Water-retaining liquid lip gloss and preparation method thereof

Abstract

The present application relates to the field of fine chemical technology, and discloses a water-locking and moisturizing liquid lip gloss and a preparation method thereof. The present application constructs a dual-phase rheological regulation network combining rigid skeleton support and flexible hydrogen bond bridging, which significantly improves the rheological properties of the product. The liquid lip gloss comprises deionized water, a polyol moisturizing compound system composed of glycerol, propylene glycol and polyethylene glycol, a film-forming polymer, and a thixotropic regulator compounded by organoammonium salt modified hectorite and xanthan gum. The preparation process uses high-temperature and high-speed dispersion to promote the full hydration of hectorite, and after cooling, the polyol and the film-forming polymer are added to protect the active ingredients. The product of the present application recovers quickly after high shear, does not delaminate in centrifugal and high-low temperature cycle tests, and has excellent water-locking and moisturizing performance and light skin feel, realizing the synergistic optimization of processing rheology and terminal use performance.

Description

Technical Field

[0001] This invention relates to the field of fine chemical technology, and in particular to a water-locking and moisturizing liquid lip gloss and its preparation method. Background Technology

[0002] Liquid lip gloss is a lip cosmetic that combines coloring and lip care functions. Its performance involves multiple aspects such as rheological properties, skin feel, and moisturizing effects. When using it, it should be applied smoothly and form an even film, giving the lips a glossy or matte finish, while also providing some moisturizing and care functions.

[0003] In terms of rheological properties, an ideal liquid lip gloss should exhibit shear-thinning behavior, meaning that its viscosity decreases under high shear conditions (such as during filling and application) to facilitate flow, and its viscosity increases under low shear conditions (such as during static storage) to prevent sedimentation and stratification. However, conventional thickening systems often experience a lag in the recovery of their internal microstructure after undergoing high shear, making it difficult to rebuild an effective support network in a short time. This can lead to problems such as filling metering errors, pigment sedimentation, and system stratification, affecting product quality and batch stability.

[0004] In terms of moisturizing and skin feel, conventional moisturizers can improve the moisturizing effect, but they are often accompanied by increased stickiness, which affects the user experience. How to achieve a balance between moisturizing effect and refreshing skin feel is one of the challenges in formula design.

[0005] Therefore, with the increasing popularity of high-speed automated filling and the continuous improvement of consumers' requirements for product quality, it is of great significance to research and develop a liquid lip gloss that achieves a comprehensive balance in terms of rheological properties, skin feel, and moisturizing performance. Summary of the Invention

[0006] The purpose of this invention is to overcome the problems of conventional thickening systems in existing liquid lip glosses, such as delayed structural recovery after high shear, easy sedimentation and stratification, and difficulty in simultaneously achieving moisturizing effects and a refreshing feel. This invention provides a water-locking and moisturizing liquid lip gloss and its preparation method. This liquid lip gloss can quickly rebuild its internal structure after shear removal, effectively inhibiting pigment sedimentation and system stratification, while simultaneously providing long-lasting moisturizing function and a lightweight, non-sticky feel.

[0007] A first aspect of the present invention provides a water-locking and moisturizing liquid lip gloss, comprising the following components in parts by weight: 40-65 parts deionized water; A polyol moisturizing compound system of 15-25 parts, wherein the polyol moisturizing compound system is composed of glycerin, propylene glycol and polyethylene glycol with a number average molecular weight of 200-600; 3-8 parts of film-forming polymer; 0.5-3.0 parts of a thixotropic modifier, wherein the thixotropic modifier is composed of a mixture of lithium montmorillonite modified with an organic ammonium salt and xanthan gum.

[0008] Furthermore, the weight ratio of glycerin, propylene glycol and polyethylene glycol in the polyol moisturizing compound system is (3-5):(1-2):(0.5-1.5).

[0009] Furthermore, the weight ratio of the organoammonium salt-modified lithium montmorillonite to xanthan gum in the thixotropic modifier is (1-3):(1-2).

[0010] Furthermore, the lithium montmorillonite modified with organic ammonium salt is prepared by the following method: the purified and modified lithium montmorillonite is dispersed in deionized water to form a slurry, and a quaternary ammonium salt solution containing long-chain alkyl groups is added under stirring conditions to carry out an ion exchange reaction. After the reaction is completed, the solution is filtered, washed, dried, and ground to obtain the final product.

[0011] Furthermore, the purified and modified lithium montmorillonite has a cation exchange capacity of 80-120 meq / 100g.

[0012] Furthermore, the quaternary ammonium salt is at least one of distearyldimethylammonium chloride, octadecyltrimethylammonium chloride, or bis(hydrogenated tallow)dimethylammonium chloride.

[0013] Furthermore, the amount added is 0.8-1.5 times the equivalent of the cation exchange capacity.

[0014] Furthermore, the reaction temperature is 60-80℃, and the reaction time is 4-8 hours.

[0015] Furthermore, the film-forming polymer is selected from at least one of polyvinylpyrrolidone K90, polyurethane-35, and acrylate copolymers.

[0016] Furthermore, the water-locking and moisturizing liquid lip gloss also contains at least one of the following components: 5-15 parts of pigment dispersion, 2-6 parts of emulsifying and solubilizing system, 0.1-2.0 parts of active ingredient, 0.3-0.8 parts of preservative and / or 0.05-0.2 parts of pH adjuster.

[0017] Furthermore, the emulsified solubilizing system is composed of polysorbate-20 and hydrogenated castor oil derivative in a weight ratio of (1-2):(1-3).

[0018] Furthermore, the active ingredient is selected from at least one of sodium hyaluronate, vitamin E acetate, and panthenol.

