Antidiscoloration composition for selenium disulfide preparations, method of preparation and use
Patent Information
- Application Number
- CN202611052196.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-07-15
- Publication Date
- 2026-08-18
AI Technical Summary
但二硫化硒化学性质不稳定,极易被空气氧化,尤其在高浓度体系(质量分数≥10%)中,常温避光放置数小时即可出现发黄、变褐、发黑等变色现象,不仅导致产品外观不合格,还会伴随二硫化硒活性成分降解、去屑效果下降,同时可能增加产品对头皮的刺激性,严重影响产品品质与使用体验
[0033] In the aforementioned anti-discoloration composition, the composite zinc salt, through its own antioxidant properties, captures free radicals generated during the oxidation of selenium disulfide, inhibiting the oxidation reaction process. At the same time, it enhances the synergistic anti-discoloration effect of anti-discoloration agent 1 and anti-discoloration agent 2. The preservative can achieve efficient preservation without interfering with the anti-discoloration and antioxidant properties. The selenium disulfide preparation made using this anti-discoloration composition is not prone to discoloration, has high storage stability, is not prone to deterioration, and is mild and non-irritating.
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Figure CN122582029A_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the field of daily chemical raw material technology, and relates to anti-discoloration composition for selenium disulfide preparations, preparation method and application. Background Technology
[0002] Selenium disulfide, as a highly effective anti-dandruff and antifungal active ingredient, is widely used in daily chemical scalp care products, especially in high-concentration selenium disulfide powder and end-use anti-dandruff products, where its anti-dandruff effect is particularly prominent. However, selenium disulfide is chemically unstable and is easily oxidized by air, especially in high-concentration systems (mass fraction ≥10%). After being left at room temperature and away from light for several hours, it can turn yellow, brown, or black, resulting in substandard product appearance, degradation of the active ingredient, decreased anti-dandruff effect, and potentially increased scalp irritation, severely impacting product quality and user experience. Summary of the Invention
[0003] Therefore, it is necessary to provide an anti-discoloration composition for selenium disulfide preparations, a preparation method, and an application for inhibiting discoloration of selenium disulfide and improving the storage stability of selenium disulfide.
[0004] In some embodiments, an anti-coloring composition for selenium disulfide preparations is provided, comprising, by weight, 50 to 85 parts of anti-coloring agent No. 1, 30 to 68 parts of anti-coloring agent No. 2, 6 to 27 parts of compound zinc salt, and 5 to 10 parts of preservative.
[0005] The anti-discoloration agent No. 1 comprises colloidal sulfur, zinc pyrrolidone carboxylate, cationic starch and a first solvent, wherein the mass ratio of the colloidal sulfur, the zinc pyrrolidone carboxylate, the cationic starch and the first solvent is (10~20):(20~35):(2~5):(50~65).
[0006] The anti-discoloration agent No. 2 contains hymex chloride;
[0007] The composite zinc salt comprises zinc glycinate, zinc carbonate, and zinc laurate.
[0008] In some embodiments, the provided anti-coloring composition for selenium disulfide preparations comprises, by weight, 50 to 70 parts of anti-coloring agent No. 1, 30 to 50 parts of anti-coloring agent No. 2, 10 to 20 parts of compound zinc salt, and 5 to 10 parts of preservative.
[0009] In some embodiments, the provided anti-coloring composition for selenium disulfide preparations comprises, by weight, 55 to 65 parts of anti-coloring agent No. 1, 35 to 45 parts of anti-coloring agent No. 2, 13 to 18 parts of compound zinc salt, and 5 to 10 parts of preservative.
[0010] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations satisfies one or more of the following conditions:
[0011] (1) The preservative contains phenoxyethanol;
[0012] (2) The composite zinc salt contains, by weight percentage, 40%~60% zinc glycinate, 20%~30% zinc carbonate, and 10%~20% zinc laurate;
[0013] (3) The cationic starch comprises starch hydroxypropyltrimethylammonium chloride;
[0014] (4) The particle size of the sulfur particles in the colloidal sulfur is 20 nm to 200 nm;
[0015] (5) The method for preparing the colloidal sulfur includes the following steps: mixing sulfur with an aqueous solution containing a dispersant and performing wet milling to prepare the colloidal sulfur; wherein the mass fraction of the dispersant in the aqueous solution containing the dispersant is 5wt%~15wt%, the mass ratio of the sulfur to the aqueous solution containing the dispersant is 1:(3~5), the wet milling time is 2~6h, and the dispersant contains gum arabic;
[0016] (6) The first solvent contains water.
[0017] In some embodiments, a method for preparing the anti-discoloration composition for selenium disulfide formulations is provided, comprising the following steps:
[0018] The anti-discoloration agent No. 1, the anti-discoloration agent No. 2, and the composite zinc salt are mixed, and a preservative is added for further mixing to prepare the anti-discoloration composition for selenium disulfide preparations.
[0019] In some embodiments, a selenium disulfide formulation is provided, comprising, by mass fraction, 10% to 30% selenium disulfide, 9% to 13% of the anti-discoloration composition, 10% to 40% of a humectant, 10% to 30% of a surfactant, 10% to 30% of a suspending agent, and 0% to 51% of a second solvent.
