A calcium stearate gel composition, its preparation method, and its application
By preparing calcium stearate gel, its amphiphilic binary structure is used to form a stable three-dimensional network structure, which solves the problem of poor thickening and dispersion of calcium stearate powder in cosmetics, and improves the stability and moisturizing performance of cosmetics.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- GUANGZHOU CADLIN COSMETICS
- Filing Date
- 2026-03-25
- Publication Date
- 2026-06-02
AI Technical Summary
Calcium stearate powder has poor thickening and dispersing properties in cosmetic systems such as creams and lotions, resulting in a rough texture and uneven dispersion, which limits its application in the cosmetic field.
By mixing calcium stearate powder with Span emulsifiers and squalane or cetyl ethylhexanoate, heating and homogenizing, and then cooling, calcium stearate gel is formed. The amphiphilic binary structure of calcium stearate forms a stable three-dimensional network structure, which is then added to cosmetics as a thickener.
It improves the stability and smoothness of cosmetics, enhances the skin barrier function, reduces skin moisture loss, and improves the moisturizing performance of cosmetics.
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Figure CN122123893A_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the field of cosmetic raw material technology, and in particular relates to a calcium stearate gel composition, its preparation method and application. Background Technology
[0002] Calcium stearate, chemically known as calcium stearate, is a white powdery metallic soap. It is insoluble in water, cold ethanol, and ether, but soluble in hot benzene, benzene, and turpentine, and slightly soluble in hot ethanol and ether. This substance slowly decomposes at around 400°C, is flammable, and decomposes into stearic acid and the corresponding calcium salt in the presence of strong acids. As a multifunctional metallic soap compound, it can be used as a heat stabilizer and processing aid for resins, as well as a dispersant in oil-based coatings. In the cosmetics industry, it can be used in powder products such as foundation and eyeshadow, effectively improving the spreadability and compressibility of powders, giving products a smooth skin feel, and making them easier to adhere to the skin. Therefore, calcium stearate can be widely used in many fields such as plastics, coatings, and daily chemical industries.
[0003] However, the hydrophobic properties of calcium stearate powder result in poor thickening and dispersing properties in cosmetic systems such as creams, easily leading to defects such as rough texture and uneven dispersion; therefore, the direct use of calcium stearate powder in cosmetics such as creams is limited; calcium stearate, as a typical long-chain fatty acid metal soap, has the molecular structural formula (C... 17 H 35 (COO)2Ca naturally possesses an amphiphilic binary structure, including a nonpolar aliphatic chain end and a polar calcium carboxylate head end. It has ionic bonding characteristics and coordination ability, and has the potential to form a gel structure. Therefore, it is necessary to modify existing calcium stearate powder based on the characteristics of calcium stearate to improve the performance of calcium stearate powder and expand its application range in the cosmetic field. Summary of the Invention
[0004] In view of this, this application provides a calcium stearate gel composition, its preparation method, and its application, to solve the technical problem of low performance of calcium stearate in the prior art.
[0005] The first aspect of this application provides a method for preparing a calcium stearate gel composition, comprising the following steps:
[0006] Span emulsifiers, squalane, or cetyl ethylhexanoate are heated and homogenized to obtain an oil phase mixture. The low-branched long carbon chain skeletons of squalane or cetyl ethylhexanoate are highly similar to the hydrophobic long carbon chains of calcium stearate at the molecular level, with small steric hindrance. Calcium stearate can be more uniformly dispersed in these oils to form a stable gel product with high hardness.
[0007] Calcium stearate powder was added to an oil phase mixture and heated to melt. The mixture was then cooled to room temperature to obtain a calcium stearate gel composition.
[0008] Preferably, the Span emulsifier is selected from at least one of sorbitan sesquioleate, sorbitan oleate, sorbitan isostearate, sorbitan stearate, sorbitan lauryl ester, sorbitan trioleate, sorbitan palmitate, and sorbitan tristearate.
[0009] Preferably, the heating and homogenization temperature is 50℃~200℃, the rotation speed is 500rpm~10000rpm, and the time is 1min~15min; and the heating and homogenization temperature value can be selected from any positive integer between 50 and 200, the rotation speed value can be selected from any positive integer between 500 and 10000, and the time value can be selected from any positive integer between 1 and 15.