[0019] Furthermore, the preservative is a compound of phenoxyethanol and ethylhexylglycerin.

[0020] Furthermore, the pH adjuster is a citric acid solution or a sodium hydroxide solution, used to adjust the pH value of the system to 5.5-6.5.

[0021] A second aspect of the present invention provides a method for preparing the water-locking and moisturizing liquid lip gloss as described above, comprising the following steps: Step 1: At 75-85℃, disperse the thixotropic modifier in deionized water at a shear rate of 2000-3500 rpm and continue shearing for 15-25 minutes to form a gel substrate; Step 2: Lower the temperature of the gel substrate to 50-60℃, add the polyol moisturizing compound system and film-forming polymer in sequence, and stir at 30-60 rpm for 20-40 minutes.

[0022] Furthermore, the thixotropic modifier, after being pre-dry-mixed evenly in step 1, is slowly sprinkled into the center of the vortex over 3-5 minutes.

[0023] Furthermore, after step 2, at least one of the following steps is included: color paste incorporation step, emulsification step, defoaming step and / or fragrance blending step.

[0024] Furthermore, the step of incorporating the color paste is as follows: add the pigment dispersion and stir at a speed of 20-40 rpm for 10-15 minutes.

[0025] Furthermore, the emulsification step is as follows: add the emulsification solubilization system and homogenize at a rate of 1500-2500 rpm for 3-8 minutes.

[0026] Furthermore, the degassing step is as follows: degassing for 10-20 minutes under a pressure of -0.08 to -0.09 MPa.

[0027] Furthermore, the fragrance preparation step is as follows: add the fragrance and stir at a speed of 20-40 rpm for 5-10 minutes.

[0028] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention provides a water-locking and moisturizing liquid lip gloss. It utilizes a thixotropic modifier composed of an organically ammonium salt-modified lithium montmorillonite and xanthan gum, synergistically combined with a polyol moisturizing complex system consisting of glycerin, propylene glycol, and polyethylene glycol with a number-average molecular weight of 200-600, as well as a film-forming polymer, to construct a biphase rheological network with excellent shear-thinning behavior and rapid structural recovery capability. Test data shows that the liquid lip gloss prepared by this invention effectively solves the problems of delayed structural recovery after high shear in conventional thickening systems of existing liquid lip glosses, which easily lead to sedimentation and stratification, and the difficulty in simultaneously achieving moisturizing efficacy and a refreshing skin feel.

[0029] 2. This invention provides a method for preparing a water-locking and moisturizing liquid lip gloss. First, a thixotropic modifier is dispersed in deionized water at a high temperature of 75-85℃ with a high-speed shear rate of 2000-3500 rpm to form a gel base. Then, the temperature is lowered to 50-60℃, and a polyol moisturizing compound system and a film-forming polymer are added. This segmented temperature control strategy effectively promotes the interlayer exfoliation and hydration swelling of the organoammonium salt-modified lithium montmorillonite, enabling it to form a uniform physical cross-linked network with xanthan gum. Simultaneously, it effectively protects the molecular integrity of the heat-sensitive film-forming polymer and active ingredients, ensuring the stability and consistency of product quality between batches. Detailed Implementation

[0030] The present invention will now be described in further detail with reference to specific embodiments. However, this should not be construed as limiting the scope of the present invention to the following embodiments; all technologies implemented based on the content of the present invention fall within the scope of the present invention.

[0031] It should be noted that the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Furthermore, in the description of this invention, unless otherwise stated, "a plurality of" means two or more. The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein. To facilitate understanding of the invention, certain technical and scientific terms are specifically defined below. Unless otherwise expressly defined elsewhere in this document, all other technical and scientific terms used herein have the meanings commonly understood by one of ordinary skill in the art to which this invention pertains. In this document, the terms “comprising” or “including” are open-ended expressions, meaning that they include the contents specified in this invention, but do not exclude other aspects. In this document, the terms “optionally,” “optionally,” or “optionally” generally refer to an event or condition that may, but may not, occur, and the description includes both cases in which the event or condition occurs and cases in which the event or condition does not occur. The conventional thickening system in existing liquid lip glosses suffers from delayed structural recovery after high shear, which easily leads to sedimentation and stratification, and it is difficult to achieve both moisturizing effects and a refreshing feel.

[0032] The first aspect of this embodiment provides a water-locking and moisturizing liquid lip gloss, which is made of the following components in parts by weight: 40-65 parts deionized water; A polyol moisturizing compound system of 15-25 parts, wherein the polyol moisturizing compound system is composed of glycerin, propylene glycol and polyethylene glycol with a number average molecular weight of 200-600; 3-8 parts of film-forming polymer; 0.5-3.0 parts of a thixotropic modifier, wherein the thixotropic modifier is composed of a mixture of lithium montmorillonite modified with an organic ammonium salt and xanthan gum.

[0033] By employing a thixotropic modifier composed of an organically ammonium salt-modified lithium montmorillonite and xanthan gum, synergistically combining it with a polyol moisturizing complex system consisting of glycerol, propylene glycol, and polyethylene glycol with a number-average molecular weight of 200-600, as well as a film-forming polymer, a rheological network exhibiting excellent shear-thinning behavior and rapid structural recovery was constructed. This liquid lip gloss exhibits significantly reduced viscosity under high shear conditions, meeting the flowability requirements of high-speed filling. During the low-shear settling stage after shear removal, its internal microstructure rapidly reconstructs, effectively inhibiting pigment sedimentation and system stratification. Simultaneously, it combines long-lasting moisturizing with a lightweight, non-sticky feel, solving the problems of delayed structural recovery, sedimentation, and stratification in conventional thickening systems of existing liquid lip glosses after high shear, as well as the difficulty in simultaneously achieving moisturizing efficacy and a refreshing feel.

