CN114569493A - Anti-dandruff shampoo composition - Google Patents
Anti-dandruff shampoo composition Download PDFInfo
- Publication number
- CN114569493A CN114569493A CN202210399607.6A CN202210399607A CN114569493A CN 114569493 A CN114569493 A CN 114569493A CN 202210399607 A CN202210399607 A CN 202210399607A CN 114569493 A CN114569493 A CN 114569493A
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- China
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- selenium sulfide
- total mass
- deionized water
- porous micron
- micron carbon
- Prior art date
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/596—Mixtures of surface active compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/83—Electrophoresis; Electrodes; Electrolytic phenomena
Abstract
A preparation method of anti-dandruff shampoo is characterized in that two anionic surfactant alkylphenol ether sulfosuccinate sodium salt and lauryl ether sodium sulfate, a cationic regulator polyquaternium-7 and guar gum hydroxypropyl trimethyl ammonium chloride are screened out by inspecting the air bubble property and cleaning capability of the shampoo, and a thickening agent, a spice, a nursing agent, a stabilizing agent, an emulsifying agent, a preservative and anti-dandruff nano selenium sulfide/porous micron carbon spheres with components are added.
Description
Technical Field
The invention belongs to the field of daily chemicals, relates to an anti-dandruff shampoo composition, and particularly designs a selenium sulfide shampoo composition.
Background
The shampoo is a product which is mainly compounded by taking a surfactant as a main body, has the effects of cleaning the scalp and hair of a person and keeping the beauty of the scalp and hair of the person, and is a daily chemical product which is used by people in large quantity in daily life. The shampoo comprises the components of a cleanser, hair care ingredients, hair moistening grease, a conditioner, an anti-dandruff antipruritic agent, a preservative, a thickening agent, a chelating agent, a thickening agent, an ultraviolet absorbent, nutrient elements and the like, wherein the main effective substance of the shampoo is an anionic surfactant, and the proper surfactant can achieve the effects of rich foam, low irritation, high cleanliness and weak degreasing force. Earlier, people only wash hair cleanly by using the shampoo, and along with the improvement of living standard, people begin to require multiple functions, such as dandruff removal, soft hair and no sticky feeling. The anti-dandruff shampoo is a product added with anti-dandruff components such as climbazole, piroctone olamine salt, zinc pyrithione and the like, and has a great proportion in the whole shampoo market because a great number of people have dandruff.
The dandruff is the scale of our scalp, and is scientifically called as "pityriasis capitis". The horny cells on the scalp under normal conditions gradually differentiate and grow from the bottom of the epidermis layer, then gradually move to the surface layer of the scalp, and finally slowly differentiate to form the horny layer on the scalp, and finally the horny layer falls off under the influence of related body metabolic enzymes to form a fine particle which cannot be seen by naked eyes. However, if there is an abnormal increase in the keratinocytes in our scalp area, there is an increase in dandruff, and as more stratum corneum cells are sloughed off and adhered together, they become visible as flaky scales on our naked eye.
There are generally three causes of abnormal proliferation of scalp keratinocytes:
first, if the scalp microbial balance is broken and a plurality of microorganisms exist in the scalp, wherein a fungus which takes sebum as food exists, namely malassezia, if the fungus is excessively proliferated, the cuticle of the user is excessively proliferated, and the cuticle forms flaky scales. This is also the reason why many shampoos containing antifungal drugs are available on the market, and are selected according to their own actual situation.
Secondly, excessive sebum secretion is also a large reason for abnormal proliferation of malassezia, but if the sebum secretion is too low, the scalp lacks protective components, the water locking function is insufficient, the scalp is easily dried and itchy, and scalp inflammation or scalp function barrier weakening can be caused seriously. Meanwhile, daily life work and rest, mental state and eating habits are clean and sanitary, and the sebum secretion condition of the scalp of people is also influenced.
Third, the barrier function of the stratum corneum of scalp, makes a important barrier for protecting scalp against the outside, and has the function of water locking, so as to prevent the scalp from drying and itching due to water loss, therefore, the function and integrity of the stratum corneum barrier are obvious, and the importance of protecting the health of scalp is obvious.
The therapeutic medicine for dandruff mainly comprises external keratolytic agents such as sulfur, salicylic acid and the like, and broad-spectrum antifungal medicines such as ketoconava, selenium disulfide, zinc rhodanate, and proxerone ethanolamine, wherein the clinical use effect of the antifungal medicines is better, and the antifungal medicines are often prepared into shampoo for convenient use. The curative effects of the above medicines are different, and here we mainly introduce selenium sulfide antifungal shampoo.