[0020] In some embodiments, the provided selenium disulfide formulation satisfies one or more of the following conditions:
[0021] (1) The moisturizer comprises one or more of glycerin, caprylic / capric triglyceride and propylene glycol;
[0022] (2) The surfactant comprises one or more of cocamidopropyl betaine, cocoyl diethanolamide, cocoyl methyl monoethanolamide and sodium cocoyl sarcosinate;
[0023] (3) The suspending agent contains one or both of emulsified hydrogenated castor oil and tristearate;
[0024] (4) The second solvent contains water; and
[0025] (5) The dosage form of the selenium disulfide preparation includes at least one of the following: powder, suspension, cream and gel.
[0026] In some embodiments, a method for preparing the selenium disulfide preparation is provided, comprising the following steps:
[0027] The selenium disulfide, the anti-discoloration composition, the humectant, the surfactant, the suspending agent, and the second solvent are mixed and ground under stirring conditions to prepare the selenium disulfide preparation.
[0028] Optionally, the stirring speed is 300 rpm to 800 rpm, and the stirring time is 30 min to 2 h.
[0029] In some embodiments, the use of the selenium disulfide preparation is provided in the preparation of anti-dandruff care products.
[0030] In some embodiments, an anti-dandruff care product is provided, comprising the aforementioned selenium disulfide preparation;
[0031] Optionally, the selenium disulfide preparation in the dandruff care product has a mass fraction of 1% to 5%.
[0032] In some embodiments, the dandruff care product includes at least one of anti-dandruff shampoo, scalp serum, hair conditioner, and 2-in-1 shampoo and conditioner.
[0033] In the aforementioned anti-discoloration composition, the composite zinc salt, through its own antioxidant properties, captures free radicals generated during the oxidation of selenium disulfide, inhibiting the oxidation reaction process. At the same time, it enhances the synergistic anti-discoloration effect of anti-discoloration agent 1 and anti-discoloration agent 2. The preservative can achieve efficient preservation without interfering with the anti-discoloration and antioxidant properties. The selenium disulfide preparation made using this anti-discoloration composition is not prone to discoloration, has high storage stability, is not prone to deterioration, and is mild and non-irritating. Attached Figure Description
[0034] To more clearly illustrate the technical solutions in the embodiments and examples of this application, and to more completely understand this application and its beneficial effects, the accompanying drawings used in the description of the embodiments or examples will be briefly introduced below. Obviously, the drawings described below are merely some embodiments of this application. Those skilled in the art can obtain other drawings based on these drawings without any creative effort.
[0035] Fig. 1The first field of view is the transmission polarized light detection result of selenium disulfide slurry in Example 1, with a magnification of 50x and a scale bar of 500μm.
[0036] Fig. 2 The second field of view is the transmission polarized light detection result of selenium disulfide slurry in Example 1, with a magnification of 50x and a scale bar of 500μm.
[0037] Fig. 3 The third field of view is the transmission polarized light detection result of selenium disulfide slurry in Example 1, with a magnification of 100x and a scale bar of 200μm.
[0038] Fig. 4 The fourth field of view is the transmission polarized light detection result of the selenium disulfide slurry in Example 1. The magnification is 100x and the scale bar is 200μm. Detailed Implementation
[0039] To facilitate understanding of the present invention, a more complete description will be given below with reference to the accompanying drawings. Preferred embodiments of the invention are shown in the drawings. However, the invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the invention.
[0040] It should be noted that when a component is said to be "fixed to" another component, it can be directly attached to the other component or there may be an intervening component. When a component is said to be "connected to" another component, it can be directly connected to the other component or there may be an intervening component.
[0041] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.
[0042] Unless otherwise stated or in case of contradiction, the terms or phrases used herein shall have the following meanings:
[0043] The terms "and / or," "or / and," and "and / or" as used in this application encompass any one of two or more related listed items, as well as any and all combinations of the related listed items. These arbitrary and all combinations include any two related listed items, any more related listed items, or a combination of all related listed items. It should be noted that when at least three items are connected using at least two conjunctions selected from "and / or," "or / and," and "and / or," it should be understood that in this application, the technical solution undoubtedly includes solutions connected by "logical AND," and also undoubtedly includes solutions connected by "logical OR." For example, "A and / or B" includes three parallel solutions: A, B, and "a combination of A and B."
[0044] In this application, the terms "multiple", "various", "multiple times", "multi-dimensional", etc., unless otherwise specified, refer to a quantity greater than or equal to 2. For example, "one or more" means one or more than or equal to two.
[0045] The terms “combinations thereof,” “any combination thereof,” and “any combination thereof” as used in this application include all suitable combinations of any two or more of the listed items.
[0046] In this application, the term "suitable" as used in "suitable combination", "suitable method", "any suitable method", etc., refers to the ability to implement the technical solution of this application, solve the technical problem of this application, and achieve the expected technical effect of this application.
[0047] In this application, terms such as "preferred," "better," "more suitable," and "ideal" are merely used to describe implementation methods or embodiments that achieve better results, and should be understood not to limit the scope of protection of this application.
