CN115887294A - Selenium disulfide shampoo and preparation method thereof - Google Patents

Selenium disulfide shampoo and preparation method thereof Download PDF

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Publication number
CN115887294A
CN115887294A CN202211421051.2A CN202211421051A CN115887294A CN 115887294 A CN115887294 A CN 115887294A CN 202211421051 A CN202211421051 A CN 202211421051A CN 115887294 A CN115887294 A CN 115887294A
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Prior art keywords
selenium
selenium disulfide
shampoo
sodium
disulfide
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胡圣伟
邱晓锋
顾葵
肖卉玲
欧业坛
刘俊达
郑冯锋
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Nox Bellcow Cosmetics Co Ltd
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Nox Bellcow Cosmetics Co Ltd
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Abstract

The invention discloses selenium disulfide shampoo and a preparation method thereof, and the selenium disulfide shampoo comprises: 0.05-1% selenium sulphide particles; 0.5-6% of high molecular polymer capable of suspending selenium disulfide particles; 0.5-5% of a polyol; 0.05-1% of a sulfur protectant; 0.1-2% of a chelating agent; 0.02-0.2% of zinc salt; 0.1-3% of a sunscreen agent; a surfactant; and the balance water. By using the high molecular polymer capable of suspending selenium disulfide, the selenium disulfide particles are prevented from coalescing into larger particles again, so that the selenium disulfide particles can fully exert the drug effect, and the content of selenium disulfide can be reduced; the stability of the selenium sulphide is further improved by using sulphur protectors, opacifiers, chelating agents, zinc salts and the like. The selenium disulfide shampoo provided by the invention has the advantages of high stability, low irritation, good anti-dandruff effect and good washing feeling.

Description

Selenium disulfide shampoo and preparation method thereof
Technical Field
The invention relates to selenium sulfide shampoo and a preparation method thereof, and particularly relates to selenium sulfide shampoo with high stability and low irritation and a preparation method thereof.
Background
Dandruff is a phenomenon of massive desquamation caused by excessive proliferation of scalp keratinocytes and affects the lives of many people. Most researchers believe that dandruff belongs to mild seborrheic dermatitis occurring on the scalp, manifested as the shedding of clumps of dead skin cells from the scalp.
At present, it is generally accepted that the generation mechanism of seborrheic dermatitis is the uninhibited proliferation of malassezia yeasts, and the treatment aspect mainly comprises the symptomatic treatment of degreasing, inflammation diminishing, sterilization, itching relieving and the like. Common topical therapeutic agents are bifonazole, ciclopirox, ketoconazole, selenium sulphide, zinc pyrithione, tar shampoo, terbinafine and topical glucocorticoids.
The selenium disulfide has pharmacological effects of resisting seborrhea, inhibiting Malassezia reproduction and resisting epidermal hyperplasia, and has good curative effect on removing dandruff and scalp seborrheic dermatitis. However, selenium disulfide is a complex mixture with an octagon structure, has unstable performance and is easily oxidized and blackened. The color of the selenium sulphide product tends to change from reddish brown to blackish brown with increasing time and temperature.
In order to solve the problem of color change of selenium sulfide, U.S. Pat. No. 4,854,333 discloses a selenium sulfide shampoo containing a peroxide such as hydrogen peroxide, sodium percarbonate and the like. These ingredients provide anti-dandruff efficacy and do not discolor upon storage. The patent also discloses a preparation method of the color-stable selenium disulfide shampoo. However, the peroxide is inherently unstable, and when the peroxide is gradually decomposed, the color stability of the selenium disulfide cannot be guaranteed.
Chinese patent 201480045888.9 discloses a hair treatment composition comprising: a) 0.1-2% by weight selenium sulphide; b) 0.1-2% by weight zinc pyrithione; and c) 0.01 to 10 weight percent cationic guar hydroxypropyltrimonium chloride polymer. The patent is directed to the color stabilization of the composition by adding zinc pyrithione to the shampoo. However, zinc pyrithione used in this patent is a highly toxic chemical antimicrobial agent, which has been banned in many areas such as the european union, and future restrictions are increasing.
