Water-responsive film-forming composition based on calcium ion coordination enhancement and lip solid cosmetic

Abstract

The application discloses a moisture-responsive film-forming composition based on calcium ion coordination reinforcement and a solid lip cosmetic. The moisture-responsive film-forming composition comprises: 18 to 35 parts of a film-forming skeleton ester, the film-forming skeleton ester being selected from one or more of synthetic esters obtained by esterification of a polyol with a hydroxyl number greater than or equal to 3 and isostearic acid or isononyl acid; 2 to 10 parts of a film-forming trigger, the film-forming trigger being N-lauroyl-L-glutamic acid ester; 0.1 to 2 parts of a coordination crosslinking agent, the coordination crosslinking agent being an oil-phase suspended pre-dispersed slurry of anhydrous calcium chloride; the pre-dispersed slurry comprising anhydrous calcium chloride solid-phase particles and a pre-dispersed medium; and 0.5 to 3 parts of a film-forming promoter, the film-forming promoter being selected from one or more oil-soluble polyisostearic acid ester compounds. The moisture-responsive film-forming composition provided by the application has high stability, can achieve rapid film formation, stable anti-transfer non-staining cup effect, and has no tight and dry feeling after being applied to lips.

Description

Technical Field

[0001] This application belongs to the field of solid lip cosmetics technology, specifically relating to a water-responsive film-forming composition based on calcium ion coordination enhancement and a solid lip cosmetic. Background Technology

[0002] Solid lip cosmetics (lipsticks, lip balms) are the mainstream lip makeup products. In addition to basic requirements such as color payoff and smooth application, consumers increasingly demand long-lasting, transfer-resistant (non-transferable) performance. Traditional wax-based lipsticks rely on the physical adhesion of pigments through waxes and oils. When exposed to saliva, beverages, food oils, and friction from lip movements, the pigments easily migrate, leading to problems such as transfer, fading, patchiness, and smudging, significantly impacting the user experience. Film-forming technology is currently the most mainstream technology for achieving non-transferable and transfer-resistant lip products. It forms a continuous film on the lip surface, encapsulating and isolating the pigment within the film matrix, reducing color transfer to cups and food. The industry urgently needs the development and innovation of film-forming technology to obtain solid lip cosmetics with faster film-forming speed, stronger transfer resistance, and longer-lasting wear. Summary of the Invention

[0003] To address the aforementioned issues, this application provides a water-responsive film-forming composition based on calcium ion coordination enhancement and a solid cosmetic for lips. In this application, the water-responsive film-forming composition, triggered by trace amounts of moisture on the lips, releases carboxylate ions from N-lauroyl-L-glutamate, which then coordinate and crosslink with calcium ions, generating an in-situ metal-organic gel network. This metal-organic gel network, together with the synthetic ester oil phase framework, forms a biphasic composite film. The combination with specific polyisostearate esters solves the problem of film-forming instability, achieving rapid film formation, stable anti-transfer, and non-sticky properties, without causing tightness or dryness after application to the lips.

[0004] In a first aspect, embodiments of this application provide a water-responsive film-forming composition based on calcium ion coordination enhancement, comprising: a film-forming backbone ester, 18 to 35 parts, wherein the film-forming backbone ester is selected from one or more synthetic esters obtained by esterification of polyols with 3 or more hydroxyl groups with isostearic acid or isononanoic acid; a film-forming trigger, 2 to 10 parts, wherein the film-forming trigger is N-lauroyl-L-glutamate ester; a coordination crosslinking agent, 0.1 to 2 parts, wherein the coordination crosslinking agent is an oil-phase suspension pre-dispersion slurry of anhydrous calcium chloride; the pre-dispersion slurry comprises anhydrous calcium chloride solid particles and a pre-dispersion medium, wherein the pre-dispersion medium is selected from one or more of C12-C24 Gelbert alcohols; and a film-forming promoter, 0.5 to 3 parts, wherein the film-forming promoter is selected from one or more oil-soluble polyisostearate compounds; wherein the molecule of the polyisostearate compound contains two or more isostearyl hydrocarbon chains and has at least one free hydroxyl or free carboxyl group.

[0005] In some alternative embodiments, the polyol has 3 to 6 hydroxyl groups.

[0006] In some alternative embodiments, the film-forming skeleton ester includes at least one of pentaerythritol pentaisostearate, pentaerythritol tetraisostearate, pentaerythritol pentaisonononate, and trimethylolpropane triisostearate.

[0007] In some alternative embodiments, N-lauroyl-L-glutamate includes at least one of phytosterol / octyldodecyl lauroyl glutamate and phytosterol / behenol / octyldodecyl lauroyl glutamate.

[0008] In some alternative embodiments, the pre-dispersion medium includes at least one of 2-butyloctanol, 2-hexyldecanol, 2-octyldodecylol, and 2-decyltetradecylol.

[0009] In some alternative embodiments, the oil-soluble polyisostearate compound includes at least one of polyglycerol-2 diisostearate and diisostearate malate.

[0010] In some alternative embodiments, the water-responsive film-forming composition based on calcium ion coordination enhancement may further include a film phase modifier, 2 to 10 parts, wherein the film phase modifier is selected from alkyl groups. Glyceryl-based co-modified polydimethylsiloxane.

[0011] Secondly, embodiments of this application provide a solid cosmetic for lips, comprising the water-responsive film-forming composition based on calcium ion coordination enhancement of the first aspect.

[0012] In some alternative embodiments, the lip-applied solid cosmetic may further include: solvent, 5-20 parts; wax, 5-20 parts; emollient ester, 10-30 parts; pigment, 3-10 parts; antioxidant, 0-2 parts; and preservative, 0.1-2 parts.