[0048] In this application, terms such as "further," "even further," and "particularly" are used to describe purposes and indicate differences in content, but should not be construed as limiting the scope of protection of this application.
[0049] In this application, "optionally," "optionally," and "optional" mean that something is optional, that is, it means that it is selected from either "with" or "without." If there are multiple "optional" entries in a technical solution, unless otherwise specified, and there are no contradictions or mutual constraints, each "optional" entry shall be independent.
[0050] In this invention, the terms "first aspect," "second aspect," "third aspect," and "fourth aspect," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or quantity, nor should they be construed as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first," "second," "third," and "fourth," etc., serve only as a non-exhaustive enumeration and should be understood not to constitute a closed limitation on quantity.
[0051] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.
[0052] In this application, numerical intervals (i.e., numerical ranges) are involved. Unless otherwise specified, the selected numerical distributions within the aforementioned numerical intervals are considered continuous and include the two endpoints (i.e., the minimum and maximum values) of the numerical range, as well as every value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints. In this document, this is equivalent to directly listing every integer. For example, if t is an integer selected from 1 to 10, it means that t is any integer selected from the group of integers consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10. Furthermore, when multiple ranges are provided to describe features or characteristics, these ranges can be merged. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all subranges to which they are included.
[0053] Unless otherwise specified, the temperature parameters in this application are permitted to be either constant-temperature treatment or variations within a certain temperature range. It should be understood that the constant-temperature treatment allows temperature fluctuations within the precision range of the instrument control, such as ±5℃, ±4℃, ±3℃, ±2℃, or ±1℃.
[0054] In this application, % (w / w) and wt% both represent weight percentage, % (v / v) refers to volume percentage, and % (w / v) refers to mass-volume percentage.
[0055] In this application, "room temperature" generally refers to 5℃~30℃, and more preferably 25±5℃.
[0056] In this application, unless otherwise specified, "for use in selenium disulfide formulations" means that it can be used to prepare selenium disulfide formulations (that is, it can be used as a raw material for the preparation of selenium disulfide formulations) or can be used as at least a portion of the components in selenium disulfide formulations.
[0057] In this application, the mass fraction of caprylic acid in the caprylic / capric triglyceride is 55% to 65%, and the mass fraction of capric acid is 35% to 45%.
[0058] Currently, common technical means to solve the discoloration problem of selenium disulfide mainly include: 1. using reducing agents and antioxidants (such as sulfites, vitamin E, citric acid, etc.); 2. using chelating agents and light-blocking agents; 3. adjusting the pH value of the system and adopting auxiliary methods such as light-proof and sealed storage. Solutions to corrosion problems often use single preservatives without synergistic design with the anti-discoloration system.
[0059] The aforementioned existing technologies have significant drawbacks: First, current anti-discoloration methods have limited effectiveness, especially in high-concentration selenium disulfide systems, where rapid discoloration cannot be prevented. Second, due to the unique chemical properties of selenium disulfide, existing compound formulations are mostly general-purpose antioxidant combinations, which cannot effectively prevent discoloration. Third, conventional anti-discoloration agents often affect the dispersibility and suspension stability of selenium disulfide, or have poor compatibility with commonly used surfactants, humectants, and suspending agents in daily chemical products, leading to system stratification and particle agglomeration. Fourth, conventional preservatives have poor compatibility with anti-discoloration systems, failing to achieve both anti-discoloration and preservative effects, easily resulting in problems such as "effective anti-discoloration but system deterioration" or "preservative standards met but severe discoloration." Fifth, even with light-proof and sealed storage, pre-prepared high-concentration selenium disulfide slurry will still exhibit browning, activity reduction, and microbial growth after long-term storage, failing to fundamentally solve the problem.
[0060] In some embodiments, a special compound system is provided that is synergistic, efficient, compatible, and suitable for high-concentration selenium disulfide systems. It also has anti-discoloration and anti-corrosion functions without affecting the product's activity and mildness, thus solving the technical pain points of selenium disulfide being easily oxidized and discolored, the system being easily deteriorated, and difficult to maintain long-term stability in the prior art.
[0061] In some embodiments, an anti-discoloration composition is provided that can significantly inhibit the oxidative browning of selenium disulfide and improve the storage stability of selenium disulfide. Non-limitingly, the provided anti-discoloration composition can be used to prepare formulations containing high concentrations of selenium disulfide and anti-dandruff shampoos and conditioners.
[0062] In some embodiments, an anti-coloring composition for selenium disulfide preparations is provided, comprising, by weight, 50 to 85 parts of anti-coloring agent No. 1, 30 to 68 parts of anti-coloring agent No. 2, 6 to 27 parts of compound zinc salt, and 5 to 10 parts of preservative.
[0063] The anti-discoloration agent No. 1 comprises colloidal sulfur, zinc pyrrolidone carboxylate, cationic starch and a first solvent, wherein the mass ratio of colloidal sulfur, zinc pyrrolidone carboxylate, cationic starch and the first solvent is (10~20):(20~35):(2~5):(50~65).
[0064] The anti-discoloration agent No. 2 contains hymex chloride;
[0065] The composite zinc salt comprises zinc glycinate, zinc carbonate, and zinc laurate.