The selenium disulfide is almost insoluble in water or organic solvent, so that the development or application of products such as lotion and the like is influenced. The development and application of a new micronization technology improve the development of a selenium disulfide lotion product.
Chinese patent 201510880617.1 discloses a selenium sulfide ultrafine powder and a preparation method thereof, wherein the selenium sulfide ultrafine powder is prepared by medium ball milling micronization, and the quality problems of long production time, large selenium sulfide particles, uneven dispersion, instability and the like are solved. In the patent, the grain diameter of the selenium disulfide superfine powder is (1-50) mu m, and the adopted method is as follows: (1) Uniformly mixing selenium disulfide dry powder, purified water, pharmaceutical grade titanium dioxide and pharmaceutical grade glycerol, and then adding citric acid to adjust the pH value to be between 3.5 and 4.5; (2) Then the selenium sulfide superfine powder is put into a grinding type superfine pulverizer to be ground and pulverized, and the selenium sulfide superfine powder is obtained. The selenium sulfide ultrafine powder can be applied to daily chemical products such as lotions, shampoos, conditioners and the like.
Chinese patent 201510882669.2 discloses a selenium sulfide dandruff-removing hair conditioner and a preparation method thereof, wherein the selenium sulfide dandruff-removing hair conditioner is prepared from selenium sulfide composite superfine powder, lanolin, hexadecanol, octadecanol, vaseline, chitosan, 10% formic acid, dodecyl dimethylamine oxide, water-soluble essence and deionized water; the grain size of the used selenium disulfide compound superfine powder is 1-50 mu m. The patent tries to solve the technical defects of the prior selenium disulfide lotion, such as high irritation, easy dryness of hair after use and difficult combing.
Chinese patent application 202111167690.6 discloses a new selenium disulfide ultrafine powder and a selenium disulfide lotion composition, the particle size of the selenium disulfide ultrafine powder is 1.0-50.0 μm, and the particle size distribution of D90 is 1.0-15.0 μm. Compared with the prior art, the selenium disulfide ultramicro powder is beneficial to the preparation of a selenium disulfide lotion product, the improvement of the quality of the selenium disulfide lotion product and the like.
Chinese patent application 202111496379.6 discloses a selenium sulfide shampoo and a method for improving stability thereof, wherein the shampoo comprises: 0.5 to 1.0 percent of selenium disulfide, 0.2 to 0.5 percent of panthenol, 0.2 to 0.5 percent of salicylic acid, 0.05 to 0.2 percent of disodium ethylene diamine tetraacetate, 15 to 20 percent of surfactant, 1.0 to 5.0 percent of conditioner for hair, 70 to 80 percent of solvent, 0.6 to 1 percent of preservative and 0.2 to 0.4 percent of pH regulator. According to the application, the stability of the selenium sulfide shampoo is improved through salicylic acid, D-panthenol and disodium ethylene diamine tetraacetate, and the problem of color change of selenium sulfide at high temperature is solved.
In Chinese patent 201510880617.1, chinese patent 201510882669.2 and Chinese patent application 202111167690.6, selenium disulfide ultrafine powder with the particle size of 1-50 μm is used for preparing lotion products; compared with other selenium disulfide lotion products, the selenium disulfide lotion overcomes the unstable phenomenon that the particle size of selenium disulfide in the traditional selenium disulfide lotion is too large (such as larger than 50 mu m) to cause easy layering of the selenium disulfide lotion, or the particle size of selenium disulfide is too small (such as smaller than 1 mu m) to increase the probability of passing through a skin barrier and cause the risk of toxic and side effects of the selenium disulfide lotion on the skin.