[0010] Preferably, the heating and melting temperature is 110℃~170℃, and the time is 5min~30min; and the heating and melting temperature value can be selected from any positive integer between 110 and 170, such as 110, 140, etc., and the time value can be selected from any positive integer between 5 and 30.
[0011] Preferably, the rotation speed during the heating and melting process is 500 rpm to 10000 rpm, and the rotation speed value can be selected from any positive integer between 500 and 10000.
[0012] Preferably, the homogenization temperature before the heating and melting process is 50℃~200℃, the rotation speed is 500rpm~10000rpm, and the time is 1min~15min; and the heating and homogenization temperature can be selected from any positive integer between 50 and 200, the rotation speed can be selected from any positive integer between 500 and 10000, and the time can be selected from any positive integer between 1 and 15.
[0013] Preferably, the cooling to room temperature process is: cooling to room temperature under conditions of 0℃~30℃, and the temperature value can be selected from any positive integer between 0 and 30.
[0014] Preferably, the mass ratio of the Span emulsifier to squalane or cetyl ethylhexanoate is 0.01 to 0.5:1, and more preferably 0.1 to 0.2:1.
[0015] The calcium stearate powder is mixed with the oil phase in a mass ratio of 0.01 to 0.5:1, and further in a mass ratio of 0.05 to 0.4:1 and 0.1 to 0.3:1.
[0016] The second aspect of this application provides a calcium stearate gel composition, which is prepared by the method for preparing a calcium stearate gel composition as described in the first aspect.
[0017] The third aspect of this application provides the use of the calcium stearate gel composition described in the second aspect in the preparation of cosmetics.
[0018] Preferably, the cosmetic is selected from emulsions, creams, ointments, or gels.
[0019] The fourth aspect of this application provides a cream comprising the calcium stearate gel composition described in the second aspect.
[0020] Preferably, the cream further includes:
[0021] Oil phases of PEG-10 polydimethylsiloxane, polydimethylsiloxane, polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, etc.
[0022] Aqueous phases include polyethylene, butanediol dioctanoic acid / didecanoate, deionized water, glycerol, 1,2-pentanediol, butanediol, magnesium sulfate, phenoxyethanol, ethylhexylglycerol, and polyethylene glycol-8.
[0023] Compared with the prior art, the method for preparing a calcium stearate gel composition provided in this application has at least the following beneficial effects:
[0024] 1. In the preparation method of the calcium stearate gel composition provided in this application, calcium stearate powder is added to a mixed oil phase system of Span emulsifier and squalane or cetyl ethylhexanoate and heated to melt to form a uniform and stable calcium stearate melt system. During the cooling process, a gel-like product with a stable three-dimensional network structure is formed by taking advantage of the amphiphilic binary structure of calcium stearate molecules. When added as a thickener to creams and other cosmetics, it can improve the stability of creams and other cosmetics, make them smooth to apply, form a high-quality skin barrier, improve moisturizing performance and reduce skin moisture loss.
[0025] 2. In the preparation method of the calcium stearate gel composition provided in this application, by selecting oils with different structures, such as cetyl ethylhexanoate and other thermally stable saturated oils with long carbon chain skeletons, the steric hindrance of the non-polar fatty chain ends of calcium stearate is reduced, forming a more stable thickener, which has a better thickening effect on creams and other cosmetics, and forms a higher quality skin barrier. Attached Figure Description
[0026] To more clearly illustrate the technical solutions in the specific embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0027] Figure 1 A photograph of the calcium stearate gel composition prepared by the method provided in this application. Detailed Implementation
[0028] This application provides a calcium stearate gel composition, its preparation method, and its application, which addresses the technical problem of low performance of calcium stearate in the prior art.
[0029] The technical solutions of this application will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.
[0030] Example 1
[0031] This embodiment provides a method for preparing a calcium stearate gel composition, the method including a raw material weighing step, an oil phase mixture preparation step, and a calcium stearate gel preparation step.
[0032] The steps for weighing raw materials include:
[0033] Weigh calcium stearate powder, sorbitan sesquioleate (SPAN 83), and squalane according to a mass ratio of 15:10:75.
[0034] The preparation steps of the oil phase mixture include:
[0035] Weigh out sorbitan sesquioleate (SPAN83) and squalane, mix and heat to 80°C, and homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0036] The preparation steps of calcium stearate gel include:
[0037] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0038] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0039] The mixture was then placed in 5°C cold water to cool to room temperature, while stirring at 80 rpm to obtain the calcium stearate gel composition. (See image below.) Figure 1 As shown.