In the prior art, selenium sulfide is prepared by reacting selenious acid with hydrogen sulfide, hydrogen sulfide gas is introduced into selenious acid solution to generate selenium sulfide, and the product selenium sulfide is obtained after filtering, drying and crushing, wherein the method has low utilization rate of hydrogen sulfide, and hydrogen sulfide is easy to pollute the environment, such as a CN102060277A selenium sulfide production method, which comprises the following steps: according to the concentration of 100-200 g/L, preparing a selenium dioxide aqueous solution under a stirring state, filtering, preparing a filtered sodium sulfide aqueous solution according to the concentration of 150-350 g/L, simultaneously dropwise adding sodium sulfide glacial acetic acid into the stirred selenium dioxide aqueous solution, continuously stirring to promote reaction, putting the solution after the reaction into a centrifugal machine for centrifugal separation to obtain a selenium disulfide product, washing the product to be neutral, and drying to obtain the selenium disulfide product, wherein the yield and the purity obviously need to be improved.
For example, CN109650353A discloses a preparation method of high-purity selenium disulfide, which is characterized by comprising the following steps: A. dissolving raw material selenium in a nitric acid solution; B. crystallizing and separating out selenious acid after reaction in the solution; C. dissolving selenious acid crystals in water and filtering to prepare a saturated solution; D. stirring the saturated solution, and adding an ammonium sulfide solution and a glacial acetic acid solution into the saturated solution, or adding an ammonium hydrogen sulfide solution and a glacial acetic acid solution; E. adding absolute ethyl alcohol or absolute methyl alcohol into the mixed solution obtained in the step D, and then continuing stirring; stirring, standing and aging; F. filtering, and washing the filtrate with alcohol for several times; and drying after washing. The purity of the selenium disulfide finally prepared by the process is as high as 99.99 percent, which is enough to meet the requirement of high purity. Although the purity is high, the obvious preparation process is extremely complex, and the purity is high, but the yield is insufficient.
In addition, regarding electrochemical synthesis of selenium sulfide, the prior art has been on the way, but a preparation method of electrochemically synthesizing a selenium simple substance is disclosed, for example, CN202110797078 discloses a selenium sulfide composite powder for hair washing, wherein the selenium sulfide is uniformly dispersed on the surface of a nano microsphere in a nano form, and can be directly mixed with a hair washing composition for use, sedimentation separation does not easily occur in the composition, and the mixing of the selenium sulfide and the hair washing solution is not required during use, so that the selenium sulfide composite powder is simple and convenient, carbon sphere particles can be used as an active carbon hair washing water additive, the generation of dandruff can be reduced, the secretion of grease can be reduced, and the selenium sulfide composite powder has an obvious inhibiting effect on malassezia, and the electrochemical deposition principle is 6H++SeO3 2-+4e-→3H2O + Se, then preparing selenium sulfide through vulcanization, and then removing excessive sulfur through sublimed sulfur to obtain high-purity selenium sulfide.
Disclosure of Invention
Based on the technical problems of complex preparation process, low purity and low yield of selenium sulfide preparation in the prior art, the invention provides a preparation method of anti-dandruff shampoo, which comprises the steps of screening out two anionic surfactant alkylphenol ether sulfosuccinate sodium salt and lauryl ether sodium sulfate, a cationic regulator polyquaternium-7 and guar gum hydroxypropyl trimonium chloride by observing the air bubble property and cleaning capability of the shampoo, adding a thickening agent, a spice, a nursing agent, a stabilizer, an emulsifier, a preservative and anti-dandruff ingredient nano selenium sulfide/porous micron carbon spheres, wherein the shampoo is simple in overall preparation, easily available in raw materials and good in washing and protecting effects, the selenium sulfide is prepared by an electrochemical method, the balance moving direction of electrolyte is reasonably controlled by adding a pH value and a complexing agent, and nano selenium sulfide particles are uniformly deposited on the surfaces of the carbon microspheres intermittently contacted with a cathode, although the selenium sulfide has a nanometer size, the selenium sulfide is attached to the surface of carbon spheres in a micrometer range, so that the selenium sulfide cannot poison the scalp due to an excessively small size, and on the premise of maintaining high purity and high dandruff removal, the preparation process is simple and easy to obtain, the selenium sulfide is synthesized in one step, and the yield and the efficiency are far higher than those of similar products.