However, in order to uniformly disperse the selenium disulfide ultrafine powder, the content of glycerin in the selenium disulfide ultrafine powder prepared by the above patent technology exceeds 40%, and the preparation of a lotion product by using a large amount of glycerin affects or limits the preparation of the selenium disulfide ultrafine powder and a matrix, for example, the selenium disulfide ultrafine powder is difficult to be prepared into a uniformly dispersed stable selenium disulfide lotion by using a water-in-oil emulsion matrix; in addition, the prepared selenium disulfide ultrafine powder has a large particle range, the D90 is more than 30 microns, the particle distribution uniformity is not good enough, and the stability of a selenium disulfide lotion product is not good, so that the content of selenium disulfide in the lotion is difficult to reach 2% or more, otherwise, the lotion product is easy to generate unstable phenomena such as layering and the like.
Since the selenium disulfide does not dissolve in the lotion matrix, the dispersion uniformity and suspension stability of the selenium disulfide in the lotion matrix directly influence the product quality of the selenium disulfide lotion. Further improvements in the uniformity of dispersion, suspension stability and safety of use of selenium sulfide lotion products are desirable to improve the safety, effectiveness and compliance of the product in use.
Disclosure of Invention
The invention aims to provide selenium disulfide shampoo with small and low content of selenium disulfide particles, high stability, low irritation, good anti-dandruff effect and good washing feeling and a preparation method thereof.
On one hand, in order to achieve the above object, the invention provides a selenium sulfide shampoo, wherein the selenium sulfide shampoo comprises, by weight:
0.05-1% selenium sulphide particles;
0.5-6% of high molecular polymer capable of suspending selenium disulfide particles;
0.5-5% of a polyol;
0.05-1% of a sulfur protectant;
0.1-2% of a chelating agent;
0.02-0.2% of zinc salt;
0.1-3% of a sunscreen agent;
a surfactant; and
the balance of water.
Compared with the selenium disulfide shampoo in the prior art, the selenium disulfide shampoo has the advantages of less selenium disulfide addition amount, lower irritation, better safety and better washing feeling. Preferably, in the selenium disulfide shampoo, the addition amount of selenium disulfide is 0.1-0.8%; more preferably, the selenium disulfide is added in the shampoo of the invention in an amount of 0.2-0.7%.
In the present invention, all the percentages are by weight unless otherwise specified.
The inventors of the present invention have found that the use of a high molecular weight polymer capable of suspending selenium sulphide particles helps to disperse and stabilize the selenium sulphide: on one hand, during the preparation of the selenium disulfide shampoo, particularly during the preparation of the selenium disulfide dispersion liquid, the steric hindrance (such as microcrystalline cellulose) of the selenium disulfide can be utilized to inhibit the reagglomeration of selenium disulfide particles; on the other hand, after the selenium sulfide shampoo base is added, the suspension effect (such as the combined effect of microcrystalline cellulose and acrylic acid (ester) copolymer) can be utilized, so that the stabilization of the selenium sulfide shampoo is facilitated.
In principle, any high molecular weight polymer capable of suspending selenium sulphide particles may be used as suspending agent in the present invention. Preferably, the high molecular polymer used is one or more selected from the following group: acrylic acid (ester) copolymer, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, acrylic acid (ester)/stearyl alcohol polyether-20 methacrylate copolymer, acrylic acid (ester)/palm oil alcohol polyether-25 acrylate copolymer, microcrystalline cellulose, magnesium aluminum silicate, modified corn starch, acrylamide copolymer and trihydroxy stearin. More preferably, the high molecular polymer used is microcrystalline cellulose and/or an acrylic acid (ester) copolymer.
Compared with the selenium disulfide homogeneous dispersion liquid in the prior art, the selenium disulfide shampoo liquid provided by the invention adopts the selenium disulfide dispersion liquid with the particle size of 1-5 microns, so that the uniformity and stability of selenium disulfide powder in lotion are improved, the particle size of selenium disulfide particles is reduced, the specific surface area of the selenium disulfide particles is increased, the adhesiveness of the selenium disulfide particles to the surfaces of skin and hair is also increased, the contact surface area and the contact time of the selenium disulfide particles to the skin are increased, and the drug effect of the selenium disulfide particles can be fully and effectively exerted.