[0013] In some alternative implementations, the solvent is selected from hydrophobic oils and fats.

[0014] Compared with existing technologies, the water-responsive film-forming composition based on calcium ion coordination enhancement of this application has at least the following beneficial effects: The water-responsive film-forming composition based on calcium ion coordination enhancement of this application uses a synthetic ester with a specific structure as the oil phase film-forming framework, providing a basic oil phase film matrix; it uses N-lauroyl-L-glutamate esters as film-forming triggers; anhydrous calcium chloride is pre-prepared as a pre-dispersion slurry for Guerbert alcohol oil seal before being introduced into the formulation, achieving oil seal isolation to avoid premature coordination during storage, while improving the micro-dispersion of calcium salts; and it is compounded with polyisostearate esters with free hydroxyl or carboxyl groups as film-forming promoters. When the product is applied to the lips, under the triggering effect of trace amounts of moisture on the lips, N-lauroyl-L-glutamate releases carboxylate ions, which coordinate and crosslink with calcium ions, generating metal in situ. Organic gel network, the metal The organic gel network and the synthetic ester oil phase skeleton together form a biphase composite film; the combination with specific polyisostearate solves the problem of film instability, achieving rapid film formation, stable anti-transfer and non-sticky effect, and no tightness or dryness after application to the lips. Attached Figure Description

[0015] Figure 1 The images show the 0-6 hour makeup retention effect of the solid lip cosmetic prepared in Example 5. Detailed Implementation

[0016] To make the purpose, technical solution, and beneficial technical effects of this application clearer, the following detailed description is provided in conjunction with embodiments. It should be understood that the embodiments described in this specification are merely for explaining this application and are not intended to limit it.

[0017] For simplicity, this application only explicitly discloses some numerical ranges. However, any lower limit can be combined with any upper limit to form a range not explicitly stated; and any lower limit can be combined with other lower limits to form a range not explicitly stated, just as any upper limit can be combined with any other upper limit to form a range not explicitly stated. Furthermore, although not explicitly stated, every point or individual value between the endpoints of the range is included within that range. Therefore, each point or individual value can be used as its own lower or upper limit and combined with any other point or individual value or with other lower or upper limits to form a range not explicitly stated.

[0018] In the description of this application, it should be noted that, unless otherwise stated, "above" and "below" include the stated number, and "multiple" in "one or more" means two or more.

[0019] The foregoing description of this application is not intended to describe every disclosed implementation or method. Instead, the following description provides more specific examples of exemplary embodiments. Throughout the application, guidance is provided through a series of embodiments that can be used in various combinations. The examples listed are representative only and should not be construed as exhaustive.

[0020] To address the problems mentioned in the background art, this application provides a water-responsive film-forming composition based on calcium ion coordination enhancement and a solid cosmetic for lips. In this application, the water-responsive film-forming composition, triggered by trace amounts of moisture on the lips, releases carboxylate ions from N-lauroyl-L-glutamate, which then coordinate and crosslink with calcium ions, generating a metal in situ. Organic gel network, the metal The organic gel network and the synthetic ester oil phase skeleton together form a biphase composite film; the combination with specific polyisostearate solves the problem of film instability, achieving rapid film formation, stable anti-transfer and non-sticky effect, and no tightness or dryness after application to the lips.

[0021] The following will describe the water-responsive film-forming composition based on calcium ion coordination enhancement and the solid cosmetic for lips based on the embodiments of this application.

[0022] In a first aspect, embodiments of this application provide a water-responsive film-forming composition based on calcium ion coordination enhancement, comprising: The film-forming skeleton ester, ranging from 18 to 35 parts, is selected from one or more synthetic esters obtained by esterification of polyols with 3 or more hydroxyl groups with isostearic acid or isononanoic acid. As an example, the mass fraction of the film-forming skeleton ester can be 18, 20, 22, 25, 28, 30, 32, 35 parts, or any range of the above values. After esterification, polyols with 3 or more hydroxyl groups can form multi-side-chain macromolecular esters. Multiple fatty acid side chains provide the cohesive force required for the formation of a continuous film, serving as the framework for the coordination film. Simultaneously, isostearic acid or isononanoic acid are both branched saturated fatty acids, further endowing the esterified oil with good antioxidant stability and ensuring the controllability of the calcium ion coordination film-forming process.

[0023] Film-forming trigger, 2 to 10 parts, wherein the film-forming trigger is N-lauroyl-L-glutamate. As an example, the mass fraction of the film-forming trigger can be 2, 3, 4, 5, 6, 7, 8, 9, 10 parts, or any combination thereof. N-lauroyl-L-glutamate has a fixed chiral backbone, and the two carboxyl groups on the molecule are spatially adapted to calcium ion coordination, enabling rapid coordination crosslinking.