Specifically, the method comprises the following steps:
an anti-dandruff shampoo composition is characterized by comprising the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (0.8-1.1), 25-27wt.% of total mass;
the mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (1.7-2.2) is 1, which accounts for 2-3wt.% of the total mass;
nano selenium sulfide/porous micron carbon sphere deionized water;
sodium carboxymethylcellulose thickener, 1-1.5wt.% of the total mass;
citronellol perfume, accounting for 0.1-0.2wt.% of the total mass;
caprylic/capric triglyceride care agent accounting for 0.5-0.75wt.% of the total mass;
cetyl alcohol emulsion stabilizer, accounting for 0.4-0.6wt.% of the total mass;
monoglyceride emulsifier 0.6-0.7wt.% of the total mass;
opening accounts for 0.03-0.05wt.% of the total mass;
adjusting the pH value to 5.5-6.0 by citric acid;
the balance of deionized water
The mass percentage content of the selenium sulfide in the shampoo is not more than 1.0 wt.%;
the preparation process of the nano selenium sulfide/porous micron carbon sphere deionized water comprises the following steps:
(1) pretreatment of porous micron carbon spheres: adding a proper amount of porous carbon microspheres into a multi-neck flask, then adding 200-300ml of 1-2M sodium hydroxide aqueous solution, heating to 97-100 ℃ under the stirring condition, condensing and refluxing cooling water for 40-60min, naturally cooling, washing and filtering a large amount of deionized water until the pH value is 7.5 +/-0.3, and preparing into 10-12g/L of hydroxylated porous carbon microsphere suspension;
(2) the nano selenium sulfide/porous micron carbon spheres are synthesized through electrochemistry, and the preparation process is as follows:
(a) dissolving 30-40 mM sodium selenate decahydrate and 90-120 mM ammonium bisulfide in deionized water, adding 0.03-0.05g of diethylenetriamine pentacarboxylate, stirring uniformly, and adjusting the pH value to 8-9 by using hydrochloric acid to obtain electrolyte;
(b) inserting an inert anode and a cathode into the electrolyte, dividing the electrolyte into catholyte and anolyte by using an ion exchange membrane, introducing the hydroxylated porous micron carbon sphere suspension obtained in the step (1) into a cathode chamber, adjusting the pH of the catholyte to 7.5 +/-0.3, switching on a power supply under stirring adjustment, performing cathodic electrolysis reduction, wherein the electrolysis voltage is 3-5V, the time is 15-20min, the stirring speed is 300-500rpm, monitoring the pH concentration of the catholyte in real time during the electrolysis process, and adding sulfuric acid at a proper time to maintain the pH value to be constant to 7.5 +/-0.3;
(c) stopping the power supply, and leading out catholyte;
(3) and filtering and washing the catholyte to obtain the nano selenium sulfide/porous micron carbon sphere deionized water.
Furthermore, the purity of the selenium sulfide is more than 99.99%, and the particle size of the nano selenium sulfide is 20-200 nm.
Further, the porous micron carbon spheres have a particle size distribution with D90 of 7-12 μm.
The preparation method of the anti-dandruff shampoo comprises the following steps:
(1) mixing alkylphenol ether sulfosuccinate sodium salt and sodium lauryl ether sulfate anionic surfactant in a ratio of 1: and (0.95) dissolving the solution in the deionized water containing the nano selenium sulfide/porous micron carbon spheres in the mass ratio of 72.5 ℃, stirring at the speed of 150rpm for 4.5 hours to obtain a solution A.
(2) And (3) mixing the polyquaternium-7 and guar gum hydroxypropyl trimethyl ammonium chloride in a mass ratio of (1.95):1 in deionized water, dissolving at 55 ℃, stirring at 150rpm for 0.75h to obtain a solution B.
(3) Cooling the solution A obtained in the step (1) to 55 ℃, then adding the solution B, uniformly stirring, then sequentially adding a citric acid pH regulator, a sodium carboxymethylcellulose thickener, a citronellol perfume, a caprylic/capric triglyceride care agent, a cetyl alcohol emulsion stabilizer and a monoglyceride emulsifier, stirring at the speed of 450pm for 1.5h, cooling to 35 ℃, then adding an opening preservative, uniformly stirring, cooling to normal temperature, and supplementing the rest of water.
The principle of electrochemical preparation of nano selenium sulfide/porous micron carbon spheres is as follows:
firstly, regarding porous micron carbon sphere suspension, the porous micron carbon sphere is purchased from the market, the porous micron carbon sphere has the particle size distribution that D90 is 7-12 μ M, but the surface has a large amount of grease and amorphous carbon sheets or other impurities and is hydrophobic, so the surface pretreatment is necessary, the pretreatment mode is that a proper amount of porous micron carbon spheres are added into a multi-mouth flask, then 200ml of 1-2M sodium hydroxide aqueous solution is added, the mixture is heated to 97-100 ℃ under the stirring condition, cooling water is condensed and refluxed for 40-60min, the mixture is naturally cooled, a large amount of deionized water is washed and filtered until the pH value is 7.5 +/-0.3, and the hydroxylated porous micron carbon sphere suspension is prepared to be 10-12 g/L; the existence of the hydroxyl groups effectively improves the suspension effect of the carbon spheres in the subsequent catholyte, and avoids agglomeration and suspension on the surface of the catholyte.