[0066] In a non-limiting sense, Anti-coloring Agent 1 is the core anti-coloring component, whose main function is to capture some of the free radicals generated during the oxidation of selenium disulfide, inhibit the change in the valence state of selenium, delay the color change process, and form a basic anti-coloring synergistic system with hyaluronic acid chloride. Anti-coloring Agent 2 is an auxiliary anti-coloring component, which can stabilize the crystal form of selenium disulfide, reduce particle agglomeration, and at the same time help inhibit the oxidation reaction. It works synergistically with Anti-coloring Agent 1 to enhance the anti-coloring effect and improve the dispersion stability of the system. The composite zinc salt can play an antioxidant role. Its mechanism of action is to remove a large number of reactive oxygen free radicals generated during the oxidation of selenium disulfide, inhibit the oxidation chain reaction, delay the oxidation and color change of selenium disulfide from the root, and at the same time enhance the anti-coloring synergistic effect of Anti-coloring Agent 1 and Anti-coloring Agent 2, regulate the rheological properties of the system, further improve the dispersibility of selenium disulfide particles, and has no antagonistic effect with the first two anti-coloring agents. Preservatives, such as phenoxyethanol, can effectively inhibit the growth of bacteria, fungi and other microorganisms, and extend the shelf life of selenium disulfide preparations. Their mechanism of action is to destroy the cell membrane structure of microorganisms and interfere with ATP synthesis. They have an inhibitory effect on bacteria, yeast and some molds. They also have excellent compatibility with the anti-discoloration-antioxidant core system (anti-discoloration agent 1 + anti-discoloration agent 2 + compound zinc salt), do not interfere with the anti-discoloration and antioxidant effects, do not increase the irritation of the system, and can also be used as a solvent to help dissolve some fat-soluble components and improve the stability of the formula.
[0067] In some embodiments, the mass ratio of anti-discoloration agent 1, anti-discoloration agent 2, composite zinc salt, and preservative in the provided anti-discoloration composition can be 6:4:1.5:0.8.
[0068] The components in the provided anti-discoloration composition work synergistically to achieve anti-discoloration, antioxidant, and preservative effects. Excessive addition of the complex zinc salt can cause agglomeration of the selenium disulfide formulation system, while insufficient addition will fail to achieve the desired antioxidant effect. Excessive addition of the preservative will cause irritation, while insufficient addition will fail to meet the preservative requirements.
[0069] Understandably, in the provided anti-coloring composition for selenium disulfide preparations, anti-coloring agent No. 1 can be 50 to 85 parts by weight, or 50 to 70 parts, or even 55 to 65 parts, for example, 50, 55, 60, 65, 70, 75, 80, 85 parts, etc., or any range of the aforementioned two values.
[0070] Understandably, in the provided anti-coloring composition for selenium disulfide preparations, anti-coloring agent No. 2 can be 30 to 68 parts by weight, or 30 to 50 parts, or even 35 to 45 parts, for example, 30, 35, 40, 45, 50, 55, 60, 65, 68 parts, etc., or any range of the aforementioned two values.
[0071] Understandably, in the provided anti-discoloration composition for selenium disulfide preparations, the composite zinc salt, by weight, can be 6 to 27 parts, or 10 to 20 parts, or even 13 to 18 parts, for example, 6 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 25 parts, 27 parts, etc., or any range of the aforementioned two values.
[0072] Understandably, in the provided anti-discoloration composition for selenium disulfide preparations, the preservative may be 5 to 10 parts by weight, for example, 5, 6, 7, 8, 9, 10 parts, etc., or may be a range of any two of the aforementioned values.
[0073] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations includes phenoxyethanol as the preservative. Using the aforementioned preservative can achieve highly efficient corrosion protection without interfering with anti-discoloration and antioxidant properties.
[0074] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations comprises, by weight percentage, 40% to 60% zinc glycinate, 20% to 30% zinc carbonate, and 10% to 20% zinc laurate.
[0075] Understandably, the complex zinc salt may contain, by weight percentage, 40%, 45%, 50%, 55%, 60% zinc glycinate, or any range of any two of the aforementioned values; by weight percentage, it may contain 20%, 25%, 30% zinc carbonate, or any range of any two of the aforementioned values; by weight percentage, it may contain 10%, 15%, 20% zinc laurate, or any range of any two of the aforementioned values.
[0076] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations includes a cationic starch comprising starch hydroxypropyltrimethylammonium chloride. Starch hydroxypropyltrimethylammonium chloride is obtained by chemically attaching a positively charged group (hydroxypropyltrimethylammonium chloride) to the starch molecule. In some embodiments, the degree of substitution of starch hydroxypropyltrimethylammonium chloride is ≥0.03%, and the nitrogen content is 0.15~0.5%. In some embodiments, starch hydroxypropyltrimethylammonium chloride is available from Dongguan Dongmei Food Co., Ltd.
[0077] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations has a particle size of 20nm to 200nm in the colloidal sulfur, for example, 20nm, 50nm, 100nm, 150nm, 200nm, etc., or it can be a range composed of any two of the aforementioned values.