[0040] Example 2
[0041] This embodiment provides a method for preparing a calcium stearate gel composition. The difference from Example 1 is that the squalane in the oil is adjusted. The preparation method includes a weighing step of raw materials, a preparation step of oil phase mixture, and a preparation step of calcium stearate gel.
[0042] The steps for weighing raw materials include:
[0043] Weigh calcium stearate powder, sorbitan sesquioleate (SPAN83), and cetyl ethylhexanoate according to a mass ratio of 15:10:75.
[0044] The preparation steps of the oil phase mixture include:
[0045] Weigh out sorbitan sesquioleate (SPAN83) and cetyl ethylhexanoate, mix and heat to 80°C, then homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0046] The preparation steps of calcium stearate gel include:
[0047] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0048] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0049] The mixture was then placed in 5°C cold water to cool to room temperature, and cooled while stirring at a speed of 80 rpm to obtain the calcium stearate gel composition.
[0050] Example 3
[0051] This embodiment provides a method for preparing a calcium stearate gel composition. The difference from Example 1 is that the emulsifier sorbitan sesquioleate is adjusted. The preparation method includes a raw material weighing step, an oil phase mixture preparation step, and a calcium stearate gel preparation step.
[0052] The steps for weighing raw materials include:
[0053] Weigh calcium stearate powder, sorbitan isostearate (SPAN120), and squalane according to a mass ratio of 15:10:75.
[0054] The preparation steps of the oil phase mixture include:
[0055] Weigh out sorbitan isostearate (SPAN120) and squalane, mix and heat to 80°C, and homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0056] The preparation steps of calcium stearate gel include:
[0057] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0058] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0059] The mixture was then placed in 5°C cold water to cool to room temperature, and cooled while stirring at a speed of 80 rpm to obtain the calcium stearate gel composition.
[0060] Comparative Example 1
[0061] This comparative example provides a method for preparing a calcium stearate composition. The difference from Example 1 is that the squalane in the oil is adjusted. The preparation method includes the steps of weighing raw materials, preparing the oil phase mixture, and preparing the calcium stearate composition.
[0062] The steps for weighing raw materials include:
[0063] Weigh calcium stearate powder, sorbitan sesquioleate (SPAN83), and isononyl isononanoate according to a mass ratio of 15:10:75.
[0064] The preparation steps of the oil phase mixture include:
[0065] Weigh out sorbitan sesquioleate (SPAN83) and isononyl isononanoate, mix and heat to 80°C, then homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0066] The preparation steps of the calcium stearate composition include:
[0067] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0068] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0069] The mixture was then placed in 5°C cold water to cool to room temperature, and cooled while stirring at a speed of 80 rpm to obtain the calcium stearate composition.
[0070] Comparative Example 2
[0071] This comparative example provides a method for preparing a calcium stearate composition. The difference from Example 1 is that the squalane in the oil is adjusted. The preparation method includes the steps of weighing raw materials, preparing the oil phase mixture, and preparing the calcium stearate composition.
[0072] The steps for weighing raw materials include:
[0073] Weigh calcium stearate powder, sorbitan sesquioleate (SPAN83), and polydimethylsiloxane according to a mass ratio of 15:10:75.
[0074] The preparation steps of the oil phase mixture include:
[0075] Weigh out sorbitan sesquioleate (SPAN83) and polydimethylsiloxane, mix and heat to 80°C, and homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0076] The preparation steps of the calcium stearate composition include:
[0077] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0078] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0079] The mixture was then placed in 5°C cold water to cool to room temperature, and cooled while stirring at a speed of 80 rpm to obtain the calcium stearate composition.
[0080] Comparative Example 3
[0081] This comparative example provides a method for preparing a calcium stearate composition. The difference from Example 1 is that the emulsifier sorbitan sesquioleate is adjusted. The preparation method includes a raw material weighing step, an oil phase mixture preparation step, and a calcium stearate composition preparation step.
[0082] The steps for weighing raw materials include:
[0083] Weigh calcium stearate powder, polyglycerol-4 isostearate, and squalane according to a mass ratio of 15:10:75.