[0034] In some embodiments, the weight ratio of glycerol, propylene glycol, and polyethylene glycol in the polyol moisturizing compound system is (3-5):(1-2):(0.5-1.5). This specific ratio can optimize the unfolding conformation of xanthan gum molecules in the aqueous phase, enhance its physical crosslinking efficiency with organoammonium salt-modified lithium montmorillonite, thereby further improving the overall strength and structural recovery rate of the biphase rheological network.

[0035] In some embodiments, the weight ratio of organoammonium salt-modified lithium montmorillonite to xanthan gum in the thixotropic modifier is (1-3):(1-2). By limiting the weight ratio of organoammonium salt-modified lithium montmorillonite to xanthan gum in the thixotropic modifier to a suitable range, a reasonable balance between the rigid framework and the flexible hydrogen bond bridging can be effectively ensured. When the ratio is within this range, the modified lithium montmorillonite provides sufficient yield stress to maintain static suspension stability, while xanthan gum provides sufficient dynamic entanglement points to buffer shear shocks and achieve rapid recovery; the two have a significant synergistic effect.

[0036] In some embodiments, the organoammonium salt modified lithium montmorillonite is prepared by the following method: the purified and modified lithium montmorillonite is dispersed in deionized water to form a slurry, and a quaternary ammonium salt solution containing long-chain alkyl groups is added under stirring conditions to carry out an ion exchange reaction. After the reaction is completed, the solution is filtered, washed, dried and ground to obtain the final product.

[0037] By employing the aforementioned specific quaternary ammonium salt intercalation modification process to prepare lithium montmorillonite modified with organic ammonium salts, the interlayer spacing can be effectively increased and the surface properties can be changed from hydrophilic to hydrophobic. This enhances the hydrophobic interaction and van der Waals force binding with xanthan gum molecular chains, forming more stable physical cross-linking points and providing a guarantee for constructing a high-quality rigid framework.

[0038] In some embodiments, the cation exchange capacity (CEC) of the purified and modified lithium montmorillonite is 80-120 meq / 100g. Controlling the CEC within a suitable range ensures that the sheets have a moderate charge density. If the CEC is too low, there are too few exchangeable sites, insufficient organic intercalation, weak hydrophobicity, and difficulty in forming effective physical cross-links. If the CEC is too high, the sheets are excessively stretched, rigidity decreases, the framework becomes brittle, and rapid reconstruction after shearing is difficult. This range achieves an optimal balance between hydrophobicity and rigidity, providing the material basis for achieving rapid structural recovery and zero centrifugal delamination.

[0039] In some embodiments, the quaternary ammonium salt is at least one of distearyldimethylammonium chloride, octadecyltrimethylammonium chloride, or bis(hydrogenated tallow)dimethylammonium chloride. Using a quaternary ammonium salt containing long-chain alkyl groups (C16-C18) can effectively transform the surface of the sheet from hydrophilic to hydrophobic after insertion into the interlayer of lithium montmorillonite, generating significant hydrophobic interactions and van der Waals forces with the xanthan gum molecular chains, forming reversible physical crosslinking points. Simultaneously, the dual long-chain structure provides sufficient steric hindrance between layers, preventing the sheets from recombining during hydration and ensuring uniform dispersion of the sheets in a monolayer or oligolayer form.

[0040] In some embodiments, the amount added is 0.8-1.5 times the equivalent of the cation exchange capacity. Controlling the amount added within this range is crucial to ensuring sufficient modification without over-addition. Below 0.8 times the equivalent, ion exchange is insufficient, hydrophilic sites remain on the sheets, hydrophobicity is insufficient, and cross-linking strength is weak. Above 1.5 times the equivalent, excess quaternary ammonium salt accumulates on the sheet surface through physical adsorption, interfering with orderly overlap, weakening the continuity of the backbone, and the residue may potentially irritate the lips. This range was determined through orthogonal experimental screening to balance sufficient modification and product purity.

[0041] In some embodiments, the reaction temperature is 60-80°C and the reaction time is 4-8 hours.

[0042] In some embodiments, the film-forming polymer is selected from at least one of polyvinylpyrrolidone K90, polyurethane-35, and acrylate copolymers.

[0043] In some embodiments, the water-locking and moisturizing liquid lip gloss further comprises at least one of the following components: 5-15 parts of pigment dispersion, 2-6 parts of emulsifying and solubilizing system, 0.1-2.0 parts of active ingredient, 0.3-0.8 parts of preservative and / or 0.05-0.2 parts of pH adjuster.

[0044] By optimizing parameters such as cation exchange capacity, quaternary ammonium salt type, addition amount, reaction temperature and time of purified and modified lithium montmorillonite to the range described above, it is possible to ensure the sufficiency of organic modification and the consistency of product quality between batches, enabling the modified lithium montmorillonite to achieve more uniform and sufficient interlayer exfoliation during subsequent hydration and dispersion processes.

[0045] In some embodiments, the emulsified solubilizing system consists of polysorbate-20 and hydrogenated castor oil derivative in a weight ratio of (1-2):(1-3).

[0046] In some embodiments, the active ingredient is selected from at least one of sodium hyaluronate, vitamin E acetate, and panthenol.

[0047] In some embodiments, the preservative is a mixture of phenoxyethanol and ethylhexylglycerin.

[0048] In some embodiments, the pH adjuster is a citric acid solution or a sodium hydroxide solution, used to adjust the pH of the system to 5.5-6.5.