[0024] The coordination crosslinking agent, 0.1 to 2 parts, is an oil-phase suspension pre-dispersion slurry of anhydrous calcium chloride; the pre-dispersion slurry contains anhydrous calcium chloride solid particles and a pre-dispersion medium selected from C12. One or more of C24 Gelbert alcohols. As an example, the mass fraction of the coordination crosslinking agent can be 0.1 parts, 0.2 parts, 0.5 parts, 0.8 parts, 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, or any range of the above values. C12 C24 Guerbert alcohol refers to one or more Guerbert alcohols with a total number of carbon atoms between 12 and 24. Guerbert alcohol is a class of saturated primary alcohols with a branched chain attached to the second carbon atom, chemically named 2-alkyl-1-alkanol. C12-C24 Guerbert alcohols are transparent oily liquids at room temperature; they have low molecular polarity, are insoluble in anhydrous calcium chloride solid, and possess excellent powder wetting ability, forming a continuous oil film on the surface of calcium chloride particles. This prevents moisture in the air from contacting the inorganic salt, inhibiting calcium chloride from absorbing moisture, agglomerating, and prematurely crosslinking. In this application, anhydrous calcium chloride remains stable during product storage after being sealed with oil, and is less prone to premature crosslinking. When applied to the lips, calcium ions are released under the triggering effect of trace amounts of moisture. The calcium ions form coordination crosslinks with the free hydroxyl or carboxyl groups of the film-forming promoter, constructing a crosslinked network in the organic film-forming framework to form a dense coordination film, achieving color locking and anti-sticking effects. Compared to other metal ions that also have coordination effects (such as magnesium ion coordination or zinc ion coordination), calcium ions have moderate hydration kinetics and a relatively slow water-binding rate; they are easy to seal with oil and not prone to deliquescence; the coordination film formed has moderate brittleness and rigidity and will not cause a tight feeling on the lips. Therefore, they are more suitable for the coordination film-forming system of the lip solid cosmetic provided in this application.

[0025] A film-forming accelerator, ranging from 0.5 to 3 parts, is selected from one or more oil-soluble polyisostearate compounds; the polyisostearate compound contains two or more isostearyl hydrocarbon chains and has at least one free hydroxyl or free carboxyl group. As an example, the mass fraction of the film-forming accelerator can be 0.5 parts, 0.8 parts, 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts, 2.8 parts, 3 parts, or any range of the above values. This system relies on the release of calcium ions from anhydrous calcium chloride in the oil seal upon contact with water vapor, which then coordinate and crosslink with the free carboxyl or hydroxyl groups of the film-forming accelerator. The uniformity of crosslinking is highly dependent on the spatial distribution of calcium ions within the film layer. If local enrichment or deficiency of calcium ions occurs due to factors such as coating shearing and uneven random distribution of water vapor at the lip, film formation will occur in some areas while no film formation occurs in others, ultimately resulting in unstable film formation. The film-forming accelerator in this invention can be adsorbed onto the surface of calcium chloride particles, improving their dispersibility in the oil phase and alleviating the film-forming instability caused by uneven calcium ion distribution, thus ensuring uniform and controllable coordination crosslinking. Specifically, the multiple isostearyl branched hydrocarbon chains in the film-forming accelerator give the compound excellent compatibility with the film-forming skeleton ester and Guerbert alcohol oil phase in the system; the free hydroxyl or free carboxyl groups retained on the molecule serve as polar coordination sites, which can be adsorbed onto the surface of anhydrous calcium chloride particles, improving their dispersibility in the oil phase, alleviating the local enrichment or deficiency of calcium ions, solving the problem of film instability, and assisting in the formation of a uniform and continuous coordination film, achieving long-lasting color locking and reducing cup sticking. If the film-forming accelerator lacks multiple isostearyl hydrocarbon chains, it cannot be stably anchored in the film skeleton and is prone to migration and loss; if the film-forming accelerator lacks free hydroxyl or free carboxyl groups, it lacks polar sites for interaction with calcium ions, cannot play the role of interfacial bridging and improving dispersibility, and cannot achieve the technical effect of promoting stable film formation.

[0026] According to the embodiments of this application, the water-responsive film-forming composition based on calcium ion coordination enhancement provided in this application uses a synthetic ester with a specific structure as the oil phase film-forming framework to provide a basic oil phase film matrix; N-lauroyl-L-glutamate esters are used as film-forming triggers; anhydrous calcium chloride is pre-prepared as a Gerbert alcohol oil seal pre-dispersion slurry and then introduced into the formulation to achieve oil seal isolation to avoid premature coordination during storage, while improving the micro-dispersion of calcium salts; and polyisostearate with free hydroxyl or carboxyl groups is compounded as a film-forming promoter. When the product is applied to the lips, triggered by the trace moisture on the lips, N-lauroyl-L-glutamate releases carboxylate ions, which coordinate and crosslink with calcium ions, generating a metal-organic gel network in situ. This metal-organic gel network, together with the synthetic ester oil phase skeleton, forms a biphase composite film. Combined with specific polyisostearate esters, it improves the wetting and dispersibility of the interface, alleviates the local enrichment or deficiency of calcium ions, solves the problem of unstable film formation, and achieves a long-lasting non-stick effect with rapid film formation and stable anti-transfer properties. Moreover, it does not cause any tightness or dryness after being applied to the lips.

[0027] In some embodiments of this application, the polyol has 3 to 6 hydroxyl groups. As an example, the polyol may have 3, 4, 5, or 6 hydroxyl groups.

[0028] In some embodiments of this application, the film-forming skeleton ester includes at least one of pentaerythritol pentaisostearate, pentaerythritol tetraisostearate, pentaerythritol pentaisonononate, and trimethylolpropane triisostearate.

[0029] In some embodiments of this application, N-lauroyl-L-glutamate includes at least one of phytosterol / octyldodecyl lauroyl glutamate and phytosterol / behenol / octyldodecyl lauroyl glutamate.

[0030] In some embodiments of this application, the pre-dispersion medium includes at least one of 2-butyloctanol, 2-hexyldecanol, 2-octyldodecylol, and 2-decyltetradecylol.

[0031] In some embodiments of this application, the oil-soluble polyisostearate compound includes at least one of polyglycerol-2 diisostearate and diisostearate malate.