[0084] The preparation steps of the oil phase mixture include:
[0085] Weigh out polyglycerol-4 isostearate and squalane, mix and heat to 80°C, then homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0086] The preparation steps of the calcium stearate composition include:
[0087] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0088] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0089] The mixture was then placed in 5°C cold water to cool to room temperature, and cooled while stirring at a speed of 80 rpm to obtain the calcium stearate composition.
[0090] Comparative Example 4
[0091] This comparative example provides a method for preparing a calcium stearate composition. The difference from Example 1 is that the emulsifier sorbitan sesquioleate is adjusted. The preparation method includes a raw material weighing step, an oil phase mixture preparation step, and a calcium stearate composition preparation step.
[0092] The steps for weighing raw materials include:
[0093] Weigh calcium stearate powder, cetyl PEG / PPG-10 / 1 polydimethylsiloxane, and squalane according to a mass ratio of 15:10:75.
[0094] The preparation steps of the oil phase mixture include:
[0095] Weigh out cetyl PEG / PPG-10 / 1 polydimethylsiloxane and squalane, mix and heat to 80°C, and homogenize at 2000 rpm for 2 min to obtain a uniformly dispersed oil phase mixture.
[0096] The preparation steps of the calcium stearate composition include:
[0097] First, add the weighed calcium stearate powder to the oil phase mixture and homogenize it at 3000 rpm for 3 minutes at 80°C to ensure that the calcium stearate powder and the oil phase are evenly mixed.
[0098] Continue heating until the temperature reaches 120°C, until the system becomes translucent. Maintain this temperature and homogenize at 3000 rpm for 10 minutes.
[0099] The mixture was then placed in 5°C cold water to cool to room temperature, and cooled while stirring at a speed of 80 rpm to obtain the calcium stearate composition.
[0100] Example 4
[0101] To further investigate the performance of the calcium stearate gel composition provided in Example 1 of this application, this example provides a water-in-oil cream, the preparation process of which includes: weighing the raw materials and preparing the cream.
[0102] The steps for weighing raw materials include:
[0103] Weigh the following components according to the mass ratio of 4:2:18:5:1:1.5:4:0.5:3:45.3:7:1.5:5:1:0.4:0.8: calcium stearate gel composition provided in Example 1, PEG-10 polydimethylsiloxane, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, butanediol dioctanoic acid / didecanoic acid ester, deionized water, glycerin, 1,2-pentanediol, butanediol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio of 9:1), and polyethylene glycol-8.
[0104] The preparation steps of the cream include:
[0105] The calcium stearate gel composition provided in Example 1, PEG-10 polydimethylsiloxane, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, and butanediol dioctanoic acid / didecanoic acid ester were weighed as the oil phase, heated to 90°C to dissolve, and then homogenized at 3000 rpm for 2 min.
[0106] Weigh out deionized water, glycerin, 1,2-pentanediol, butylene glycol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio 9:1), and polyethylene glycol-8 as the aqueous phase. Heat to 75°C to dissolve. Slowly add the aqueous phase to the oil phase while stirring, and homogenize and emulsify at 6000 rpm for 5 minutes. Continue stirring and cool to room temperature to obtain a water-in-oil cream.
[0107] Comparative Example 5
[0108] To further investigate the performance of the calcium stearate gel composition provided in Example 1 of this application, this comparative example provides a water-in-oil cream, the preparation process of which includes: weighing the raw materials and preparing the cream.
[0109] The steps for weighing raw materials include:
[0110] Weigh the following components according to the mass ratio of 0.6:2:0.4:18:5:4:1.5:4:0.5:3:45.3:7:1.5:5:1:0.4:0.8: calcium stearate powder, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, butanediol dioctanoate / didecanoate, deionized water, glycerin, 1,2-pentanediol, butanediol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio of 9:1), and polyethylene glycol-8.
[0111] The preparation steps of the cream include:
[0112] The weighed calcium stearate powder, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, and butanediol dioctanoic acid / didecanoate were used as the oil phase and heated to 90°C to dissolve. The mixture was then homogenized at 3000 rpm for 2 min.
[0113] Weigh out deionized water, glycerin, 1,2-pentanediol, butylene glycol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio 9:1), and polyethylene glycol-8 as the aqueous phase. Heat to 75°C to dissolve. Slowly add the aqueous phase to the oil phase while stirring, and homogenize and emulsify at 6000 rpm for 5 minutes. Continue stirring and cool to room temperature to obtain a water-in-oil cream.
