paste structure.

[0037] S5 Filling and Cooling: Cool to 44℃ at a rate of 0.5℃ / min, and degas for 4 minutes under a vacuum of -0.1MPa. Fill at 43℃, and allow to cool to room temperature to obtain the moisturizing skin cream.

[0038] Comparative Example 1: This comparative example uses a traditional wax-based emulsification process, without distinguishing between high and low melting point waxes. The specific steps are as follows: Raw material preparation: Weigh out 12 parts beeswax, 25 parts isononyl isononanoate, 5 parts glyceryl stearate, 1.5 parts cetearyl alcohol, 8 parts glycerin, and 25 parts deionized water by weight.

[0039] Emulsification: The oil phase raw materials are mixed and heated to 90°C, and the water phase is heated to 90°C. Under high-speed stirring at 1000 rpm, the water phase is quickly poured into the oil phase, and then cooled to 70°C.

[0040] Homogenization and cooling: Process using a homogenizer at 4000 rpm for 3 minutes. Then turn off the homogenizer and allow to cool naturally to 45°C. Add heat-sensitive ingredients and preservatives, fill into containers, and cool to room temperature.

[0041] Performance testing: The finished products obtained from the three embodiments and Comparative Example 1 were subjected to the following performance tests. Specific data can be found in [the relevant documentation]. Figure 2 .

[0042] 1. Stability Testing: Centrifugation stability: Take an appropriate amount of sample and place it in a centrifuge tube. Centrifuge at 3000 rpm for 30 minutes and observe whether the sample shows stratification, oil-water separation or precipitation. Thermal cycling stability: The sample was placed in an environment of -15℃ (24h) and 40℃ (24h) respectively, and cycled 5 times. The changes in the appearance of the paste (oil seepage, powdering, deformation, etc.) were observed.

[0043] Test results are as follows Figure 2 As shown in the results analysis, Examples 1 and 2 of this invention, through the use of high and low melting point wax blending and homogenization refining treatment, stabilized the entire emulsion system and created a dense wax crystal network structure, thus exhibiting excellent weather resistance. Comparative Example 1, due to the use of a single wax and the lack of homogenization refining, had poor system stability and was prone to oil phase precipitation at high temperatures.

[0044] 2. Microstructure observation: Test method: Take the cured sample and observe the morphology of the wax crystals using a polarizing microscope (PLM) at a magnification of 200x.

[0045] Test results are as follows Figure 2 As shown in the results analysis, the present invention, through scraping and stirring along the wall and cooling at a stable rate of 0.5℃ / min-2℃ / min, causes the wax to form fine and regular crystals, resulting in a delicate paste. This not only avoids the grainy feel and skin-pulling sensation produced when applying products prepared by traditional processes, but also improves the smoothness, delicacy, and gloss of the product while maintaining the hardness of the paste.

[0046] Comparative Example 1 used natural cooling, but the cooling rate was uncontrollable, which caused the wax to form crystals of inconsistent sizes and agglomerate, directly affecting the particle size of the entire product.

[0047] The above description is merely a preferred embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

[0048] Furthermore, the technical solutions of the various embodiments of the present invention can be combined with each other, but only if they are feasible for those skilled in the art. If the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by the present invention.

[0049] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the appended claims.

Claims

1. A wax-based emulsification method, characterized in that, Includes the following steps: S1 Raw Material Preparation and Pretreatment: Weigh out 8-20 parts by weight of wax-based raw material, 15-35 parts of liquid oil, 2-8 parts of nonionic emulsifier, 0.5-3 parts of additives, 5-15 parts of polyol, and 20-30 parts of deionized water. The wax-based raw material, liquid oil, nonionic emulsifier and additives are added to an oil phase pot, heated to 80℃-85℃, and stirred until completely melted to obtain an oil phase; then the polyol and deionized water are added to an aqueous phase pot, heated to 78℃-83℃, and stirred evenly to obtain an aqueous phase; S2 Oil-Water Initial Mixing: Controlling the temperature difference between the oil phase and the water phase to within 2°C, the water phase is added to the oil phase under stirring conditions to form a water-in-oil primary emulsion; S3 Homogenization and Refinement: Pour the above water-in-oil pre-emulsion into a homogenizer and perform high-speed shearing on the obtained water-in-oil pre-emulsion at a speed of 2500rpm-3500rpm for 5min-10min to obtain a fine homogenized emulsion. S4 Cooling and Stirring and Wax Crystal Formation: The homogenized emulsion obtained above is transferred to a cooling reaction vessel equipped with a wall-scraping stirring device. Stir at low speed and slowly cool to 58℃-62℃ at a rate of 0.5℃ / min-2℃ / min. Add 0.1-0.5 parts of heat-sensitive ingredients, 0.2-0.2 parts of preservatives and 0.5-2 parts of fragrance, and maintain stirring within this temperature range for 8min-15min to allow the wax to crystallize and precipitate, forming a semi-paste structure. S5 Filling and Cooling: Continue cooling at a rate of 0.5℃ / min-1℃ / min to 43℃-47℃, then perform vacuum degassing, and fill at 40℃-45℃. Cool to room temperature to obtain the wax-based emulsion product.

2. The wax-based emulsification method according to claim 1, characterized in that, In step S1: the wax base material is composed of high melting point wax and low melting point wax. The high melting point wax is one or two of carnauba wax and candelilla wax, and the low melting point wax is beeswax or microcrystalline wax.

3. The wax-based emulsification method according to claim 1, characterized in that, In step S1: the additive is cetearyl alcohol or behenyl alcohol.

4. The wax-based emulsification method according to claim 1, characterized in that, In step S1: the HLB value of the nonionic emulsifier is between 8 and 12, and the nonionic emulsifier is one or more of cetearyl oleate, sorbitan oleate, and glyceryl stearate; the liquid oil is one or more of isononyl isononanoate, caprylic / capric triglyceride, and jojoba seed oil.

5. The wax-based emulsification method according to claim 1, characterized in that, In step S1: the polyol is one or more of glycerol, butanediol, 1,3-propanediol, and panthenol.

6. The wax-based emulsification method according to claim 1, characterized in that, In step S1: the heat-sensitive component is one or more of acetyl hexapeptide-8, sodium hyaluronate, nicotinamide, and plant extracts.

7. The wax-based emulsification method according to claim 1, characterized in that, The stirring speed in step S2 is 300 rpm-800 rpm; the time for adding the aqueous phase to the oil phase is controlled at 2 min-5 min to maintain uniform mixing.

8. The wax-based emulsification method according to claim 7, characterized in that, In step S3: the homogenizer is maintained at a temperature of 80℃-85℃.

9. The wax-based emulsification method according to claim 8, characterized in that, In step S4, the low-speed stirring speed is 250 rpm to 400 rpm, and the stirring temperature is maintained between 58℃ and 62℃ to stably control the crystallization rate and crystal morphology of the wax.

10. The wax-based emulsification method according to claim 9, characterized in that, The vacuum degree of vacuum degassing in step S5 is -0.06MPa to -0.9MPa, and the processing time is 2min to 5min, to remove air bubbles from the paste.

Images