[0032] In some embodiments of this application, the water-responsive film-forming composition based on calcium ion coordination enhancement may further include a film phase modifier, 2 to 10 parts, wherein the film phase modifier is selected from alkyl groups. Glyceryl-based co-modified polydimethylsiloxane. As an example, the membrane phase modifier can be bis-C16-18 alkylglycerol undecyl polydimethylsiloxane, and the mass fraction of the membrane phase modifier can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, or any of the above-mentioned values. In this application, the water-responsive membrane is strengthened by calcium ion coordination. Although compared to other coordination metal ion strengthening effects, it has the characteristics of moderate membrane brittleness and rigidity, and does not cause a tight feeling at the lip, it was found in testing that the membrane layer layout cracked when the lip moved significantly. Therefore, it is preferable to further add alkyl-glycerol-based co-modified polydimethylsiloxane as a membrane phase modifier to the water-responsive film-forming composition. Alkyl-glycerol-modified polydimethylsiloxane has highly flexible siloxane segments. These highly flexible segments are dispersed and embedded in the cross-linked network. When the membrane is subjected to large deformation, the siloxane segments preferentially twist, dispersing and releasing the internal stress of the membrane layer. Without destroying the overall membrane continuity or losing the anti-sticking and color-locking ability, it improves the elongation at break of the membrane and reduces the cracking of the membrane layer layout when the lip opens and closes.

[0033] In some embodiments of this application, the mass ratio of anhydrous calcium chloride solid particles to predispersing medium in the oil-phase suspension predispersed slurry of anhydrous calcium chloride is 0.5:1 to 2:1. As examples, it can be 0.5:1, 0.8:1, 1:1, 1.2:1, 1.5:1, 1.8:1, 2:1, or any range of the above values. Optionally, the mass ratio of anhydrous calcium chloride solid particles to predispersing medium in the oil-phase suspension predispersed slurry of anhydrous calcium chloride is 0.5:1 to 1:1.

[0034] Secondly, embodiments of this application provide a solid cosmetic for lips, comprising the water-responsive film-forming composition based on calcium ion coordination enhancement of the first aspect.

[0035] In some embodiments of this application, the lip-applied solid cosmetic may further include: solvent, 5-20 parts; wax, 5-20 parts; emollient ester, 10-30 parts; pigment, 3-10 parts; antioxidant, 0-2 parts; and preservative, 0.1-2 parts.

[0036] As examples, the mass fractions of the solvent can be 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, or any combination of the above values. The mass fractions of the wax can be 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, or any combination of the above values. The mass fractions of the emulsifying oil can be 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 22 parts, 25 parts, 28 parts, 30 parts, or any combination of the above values. The mass fractions of the pigment can be 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, or any combination of the above values. The mass fractions of the antioxidant can be 0 parts, 0.2 parts, 0.5 parts, 0.8 parts, 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, or any combination of the above values. The mass fraction of the preservative can be 0.1 parts, 0.2 parts, 0.5 parts, 0.8 parts, 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, or any range of the above values.

[0037] In some embodiments of this application, the solvent is selected from hydrophobic oils and fats.

[0038] Example The following embodiments describe the disclosure of this application in more detail. These embodiments are merely illustrative, as various modifications and variations will be apparent to those skilled in the art within the scope of the disclosure of this application. Unless otherwise stated, all parts, percentages, and ratios reported in the following embodiments are based on mass, and all reagents used in the embodiments are commercially available or synthesized by conventional methods and can be used directly without further processing, and the instruments used in the embodiments are commercially available.

[0039] Example 1 A solid cosmetic product for lips, the components of which are shown in Table 1.

[0040] Table 1. Component formulation of the solid lip cosmetic of Example 1

[0041] Note: In Table 1, “anhydrous calcium chloride, 2-butyloctol (1:2)” means that anhydrous calcium chloride powder and 2-butyloctol form an oil phase suspension pre-dispersion slurry of anhydrous calcium chloride in a mass ratio of 1:2.

[0042] Solid cosmetic products for lips are prepared using the following steps: In step S100, the analytical grade anhydrous calcium chloride is placed in a constant temperature oven at 105℃ and dried continuously for 2 hours to completely remove adsorbed water and trace amounts of crystal water from the surface of the raw material. After drying, the material is taken out, cooled to room temperature, and immediately ground. It is then passed through a 150-mesh sieve twice to obtain anhydrous calcium chloride powder.

[0043] In step S200, the above-mentioned anhydrous calcium chloride powder is mixed with 2-butyloctanol at a mass ratio of 1:2 and ground at low speed to obtain an oil phase suspension pre-dispersion slurry of anhydrous calcium chloride.

[0044] In step S300, solvent, emollient, wax, film phase modifier, film-forming promoter, film-forming trigger and film-forming skeleton ester are added to the reaction vessel, heated to 98°C, and stirred at a constant temperature until all raw materials are completely melted and the system is clear and transparent to obtain the first oil phase.

[0045] In step S400, the first oil phase is cooled to 78°C, and the above-mentioned anhydrous calcium chloride oil phase suspension pre-dispersion slurry is added. The mixture is kept at 78°C and stirred continuously for 15 minutes to ensure uniform dispersion of the metal salt. If trace amounts of insoluble impurities appear in the system, it is filtered while hot using a 200-mesh nylon filter to obtain the second oil phase.

[0046] In step S500, color powder is added to the second oil phase and stirred until the system is uniform to obtain the third oil phase.

[0047] In step S600, after the third oil phase cools down to below 60°C, antioxidants and preservatives are added sequentially and stirred at low speed to obtain the paste to be formed.

[0048] Step S700: Degas the finished product to be molded in a vacuum environment at 78°C for 20 minutes to fully remove air bubbles from the system; then adjust the temperature to 60-65°C and inject it into a mold preheated to 35-38°C; place it in a 4°C environment to cool for 30 minutes, remove it from the mold and place it at room temperature to obtain a solid lip cosmetic.