With respect to the principle of the present invention for preparing high purity selenium sulfide,
the main components of the electrolyte are sodium selenate decahydrate, ammonium bisulfide and diethylenetriamineAmine pentacarboxylates, i.e. Na in water+、NH4+、SeO4 2-And HS-When the electrolyte is alkaline, the pH value is adjusted to 8-9 by adding acid such as sulfuric acid and hydrochloric acid, so that the solution is ionized and moved, and the reaction formula is shown as follows, SeO4 2- + 4HS- + 4H+ ⇌ SeS4 2- + 4H2O, the equilibrium of ionization occurring during the lowering of the pH value of the solution, is shifted to the right, and in addition, the complexing agent is diethylenetriamine pentacarboxylate to SeS4 2-Has a complexing power significantly greater than SeO4 2-Further increasing the balance to move to the right, forming more SeS4 2-。
Then, when a voltage is applied to the electrolyte, the following reaction [ SeS ] occurs4]2- + 2e- + 2H2O → SeS2 +2HS- +2OH-I.e. SeS formation on the cathode surface2Particles, SeS accompanying the occurrence of electrolysis2Particles forming a film covering the cathode surface, said SeS2The film has strong binding force on the surface of the cathode and cannot be effectively stripped, particularly for a porous inert titanium plate cathode, SeS deposited on the surface of the cathode2Difficult to recycle and may affect the conductivity of the cathode.
The hydroxylated porous micron carbon spheres are introduced into the cathode, the carbon spheres are conductive microspheres, the microspheres continuously impact the cathode under the condition of stirring speed of 300-500rpm, and electrolytic reduction [ SeS ] occurs in the process of contacting with the surface of the cathode4]2- + 2e- + 2H2O → SeS2 +2HS- +2OH-As mentioned above, a local alkaline environment is formed on the surface of the carbon spheres contacted with the cathode, so that the pH of the catholyte is reduced, and the selenium sulfide deposition on the cathode is facilitated, therefore, the pH concentration of the catholyte needs to be monitored in real time in the electrolytic process, and the pH value is maintained to be constant at 7.5 +/-0.3 by adding sulfuric acid at a proper time, and is consistent with the concentration of the hydroxylated porous micron carbon spheres, and the optimal microsphere deposition SeS is obtained in the pH concentration range2The range is a requirement.
The shampoo disclosed by the invention has the following components:
the anionic surfactant can generate active anionic parts after being dissociated in water, so that the foaming performance and the decontamination performance are good, and in addition, the ether group can improve the hydrophilicity of the surfactant, the foaming is fast, and the foam is more dense and stable.
Polyquaternium-7 and guar hydroxypropyltrimonium chloride are composed of cationic polymers. When the hair is washed, the carried cation can neutralize a part of negative charges of the hair, and the effect of improving combing property is achieved. The action mechanism is as follows: the cationic polymer can be adsorbed on the hair surface to perform electrostatic reaction with the negative charges on the hair surface, and because the cationic polymer is a high-molecular polymer, a film can be formed on the hair, so that the cationic polymer has a lubricating effect and reduces the friction force between hair fibers.
In addition, the characteristics of the shampoo such as adhesiveness, lubricity, film-forming property, chelating property, colloid-forming dispersibility, thickening property, foam stabilization, foam enhancement, solubilization and the like are improved by a citric acid pH regulator, a sodium carboxymethylcellulose thickener, a citronellol perfume, a caprylic/capric triglyceride care agent, a cetyl alcohol emulsion stabilizer and a monoglyceride emulsifier.
The beneficial technical effects are as follows:
(1) the selenium sulfide is prepared by an electrochemical method, the balance moving direction of electrolyte is reasonably controlled by adding a pH value and a diethylenetriamine pentacarboxylate complexing agent, nano selenium sulfide particles are uniformly deposited on the surface of the carbon microsphere intermittently contacted with a cathode, the preparation process is simple and easy to obtain, the selenium sulfide is synthesized by one step, and the yield and the efficiency are far higher than those of similar products.
(2) The relative sizes of the selenium sulfide and the carbon spheres are reasonably controlled, and the relative sizes of the selenium sulfide and the carbon spheres are cooperated with the nanometer active component and the micron macroscopic carrier, so that the unstable phenomena that the selenium sulfide lotion is easy to layer and the like due to overlarge particle size (such as larger than 50 mu m) of the selenium sulfide in the selenium sulfide lotion are effectively overcome, or the risk that the selenium sulfide lotion passes through a skin barrier probability and causes toxic and side effects on the skin due to overlarge particle size (such as smaller than 1 mu m) of the selenium sulfide is increased.