[0049] By selecting an emulsification and solubilization system composed of polysorbate-20 and hydrogenated castor oil derivatives in a specific ratio, uniform emulsification of the oil and water phases can be effectively achieved. By selecting active ingredients such as sodium hyaluronate, vitamin E acetate, and panthenol, the product is endowed with additional moisturizing, antioxidant, and repairing effects. By adjusting the pH value of the system to 5.5-6.5, not only can the preservatives exert their optimal efficacy, but the electrostatic balance between the modified lithium montmorillonite flakes is also ensured to be preserved, maintaining the long-term stability of the network.

[0050] The second aspect of this embodiment provides a method for preparing a water-locking and moisturizing liquid lip gloss as described above, comprising the following steps: Step 1: At 75-85℃, disperse the thixotropic modifier in deionized water at a shear rate of 2000-3500 rpm and continue shearing for 15-25 minutes to form a gel substrate; Step 2: Lower the temperature of the gel substrate to 50-60℃, add the polyol moisturizing compound system and film-forming polymer in sequence, and stir at 30-60 rpm for 20-40 minutes.

[0051] By first dispersing the thixotropic modifier in deionized water at a high temperature of 75-85℃ and a high-speed shearing speed of 2000-3500rpm to form a gel substrate, and then lowering the temperature to 50-60℃ to add a polyol moisturizing compound system and a film-forming polymer, this segmented temperature control strategy can fully promote the interlayer exfoliation and hydration swelling of the organoammonium salt modified lithium montmorillonite, enabling it to form a uniform physical cross-linking network with xanthan gum. At the same time, it effectively protects the molecular integrity of the heat-sensitive film-forming polymer and active ingredients, ensuring the stability and consistency of product quality between batches.

[0052] Through extensive experimentation, the inventors unexpectedly discovered that applying high shear to the lithium montmorillonite and xanthan gum composite system within a specific high-temperature window of 75-85℃ not only did not cause system failure, but the high temperature also promoted the hydration expansion and exfoliation of the modified lithium montmorillonite layers, while simultaneously allowing the xanthan gum molecular chains to fully extend. During this dynamic process, the two components formed a more uniform and dense physical cross-linked network that cannot be achieved through conventional low-temperature mixing. Subsequently, by rapidly cooling and fixing this network, rheological effects unattainable through low-temperature processes were achieved.

[0053] Meanwhile, when polyols and film-forming polymers are added to the aqueous phase before lithium montmorillonite, their molecules preferentially occupy water molecules and encapsulate the subsequently added lithium montmorillonite sheets, hindering their interlayer hydration and delamination; at the same time, xanthan gum cannot fully expand due to insufficient free water. Zero-shear viscosity is significantly reduced, structural recovery is delayed, and the sustained-release capacity of moisturizing components decreases.

[0054] In some embodiments, the thixotropic modifier is pre-dry-mixed in step 1 and then slowly sprinkled into the center of the vortex over 3-5 minutes.

[0055] In some embodiments, after step 2, at least one of the following steps is included: a color paste incorporation step, an emulsification step, a defoaming step, and / or a fragrance blending step.

[0056] By pre-drying and uniformly mixing the thixotropic modifier before slowly adding it to the center of the vortex over 3-5 minutes, it is ensured that the modified lithium montmorillonite and xanthan gum have achieved uniform microscale distribution before being added to the aqueous phase, avoiding local agglomeration or network inhomogeneity caused by differences in hydration rates when added separately. Furthermore, by adding color paste incorporation, emulsification, defoaming, and / or flavoring steps after the core steps, the preparation process can be flexibly adapted to various product formulation requirements.

[0057] In some embodiments, the color paste incorporation step is: adding the pigment dispersion and stirring at a speed of 20-40 rpm for 10-15 minutes.

[0058] In some embodiments, the emulsification step is: adding an emulsification solubilization system and homogenizing at a rate of 1500-2500 rpm for 3-8 minutes.

[0059] In some embodiments, the degassing step is: degassing for 10-20 minutes at a pressure of -0.08 to -0.09 MPa.

[0060] In some embodiments, the fragrance preparation step is as follows: add fragrance and stir at a speed of 20-40 rpm for 5-10 minutes.

[0061] By optimizing process parameters such as rotation speed, time, and vacuum degree in each auxiliary step of color paste incorporation, emulsification, defoaming, and fragrance blending to the aforementioned range, it is possible to achieve uniform color distribution, thorough oil-water emulsification, complete removal of micro-bubbles, and uniform fragrance distribution while protecting the formed gel network structure from damage, ultimately obtaining a liquid lip gloss product with stable quality and excellent performance.

[0062] To better understand the technical solutions of the above embodiments, the following more detailed experimental examples are provided for further explanation. Those skilled in the art will understand that the following examples are for illustrative purposes only and should not be considered as limiting the scope of this disclosure. Where specific techniques or conditions are not specified in the examples, they are performed according to the techniques or conditions described in the literature in the art or according to the product instructions. Reagents or instruments used, unless otherwise specified, are all commercially available conventional products.

[0063] The sources of raw materials for the following examples and comparative examples are shown in Table 1.

[0064] Table 1 Raw material specifications and sources Example 1 Preparation of lithium montmorillonite modified with organic ammonium salt Step 1: Add water to the natural lithium montmorillonite ore to make a slurry. Remove associated impurities such as quartz and feldspar by gravity sedimentation and centrifugal classification to make the montmorillonite content reach more than 90% by weight. Disperse the purified lithium montmorillonite in a 1 mol / L sodium chloride solution and stir at 60℃ for 4 hours to perform sodium modification. After filtration, wash with deionized water until no white precipitate is formed when the filtrate is tested with silver nitrate solution. After drying, obtain modified lithium montmorillonite with a cation exchange capacity (CEC) of 100 meq / 100g.