[0114] Comparative Example 6
[0115] To further investigate the performance of the calcium stearate gel composition provided in Example 1 of this application, this comparative example provides a water-in-oil cream, the preparation process of which includes: weighing the raw materials and preparing the cream.
[0116] The steps for weighing raw materials include:
[0117] Weigh the following components according to the mass ratio of magnesium stearate powder, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, butanediol dioctanoate / didecanoate, deionized water, glycerin, 1,2-pentanediol, butanediol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio of 9:1), and polyethylene glycol-8.
[0118] The preparation steps of the cream include:
[0119] The weighed magnesium stearate powder, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, and butanediol dioctanoic acid / didecanoate were used as the oil phase and heated to 90°C to dissolve. The mixture was then homogenized at 3000 rpm for 2 min.
[0120] Weigh out deionized water, glycerin, 1,2-pentanediol, butylene glycol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio 9:1), and polyethylene glycol-8 as the aqueous phase. Heat to 75°C to dissolve. Slowly add the aqueous phase to the oil phase while stirring, and homogenize and emulsify at 6000 rpm for 5 minutes. Continue stirring and cool to room temperature to obtain a water-in-oil cream.
[0121] Comparative Example 7
[0122] To further investigate the performance of the calcium stearate gel composition provided in Example 1 of this application, this comparative example provides a water-in-oil cream, the preparation process of which includes: weighing the raw materials and preparing the cream.
[0123] The steps for weighing raw materials include:
[0124] Weigh the following components according to the mass ratio of 0.6:2:0.4:18:5:4:1.5:4:0.5:3:45.3:7:1.5:5:1:0.4:0.8: Quaternary ammonium salt-18 bentonite, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, butanediol dioctanoic acid / didecanoate, deionized water, glycerin, 1,2-pentanediol, butanediol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio of 9:1), and polyethylene glycol-8.
[0125] The preparation steps of the cream include:
[0126] The weighed quaternary ammonium salt-18 bentonite, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, and butanediol dioctanoic acid / didecanoate were used as the oil phase and heated to 90°C to dissolve. The mixture was then homogenized at 3000 rpm for 2 min.
[0127] Weigh out deionized water, glycerin, 1,2-pentanediol, butylene glycol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio 9:1), and polyethylene glycol-8 as the aqueous phase. Heat to 75°C to dissolve. Slowly add the aqueous phase to the oil phase while stirring, and homogenize and emulsify at 6000 rpm for 5 minutes. Continue stirring and cool to room temperature to obtain a water-in-oil cream.
[0128] Comparative Example 8
[0129] To further investigate the performance of the calcium stearate gel composition provided in Example 1 of this application, this comparative example provides a water-in-oil cream, the preparation process of which includes: weighing the raw materials and preparing the cream.
[0130] The steps for weighing raw materials include:
[0131] Weigh the following components according to the mass ratio of 0.6:2:0.4:18:5:4:1.5:4:0.5:3:45.3:7:1.5:5:1:0.4:0.8: montmorillonite, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, butanediol dioctanoic acid / didecanoate, deionized water, glycerin, 1,2-pentanediol, butanediol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio of 9:1), and polyethylene glycol-8.
[0132] The preparation steps of the cream include:
[0133] The weighed montmorillonite, PEG-10 polydimethylsiloxane, sorbitan sesquioleate, polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, polydimethylsiloxane, squalane, C8-12 triglyceride, isohexadecane, polyethylene, and butanediol dioctanoic acid / didecanoate were used as the oil phase and heated to 90°C to dissolve. The mixture was then homogenized at 3000 rpm for 2 min.
[0134] Weigh out deionized water, glycerin, 1,2-pentanediol, butylene glycol, magnesium sulfate, phenoxyethanol / ethylhexylglycerin (phenoxyethanol:ethylhexylglycerin ratio 9:1), and polyethylene glycol-8 as the aqueous phase. Heat to 75°C to dissolve. Slowly add the aqueous phase to the oil phase while stirring, and homogenize and emulsify at 6000 rpm for 5 minutes. Continue stirring and cool to room temperature to obtain a water-in-oil cream.