(3) Although the selenium sulfide has a nanometer size, the selenium sulfide is attached to the surface of a carbon sphere in a micrometer range, so that the selenium sulfide does not poison the scalp due to the fact that the selenium sulfide is too small in size, the preparation process is simple and easy to obtain on the premise of maintaining high purity and high dandruff removal, the yield and the efficiency are far higher than those of similar products due to one-step synthesis.
(4) The shampoo disclosed by the invention has a washing and protecting function, can endow hair with excellent wetting and combing properties, and enables the hair to be bright, smooth, moist and soft.
Drawings
FIG. 1 test optical patterns for the elimination of redness for shampoo prepared in example 2.
Fig. 2 test optical patterns of the shampoo prepared in example 2 for dandruff removal from the scalp (hairless).
Fig. 3 test optical diagram of dandruff (hair root) removal by shampoo prepared in example 2.
Detailed Description
Example 1
The shampoo preparations of examples 1 to 3 of the present invention, and comparative examples 1 to 2 were prepared in principle by the following methods:
(1) mixing alkylphenol ether sulfosuccinate sodium salt and sodium lauryl ether sulfate anionic surfactant in a ratio of 1: (0.95) is dissolved in the deionized water of nano selenium sulfide/porous micron carbon spheres at the dissolving temperature of 72.5 ℃, the stirring speed of 150rpm and the stirring time of 4.5h to obtain a solution A.
(2) And (3) mixing the polyquaternium-7 and guar gum hydroxypropyl trimethyl ammonium chloride in a mass ratio of (1.95):1 in deionized water, dissolving at 55 ℃, stirring at 150rpm for 0.75h to obtain a solution B.
(3) Cooling the solution A obtained in the step (1) to 55 ℃, then adding the solution B, uniformly stirring, then sequentially adding a citric acid pH regulator, a sodium carboxymethylcellulose thickener, a citronellol perfume, an octanoic acid/capric acid triglyceride care agent, a cetyl alcohol emulsion stabilizer and a monoglyceride emulsifier, stirring at a speed of 450pm for 1.5h, cooling to 35 ℃, then adding an opening preservative, uniformly stirring, cooling to normal temperature, and supplementing the balance of water. If some components are not contained, the components are deleted adaptively.
The shampoo comprises the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (0.8) in 25wt.% of the total mass.
The mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (1.7) is 1, and the mass ratio accounts for 2 wt% of the total mass.
Nano selenium sulfide/porous micron carbon sphere deionized water.
Sodium carboxymethylcellulose thickener, 1wt.% of the total mass.
Citronellol perfume, accounting for 0.1wt.% of the total mass.
Caprylic/capric triglyceride care agent accounting for 0.5 wt% of the total mass.
Cetyl alcohol emulsion stabilizer, accounting for 0.4wt.% of the total mass.
Monoglyceride emulsifier accounted for 0.6wt.% of the total mass.
Opening accounts for 0.03 wt% of the total mass.
Citric acid adjusted the pH to 5.5.
The balance being deionized water.
The preparation process of the nano selenium sulfide/porous micron carbon sphere deionized water comprises the following steps:
(1) pretreatment of porous micron carbon spheres: adding a proper amount of porous micron carbon spheres into a multi-mouth flask, then adding 200ml of 1M sodium hydroxide aqueous solution, heating to 97 ℃ under the condition of stirring, condensing and refluxing cooling water for 40min, naturally cooling, washing with a large amount of deionized water, filtering until the pH value is 7.5 +/-0.3, and preparing into a 10g/L hydroxylated porous micron carbon sphere suspension.
(2) The nano selenium sulfide/porous micron carbon spheres are synthesized through electrochemistry, and the preparation process is as follows:
(a) dissolving 30mM sodium selenate decahydrate and 90mM ammonium bisulfide in deionized water, adding 0.03g of diethylenetriamine pentacarboxylate, stirring uniformly, and adjusting the pH value to 8 by using hydrochloric acid to obtain the electrolyte.
(b) Inserting an inert anode and a cathode into the electrolyte, dividing the electrolyte into catholyte and anolyte by using an ion exchange membrane, introducing the hydroxylated porous micron carbon sphere suspension obtained in the step (1) into a cathode chamber, adjusting the pH of the catholyte to 7.5 +/-0.3, switching on a power supply under the condition of stirring, carrying out cathodic electrolysis reduction, wherein the electrolysis voltage is 3V, the time is 15min, the stirring speed is 300rpm, monitoring the pH concentration of the catholyte in real time during electrolysis, and adding sulfuric acid at a proper time to maintain the pH value to be 7.5 +/-0.3.
(c) And stopping the power supply and leading out the catholyte.
(3) And filtering and washing the catholyte to obtain the nano selenium sulfide/porous micron carbon sphere deionized water.
Example 2
The shampoo comprises the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (0.95) in 26wt.% of the total mass.
The mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (1.95) is 1, and the mass ratio accounts for 2.5 wt% of the total mass.
Nano selenium sulfide/porous micron carbon sphere deionized water.
Sodium carboxymethylcellulose thickener, 1.25wt.% of the total mass.
Citronellol perfume, accounting for 0.15wt.% of the total mass.
Caprylic/capric triglyceride care agent accounting for 0.625 wt% of the total mass.
Cetyl alcohol emulsion stabilizer, accounting for 0.5wt.% of the total mass.
Monoglyceride emulsifier accounted for 0.65wt.% of the total mass.
Opening accounts for 0.04 wt% of the total mass.
Citric acid adjusted the pH to 5.75.
The balance being deionized water.
The preparation process of the nano selenium sulfide/porous micron carbon sphere deionized water comprises the following steps:
(1) pretreatment of porous micron carbon spheres: adding a proper amount of porous micron carbon spheres into a multi-mouth flask, then adding 250ml of 1.5M sodium hydroxide aqueous solution, heating to 98.5 ℃ under the condition of stirring, condensing and refluxing cooling water for 50min, naturally cooling, washing and filtering by a large amount of deionized water until the pH value is 7.5 +/-0.3, and preparing into 11g/L hydroxylated porous micron carbon sphere suspension.
(2) The nano selenium sulfide/porous micron carbon spheres are synthesized through electrochemistry, and the preparation process is as follows:
(a) dissolving 35 mM sodium selenate decahydrate and 105 mM ammonium bisulfide in deionized water, adding 0.04g diethylenetriamine pentacarboxylate, stirring uniformly, and adjusting pH to 8.5 with hydrochloric acid to obtain electrolyte.
(b) Inserting an inert anode and a cathode into the electrolyte, dividing the electrolyte into catholyte and anolyte by using an ion exchange membrane, introducing the hydroxylated porous micron carbon sphere suspension obtained in the step (1) into a cathode chamber, adjusting the pH of the catholyte to 7.5 +/-0.3, switching on a power supply under the condition of stirring, carrying out cathodic electrolysis reduction, wherein the electrolysis voltage is 4V, the time is 17.5min, the stirring speed is 400rpm, monitoring the pH concentration of the catholyte in real time during electrolysis, and adding sulfuric acid at a proper time to maintain the pH value to be 7.5 +/-0.3.
(c) And stopping the power supply and leading out the catholyte.
(3) And filtering and washing the catholyte to obtain the nano selenium sulfide/porous micron carbon sphere deionized water.
Example 3
The shampoo comprises the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (1.1) 27wt.% of total mass.
The mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (2.2) is 1, and the mass ratio accounts for 3 wt% of the total mass.
Nano selenium sulfide/porous micron carbon sphere deionized water.
Sodium carboxymethylcellulose thickener, 1.5wt.% of the total mass.
Citronellol perfume, accounting for 0.2wt.% of the total mass.
Caprylic/capric triglyceride care agent accounting for 0.75 wt% of the total mass.
Cetyl alcohol emulsion stabilizer, accounting for 0.6wt.% of the total mass.
Monoglyceride emulsifier accounted for 0.7wt.% of the total mass.
Opening accounts for 0.05 wt% of the total mass.
Citric acid adjusted the pH to 6.0.
The balance being deionized water.
The preparation process of the nano selenium sulfide/porous micron carbon sphere deionized water comprises the following steps:
(1) pretreatment of porous micron carbon spheres: adding a proper amount of porous micron carbon spheres into a multi-neck flask, then adding 300ml of 2M sodium hydroxide aqueous solution, heating to 100 ℃ under the condition of stirring, condensing and refluxing cooling water for 60min, naturally cooling, washing with a large amount of deionized water, filtering until the pH value is 7.5 +/-0.3, and preparing into 12g/L hydroxylated porous micron carbon sphere suspension.
(2) The nano selenium sulfide/porous micron carbon spheres are synthesized through electrochemistry, and the preparation process is as follows:
(a) dissolving 40 mM sodium selenate decahydrate and 120 mM ammonium bisulfide in deionized water, adding 0.05g of diethylenetriamine pentacarboxylate, stirring uniformly, and adjusting the pH value to 9 by using hydrochloric acid to obtain the electrolyte.
(b) Inserting an inert anode and a cathode into the electrolyte, dividing the electrolyte into catholyte and anolyte by using an ion exchange membrane, introducing the hydroxylated porous micron carbon sphere suspension obtained in the step (1) into a cathode chamber, adjusting the pH of the catholyte to 7.5 +/-0.3, switching on a power supply under stirring adjustment, carrying out cathodic electrolytic reduction, wherein the electrolytic voltage is 5V, the time is 20min, the stirring speed is 500rpm, monitoring the pH concentration of the catholyte in real time in the electrolytic process, and adding sulfuric acid at a proper time to maintain the pH constant to 7.5 +/-0.3.