[0049] Example 2 The only difference between the solid lip cosmetic of Example 2 and that of Example 1 is the formulation of the solid lip cosmetic; the preparation method is the same as that of Example 1. See Table 2 for details.

[0050] Table 2. Component formulation of the solid lip cosmetic product in Example 2

[0051] Note: In Table 2, “anhydrous calcium chloride, 2-hexyldecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-hexyldecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension pre-dispersion slurry of anhydrous calcium chloride.

[0052] Example 3 The only difference between the solid lip cosmetic of Example 3 and that of Example 1 is the formulation of the solid lip cosmetic; the preparation method is the same as that of Example 1. See Table 3 for details.

[0053] Table 3. Component formulation of the solid lip cosmetic product in Example 3

[0054] Note: In Table 3, “anhydrous calcium chloride, 2-decyltetradecyl alcohol (2:1)” means that anhydrous calcium chloride powder and 2-decyltetradecyl alcohol are mixed in a mass ratio of 2:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0055] Example 4 The only difference between the solid lip cosmetic of Example 4 and that of Example 1 is the formulation of the solid lip cosmetic; the preparation method is the same as that of Example 1. See Table 4 for details.

[0056] Table 4. Component formulation of the solid lip cosmetic product in Example 4

[0057] Note: In Table 4, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0058] Example 5 The only difference between the solid lip cosmetic of Example 5 and that of Example 1 is the formulation of the solid lip cosmetic; the preparation method is the same as that of Example 1. See Table 5 for details.

[0059] Table 5. Component formulation of the lip solid cosmetic of Example 5

[0060] Note: In Table 5, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0061] Example 6 The only difference between the solid lip cosmetic of Example 6 and that of Example 1 is the formulation of the solid lip cosmetic; the preparation method is the same as that of Example 1. See Table 6 for details.

[0062] Table 6. Component formulation of the lip solid cosmetic of Example 6

[0063] Note: " / " in Table 6 indicates that the substance was not added. "Anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)" means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension pre-dispersion slurry of anhydrous calcium chloride.

[0064] Comparative Example 1 The only difference between the solid lip cosmetic of Comparative Example 1 and Example 5 is that the formulation of the solid lip cosmetic is different (the film-forming skeleton ester component is omitted), while the preparation method is the same as that of Example 5. See Table 7 for details.

[0065] Table 7. Component formulation of the solid lip cosmetic product in Comparative Example 1

[0066] Note: " / " in Table 7 indicates that the substance was not added. "Anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)" means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension pre-dispersion slurry of anhydrous calcium chloride.

[0067] Comparative Example 2 The only difference between the solid lip cosmetic of Comparative Example 2 and Example 5 is that the formulation of the solid lip cosmetic is different (propylene glycol diisostearate is used instead of the original film-forming backbone ester component dipolypentaerythritol pentaisostearate), while the preparation method is the same as that of Example 5. See Table 8 for details.

[0068] Table 8. Component formulation of the solid lip cosmetic product in Comparative Example 2

[0069] Note: In Table 8, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0070] Comparative Example 3 The only difference between the solid lip cosmetic of Comparative Example 3 and Example 5 is that the formulation of the solid lip cosmetic is different (anhydrous calcium chloride in the coordination crosslinking agent is replaced with anhydrous magnesium chloride), while the preparation method is the same as that of Example 5. See Table 9 for details.

[0071] Table 9. Component formulation of the solid lip cosmetic product in Comparative Example 3

[0072] Note: In Table 9, “anhydrous magnesium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous magnesium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous magnesium chloride.

[0073] Comparative Example 4 The only difference between the solid lip cosmetic of Comparative Example 4 and Example 5 is that the formulation of the solid lip cosmetic is different (anhydrous calcium chloride in the coordination crosslinking agent is replaced with anhydrous zinc chloride), while the preparation method is the same as that of Example 5. See Table 10 for details.

[0074] Table 10. Component formulation of the solid lip cosmetic product in Comparative Example 4

[0075] Note: In Table 10, “anhydrous zinc chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous zinc chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous zinc chloride.

[0076] Comparative Example 5 The only difference between the solid lip cosmetic of Comparative Example 5 and Example 5 is that the formulation of the solid lip cosmetic is different (anhydrous calcium chloride was not pre-dispersed with Guerbert alcohol oil), and the preparation method is different from that of Example 5 in that it does not include the step of preparing the pre-dispersed slurry. See Table 11 for details.

[0077] Table 11. Component formulation of the solid lip cosmetic product in Comparative Example 5

[0078] Comparative Example 6 The only difference between the solid lip cosmetic of Comparative Example 6 and Example 5 is that the formulation of the solid lip cosmetic is different (ethanol is used instead of C12-C24 Guerbert alcohol as the pre-dispersion medium), while the preparation method is the same as that of Example 5. See Table 12 for details.

[0079] Table 12. Component formulation of the solid lip cosmetic product in Comparative Example 6

[0080] Note: In Table 12, “anhydrous calcium chloride, ethanol (1:1)” means that anhydrous calcium chloride powder and ethanol are mixed in a mass ratio of 1:1 to form a pre-dispersed slurry.

[0081] Comparative Example 7 The only difference between the solid lip cosmetic of Comparative Example 7 and Example 5 is that the formulation of the solid lip cosmetic is different (stearyl alcohol is used instead of C12-C24 Guerbert alcohol as the pre-dispersion medium), while the preparation method is the same as that of Example 5. See Table 13 for details.

[0082] Table 13. Component formulation of the solid lip cosmetic product in Comparative Example 7

[0083] Note: In Table 13, “anhydrous calcium chloride, stearyl alcohol (1:1)” means that anhydrous calcium chloride powder and stearyl alcohol are mixed in a mass ratio of 1:1 to form a pre-dispersion slurry.