[0135] Experimental Example 1
[0136] This experiment tested the performance of the calcium stearate gel compositions provided in Examples 1-3, the calcium stearate compositions provided in Comparative Examples 1-4, and the water-in-oil creams provided in Examples 4 and Comparative Examples 5-8.
[0137] In the performance tests, a Brookfield CT3 texture analyzer was used to test the hardness of the calcium stearate gel compositions provided in Examples 1-3 and the calcium stearate compositions provided in Comparative Examples 1-4 at 25°C. Centrifugal stability was tested by centrifuging at 3000 r / min for 30 min. Heat resistance was tested by incubating at 45°C for one week. Cold resistance was tested by incubating at -15°C for one week. The results are shown in Table 1.
[0138] In addition, the viscosity of the water-in-oil creams provided in Example 4 and Comparative Examples 5-8 was tested at 25°C using a Brookfield DV2T viscometer; the centrifugal stability of the water-in-oil creams provided in Example 4 and Comparative Examples 5-8 was tested by centrifuging at 3000 r / min for 30 min; the heat resistance stability of the water-in-oil creams provided in Example 4 and Comparative Examples 5-8 was tested by incubating at 45°C for one week using a constant temperature incubator; and the cold resistance stability of the water-in-oil creams provided in Example 4 and Comparative Examples 5-8 was tested by incubating at -15°C for one week using a refrigerator. The results are shown in Table 2.
[0139] Table 1: Performance test results of the calcium stearate gel compositions provided in Examples 1-3 and the calcium stearate compositions provided in Comparative Examples 1-4
[0140]
[0141] Table 2: Performance test results of the water-in-oil creams provided in Example 4 and Comparative Examples 5-8
[0142]
[0143] As shown in Table 1, the performance test results indicate that, compared with the calcium stearate compositions provided in Comparative Examples 1-4, the calcium stearate gel compositions provided in Examples 1-3 have a hardness between 881 and 1263 g, indicating that the calcium stearate gel compositions provided in Examples 1-3 are well-formed gels. Furthermore, they exhibit good centrifugal stability, heat resistance, and cold resistance; no stratification occurred after centrifugation at 3000 r / min for 30 min, storage at 45℃ for one week, and storage at -15℃ for one week. This demonstrates that the calcium stearate gel compositions provided in Examples 1-3 are structurally stable, cold-resistant, and heat-resistant stable gel products. This is because Span-type emulsifiers and squalane or cetyl ethylhexanoate are used as the molten oil phase of the calcium stearate powder. During the heating and melting process, the long-chain fatty acid portion of Span-type emulsifiers such as sorbitan sesquioleate reacts with the non-polar fatty chain ends of calcium stearate and the squalane or cetyl ethylhexanoate... Cetyl ethylhexanoate exhibits good compatibility, forming a uniform and stable calcium stearate melt system. During the cooling process after the calcium stearate melts at high temperature, the calcium stearate molecules, including the nonpolar aliphatic chain ends and the polar head ends of calcium carboxylate, begin to align as amphiphilic binary molecules. The nonpolar aliphatic chain ends combine with squalane or cetyl ethylhexanoate, while the polar head ends of calcium carboxylate aggregate to form reverse micelles and layered crystals. Through the bridging effect of calcium ions and the van der Waals forces between molecules, a gel-like product with a stable three-dimensional network structure is formed. The performance test results shown in Table 1 also show that, due to the use of squalane or cetyl ethylhexanoate as the oil in Examples 1 and 2, the structure of squalane is shown in Formula 1, and the structure of cetyl ethylhexanoate is shown in Formula 2. Both have long carbon chain skeleton structures, low branching, and small steric hindrance, resulting in a stable gel structure with high hardness when combined with calcium stearate.
[0144] Formula 1;
[0145] Equation 2.
[0146] As can be seen from the performance test results shown in Table 2, compared with the water-in-oil creams provided in Comparative Examples 5-8, the water-in-oil cream provided in Example 4 has a higher viscosity, indicating that the calcium stearate gel composition used in the water-in-oil cream provided in Example 4 has a better thickening effect. At the same time, the water-in-oil cream provided in Example 4 has better stability. This is because the calcium stearate gel composition used in the water-in-oil cream provided in Example 4, as a thickener with a stable three-dimensional network structure, significantly improves the thickening effect and stability of the water-in-oil cream, which is significantly higher than that of simple powdered thickeners such as calcium stearate powder, magnesium stearate powder, quaternary ammonium salt-18 bentonite, and montmorillonite.