(c) And stopping the power supply and leading out the catholyte.
(3) And filtering and washing the catholyte to obtain the nano selenium sulfide/porous micron carbon sphere deionized water.
Comparative example 1
The shampoo comprises the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (0.95) in 26wt.% of the total mass.
The mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (1.95) is 1, and the mass ratio accounts for 2.5 wt% of the total mass.
Sodium carboxymethylcellulose thickener, 1.25wt.% of the total mass.
Citronellol perfume, accounting for 0.15wt.% of the total mass.
Caprylic/capric triglyceride care agent accounting for 0.625 wt% of the total mass.
Cetyl alcohol emulsion stabilizer, accounting for 0.5wt.% of the total mass.
Monoglyceride emulsifier accounted for 0.65wt.% of the total mass.
Opening accounts for 0.04 wt% of the total mass.
Citric acid adjusted the pH to 5.75.
The balance being deionized water.
Comparative example 2
The shampoo comprises the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (0.95) in 26wt.% of the total mass.
The mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (1.95) is 1, and the mass ratio accounts for 2.5 wt% of the total mass.
Nano selenium sulfide/porous micron carbon sphere deionized water.
Sodium carboxymethylcellulose thickener, 1.25wt.% of the total mass.
Citronellol perfume, accounting for 0.15wt.% of the total mass.
Caprylic/capric triglyceride care agent accounting for 0.625 wt% of the total mass.
Cetyl alcohol emulsion stabilizer, accounting for 0.5wt.% of the total mass.
Monoglyceride emulsifier accounted for 0.65wt.% of the total mass.
Opening accounts for 0.04 wt% of the total mass.
Citric acid adjusted the pH to 5.75.
The balance being deionized water.
The preparation process of the nano selenium sulfide/porous micron carbon sphere deionized water comprises the following steps:
(1) pretreatment of porous micron carbon spheres: adding a proper amount of porous micron carbon spheres into a multi-mouth flask, then adding 250ml of 1.5M sodium hydroxide aqueous solution, heating to 98.5 ℃ under the condition of stirring, condensing and refluxing cooling water for 50min, naturally cooling, washing and filtering by a large amount of deionized water until the pH value is 7.5 +/-0.3, and preparing into 11g/L hydroxylated porous micron carbon sphere suspension.
(2) The nano selenium sulfide/porous micron carbon spheres are synthesized through electrochemistry, and the preparation process is as follows:
(a) dissolving 35 mM sodium selenate decahydrate and 105 mM ammonium bisulfide in deionized water, and uniformly stirring to obtain the electrolyte.
(b) Inserting an inert anode and a cathode into the electrolyte, dividing the electrolyte into catholyte and anolyte by using an ion exchange membrane, introducing the hydroxylated porous micron carbon sphere suspension obtained in the step (1) into a cathode chamber, adjusting the pH of the catholyte to 7.5 +/-0.3, switching on a power supply under the condition of stirring, carrying out cathodic electrolysis reduction, wherein the electrolysis voltage is 4V, the time is 17.5min, the stirring speed is 400rpm, monitoring the pH concentration of the catholyte in real time during electrolysis, and adding sulfuric acid at a proper time to maintain the pH value to be 7.5 +/-0.3.
(c) And stopping the power supply and leading out the catholyte.
(3) And filtering and washing the catholyte to obtain the nano selenium sulfide/porous micron carbon sphere deionized water.