[0065] Step 2: Disperse the modified lithium montmorillonite in deionized water to form a slurry with a solid content of 5% by weight; under stirring at 75°C, slowly add an ethanol solution of distearate dimethyl ammonium chloride, the amount of quaternary ammonium salt added being 1.2 times the equivalent of the modified lithium montmorillonite CEC; after reacting at a constant temperature for 6 hours, filter, and wash repeatedly with deionized water until no white precipitate is formed when the filtrate is tested with 0.1 mol / L silver nitrate solution; dry the filter cake at 80°C to constant weight, and grind it to a particle size D90≤10μm to obtain the lithium montmorillonite modified with organic ammonium salt.

[0066] By weight, the raw material composition of this embodiment is as follows: 52.0 parts deionized water; 12.0 parts glycerin; 5.0 parts propylene glycol; 3.0 parts polyethylene glycol-400; 5.0 parts polyvinylpyrrolidone K90; 1.2 parts lithium montmorillonite modified with organic ammonium salts as prepared above; 0.6 parts xanthan gum; 10.0 parts iron oxide red dispersion; 1.5 parts polysorbate-20; 2.5 parts hydrogenated castor oil derivative; 1.0 part sodium hyaluronate; 0.6 parts phenoxyethanol / ethylhexylglycerin compound; 0.1 parts 10% citric acid solution; and 0.3 parts fragrance.

[0067] Preparation process: S1. Aqueous phase pretreatment: Deionized water is added to a vacuum emulsifying pot equipped with a vacuum system and a heating jacket. Phenoxyethanol / ethylhexylglycerin compound is added, heated to 80°C, and stirred for 15 minutes.

[0068] S2. Powder Dispersion: Pre-mix the organoammonium salt modified lithium montmorillonite with xanthan gum until homogeneous. Maintain the aqueous phase temperature at 80℃, start a high-speed shear emulsifier, set the shear rate to 3000 rpm, and slowly sprinkle the mixed powder into the center of the vortex over 4 minutes. After the addition is complete, continue shear dispersion at 3000 rpm for 20 minutes until a uniform, transparent gel matrix free of lumps is formed.

[0069] S3. Dissolving and Mixing: Turn on the cooling water system and gradually lower the system temperature to 55°C. Add glycerin, propylene glycol, polyethylene glycol-400, polyvinylpyrrolidone K90, and sodium hyaluronate in sequence. Switch to anchor stirring at 45 rpm and stir for 30 minutes, until all solid components are completely dissolved and the system has a homogeneous, viscous consistency.

[0070] S4. Add color paste: Keep the speed at 30 rpm and slowly add the iron oxide red dispersion paste to the main pot. Continue stirring for 12 minutes to ensure uniform color distribution.

[0071] S5. Emulsification and Fragrance: Add polysorbate-20 and hydrogenated castor oil derivative, start the homogenizer, and homogenize at 2000 rpm for 5 minutes. Then add 10% citric acid solution dropwise to adjust the pH of the system to 6.0. Add fragrance and stir at 30 rpm for 8 minutes.

[0072] S6. Degassing and Filling: Turn on the vacuum system and evacuate the pressure inside the pot to -0.085MPa, maintaining this pressure for 15 minutes to remove microbubbles. Continue cooling to 35℃, then discharge and fill.

[0073] Example 2 This embodiment includes five groups (2a to 2e). Based on the formulation of Example 1, only the internal ratio of the polyol moisturizing compound system is changed. The total amount of polyol remains unchanged at 20.0 parts. The types and amounts of other components and the preparation process are the same as in Example 1.

[0074] Polyol composition of each group: Example 2a: 3.1 parts glycerol, 9.2 parts propylene glycol, 7.7 parts polyethylene glycol-400.

[0075] Example 2b: 10.0 parts glycerol, 6.7 parts propylene glycol, and 3.3 parts polyethylene glycol-400.

[0076] Example 2c: 12.3 parts glycerol, 4.6 parts propylene glycol, and 3.1 parts polyethylene glycol-400.

[0077] Example 2d: 14.3 parts glycerol, 2.9 parts propylene glycol, 2.8 parts polyethylene glycol-400.

[0078] Example 2e: 15.4 parts glycerol, 2.0 parts propylene glycol, 2.6 parts polyethylene glycol-400.

[0079] Example 3 This embodiment includes five groups (3a to 3e), based on the formulation of Example 1, except that the weight ratio of lithium montmorillonite modified with organic ammonium salt to xanthan gum in the thixotropic modifier is changed. The total amount of thixotropic modifier remains unchanged at 1.8 parts. The types and amounts of other components and the preparation process are the same as in Example 1.

[0080] Composition of thixotropic modifiers in each group: Example 3a: 0.36 parts of lithium montmorillonite modified with organic ammonium salt and 1.44 parts of xanthan gum.

[0081] Example 3b: 0.60 parts of lithium montmorillonite modified with organic ammonium salt and 1.20 parts of xanthan gum.

[0082] Example 3c: 0.90 parts of lithium montmorillonite modified with organic ammonium salt and 0.90 parts of xanthan gum.

[0083] Example 3d: 1.35 parts of lithium montmorillonite modified with organic ammonium salt and 0.45 parts of xanthan gum.

[0084] Example 3e: 1.50 parts of lithium montmorillonite modified with organic ammonium salt and 0.30 parts of xanthan gum.