[0147] Experiment Example 2
[0148] The performance of the oil-in-water creams provided in Example 4 and Comparative Examples 5-8 was tested. The performance tests included sensory evaluation, moisturizing performance test, and transdermal water loss performance test.
[0149] In the performance testing, sensory evaluation included: The oil-in-water creams provided in Example 4 and Comparative Examples 5-8 were given to approximately 15 volunteers who had received sensory evaluation training for trial use. The volunteers evaluated the products based on sensory indicators such as color, texture, fineness, stickiness, spreadability, moisturizing feel, and absorption speed. The scores were the statistical average of each volunteer's score, as shown in Table 3. In Table 3, texture refers to the cream's thickness; the thicker the cream, the higher the score (9 points or above is very thick), 7-8 points is relatively thick, and 6 points or below is not thick. Fineness refers to the cream's particle or roughness; 9 points or above is very fine, 7-8 points is relatively fine with no particles, and 6 points or below is not fine with large particles or a very rough surface. Stickiness refers to the cream's stickiness; 9 points or above indicates no stickiness. 7-8 points: No noticeable stickiness; 6 points and below: Noticeable stickiness; Spreadability: Silky smoothness and pilling sensation when applying the cream; 9 points and above: Good smoothness with no pilling; 7-8 points: Smoothness with no noticeable pilling; 6 points and below: No silky smoothness and noticeable pilling; Moisturizing effect: How well the cream moisturizes and relieves dryness; 9 points and above: Noticeable relief from dryness and hydration; 7-8 points: Relief from dryness and hydration; 6 points and below: No noticeable hydration; Absorption speed: How well the cream is absorbed; 9 points and above: Very fast absorption; 7-8 points: Moderate absorption; 6 points and below: Very slow absorption.
[0150] Furthermore, the stratum corneum of the skin is composed of keratinocytes and intercellular lipids, and has a naturally low dielectric constant. Water, however, is mainly found in the intercellular lipid matrix, forming localized areas of high dielectric constant. When the skin is dry and dehydrated, its conductivity is poor; when the water content is high, its conductivity is good. Therefore, the capacitance value after contact with the skin can reflect skin moisture and thus moisturizing performance. Thus, the CORNEOMETER-capacitance method was used to test the moisturizing performance. The procedure included: before testing, the inner sides of both arms were cleansed with facial cleanser at 20°C and 50% relative humidity, and the volunteers sat quietly in this environment for 20 minutes. The inner sides of the forearms of both volunteers were divided into symmetrical chambers with an area of 4cm × 3cm using a marker pen. Blank values were measured for each test area as a blank control. Then, using latex finger cots, the oil-in-water creams provided in Example 4 and Comparative Examples 5-8 were applied at a concentration of 2.0 ± 0.1 mg / cm³. 2The product was evenly applied to the test area; then, data was collected at 4 or 8 hours using a Corneometer CM825 skin moisture meter. During the test, the moisture test probe was simply pressed vertically onto the surface of the skin being tested. The data was recorded and displayed according to the machine prompts. The skin moisture content before and after using the oil-in-water cream provided in Example 4 and Comparative Examples 5-8 was measured respectively. The skin hydration status was obtained using the formula: △ rate of change of skin stratum corneum moisture content = (n-hour moisture content - baseline value) / baseline value × 100%. The results are shown in Table 4.
[0151] The transdermal water loss performance test method is based on Fick's law of diffusion, which states that the rate of skin water evaporation is directly proportional to the water vapor concentration gradient. The rate of water evaporation is quantified by measuring the water vapor pressure gradient on the skin surface. The transdermal water loss tester captures this gradient to calculate TEWL (Transdermal Water Loss Level). The TEWL value is a physical parameter representing the normal and continuous diffusion of water through the stratum corneum of the skin, and is the most important indicator reflecting the quality of the human skin barrier function. The process includes: before the test, in an environment of 20°C and 50% relative humidity, the inner sides of both forearms were cleaned with facial cleanser, and the participants sat quietly in this environment for 20 minutes. The inner sides of the volunteers' forearms were divided into symmetrical chambers with an area of 4cm × 3cm using a marker pen. The blank values of each test area were measured first. Then, using latex finger cots, the oil-in-water creams provided in Example 4 and Comparative Example 5 were applied at a concentration of 2.0 ± 0.1 mg / cm³. 2 The product was evenly applied to the test area. Subjects were required to refrain from applying makeup and skincare products on the day of each test. They were to sit quietly and relax in an environment of 20°C and 50% relative humidity. The transepidermal water loss (TEWL) values before and after using the water-in-oil cream provided in Example 4 and Comparative Example 5 were measured using a Tewameter® TMHex probe. The transepidermal water loss was obtained using the formula: △TEWL=(TEWL before using the water-in-oil cream - TEWL after using the water-in-oil cream) / TEWL after using the water-in-oil cream×100%. The results are shown in Table 5.
