Highly transparent fixing powder and preparation method and application thereof

Abstract

The application discloses a kind of high transparent setting powder and preparation method thereof.Preparation method is composed of the following steps: step one, filler is uniformly dispersed with colorant, and powder phase is obtained;Step two, emollient, thickening agent, film-forming agent, antioxidant, anti-allergic agent and emulsifier are mixed and homogenized, and oil phase is obtained;Step three, slowly pour the powder phase into the oil phase, and stir while pouring until the flow liquid without obvious particles;Step four, the liquid obtained in step three is homogenized;Step five, the liquid obtained in step four is poured into a mold or a package material to release and form, and a high transparent setting powder is obtained.The method has high production intensity, and has the advantages of efficient purification process, low cost, no need to use a large amount of organic solvents and resins, less waste, high product purity, etc., and has important value for promoting the application of high transparent setting powder, especially in cosmetics.

Description

Technical Field

[0001] This invention discloses a method for preparing a highly transparent setting powder cream, a self-assembled nanoemulsion, and also discloses the preparation method and application of the highly transparent setting powder cream, belonging to the field of daily chemical raw materials. Background Technology

[0002] In the cosmetics industry, setting powder creams typically appear as a mixture of powder and oil phases, used to provide a long-lasting makeup setting effect after makeup application. Traditional formulas often use high-coverage pigments such as titanium dioxide or a large amount of mineral fillers such as talc as the main solid components, combined with oil phase components such as emollients, thickeners, and film-forming agents. These cream products are prepared through processes such as heating, grinding, and homogenization, and are widely used in everyday makeup and professional makeup occasions to achieve functions such as oil absorption, shine adjustment, and makeup setting.

[0003] However, existing technologies of this kind generally have several shortcomings. First, due to the use of high-coverage titanium dioxide or a large amount of talc, the powder cream tends to form a heavy mask-like feel when applied, lacking transparency and making it difficult to achieve a light and natural "no-makeup" effect. Second, to enhance oil control, fillers with extremely high oil absorption values ​​are often added, leading to excessive absorption of moisture from the skin surface, resulting in dryness, peeling, or caking, significantly reducing the user experience. Third, traditional production processes generally require heat treatment, which can easily cause the loss of volatile components or the deactivation of active ingredients. Furthermore, the product is prone to cracking and shrinkage after cooling, increasing the complexity and cost of the process. Fourth, it is difficult to achieve uniform dispersion of powder in the oil phase, resulting in a rough surface or a grainy feel when applied, further affecting the longevity and comfort of the makeup. These shortcomings collectively indicate that existing setting powder creams still have significant shortcomings in meeting users' needs for a light and transparent finish, comfortable oil control, and simplified production processes. Summary of the Invention

[0004] To address the shortcomings of current methods, the first objective of this invention is to provide a method for preparing a highly transparent setting powder. This method boasts high production intensity and advantages such as efficient purification processes, low cost, no need for large amounts of organic solvents and resins, minimal waste, and high product purity. It is of significant value in promoting the application of highly transparent setting powders, especially in cosmetics.

[0005] To achieve the above objectives, the specific technical solution is as follows:

[0006] A method for preparing a highly transparent setting powder cream comprises the following steps:

[0007] Step 1: Disperse the filler and colorant evenly to obtain a powder phase;

[0008] Step 2: Mix and homogenize the emollient, thickener, film-forming agent, antioxidant, anti-allergen, and emulsifier to obtain the oil phase;

[0009] Step 3: Slowly pour the powder phase into the oil phase while stirring until a smooth, flowing liquid without obvious particles is formed.

[0010] Step 4: Homogenize the liquid obtained in Step 3;

[0011] Step 5: Pour the liquid obtained in Step 4 into a mold or packaging material to demold and shape, and you will get a highly transparent setting powder.

[0012] Furthermore, the process of dispersing and homogenizing the filler in step one is as follows: the filler is added to a mixing pot and dispersed twice at 3000 rpm, each time for 30-60 seconds, to obtain a powder phase.

[0013] Furthermore, the mixing and homogenizing process parameters in step two are as follows: using a homogenizer to process the mixture at a rotation speed of 1000~5000 rpm for 10~15 minutes.