[0084] Comparative Example 8 The only difference between the solid lip cosmetic of Comparative Example 8 and Example 5 is that the formulation of the solid lip cosmetic is different (the amount of coordination crosslinking agent is insufficient), while the preparation method is the same as that of Example 5. See Table 14 for details.

[0085] Table 14. Component formulation of the solid lip cosmetic product in Comparative Example 8

[0086] Note: In Table 14, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0087] Comparative Example 9 The only difference between the solid lip cosmetic of Comparative Example 9 and Example 5 is that the formulation of the solid lip cosmetic is different (the amount of coordination crosslinking agent is too large), while the preparation method is the same as that of Example 5. See Table 15 for details.

[0088] Table 15. Component formulation of the solid lip cosmetic product in Comparative Example 9

[0089] Note: In Table 15, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0090] Comparative Example 10 The only difference between the solid lip cosmetic of Comparative Example 10 and Example 5 is that the formulation of the solid lip cosmetic is different (no film-forming accelerator is added), while the preparation method is the same as that of Example 5. See Table 16 for details.

[0091] Table 16. Component formulation of the solid lip cosmetic product in Comparative Example 10

[0092] Note: " / " in Table 16 indicates that the substance was not added. "Anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)" means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension pre-dispersion slurry of anhydrous calcium chloride.

[0093] Comparative Example 11 The only difference between the solid lip cosmetic of Comparative Example 11 and Example 5 is that the formulation of the solid lip cosmetic is different (using glyceryl triisostearate instead of the original film-forming promoter polyglyceryl-2 diisostearate), while the preparation method is the same as that of Example 5. See Table 17 for details.

[0094] Table 17. Component formulation of the solid lip cosmetic product in Comparative Example 11

[0095] Note: In Table 17, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0096] Comparative Example 12 The only difference between the solid lip cosmetic of Comparative Example 12 and Example 5 is that the formulation of the solid lip cosmetic is different (isopropyl isostearate is used instead of the original film-forming promoter polyglycerol-2 diisostearate), while the preparation method is the same as that of Example 5. See Table 18 for details.

[0097] Table 18. Component formulation of the solid lip cosmetic product in Comparative Example 12

[0098] Note: In Table 18, “anhydrous calcium chloride, 2-octyldodecyl alcohol (1:1)” means that anhydrous calcium chloride powder and 2-octyldodecyl alcohol are mixed in a mass ratio of 1:1 to form an oil phase suspension predispersed slurry of anhydrous calcium chloride.

[0099] Product performance testing Stability studies (production process stability study, room temperature stability study, accelerated stability study), non-stickiness tests (film formation test within 40 seconds, makeup residue rate test after 6 hours) and skin feel evaluation (whether there is a tightness or dryness, whether there is cracking or peeling) were conducted on the solid lip cosmetics obtained in Examples 1 to 6 and Comparative Examples 1 to 12. The specific results are shown in Table 19. Among them, Comparative Examples 5 and 6 failed the room temperature stability study, so the non-stickiness test and skin feel evaluation were not conducted.

[0100] (1) Stability test Production process stability study: Ten samples were prepared for each of Examples 1-6 and Comparative Examples 1-12. The entire process of sample preparation, grinding, degassing, and filling was monitored to observe whether the material exhibited localized thickening, clumping, or stratification. The phenomena observed in 80% or more of the samples in each group were recorded as the study results.

[0101] Room temperature stability test: Ten samples in each group were stored at 25±2℃ and 45%~55% relative humidity for 90 days, and the presence of oil release or discoloration was observed. If no oil release or discoloration was observed in more than 90% of the samples in each group, the sample was recorded as stable; otherwise, it was recorded as unstable. If severe clumping and stratification occurred during the preparation process, the room temperature stability test was not conducted.

[0102] Accelerated stability test: Place 10 samples in each group in an oven at 48±2℃ for 30 days and observe whether the paste shows any signs of oiling or discoloration. If no oiling or discoloration is observed in 90% or more of the samples in each group, the paste is recorded as stable; otherwise, it is recorded as unstable.

[0103] (2) Non-stick cup test 40-second film-forming test: Five samples were used in each group for volunteer testing. After cleaning their lips, volunteers applied a measured amount of sample, started the timer, and waited 40 seconds. First, they pressed their lips with a tissue to remove surface pigment, leaving some residual color on the lips. Second, they pressed their lips with a tissue and observed whether there was any pigment on the tissue and whether the residual color on the lips had decreased. If there was no pigment on the tissue and no decrease in residual color after the second pressing, film formation was considered successful in 40 seconds; if there was pigment on the tissue and a decrease in residual color, film formation was not successful in 40 seconds. In each group of five parallel samples, if ≥4 samples formed a film within 40 seconds, the 40-second film-forming test was considered successful; otherwise, it was considered unsuccessful.

[0104] Comparative observation of makeup effects at 1, 2, and 6 hours: The makeup-holding properties of the solid lip cosmetic prepared in Example 5 were compared at 1, 2, and 6 hours. After cleaning their arms, volunteers applied a quantitative amount of the sample at time T0 (after waiting 2 minutes, the surface color was removed by pressing the lips with a tissue), leaving residual color 1; at time T0+4, a quantitative amount of the sample was applied again (after waiting 2 minutes, the surface color was removed by pressing the lips with a tissue), leaving residual color 2; at time T0+5, a quantitative amount of the sample was applied again (after waiting 2 minutes, the surface color was removed by pressing the lips with a tissue), leaving residual color 3; at time T0+6, a quantitative amount of the sample was applied again (after waiting 2 minutes, the surface color was removed by pressing the lips with a tissue), leaving residual color 4; photos of residual color 1, residual color 2, residual color 3, and residual color 4 were immediately taken for comparison. Residual color 4 represents the initial makeup effect, residual color 3 represents the 1-hour makeup effect, residual color 2 represents the 2-hour makeup effect, and residual color 1 represents the 6-hour makeup effect. Figure 1 As shown, there was no significant change in the makeup effect at the initial, 1-hour, 2-hour, and 6-hour intervals, indicating that the lip solid cosmetic prepared in Example 5 has a good 6-hour makeup-holding effect.