[0078] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations includes a method for preparing colloidal sulfur comprising the following steps: mixing sulfur with an aqueous solution containing a dispersant and performing wet milling to prepare the colloidal sulfur; wherein the mass fraction of the dispersant in the aqueous solution containing the dispersant is 5wt%~15wt%, the mass ratio of the sulfur to the aqueous solution containing the dispersant is 1:(3~5), the wet milling time is 2~6h, and the dispersant comprises gum arabic;
[0079] In some embodiments, the provided anti-discoloration composition for selenium disulfide preparations includes a first solvent comprising water.
[0080] In some embodiments, a method for preparing the anti-discoloration composition for selenium disulfide formulations is provided, comprising the following steps:
[0081] The anti-discoloration agent No. 1, the anti-discoloration agent No. 2, and the composite zinc salt are mixed, and a preservative is added for further mixing to prepare the anti-discoloration composition for selenium disulfide preparations.
[0082] In some embodiments, in the preparation method of the provided anti-discoloration composition, the preservative is added when the system is cooled to below 45°C to avoid its volatilization due to high temperature, which would affect the anti-corrosion effect.
[0083] In some embodiments, a selenium disulfide formulation is provided, comprising, by mass fraction, 10% to 30% selenium disulfide, 9% to 13% of the anti-discoloration composition, 10% to 40% of a humectant, 10% to 30% of a surfactant, 10% to 30% of a suspending agent, and 0% to 51% of a second solvent.
[0084] Understandably, in the provided selenium disulfide preparation, by mass fraction, selenium disulfide can be 10% to 30%, for example, 10%, 15%, 20%, 25%, 30%, etc., or any range of any two of the aforementioned values; the anti-discoloration composition can be 9% to 13%, or 10% to 11%, for example, 9%, 10%, 11%, 12%, 13%, etc., or any range of any two of the aforementioned values; the humectant can be 10% to 40%, for example, 10%, 15%, 20%, 25%, 30%, 35%, 40%, etc., or any two of the aforementioned values. The range of values for the surfactant can be 10% to 30%, for example, 10%, 15%, 20%, 25%, 30%, etc., or any two of the aforementioned values; the range of values for the suspending agent can be 10% to 30%, for example, 10%, 15%, 20%, 25%, 30%, etc., or any two of the aforementioned values; the range of values for the second solvent can be 0% to 51%, for example, 0%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 51%, etc., or any two of the aforementioned values.
[0085] In some embodiments, the provided selenium disulfide formulation includes a humectant comprising one or more of glycerin, caprylic / capric triglyceride, and propylene glycol.
[0086] In some embodiments, the provided selenium disulfide formulation contains a surfactant comprising one or more of cocamidopropyl betaine, cocoyl diethanolamide, cocoyl methyl monoethanolamide, and sodium cocoyl sarcosinate.
[0087] In some embodiments, the provided selenium disulfide formulation includes a suspension comprising one or both of emulsified hydrogenated castor oil and tristearate.
[0088] In some embodiments, the method for preparing emulsified hydrogenated castor oil includes the following steps:
[0089] Hydrogenated castor oil was mixed with cocamidomethyl monoethanolamine (cocamidomethyl MEA) under first heating and first stirring conditions to prepare an oil phase;
[0090] Aqueous phase was prepared by mixing water and disodium lauryl sulfosuccinate, and then adding cocamidopropyl betaine.
[0091] Under the conditions of second heating and second stirring of the aqueous phase, the oil phase is added to the aqueous phase and dispersed and crystallized under the conditions of third stirring to prepare the emulsified hydrogenated castor oil; in some embodiments, the temperatures of the first heating and the second heating are each independently 80°C to 90°C, the speeds of the first stirring and the second stirring are each independently 300 rpm to 800 rpm, and the speed of the third stirring is 3000 rpm to 8000 rpm.
[0092] In some embodiments, the provided selenium disulfide formulation has a second solvent comprising water.
[0093] In some embodiments, the provided selenium disulfide formulation comprises at least one of a powder, suspension, cream, and gel.
[0094] In some embodiments, a method for preparing the selenium disulfide preparation is provided, comprising the following steps:
[0095] The selenium disulfide, the anti-discoloration composition, the humectant, the surfactant, the suspending agent, and the second solvent are mixed and ground under stirring conditions to prepare the selenium disulfide preparation.
[0096] In some embodiments, the preparation method of the provided selenium disulfide preparation involves a stirring speed of 300 rpm to 800 rpm and a stirring time of 30 min to 2 h.
[0097] In some embodiments, the use of the selenium disulfide preparation is provided in the preparation of anti-dandruff care products.
[0098] In some embodiments, an anti-dandruff care product is provided, comprising the aforementioned selenium disulfide preparation.
[0099] For example, anti-dandruff care products may also include one or more of solvents, surfactants, thickeners, suspending agents, emulsifiers, preservatives, pH adjusters, chelating agents, fragrances, and colorants.
[0100] In some embodiments, the raw materials for preparing the anti-dandruff care product include the aforementioned selenium disulfide preparation.
[0101] In some embodiments, the anti-dandruff care product includes a non-solvent component of a selenium disulfide formulation.