[0085] Example 4 By weight, the raw material composition of this embodiment is as follows: 65.0 parts deionized water; 14.0 parts glycerin; 7.0 parts propylene glycol; 4.0 parts polyethylene glycol-400; 3.0 parts polyvinylpyrrolidone K90; 0.33 parts lithium montmorillonite modified with organic ammonium salts as prepared above; 0.17 parts xanthan gum; 10.0 parts iron oxide red dispersion; 1.5 parts polysorbate-20; 2.5 parts hydrogenated castor oil derivative; 1.0 part sodium hyaluronate; 0.6 parts phenoxyethanol / ethylhexylglycerin compound; 0.1 parts 10% citric acid solution; and 0.3 parts fragrance.

[0086] Liquid lip gloss was prepared using the same method as in Example 1.

[0087] Example 5 By weight, the raw material composition of this embodiment is as follows: 40.0 parts deionized water; 9.0 parts glycerin; 4.0 parts propylene glycol; 2.0 parts polyethylene glycol-400; 8.0 parts polyvinylpyrrolidone K90; 2.0 parts lithium montmorillonite modified with organic ammonium salts as prepared above; 1.0 part xanthan gum; 15.0 parts iron oxide red dispersion; 2.0 parts polysorbate-20; 4.0 parts hydrogenated castor oil derivative; 2.0 parts sodium hyaluronate; 0.8 parts phenoxyethanol / ethylhexylglycerin compound; 0.2 parts 10% citric acid solution; and 0.5 parts fragrance.

[0088] Liquid lip gloss was prepared using the same method as in Example 1.

[0089] Performance testing (1) Rheological property testing Experimental equipment: Rotational rheometer (Anton Paar, MCR 302), with a matching flat plate measuring system (50 mm in diameter, 1.0 mm gap).

[0090] Test conditions: All samples were placed at a constant temperature of 25±1℃ for 24 hours to eliminate historical shear effects before testing.

[0091] Zero-shear viscosity test: Set the shear rate from 0.01 s⁻¹ -1 Linearly increase to 1000 s -1 Record the viscosity as a function of shear rate. Use a time interval of 0.01 s⁻¹. -1 The viscosity value below is zero shear viscosity.

[0092] Structural recovery time t90 test: The sample is subjected to 1000 s... -1 Pre-shear at a high shear rate for 60 seconds (simulating the filling process), then instantly reduce the shear rate to 0.1 s⁻¹ (simulating post-filling resting), and record the viscosity change curve over time. Measure the time t₉₀ required for the viscosity to recover to 90% of its initial value. Each sample was tested three times, and the average value was taken.

[0093] (2) Accelerated stability test Centrifugation test: Take 10g of sample and put it into a centrifuge tube. Centrifuge at 4000rpm for 30 minutes using a high-speed centrifuge (Eppendorf, 5810R) (equivalent to a centrifugal acceleration of about 2000g). Visually observe whether there is oil-water separation, pigment sedimentation or water separation. Measure the layer height, accurate to 0.1mm.

[0094] High and low temperature cycling test: The sample was placed in a 45℃ oven for 24 hours, and then transferred to a -15℃ freezer for 24 hours. This is one cycle, and a total of 5 cycles were performed. After each cycle, the sample was allowed to return to room temperature and the appearance changes were visually observed and rated on a scale of 1 to 5 (5 points = no change; 4 points = slight change but acceptable; 3 points = significant change; 2 points = severe change; 1 point = complete demulsification / delamination).

[0095] (3) Sensory evaluation and moisturizing performance test Experimental conditions: constant temperature and humidity chamber (22±1℃, 50±5% RH).

[0096] Subjects: 30 female volunteers aged 20-45 years with skin types including dry, normal and oily.

[0097] Testing equipment: Corneometer CM 825.

[0098] Moisturizing Increment Test Steps: After volunteers sat quietly in a constant temperature and humidity room for 30 minutes, the initial stratum corneum moisture content of their lips was measured as a baseline. Apply 20mg of the sample to the lower lip and allow it to form a film naturally. The moisture content of the lip stratum corneum was measured at 4 hours and 8 hours after application, and the increase in moisture content ΔHydration (%) was calculated.

[0099] Sensory blind rating process: After application, volunteers conducted a subjective blind evaluation on a scale of 1-10: Stickiness (0 points = extremely sticky and uncomfortable, 10 points = silky smooth and refreshing with no stickiness; the evaluation is based on the resistance felt when separating the lips after lightly touching them with the fingertips). Tightness (0 points for obvious dryness and tightness, 10 points for soft skin with no dryness); Overall recommendation rating (10 points = very willing to recommend).

[0100] Before each evaluation, the lips were calibrated with a standard sample, with a test interval of at least 2 hours. During this period, the lips were cleaned and rested using a gentle makeup remover provided by the company.

[0101] The products prepared in Examples 1-5 were subjected to performance tests, and the test results are shown in Tables 2 and 3.

[0102] Table 2 Table 3 Comparative Example 1 The thixotropic modifier was adjusted to contain only 1.8 parts xanthan gum, without the addition of organoammonium salt modified lithium montmorillonite. The remaining formulation and process are the same as in Example 1.

[0103] Comparative Example 2 The thixotropic modifier was adjusted to contain only 1.8 parts of organoammonium salt modified lithium montmorillonite, without the addition of xanthan gum. The remaining formulation and process are the same as in Example 1.

[0104] Comparative Example 3 In Example 1, the organoammonium salt modified lithium montmorillonite was replaced with an equal amount of unmodified natural lithium montmorillonite (i.e., without quaternary ammonium salt intercalation treatment), while the amount of xanthan gum remained unchanged at 0.6 parts. The remaining formulation and process were the same as in Example 1.

[0105] Comparative Example 4 The thixotropic modifier was adjusted to contain only 1.8 parts of unmodified natural lithium montmorillonite, without the addition of xanthan gum. The remaining formulation and process are the same as in Example 1.