[0105] 6-Hour Makeup Residue Rate Test: Five samples were taken from each group for volunteer testing. After cleansing their lips, volunteers applied a measured amount of sample, started the timer, and waited for 2 minutes. They then used a tissue to press away any surface color, leaving some residual color on their lips. The initial redness value A-0 of the test area was collected using a spectrophotometer. For the next 6 hours, standardized simulated daily activities were observed: drinking room-temperature purified water four times, and eating uncolored white bread at the 3rd hour. Licking, wiping, and reapplying makeup were prohibited during the test. After 6 hours, the redness value A-6 was collected from the original test area. The makeup residue rate was calculated as follows: Makeup Residue Rate (%) = (A-6 / A-0) × 100%. The average of the results from the five volunteers in each group was used.

[0106] (3) Skin feel evaluation: Five samples were taken from each group for volunteer use testing. After cleaning their lips, volunteers applied a quantitative amount of the sample, lived normally for 2 hours, and filled out a volunteer evaluation form to evaluate whether their lips felt tight and dry, and whether the film layer cracked and peeled when the lips were opened and closed. The evaluation results of more than 80% of the samples in each group were recorded.

[0107] Table 19 Detection results of Examples 1-6 and Comparative Examples 1-12

[0108] Table 19, based on Examples 1 to 6, shows that a specific synthetic ester was used as the oil phase film-forming framework to construct the basic film matrix. N-lauroyl-L-glutamate was used as the film-forming trigger. Anhydrous calcium chloride was incorporated into the system as a Gerbert alcohol oil-sealing pre-dispersion slurry, effectively isolating moisture, avoiding premature coordination during storage, and optimizing the micro-dispersion of calcium salts. Polyisostearate containing free hydroxyl or carboxyl groups was used as a film-forming promoter. After the product was applied to the lips, triggered by trace amounts of moisture on the lips, N-lauroyl-L-glutamate released carboxyl groups, which then coordinated and crosslinked with calcium ions in situ to form a metal. Organic gel network, the metal An organic gel network and a synthetic ester oil phase skeleton are used to construct a biphase composite film. Specific polyisostearate is added to improve interfacial wetting and dispersibility, alleviating localized calcium ion enrichment or deficiency and solving the problem of film instability. The samples from Examples 1 to 6 of this application exhibit good stability during production and storage, achieving rapid film formation, anti-transfer, and non-stick properties. The lips do not experience tightness or dryness after applying the product due to film formation.

[0109] Compared to Examples 1 to 5, Example 6 reduced the amount of alkyl membrane phase modifier. The glycerol-based co-modified polydimethylsiloxane component exhibits poor film extensibility and a brittle texture after film formation, making it prone to cracking and peeling during lip opening and closing activities, thus affecting the makeup feel and user comfort. However, in Examples 1 to 5, which used the alkyl-glycerol-based co-modified polydimethylsiloxane component as a film phase modifier, no cracking or peeling was observed during lip opening and closing activities. Therefore, the alkyl-glycerol-based co-modified polydimethylsiloxane component, in addition to improving the moisture-responsive film-forming composition, further enhances the elongation at break of the film, reducing the likelihood of film cracking during lip opening and closing activities.

[0110] The formulation of Comparative Example 1 omitted the film-forming skeleton ester component. Even with increased amounts of film-forming trigger, coordination crosslinking agent and film-forming promoter, the lack of a hydrophobic skeleton film after application to the lips prevented rapid film formation and long-lasting makeup. Furthermore, the stability of the balm was poor, with localized thickening and clumping of the material during preparation, resulting in a decreased yield and failure to pass the accelerated stability test.

[0111] Comparative Example 2 used propylene glycol diisostearate to replace the original film-forming backbone ester component, pentaerythritol pentaisostearate. Propylene glycol diisostearate is a diol diester containing only two ester bonds. Its low degree of molecular branching and small molecular weight prevent it from forming a continuous hydrophobic backbone film with sufficient cohesive strength when applied to the lips, thus affecting its non-stick properties. Furthermore, the thermal stability of the lipstick decreased, and oil seepage occurred during accelerated stability testing.

[0112] In Comparative Examples 3 and 4, anhydrous calcium chloride in the coordination crosslinking agent was replaced with anhydrous magnesium chloride and anhydrous zinc chloride. Zinc and magnesium ions have extremely high coordination reactivity, and the raw materials are prone to premature crosslinking and gelation during mixing and storage, resulting in abnormal thickening of the cream. Although it can also form a film quickly and provide long-lasting makeup, in terms of skin feel, if the amount of zinc and magnesium compounds added exceeds the appropriate range, it will lead to a significant increase in film hardness, causing problems such as tightness and dryness on the lips, making it difficult to simultaneously achieve high makeup-holding performance and a comfortable skin feel.