[0102] In this application, unless otherwise specified, "non-solvent components" in a selenium sulfide formulation refers to components in a selenium sulfide formulation other than solvent components (such as water). Typically, when a selenium sulfide formulation is concentrated, at least a portion of the solvent components can evaporate, while the non-solvent components are retained in the concentrate.
[0103] In some embodiments, the selenium disulfide preparation in the provided anti-dandruff care product has a mass fraction of 1% to 5%.
[0104] In some embodiments, the dandruff care product includes at least one of anti-dandruff shampoo, scalp serum, hair conditioner, and 2-in-1 shampoo and conditioner.
[0105] The following are specific embodiments. They are intended to provide a further detailed description of this application to help those skilled in the art and researchers better understand it. The technical conditions and other details do not constitute any limitation on this application. Any modifications made within the scope of the claims of this application are within the protection scope of the claims.
[0106] Unless otherwise stated, all raw materials and reagents used in the following examples are commercially available or can be prepared by known methods. Experimental methods not specifying particular conditions in the examples were performed under conventional conditions, such as those described in literature, books, or methods recommended by the manufacturer.
[0107] The preparation method of colloidal sulfur includes the following steps: dissolving gum arabic in water to prepare a 10wt% gum arabic aqueous solution; adding sulfur powder to the gum arabic aqueous solution at a mass ratio of 1:4; wet grinding for 5 hours in a circulating manner; grinding the sulfur particles to 20~200nm; allowing the dispersant gum arabic to coat the sulfur particles to form water-based colloidal sulfur; filtering out coarse particles to obtain the finished product.
[0108] The preparation method of emulsified hydrogenated castor oil includes the following steps:
[0109] 1. Preparation of the oil phase: Hydrogenated castor oil solid was mixed with cocoamide MEA and heated to 85°C while stirring until it was completely melted into a yellow transparent oily liquid;
[0110] 2. Aqueous phase preparation: Add deionized water and disodium lauryl sulfosuccinate, stir for 5 minutes until completely dissolved, then add cocamidopropyl betaine, stir for 5 minutes until completely dissolved;
[0111] 3. At 85℃, slowly add the oil phase to the aqueous phase while keeping the aqueous phase stirred at high speed. After adding the oil phase, keep stirring at high speed for 30 minutes to fully disperse the hydrogenated castor oil into tiny droplets.
[0112] 4. Cool down and crystallize to prepare emulsified hydrogenated castor oil.
[0113] The starch used is hydroxypropyltrimethylammonium chloride, manufactured by Dongguan Dongmei Food Co., Ltd., and its product model is DM-858F.
[0114] Examples 1 to 7 and Comparative Examples 1 to 9
[0115] Examples 1 to 7 and Comparative Examples 1 to 9 each provide an anti-discoloration composition for selenium disulfide preparations. The content of each component is in parts by weight, and the formulation is shown in Table 1 below.
[0116] Table 1
[0117]
[0118] In Table 1 above, Anti-discoloration Agent No. 1 contains colloidal sulfur, zinc pyrrolidone carboxylate, starch hydroxypropyltrimethylammonium chloride, and water. The mass ratio of colloidal sulfur, zinc pyrrolidone carboxylate, starch hydroxypropyltrimethylammonium chloride, and water is 15:30:3:55. KP70 Composite Zinc Salt contains zinc glycinate, zinc carbonate, and zinc laurate. In KP70 Composite Zinc Salt, the mass fraction of zinc glycinate is 50%, the mass fraction of zinc carbonate is 30%, and the mass fraction of zinc laurate is 20%.
[0119] The preparation methods of the anti-coloring compositions of Examples 1 to 7 and Comparative Examples 1 to 9 are as follows: Anti-coloring agent No. 1, Haimei ammonium chloride and KP70 composite zinc salt are mixed evenly, preservative is added and mixed, and stirred at 100-200 r / min for 5 min to prepare the anti-coloring composition.
[0120] Application Example 1
[0121] Selenium disulfide slurry was prepared from the anti-discoloration compositions obtained in each embodiment and comparative example. By mass fraction, the selenium disulfide slurry contained 20% selenium disulfide, 25% glycerol, 20% cocamidopropyl betaine (CAB), 20% emulsified hydrogenated castor oil, and 10% anti-discoloration composition, with water added to bring the total to 100%. The preparation method of the selenium disulfide slurry is as follows:
[0122] The above raw materials were mixed and ground under stirring conditions. The stirring speed was 500 rpm and the stirring time was 1 hour to prepare the selenium disulfide preparation.