[0014] Furthermore, the specific process of stirring in the mixing pot in step three is as follows: slowly stirring with a stirrer at a speed of 50~300 rpm.

[0015] Furthermore, the homogenization process in step four is as follows: after grinding with a three-roll mill 1 to 2 times, stir with a stirrer at a speed of 200 to 500 rpm for 10 to 15 minutes.

[0016] Furthermore, the homogenization process in step four is as follows: using a homogenizer, homogenizing at a speed of 1000~5000 rpm for 30~45 minutes.

[0017] Furthermore, the demolding process in step five is as follows: the powder is placed in a powder press and the pressure of the powder press is adjusted to 0.1~5kg, and it is extruded 1~2 times.

[0018] The second technical solution provided by the present invention is: a high-transparency setting powder cream, prepared according to the above preparation method, wherein the high-transparency setting powder cream is composed of fillers, colorants, emollients, thickeners, film-forming agents, antioxidants, anti-allergens and emulsifiers.

[0019] Further, the filler is polymethylsilsesquioxane, vinyl polydimethylsiloxane / polymethylsiloxane-silsesquioxane crosspolymer, or silica; the colorant is one or more of iron oxide pigments or plant pigments; and the emollient is polydimethylsiloxane, isononyl isononanoate, octyl polymethylsiloxane, C12-15 alcohol benzoate, phenyl polytrimethylsiloxane, propylene glycol dioctyl ester / didecanoate, caprylic / capric triglyceride, or olive fruit oil.

[0020] Further, the thickener is a cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer composition, cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer, polydimethylsiloxane, hydrogenated polyisobutylene, or octyl polymethylsiloxane; the film-forming agent is polymethylsilsesquioxane; the antioxidant is tocopheryl acetate; the anti-sensitizing agent is bisabolol; and the emulsifier is cetyl PEG / PPG~10 / 1 polydimethylsiloxane.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] 1. In addition to the necessary pulverizer dispersion, this invention also uses a stirrer to agitate the powder at 50-300 rpm until it reaches a flowing liquid state. It incorporates a three-roll mill grinding process and a homogenizer homogenization process, resulting in more uniform powder dispersion, reducing uneven dispersion and agglomeration, and making the powder finer. Since the machines used are commonly found in cosmetics, no additional production equipment is needed (even skincare factories without cosmetic equipment can use a homogenizer for uniform dispersion and then use a capping machine). It is suitable for large-scale production, offering high production smoothness. Furthermore, the semi-finished material is in liquid form, allowing for direct quantitative filling and pressing into solid form, reducing labor costs and aligning with the company's cost reduction and efficiency improvement goals.

[0023] 2. This invention does not require baking or freeze-drying processes (compared to baked powder cakes), nor does it require heating treatment. After grinding at room temperature (1-2 times is sufficient) or homogenization, it can be directly pressed into shape (pressure 0.1-5kg, pressing time 1s, pressing times 1-2 times is sufficient), reducing production time and energy costs by more than 50%.

[0024] 3. The emollients added in this patent (isononyl isononanoate, octyl polymethylsiloxane, C12-15 alcohol benzoate, phenyl polytrimethylsiloxane) have good compatibility, allowing for the inclusion of more non-silicone raw materials in the formulation, enriching the efficacy and ingredient composition of the formula and better meeting consumer needs. Furthermore, for ointments that are opaque due to impurities or different processing methods, the addition of these emollients greatly increases their compatibility with fillers (polymethylsilsesquioxane, vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosspolymer, silica), thus enhancing transparency and significantly increasing the range of raw materials that can be selected from different manufacturers, allowing formulators to flexibly choose different raw materials.

[0025] 4. This invention uses 35-55.2 parts of a composition of polymethylsilsesquioxane, vinyl polydimethylsiloxane / polymethylsilsesquioxane crosslinked polymer, and cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer. It has a strong soft-focus effect, provides a natural matte finish, and allows for setting makeup with very little powder, resulting in a more natural makeup look. See details for specific effects. Figure 1 and Figure 2 .