[0113] Comparative Example 5 did not pre-disperse anhydrous calcium chloride with Guerbert alcohol; instead, it directly introduced anhydrous calcium chloride into the formulation. This resulted in the paste easily agglomerating and clumping, leading to poor stability during preparation and storage. Comparative Example 6 used ethanol instead of C12-C24 Guerbert alcohol as the pre-dispersion medium. The results showed that ethanol formed an insoluble crystalline alcohol complex with anhydrous calcium chloride, causing precipitation and stratification of the pre-dispersion slurry. Furthermore, ethanol evaporation led to instability in the slurry composition. Comparative Example 7 used stearyl alcohol instead of C12-C24 Guerbert alcohol as the pre-dispersion medium. However, stearyl alcohol is solid at room temperature and cannot form a liquid suspension slurry under normal conditions. After preparation by heating and melting, the stearyl alcohol solidified upon cooling, embedding CaCl2 particles within the waxy matrix. These particles could not be effectively released upon contact with water, preventing coordination and cross-linking, thus affecting the non-stick effect. Moreover, the introduction of stearyl alcohol negatively impacted the skin feel after makeup application.

[0114] In Comparative Example 8, the amount of coordination crosslinking agent was insufficient, resulting in insufficient coordination crosslinking sites, which affected the non-stick effect and reduced film strength, oil resistance, and makeup holding power. In Comparative Example 9, the amount of coordination crosslinking agent was excessive, resulting in an overly rigid film that was prone to cracking and crumbling, and also reduced the storage stability of the paste.

[0115] According to Comparative Example 10, when no film-forming promoter is added to the system, even if the amount of film-forming trigger is appropriately increased, after the product is applied to the lips, although it contains a film-forming skeleton, lauroyl glutamate, and calcium ion source, the uniformity of cross-linking is highly dependent on the spatial distribution of calcium ions in the film layer. Under the influence of application shearing and uneven random distribution of moisture on the lips, local enrichment or deficiency of calcium ions occurs, and the film cannot be stably formed within 40 seconds or cannot be formed in some areas, resulting in a significant decrease in long-lasting makeup retention.

[0116] Although the glyceryl triisostearate of Comparative Example 11 has multiple isostearyl hydrocarbon chains, it lacks free hydroxyl or carboxyl groups; the isostearate isopropyl isostearate of Comparative Example 12 has only one isostearyl hydrocarbon chain and lacks free polar groups. Neither of them falls within the structural characteristics of film-forming accelerators defined in this application, and neither can effectively control the film-forming process of calcium chloride coordination crosslinking; after application, it is difficult to form a uniform and continuous coordination film, the film formation is unstable, it easily sticks to cups, and the color-locking effect is poor, failing to achieve the technical effect of this application.

[0117] The above description is merely a specific embodiment of this application, but the scope of protection of this application is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in this application, and these modifications or substitutions should all be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A water-responsive film-forming composition based on calcium ion coordination enhancement, characterized in that, include: Film-forming skeleton ester, 18 to 35 parts, wherein the film-forming skeleton ester is selected from one or more synthetic esters obtained by esterification of polyols with 3 or more hydroxyl groups with isostearic acid or isononanoic acid. Film-forming trigger, 2 to 10 parts, wherein the film-forming trigger is N-lauroyl-L-glutamate; The coordination crosslinking agent, 0.1 to 2 parts, is an oil-phase suspension pre-dispersion slurry of anhydrous calcium chloride; the pre-dispersion slurry comprises anhydrous calcium chloride solid particles and a pre-dispersion medium selected from C12. One or more of C24 Gelbert alcohols; Film-forming accelerator, 0.5 to 3 parts, wherein the film-forming accelerator is selected from one or more oil-soluble polyisostearate compounds; wherein the polyisostearate compound contains two or more isostearyl hydrocarbon chains and has at least one free hydroxyl or free carboxyl group.

2. The water-responsive film-forming composition based on calcium ion coordination enhancement according to claim 1, characterized in that, The polyol has 3 to 6 hydroxyl groups.

3. The water-responsive film-forming composition based on calcium ion coordination enhancement according to claim 2, characterized in that, The film-forming backbone ester includes at least one of pentaerythritol pentaisostearate, pentaerythritol tetraisostearate, pentaerythritol pentaisonononate, and trimethylolpropane triisostearate.

4. The water-responsive film-forming composition based on calcium ion coordination enhancement according to claim 1, characterized in that, The N-lauroyl-L-glutamate includes at least one of phytosterol / octyldodecyl lauroyl glutamate and phytosterol / behenol / octyldodecyl lauroyl glutamate.

5. The water-responsive film-forming composition based on calcium ion coordination enhancement according to claim 1, characterized in that, The pre-dispersion medium includes at least one of 2-butyloctanol, 2-hexyldecanol, 2-octyldodecylol, and 2-decyltetradecylol.

6. The water-responsive film-forming composition based on calcium ion coordination enhancement according to claim 1, characterized in that, The oil-soluble polyisostearate compound includes at least one of polyglycerol-2 diisostearate and diisostearate malate.

7. The water-responsive film-forming composition based on calcium ion coordination enhancement according to claim 1, characterized in that, It also includes a membrane phase modifier, 2 to 10 parts, said membrane phase modifier being selected from alkyl groups. Glyceryl-based co-modified polydimethylsiloxane.

8. A solid cosmetic product for lips, characterized in that, The water-responsive film-forming composition based on calcium ion coordination enhancement as described in any one of claims 1 to 7.

9. The lip-applied solid cosmetic according to claim 8, characterized in that, Also includes: Solvent, 5-20 parts; wax, 5-20 parts; emollient ester, 10-30 parts; pigment, 3-10 parts; antioxidant, 0-2 parts; preservative, 0.1-2 parts.

10. The lip-applied solid cosmetic according to claim 9, characterized in that, The solvent is selected from hydrophobic oils and fats.

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