[0123] Application Example 2
[0124] The selenium disulfide powder slurry containing the anti-color-changing compositions of each embodiment and comparative example was used to prepare a shampoo. The preparation method of the shampoo is as follows: 55.47 parts of deionized water were added to a mixing tank, along with 0.2 parts of disodium ethylenediaminetetraacetate and 0.2 parts of allantoin, and stirred at room temperature to dissolve and disperse. The temperature was raised to 75-80°C, and 15 parts of sodium lauryl ether sulfate (AES), 6 parts of sodium α-olefin sulfonate, 3.5 parts of coconut oil monoethanolamide (CMEA), and 6 parts of cocamidopropyl betaine were added sequentially to construct a stable anionic cleaning system. The temperature was lowered to 50°C, and 2.5 parts of emulsified hydrogenated castor oil were added and stirred to disperse evenly. The temperature was further lowered to below 45°C, and 0.3 parts of pre-dispersed polyquaternium-10, 0.5 parts of polyquaternium-87, 0.4 parts of polyquaternium-7, and 0.25 parts of conditioning agent (manufactured by Guangzhou Gaoju Biotechnology Co., Ltd.) were added sequentially. The product, composed of diC14-15 alcohol carbonate and water, is thoroughly mixed and introduced into the cationic conditioning system. The temperature is lowered to below 40°C, and 5 parts of 20% selenium disulfide slurry, 1 part of pearlescent paste (LP3201 pearlescent paste, manufactured by Guangdong Liangpeng Biotechnology Co., Ltd., composed of water, ethylene glycol monostearate, sodium lauryl ether sulfate, and coconut oil monoethanolamide), 0.3 parts of D-panthenol, 0.1 parts of zinc pyrrolidone carboxylate, 0.05 parts of natural vitamin E, 0.03 parts of menthol, 0.35 parts of fragrance, and 0.4 parts of 1,3-dihydroxymethyl-5,5-dimethylhydantoin (DMDMH) are added. The pH is finely adjusted twice with 0.25 parts of citric acid, and finally, 0.2 parts of sodium chloride are added to adjust the viscosity of the system. After homogenization, the product is discharged.
[0125] Performance testing
[0126] (1) Stability test
[0127] The selenium disulfide slurry prepared in Application Example 1 and the shampoo prepared in Application Example 2 were placed at room temperature and 50°C for one month respectively. The properties of the samples before and after storage under different conditions were checked. The experimental results are shown in Table 2 below.
[0128] Table 2
[0129]
[0130] Table 2 shows the color change grades of selenium disulfide powder and shampoo as follows: No color change means the color is normal orange-yellow; slight color change means the color is slightly darker, changing from orange-yellow to orange-red; significant color change means the color changes to reddish-brown; severe color change means the color changes to brownish-black or even dark brown. The stratification grades of selenium disulfide powder and shampoo are as follows: No stratification, i.e., no visible stratification; slight stratification, i.e., trace amounts of sediment at the bottom of the bottle; obvious stratification, i.e., obvious stratification or clumping; significant stratification, i.e., complete stratification or sandy sedimentation.
[0131] As can be seen from Table 2, the slurry of Example 1 did not show discoloration, stratification, sedimentation, or particle agglomeration after being stored at room temperature and 52°C for one month. Figs. 1-4 The image shows that the particles in the slurry of Example 1 were uniformly dispersed under a polarizing microscope after being stored at 52°C for one month. In contrast, the slurries in Comparative Examples 1 to 9 showed varying degrees of discoloration and stratification after being stored at room temperature or 52°C for one month. This demonstrates that the anti-discoloration composition provided in this application can stabilize the crystal form and dispersion of selenium disulfide, inhibit discoloration of selenium disulfide, improve the storage stability of selenium disulfide, and does not affect the dispersibility and suspension stability of selenium disulfide, exhibiting excellent compatibility.
[0132] (2) Test of dandruff removal, oil control and anti-itch effects
[0133] The following method was used to test the dandruff-removing, oil-controlling, and itch-relieving effects of the shampoo prepared in Application Example 2: Volunteers with dandruff were divided into 14 groups of 50 people each. They used the test sample shampoo twice a week, and the safety and dandruff-removing efficacy were evaluated based on the volunteers' user experience. The number of people in each group who reported effective, moderate, or ineffective dandruff-removing, oil-controlling, and itch-relieving effects were counted according to the following evaluation criteria.
[0134] The evaluation criteria for dandruff removal are as follows:
[0135] Effective: No dandruff; Normal: A small amount of dandruff remains; Ineffective: No reduction in dandruff.
[0136] Dandruff improvement rate (%) = (effective + average) / 50 × 100%.
[0137] Oil control evaluation criteria:
[0138] Effective: Not greasy; Average: Slightly greasy; Ineffective: Still very greasy.
[0139] Oil control improvement rate (%) = (effective + average) / 50 × 100%.
[0140] Antipruritic evaluation criteria:
[0141] Effective: No itching; Moderate: Slight itching; Ineffective: Still very itchy.
[0142] Itching relief rate (%) = (effective + average) / 50 × 100%.
[0143] The results are shown in Table 3.
[0144] Table 3
[0145]
[0146] As shown in Table 3, the shampoo prepared using the anti-color-changing composition of Example 1 achieved a 100% dandruff removal rate and oil control rate, and a 98% anti-itch rate, demonstrating superior efficacy. Comparative Examples 6-9 show that adding only a single component or using the blank group resulted in dandruff removal, oil control, and anti-itch rates of only 36%-74%, significantly lower than Example 1. This proves that anti-color-changing agent 1, anti-color-changing agent 2, and the compound zinc salt are all indispensable; using them alone cannot achieve highly effective dandruff removal, oil control, and anti-itch relief. Comparative Examples 2 and 4 show that excessively low levels of anti-color-changing agent 1 or anti-color-changing agent 2 lead to reduced efficacy. Comparative Examples 1, 3, and 5 show that the absence of any one of anti-color-changing agent 1, anti-color-changing agent 2, or the compound zinc salt significantly reduced efficacy, indicating that the three components must be used synergistically; the absence of any one component prevents the achievement of optimal results.