[0026] 5. The national standard for the maximum usage of polymethylsilsesquioxane in this invention is 55.2%. Therefore, in order to make it flowable and compressible, 10-15 mg of silica (with an oil absorption value ≤250 ml / 100 g) was added. When the silica particle size is less than 10 mg, it will be difficult to make the formula flowable. When the silica particle size is greater than 15 mg, the resulting cream will have a certain grainy texture, and the skin feel will be worse.

[0027] 6. The polydimethylsiloxane in this patent can be a small amount of volatile (0-5 parts), which can be added according to the customer's requirements for the dryness of the product. No additional baking process is required, and it can be left to stand at room temperature for 1-6 hours.

[0028] 7. This invention uses 30-45 parts of emollient to make it appear as a paste, and the powder has a brief oily feel, giving the powder a "paste to powder" effect and enhancing the user experience. Attached Figure Description

[0029] Figure 1 A diagram of the user's skin condition before using this composition product;

[0030] Figure 2 This is a diagram showing the skin condition of a user after using this composition product. Detailed Implementation

[0031] The claims of the present invention will be further described in detail below with reference to specific embodiments, but this does not constitute any limitation on the present invention. Any limited modifications made by any person within the scope of protection of the claims of the present invention are still within the scope of protection of the claims of the present invention.

[0032] Example 1

[0033] Step 1: Disperse 55.2g of polymethylsilsesquioxane, 0.5g of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer and 2.6g of silica twice at room temperature using a pulverizer, each time for 5 seconds, to obtain a powder phase;

[0034] Step 2: Homogenize 30.946g of polydimethylsiloxane, 0.3g of polymethylsilsesquioxane, 1g of isononyl isononanoate, 1g of octyl polymethylsiloxane, 1g of C12-15 alcohol benzoate, 1g of phenyl polytrimethylsiloxane, 0.3g of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 6g of cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer composition, 0.1g of bisabolol, 0.001g of caprylic / capric triglyceride, 0.001g of olive (Olea europaea) fruit oil, 0.001g of propylene glycol dicaprylate / dicaprylate, and 0.001g of tocopheryl acetate at 2000 rpm for 12 minutes at room temperature. Then add 0.05g of (daily use) fragrance and stir for 2 minutes to obtain the oil phase.

[0035] Step 3: Add the powder phase from Step 1 to the oil phase from Step 2, and stir with a stirrer at 200 rpm until a free-flowing liquid with no obvious particles is formed.

[0036] Step 4: Grind the liquid obtained in Step 3 twice using a three-roll mill, and then stir it with a stirrer at 300 rpm for 12 minutes to obtain a finer and clearer flowable liquid.

[0037] Step 5: Pour the liquid from Step 4 into the mold or packaging material according to the specified mass fraction, put it into the powder press and adjust the pressure of the powder press to 0.2 kg, the holding time to 1 second, press twice, demold and shape to obtain a highly transparent setting powder cream.

[0038] Example 2

[0039] This embodiment refers to the preparation steps of Example 1, except that 28.946g of polydimethylsiloxane and 3g of volatile polydimethylsiloxane are used, while other conditions remain unchanged.

[0040] Example 3

[0041] This embodiment refers to the preparation steps of Example 1, except that 25.946g of polymethylsilsesquioxane and 5g of volatile polydimethylsiloxane are used, while other conditions remain unchanged.

[0042] Example 4

[0043] This embodiment refers to the preparation steps of Example 1, except that 3.6g of silica, 3g of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer, 32.946g of polydimethylsiloxane, and 0.5g of cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer composition remain unchanged.

[0044] Example 5

[0045] This embodiment refers to the preparation steps of Example 1, except that 52.2g of polymethylsilsesquioxane, 5g of vinyl polydimethylsiloxane / polymethylsilsesquioxane crosslinked polymer, 27.446g of polydimethylsiloxane, and 8g of cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer composition remain unchanged.

[0046] Comparative Example 1

[0047] This comparative example follows the same preparation steps as Example 1, except that it uses 22.946g of polydimethylsiloxane and 8g of volatile polydimethylsiloxane, while other conditions remain unchanged.