[0106] Comparative Example 5 The thixotropic modifier contains: 0.36 parts of unmodified natural lithium montmorillonite and 1.44 parts of xanthan gum. The remaining formulation and process are the same as in Example 1.

[0107] Comparative Example 6 The polyol moisturizing compound system in Example 1 was completely replaced with 20.0 parts of glycerin, and propylene glycol and polyethylene glycol-400 were no longer added. The rest of the formulation and process were the same as in Example 1.

[0108] Comparative Example 7 The polyol moisturizing compound system in Example 1 was completely replaced with 20.0 parts propylene glycol, and glycerin and polyethylene glycol-400 were no longer added. The rest of the formulation and process were the same as in Example 1.

[0109] Comparative Example 8 The polyol moisturizing compound system in Example 1 was completely replaced with 20.0 parts of polyethylene glycol-400, and glycerin and propylene glycol were no longer added. The rest of the formulation and process were the same as in Example 1.

[0110] Comparative Example 9 By weight, the raw material composition of this comparative example is as follows: 35.0 parts deionized water; 7.0 parts glycerin; 3.0 parts propylene glycol; 2.0 parts polyethylene glycol-400; 2.0 parts polyvinylpyrrolidone K90; 0.24 parts lithium montmorillonite modified with organic ammonium salts as prepared above; 0.12 parts xanthan gum; 6.0 parts iron oxide red dispersion; 1.0 part polysorbate-20; 1.5 parts hydrogenated castor oil derivative; 0.5 parts sodium hyaluronate; 0.3 parts phenoxyethanol / ethylhexylglycerin complex; 0.05 parts 10% citric acid solution; and 0.2 parts fragrance.

[0111] The preparation process is the same as in Example 1.

[0112] Comparative Example 10 The raw material composition of this comparative example, by weight, is as follows: 70.0 parts deionized water; 18.0 parts glycerin; 8.0 parts propylene glycol; 5.0 parts polyethylene glycol-400; 10.0 parts polyvinylpyrrolidone K90; 2.5 parts lithium montmorillonite modified with organic ammonium salts as prepared above; 1.2 parts xanthan gum; 18.0 parts iron oxide red dispersion; 3.0 parts polysorbate-20; 5.0 parts hydrogenated castor oil derivative; 3.0 parts sodium hyaluronate; 1.0 part phenoxyethanol / ethylhexylglycerin compound; 0.3 parts 10% citric acid solution; and 0.6 parts fragrance.

[0113] The preparation process is the same as in Example 1.

[0114] Comparative Example 11 By weight, the raw material composition of this comparative example is the same as that of Example 1: 52.0 parts deionized water; 12.0 parts glycerin; 5.0 parts propylene glycol; 3.0 parts polyethylene glycol-400; 5.0 parts polyvinylpyrrolidone K90; 1.2 parts lithium montmorillonite modified with organic ammonium salt; 0.6 parts xanthan gum; 10.0 parts iron oxide red dispersion; 1.5 parts polysorbate-20; 2.5 parts hydrogenated castor oil derivative; 1.0 part sodium hyaluronate; 0.6 parts phenoxyethanol / ethylhexylglycerin compound; 0.1 parts 10% citric acid solution; and 0.3 parts fragrance.

[0115] Preparation process: S1. Aqueous phase pretreatment: Deionized water is added to a vacuum emulsifying pot equipped with a vacuum system and a heating jacket. Phenoxyethanol / ethylhexylglycerin compound is added, heated to 55°C, and stirred for 15 minutes.

[0116] S2. Dissolving and mixing: Keep the aqueous phase temperature at 55℃, add glycerol, propylene glycol, polyethylene glycol-400, polyvinylpyrrolidone K90 and sodium hyaluronate in sequence, stir with anchor stirring at 45 rpm for 30 minutes until completely dissolved, and the system is homogeneous and viscous.

[0117] S3. Heating and Dispersion: Raise the system temperature to 80℃, start the high-speed shear emulsifier, and set the shear rate to 3000 rpm. After pre-dry mixing the organoammonium salt modified lithium montmorillonite and xanthan gum evenly, slowly sprinkle it into the center of the vortex over 4 minutes. After the feeding is complete, continue to maintain shear dispersion at 3000 rpm for 20 minutes.

[0118] S4. Cooling: Turn on the cooling water system to lower the system temperature to 55℃.

[0119] S5. Add color paste: Keep the speed at 30 rpm and slowly add the iron oxide red dispersion paste, stirring for 12 minutes.

[0120] S6. Emulsification and Fragrance: Add polysorbate-20 and hydrogenated castor oil derivative, and homogenize at 2000 rpm for 5 minutes. Adjust the pH to 6.0 by adding 10% citric acid solution dropwise, add fragrance, and stir at 30 rpm for 8 minutes.

[0121] S7. Degassing and Filling: Degas for 15 minutes under a pressure of -0.085MPa, then cool to 35℃ for discharge and filling.

[0122] Comparative Example 12 Preparation of modified lithium montmorillonite: The purified and modified lithium montmorillonite was mixed with γ-aminopropyltriethoxysilane at a weight ratio of 100:3, and thiourea equivalent to 0.5% of the total powder weight was added. The mixture was then ball-milled in a planetary ball mill at 400 rpm for 2 hours. After removal, it was dried at 80℃ and ground until D90≤10μm to obtain silane coupling agent modified lithium montmorillonite.