[0147] The provided anti-discoloration composition can effectively inhibit the oxidation and discoloration of selenium disulfide, reduce the generation of irritating byproducts, and improve the storage stability of the powder paste. It can also significantly enhance the dandruff removal, oil control, and anti-itch effects of shampoo.
[0148] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0149] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention should be determined by the appended claims, and the specification and drawings can be used to interpret the content of the claims.
Claims
1. An anti-discoloration composition for selenium disulfide preparations, comprising, by weight, 50 to 85 parts of anti-discoloration agent No. 1, 30 to 68 parts of anti-discoloration agent No. 2, 6 to 27 parts of compound zinc salt and 5 to 10 parts of preservative; in, The anti-discoloration agent No. 1 comprises colloidal sulfur, zinc pyrrolidone carboxylate, cationic starch, and a first solvent, wherein the mass ratio of the colloidal sulfur, the zinc pyrrolidone carboxylate, the cationic starch, and the first solvent is (10~20):(20~35):(2~5):(50~65). The anti-discoloration agent No. 2 contains hymex chloride; The composite zinc salt comprises zinc glycinate, zinc carbonate, and zinc laurate.
2. The anti-discoloration composition for selenium disulfide preparations according to claim 1, characterized in that, By weight, it contains 50 to 70 parts of anti-discoloration agent No. 1, 30 to 50 parts of anti-discoloration agent No. 2, 10 to 20 parts of compound zinc salt and 5 to 10 parts of preservative. Optionally, by weight, it contains 55 to 65 parts of anti-discoloration agent No. 1, 35 to 45 parts of anti-discoloration agent No. 2, 13 to 18 parts of compound zinc salt, and 5 to 10 parts of preservative.
3. The anti-discoloration composition for selenium disulfide preparations according to claim 1 or 2, characterized in that, One or more of the following conditions must be met: (1) The preservative contains phenoxyethanol; (2) The composite zinc salt contains, by weight percentage, 40%~60% zinc glycinate, 20%~30% zinc carbonate and 10%~20% zinc laurate; (3) The cationic starch comprises starch hydroxypropyltrimethylammonium chloride; (4) The particle size of the sulfur particles in the colloidal sulfur is 20 nm to 200 nm; (5) The method for preparing the colloidal sulfur includes the following steps: mixing sulfur with an aqueous solution containing a dispersant, and performing wet milling to prepare the colloidal sulfur; wherein the mass fraction of the dispersant in the aqueous solution containing the dispersant is 5wt%~15wt%, the mass ratio of the sulfur to the aqueous solution containing the dispersant is 1:(3~5), the wet milling time is 2~6h, and the dispersant contains gum arabic; and (6) The first solvent contains water.
4. The method for preparing the anti-discoloration composition for selenium disulfide preparations according to any one of claims 1 to 3, characterized in that, Includes the following steps: The anti-discoloration agent No. 1, the anti-discoloration agent No. 2, and the composite zinc salt are mixed, and a preservative is added for further mixing to prepare the anti-discoloration composition for selenium disulfide preparations.
5. A selenium disulfide preparation, characterized in that, The composition comprises, by mass fraction, 10% to 30% selenium disulfide, 9% to 13% of the anti-discoloration composition according to any one of claims 1 to 3, 10% to 40% humectant, 10% to 30% surfactant, 10% to 30% suspending agent, and 0% to 51% second solvent.
6. The selenium disulfide preparation according to claim 5, characterized in that, One or more of the following conditions must be met: (1) The moisturizer comprises one or more of glycerin, caprylic / capric triglyceride and propylene glycol; (2) The surfactant comprises one or more of cocamidopropyl betaine, cocoyl diethanolamide, cocoyl methyl monoethanolamide and sodium cocoyl sarcosinate; (3) The suspending agent contains one or both of emulsified hydrogenated castor oil and tristearate; (4) The second solvent contains water; and (5) The dosage form of the selenium disulfide preparation includes at least one of the following: powder, suspension, cream and gel.
7. The method for preparing the selenium disulfide preparation according to claim 5 or 6, characterized in that, Includes the following steps: The selenium disulfide, the anti-discoloration composition, the humectant, the surfactant, the suspending agent, and the second solvent are mixed and ground under stirring conditions to prepare the selenium disulfide preparation. Optionally, the stirring speed is 300 rpm to 800 rpm, and the stirring time is 30 min to 2 h.
8. The use of the selenium disulfide preparation according to claim 5 or 6 in the preparation of anti-dandruff care products.
9. A dandruff care product, characterized in that, Contains the selenium disulfide formulation as described in claim 5 or 6; Optionally, the selenium disulfide preparation in the dandruff care product has a mass fraction of 1% to 5%.
10. The dandruff care product according to claim 9, characterized in that, The dandruff care products include at least one of the following: dandruff shampoo, scalp serum, hair conditioner, and 2-in-1 shampoo and conditioner.