[0048] Comparative Example 2

[0049] This comparative example follows the preparation steps of Example 2, except that the raw materials differ in that 23.946g of polydimethylsiloxane and 10g of the cetearyl-based polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer composition are used. After mixing in step three, the material is in a semi-solid state. In step four, the semi-solid material obtained in step three is ground four times using a three-roll mill. In step five, the material from step four is poured into a mold or packaging material according to a specific mass fraction, placed in a powder press, and the pressure of the powder press is adjusted to 0.5kg. The pressure holding time is 2 seconds, and the material is extruded twice. After demolding, a high-transparency setting powder cream is obtained, with other conditions remaining unchanged.

[0050] Comparative Example 3

[0051] This comparative example follows the preparation steps of Example 1, except that 41.6g of polymethylsilsesquioxane, 12g of silica, and 5g of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer are used, while other conditions remain unchanged.

[0052] Comparative Example 4

[0053] This comparative example follows the same preparation steps as Example 1, except that it uses 30g of polymethylsilsesquioxane and 27.8g of silica, while other conditions remain unchanged.

[0054] To better demonstrate the technical solution provided in this application, the following testing experiments are presented:

[0055] Experiment 1: Accelerated stability test.

[0056] The prepared powder paste was subjected to a 3-month stability test under the following conditions: room temperature, light exposure (natural light), low temperature (-15℃), low temperature (-10℃), high temperature (45℃), high temperature (55℃), high and low temperature cycling (45℃ / 15℃, cycled once every 6 days, tested for one month), sea transport (5~55℃, tested for one month), and refrigeration (5℃). The stability test results are as follows:

[0057] Table 1. Stability Test Results

[0058]

[0059] Table 1 shows that Examples 1-5 and Comparative Example 2 showed no significant abnormalities in stability over 3 months. Comparative Example 1 showed cloudiness and white spots in all samples during the 3-month stability test. Comparative Example 3 showed cracks in the material during low-temperature (-15℃) and high-low temperature cycling tests. Comparative Example 4 showed cracks in both low-temperature and cycling tests. The comparative examples indicate that volatile polydimethylsiloxane > 5 parts, polymethylsilsesquioxane < 35 parts, and silica > 10 parts are prone to stability issues. It is recommended that the addition of volatile polydimethylsiloxane ≤ 5 parts, polymethylsilsesquioxane ≥ 35 parts, and silica ≤ 10 parts be regulated. Although Comparative Example 2 showed no stability issues, its process was more complex and production efficiency was slower.

[0060] Experiment 2: Drop Stability Test

[0061] This test is a drop test of Examples 1-5 and Comparative Examples 1-4. Specifically, for each example, 10 products were selected and subjected to three 50cm drops, with the results of each drop recorded. See Table 2 below for details.

[0062] Table 2. Drop Stability Test Results

[0063]

[0064] As shown in Table 2, all drop tests of the embodiments passed, proving that they have strong drop resistance and are not easily damaged during normal carrying.

[0065] Experiment 3: Microbial Detection Experiment

[0066] The finished product prepared in Example 1 was used as the test sample in this experiment. The specific test method was in accordance with the "Cosmetic Safety Technical Specification". The test items included total bacterial count (≤500 CFU / g), total mold and yeast count (≤100 CFU / g), thermotolerant coliforms (not detectable), Pseudomonas aeruginosa (not detectable) and Staphylococcus aureus (not detectable). The test results are shown in Table 3.

[0067] Table 3. Microbiological Detection Results

[0068]

[0069] As shown in Table 3, the total bacterial count and the total count of mold and yeast are all less than 10 CFU / g, which is far below the implementation standard. Thermotolerant coliforms, Pseudomonas aeruginosa, and Staphylococcus aureus were not detected. Therefore, the products provided by this invention patent meet the microbiological indicators and the hygiene quality of the products is qualified and compliant.

[0070] Experiment 4: Heavy Metal Detection

[0071] The finished product prepared in Example 1 was used as the test sample in this experiment. The specific test method was in accordance with the "Cosmetic Safety Technical Specification". The test items included arsenic (≤2mg / kg), cadmium (≤5mg / kg), lead (≤10mg / kg), and mercury (≤1mg / kg). The test results are shown in Table 4 below.