[0123] The raw material composition of this comparative example, by weight, is as follows: 52.0 parts deionized water; 12.0 parts glycerin; 5.0 parts propylene glycol; 3.0 parts polyethylene glycol-400; 5.0 parts polyvinylpyrrolidone K90; 1.2 parts lithium montmorillonite modified with the silane coupling agent prepared above; 0.6 parts xanthan gum; 10.0 parts iron oxide red dispersion; 1.5 parts polysorbate-20; 2.5 parts hydrogenated castor oil derivative; 1.0 part sodium hyaluronate; 0.6 parts phenoxyethanol / ethylhexylglycerin compound; 0.1 parts 10% citric acid solution; and 0.3 parts fragrance.

[0124] The preparation process is the same as in Example 1.

[0125] Comparative Example 13 By weight, the raw material composition of this comparative example is the same as that of Example 1, except that 1.2 parts of organoammonium salt modified lithium montmorillonite and 0.6 parts of xanthan gum are replaced with 1.8 parts of BENTONE HYDROCLAY™ 700 (purchased from Elementis Specialties, INCI name: hydrangea (and) xanthan gum). The preparation process is the same as that of Example 1, namely, a segmented temperature-controlled process of high-temperature and high-speed dispersion at 75-85℃, followed by cooling to 50-60℃ and adding polyol.

[0126] Using the same performance testing method as in the above embodiments, the performance of the products in Comparative Examples 1-13 was tested, and the test results are shown in Tables 4 and 5.

[0127] Table 4 Table 5 In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," "some implementations," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0128] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A water-locking and moisturizing liquid lip gloss, characterized in that, It is made from the following components in parts by weight: 40-65 parts deionized water; A polyol moisturizing compound system of 15-25 parts, wherein the polyol moisturizing compound system is composed of glycerin, propylene glycol and polyethylene glycol with a number average molecular weight of 200-600; 3-8 parts of film-forming polymer; 0.5-3.0 parts of a thixotropic modifier, wherein the thixotropic modifier is composed of a mixture of lithium montmorillonite modified with an organic ammonium salt and xanthan gum.

2. The water-locking and moisturizing liquid lip gloss according to claim 1, characterized in that, The weight ratio of glycerin, propylene glycol and polyethylene glycol in the polyol moisturizing compound system is (3-5):(1-2):(0.5-1.5).

3. The water-locking and moisturizing liquid lip gloss according to claim 1, characterized in that, The weight ratio of lithium montmorillonite modified with organic ammonium salt to xanthan gum in the thixotropic modifier is (1-3):(1-2).

4. The water-locking and moisturizing liquid lip gloss according to claim 1, characterized in that, The modified lithium montmorillonite with organic ammonium salts is prepared by the following method: the purified and modified lithium montmorillonite is dispersed in deionized water to form a slurry, and a quaternary ammonium salt solution containing long-chain alkyl groups is added under stirring conditions to carry out an ion exchange reaction. After the reaction is completed, the solution is filtered, washed, dried and ground to obtain the final product.

5. The water-locking and moisturizing liquid lip gloss according to claim 4, characterized in that, The purified and modified lithium montmorillonite has a cation exchange capacity of 80-120 meq / 100g, and / or the quaternary ammonium salt is at least one of distearyldimethylammonium chloride, octadecyltrimethylammonium chloride, or bis(hydrogenated tallow)dimethylammonium chloride; and / or the amount added is 0.8-1.5 times the equivalent of the cation exchange capacity; and / or the reaction temperature is 60-80℃ and the reaction time is 4-8 hours.

6. The water-locking and moisturizing liquid lip gloss according to any one of claims 1-5, characterized in that, The film-forming polymer is selected from polyvinylpyrrolidone K90, polyurethane-35 and / or acrylic (ester) copolymers; and / or, the water-locking and moisturizing liquid lip gloss further comprises at least one of the following components: 5-15 parts of pigment dispersion, 2-6 parts of emulsifying and solubilizing system, 0.1-2.0 parts of active ingredient, 0.3-0.8 parts of preservative and / or 0.05-0.2 parts of pH adjuster.

7. The water-locking and moisturizing liquid lip gloss according to claim 6, characterized in that, The emulsified solubilizing system is composed of polysorbate-20 and hydrogenated castor oil derivative in a weight ratio of (1-2):(1-3); and / or, the active ingredient is selected from at least one of sodium hyaluronate, vitamin E acetate, and panthenol; and / or, the preservative is a compound of phenoxyethanol and ethylhexylglycerin; and / or, the pH adjuster is a citric acid solution or a sodium hydroxide solution, used to adjust the pH of the system to 5.5-6.

5.

8. A method for preparing a water-locking and moisturizing liquid lip gloss as described in any one of claims 1-7, characterized in that, Includes the following steps: Step 1: At 75-85℃, disperse the thixotropic modifier in deionized water at a shear rate of 2000-3500 rpm and continue shearing for 15-25 minutes to form a gel substrate; Step 2: Lower the temperature of the gel substrate to 50-60℃, add the polyol moisturizing compound system and film-forming polymer in sequence, and stir at 30-60 rpm for 20-40 minutes.

9. The preparation method according to claim 8, characterized in that, The thixotropic modifier is pre-dry-mixed in step 1 and then slowly sprinkled into the center of the vortex over 3-5 minutes; and / or, after step 2, at least one of the following steps is also included: color paste incorporation step, emulsification step, defoaming step and / or fragrance step.

10. The preparation method according to claim 9, characterized in that, The color paste incorporation step is as follows: add pigment dispersion and stir at 20-40 rpm for 10-15 minutes; the emulsification step is as follows: add emulsification and solubilization system and homogenize at 1500-2500 rpm for 3-8 minutes; the degassing step is as follows: degas at -0.08 to -0.09 MPa pressure for 10-20 minutes; the fragrance step is as follows: add fragrance and stir at 20-40 rpm for 5-10 minutes.

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