[0152] Table 3: Sensory Evaluation Results
[0153]
[0154] Table 4: Results of Moisturizing Performance Test
[0155]
[0156] Table 5: Results of transdermal water loss test
[0157]
[0158] As can be seen from Table 3, compared with the water-in-oil creams provided in Comparative Examples 5-8 that use calcium stearate powder and other thickeners, the water-in-oil cream provided in Example 4, due to the use of calcium stearate gel composition as a thickener, exhibits the best application performance. Its texture is smooth, it can significantly relieve skin dryness, and it is absorbed quickly. Moreover, the oily sheen after application is not obvious. It successfully solves the problem that thickeners such as calcium stearate powder have poor thickening and dispersing performance in cosmetic systems such as creams due to their hydrophobicity, which easily leads to defects such as rough texture and uneven dispersion, resulting in problems such as pilling and poor absorption.
[0159] As can be seen from Table 4, compared with the water-in-oil creams provided in Comparative Examples 5-8 (which served as blank controls), the water-in-oil cream provided in Example 4 exhibited stronger moisturizing performance due to the use of a calcium stearate gel composition. This is because the calcium stearate gel composition acts as a thickener to stabilize the three-dimensional network structure. When added to the water-in-oil cream, it increases the viscosity and makes the texture smoother, forming an excellent moisturizing layer after application. Therefore, its moisturizing performance is significantly higher than that of the water-in-oil creams provided in Comparative Examples 5-8, which used thickeners such as calcium stearate powder. At the same time, the transdermal water loss performance shown in Table 5 also demonstrates that the water-in-oil cream provided in Example 4 can form a better skin barrier and reduce skin moisture loss.
[0160] The above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.
Claims
1. A method for preparing a calcium stearate gel composition, characterized in that, Includes the following steps: Span-type emulsifiers, squalane, or cetyl ethylhexanoate are heated and homogenized to obtain an oil phase mixture; Calcium stearate powder was added to an oil phase mixture and heated to melt. The mixture was then cooled to room temperature to obtain a calcium stearate gel composition.
2. The method for preparing a calcium stearate gel composition according to claim 1, characterized in that, The Span emulsifier is selected from at least one of sorbitan sesquioleate, sorbitan oleate, sorbitan isostearate, sorbitan stearate, sorbitan lauryl ester, sorbitan trioleate, sorbitan palmitate, and sorbitan tristearate.
3. The method for preparing a calcium stearate gel composition according to claim 1, characterized in that, The heating and homogenization process is carried out at a temperature of 50℃ to 200℃, a rotation speed of 500 rpm to 10000 rpm, and a time of 1 min to 15 min.
4. The method for preparing a calcium stearate gel composition according to claim 1, characterized in that, The heating and melting temperature is 110℃~170℃, and the time is 5min~30min.
5. The method for preparing a calcium stearate gel composition according to claim 1, characterized in that, The cooling to room temperature process is as follows: cooling to room temperature under conditions of 0℃~30℃.
6. The method for preparing a calcium stearate gel composition according to claim 1, characterized in that, The mass ratio of the Span emulsifier to squalane or cetyl ethylhexanoate is 0.01~0.5:1; the mass ratio of the calcium stearate powder to the oil phase mixture is 0.01~0.5:
1.
7. A calcium stearate gel composition, characterized in that, It is prepared by the method for preparing a calcium stearate gel composition according to any one of claims 1-6.
8. The use of the calcium stearate gel composition according to claim 7 in the preparation of cosmetics.
9. The application according to claim 8, characterized in that, The cosmetics are selected from emulsions, creams, ointments, or gels.
10. A cream, characterized in that, Includes the calcium stearate gel composition as described in claim 7.