[0072] Table 4. Heavy Metal Detection Results

[0073]

[0074] As shown in Table 4, arsenic, cadmium, and lead were not detected. Comparative Example 4 showed a mercury content of 0.006 mg / kg, far below the standard requirement. Therefore, the products of this invention comply with national regulations on the content of heavy metals in cosmetics.

[0075] Experiment 5: Product Soft Focus Effect and Smoothness Test

[0076] Experimental Methods: The use test was conducted by 40 evaluators (aged 18-65, 9 males and 31 females in one group). The evaluators evaluated the product immediately after applying it to the face and again 2 hours later.

[0077] Table 5. Comparison of Examples and Commercially Available Examples

[0078]

[0079] As shown in Table 5, the soft-focus effect, makeup retention, and smoothness of the examples are better than those of ordinary commercially available pressed powders, giving them a certain advantage among setting products and enhancing the user experience. Comparative Example 4 had the best smoothness rating, but it also showed cracks in low-temperature and cycling tests, indicating poor stability.

[0080] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a highly transparent setting powder, characterized in that, It consists of the following steps: Step 1: Disperse the filler and colorant evenly to obtain a powder phase; Step 2: Mix and homogenize the emollient, thickener, film-forming agent, antioxidant, anti-allergen, and emulsifier to obtain the oil phase; Step 3: Slowly pour the powder phase into the oil phase while stirring until a smooth, flowing liquid without obvious particles is formed. Step 4: Homogenize the liquid obtained in Step 3; Step 5: Pour the liquid obtained in Step 4 into a mold or packaging material to demold and shape, and you will get a highly transparent setting powder.

2. The preparation method according to claim 1, characterized in that: The process of dispersing and homogenizing the filler in step one is as follows: the filler is added to a mixing pot and dispersed twice at 3000 rpm, each time for 30-60 seconds, to obtain a powder phase.

3. The preparation method according to claim 1, characterized in that: In step two, the mixing and homogenizing process parameters are as follows: use a homogenizer to process the mixture at a rotation speed of 1000~5000 rpm for 10~15 minutes.

4. The preparation method according to claim 1, characterized in that: The specific process of stirring in step three is as follows: use a stirrer to stir at a speed of 50 to 300 rpm.

5. The preparation method according to claim 1, characterized in that: The homogenization process in step four is as follows: after grinding with a three-roll mill 1 to 2 times, stir with a stirrer at a speed of 200 to 500 rpm for 10 to 15 minutes.

6. The preparation method according to claim 1, characterized in that: The homogenization process in step four is as follows: use a homogenizer at a speed of 1000~5000 rpm for 10~15 minutes.

7. The preparation method according to claim 1, characterized in that: The demolding process in step five is as follows: put it into the powder press and adjust the pressure of the powder press to 0.1~5kg, and press it 1~2 times.

8. A highly transparent setting powder, characterized in that, The high-transparency setting powder cream is prepared according to any one of claims 1 to 7, and comprises 35-60 parts of filler, 0-0.001 parts of colorant, 30-45 parts of emollient, 0-8 parts of thickener, 0-3 parts of film-forming agent, 0-0.1 parts of antioxidant, 0-0.1 parts of anti-allergen and 0-0.3 parts of emulsifier.

9. The high-transparency setting powder cream according to claim 8, characterized in that, The filler is polymethylsilsesquioxane, vinyl polydimethylsiloxane / polymethylsiloxane-silsesquioxane crosspolymer, or silica; the colorant is one or more of iron oxide pigments or plant pigments; and the emollient is polydimethylsiloxane, isononyl isononanoate, octyl polymethylsiloxane, C12-15 benzoyl alcohol, phenyl polytrimethylsiloxane, propylene glycol dioctyl ester / didecanoate, caprylic / capric triglyceride, or olive fruit oil.

10. The high-transparency setting powder cream according to claim 8, characterized in that, The thickener is a cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer composition, cetearyl polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer, polydimethylsiloxane, hydrogenated polyisobutylene, and octyl polymethylsiloxane; the film-forming agent is polymethylsilsesquioxane; the antioxidant is tocopheryl acetate; the anti-sensitizing agent is bisabolol; and the emulsifier is cetyl PEG / PPG~10 / 1 polydimethylsiloxane.

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