Finally obtained
The inventive example 2 and comparative examples 1-2 were tested, wherein the porous micro carbon spheres were not added in the comparative example 1, and thus the selenium sulfide anti-dandruff component was not contained in the comparative example 1, wherein the diethylenetriamine pentacarboxylate was not contained in the comparative example 2, and the pH of the mixed solution was not adjusted, and it can be seen from the above table that the anti-dandruff component in the shampoo of the present invention was 0.892wt.%, as shown in fig. 1, fig. 2 and fig. 3, and the shampoo of the present invention has excellent cleansing, treating and maintaining effects on redness of scalp, redness of hair roots, dandruff of scalp, and dandruff of hair roots. In addition, when the effective anti-dandruff component is prepared, if the diethylenetriamine penta-carboxylate is not added and the pH of the mixed solution is not adjusted, the balance movement is hindered and the yield is low in the process of preparing the selenium sulfide by electrochemical reduction, but the test can show that the addition of the selenium sulfide-porous micron carbon spheres in the shampoo can not generate any influence on the corresponding physicochemical properties of wet combing test, stability test, surface tension and the like of the shampoo.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (3)
1. An anti-dandruff shampoo composition is characterized by comprising the following components:
sodium alkyl phenol ether sulfosuccinate and sodium lauryl ether sulfate in a mass ratio of 1: (0.8-1.1), 25-27wt.% of total mass;
the mass ratio of the polyquaternium-7 to the guar gum hydroxypropyl trimethyl ammonium chloride (1.7-2.2) is 1, which accounts for 2-3wt.% of the total mass;
nano selenium sulfide/porous micron carbon sphere deionized water;
sodium carboxymethylcellulose thickener, 1-1.5wt.% of the total mass;
citronellol perfume, accounting for 0.1-0.2wt.% of the total mass;
caprylic/capric triglyceride care agent accounting for 0.5-0.75wt.% of the total mass;
cetyl alcohol emulsion stabilizer, accounting for 0.4-0.6wt.% of the total mass;
monoglyceride emulsifier 0.6-0.7wt.% of the total mass;
opening accounts for 0.03-0.05wt.% of the total mass;
adjusting the pH value to 5.5-6.0 by citric acid;
the balance of deionized water
The mass percentage content of the selenium sulfide in the shampoo is not more than 1.0 wt.%;
the preparation process of the nano selenium sulfide/porous micron carbon sphere deionized water comprises the following steps:
(1) pretreatment of porous micron carbon spheres: adding a proper amount of porous micron carbon spheres into a multi-mouth flask, then adding 200ml of 1-2M sodium hydroxide aqueous solution, heating to 97-100 ℃ under the condition of stirring, condensing and refluxing cooling water for 40-60min, naturally cooling, washing and filtering a large amount of deionized water until the pH value is 7.5 +/-0.3, and preparing into 10-12g/L hydroxylated porous micron carbon sphere suspension;
(2) the nano selenium sulfide/porous micron carbon spheres are synthesized through electrochemistry, and the preparation process is as follows:
(a) dissolving 30-40 mM sodium selenate decahydrate and 90-120 mM ammonium bisulfide in deionized water, adding 0.03-0.05g of diethylenetriamine pentacarboxylate, stirring uniformly, and adjusting the pH value to 8-9 by using hydrochloric acid to obtain electrolyte;
(b) inserting an inert anode and a cathode into the electrolyte, dividing the electrolyte into catholyte and anolyte by using an ion exchange membrane, introducing the hydroxylated porous micron carbon sphere suspension obtained in the step (1) into a cathode chamber, adjusting the pH of the catholyte to 7.5 +/-0.3, switching on a power supply under stirring adjustment, performing cathodic electrolysis reduction, wherein the electrolysis voltage is 3-5V, the time is 15-20min, the stirring speed is 300-500rpm, monitoring the pH concentration of the catholyte in real time during the electrolysis process, and adding sulfuric acid at a proper time to maintain the pH value to be constant to 7.5 +/-0.3;
(c) stopping the power supply, and leading out catholyte;
(3) and filtering and washing the catholyte to obtain the nano selenium sulfide/porous micron carbon sphere deionized water.
2. An anti-dandruff shampoo composition according to claim 1, wherein the selenium sulfide has a purity of greater than 99.99% and the nano-selenium sulfide has a particle size of 20-200 nm.
3. An anti-dandruff shampoo composition according to claim 1, wherein the porous carbon microspheres have a particle size distribution with a D90 of 7 to 12 μm.
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|---|---|---|---|---|
| WO2016058837A1 (en) * | 2014-10-17 | 2016-04-21 | Unilever Plc | Anti-dandruff hair composition |
| CN112691055A (en) * | 2021-02-09 | 2021-04-23 | 惠州市光大化妆品有限公司 | Anti-dandruff shampoo and preparation method thereof |
| CN113620258A (en) * | 2021-07-14 | 2021-11-09 | 郑小青 | Selenium sulfide composite powder for hair washing |
| CN113633576A (en) * | 2021-07-14 | 2021-11-12 | 郑小青 | Dandruff-removing itching-relieving hair washing composition |
| CN113633559A (en) * | 2021-07-14 | 2021-11-12 | 郑小青 | Preparation method of dandruff-removing and itching-relieving shampoo |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016058837A1 (en) * | 2014-10-17 | 2016-04-21 | Unilever Plc | Anti-dandruff hair composition |
| CN112691055A (en) * | 2021-02-09 | 2021-04-23 | 惠州市光大化妆品有限公司 | Anti-dandruff shampoo and preparation method thereof |
| CN113620258A (en) * | 2021-07-14 | 2021-11-09 | 郑小青 | Selenium sulfide composite powder for hair washing |
| CN113633576A (en) * | 2021-07-14 | 2021-11-12 | 郑小青 | Dandruff-removing itching-relieving hair washing composition |
| CN113633559A (en) * | 2021-07-14 | 2021-11-12 | 郑小青 | Preparation method of dandruff-removing and itching-relieving shampoo |
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