The inventors of the present invention have found that the particle size (e.g. D) of the selenium sulphide particles (microparticles) in the selenium sulphide dispersion is to be achieved 97 ) In the particle size range of 1-5 μm, it is critical to use a high molecular polymer that is capable of suspending the selenium sulphide particles, which would otherwise rapidly coalesce again into larger particles; in order to realize the good stability of the selenium disulfide shampoo, the high molecular polymer capable of suspending the selenium disulfide particles is necessary. By using the high molecular polymer capable of suspending the selenium disulfide particles, the selenium disulfide dispersion liquid with the selenium disulfide particles within the range of 1-5 microns can be prepared, and then the corresponding selenium disulfide shampoo is obtained.
In order to make the selenium disulfide shampoo of the invention more stable, a sulfur protectant must also be used. The inventor of the invention unexpectedly finds that the ammonium hypromellose which is rarely used in washing and protecting products but is often used as a hair conditioner in dyeing and ironing products can play a role of a sulfur protective agent when used in the selenium disulfide shampoo (washing and protecting products) of the invention, can greatly improve the stability of the selenium disulfide, and can also play a role of conditioning hair. The inventor thinks that the general protection mechanism of the Haimei ammonium chloride as the sulfur protective agent is to utilize the property of lower PH value in the Haimei ammonium chloride, have certain reducibility, inhibit the conversion of negative bivalent sulfur to negative tetravalent sulfur; in addition, the oxidation reaction can be inhibited to a certain extent by the low temperature caused by continuous heat absorption of the aqueous solution of the Heimei ammonium chloride.
Experiments show that the stability of the selenium disulfide shampoo can be improved by adding the zinc salt into the formula. The zinc salt used may be one or more selected from the following group: zinc gluconate, zinc glycinate, zinc sulfate, zinc carbonate, zinc lactate, zinc PCA, and zinc laurate.
In order to improve the light stability of the selenium disulfide shampoo, a sunscreen agent is also used in the formula of the invention. Preferred sunscreen agents may be one or more selected from the group consisting of: titanium dioxide, ethylene glycol distearate, mica, and synthetic fluorophlogopite.
Experiments of the invention also show that the addition of the chelating agent can also improve the stability of the selenium disulfide. The chelating agent used may be one or more selected from the following group: citric acid, sodium citrate, disodium EDTA, monosodium phosphate, disodium hydrogen phosphate, tetrasodium etidronate, hydroxyethylidene diphosphonic acid, HEPES buffer, salicylic acid, sodium salicylate, and diethylenetriaminepentaacetic acid (DTPA). The invention finds that the stronger the chelating ability of the chelating agent is, the more beneficial the stability of the selenium disulfide is. In view of the weak chelating ability of sodium citrate, it is preferred to use it in combination with a chelating agent having a stronger chelating ability, for example, tetrasodium etidronate, hydroxyethylidene diphosphonic acid, HEPES buffer, etc.
In the selenium disulfide shampoo, the surfactant is anionic surfactant. The anionic surfactant mainly plays a role in soil removal and foaming, and can be one or more selected from the following group: sodium laureth sulfate, ammonium laureth sulfate, C 12-14 Olefin sulfonic acid sodium salt, C 14-16 Sodium olefin sulfonate, disodium laureth sulfosuccinate, potassium laureth phosphate, sodium lauroyl sarcosinate, sodium lauroyl glutamate, sodium methylcocoyl taurate, sodium cocoyl amidopropionate, sodium cocoyl glycinate, sodium cocoyl methyltaurate, sodium cocoyl malate, sodium cocoyl isethionate, sodium laureth-6 carboxylate, potassium cocoyl hydrolyzed oat protein, andlauroyl sodium avenantamino acid.
In the selenium disulfide shampoo of the present invention, the surfactant used may further comprise an amphoteric surfactant and/or a nonionic surfactant. Wherein, the main functions of the amphoteric surfactant are thickening and irritation reduction, and the main functions of the nonionic surfactant are thickening and foam stabilization. The amphoteric surfactant can be one or more of the following substances: cocamidopropyl betaine, sodium lauroamphoacetate, sodium cocoamphoacetate, disodium cocoamphodiacetate, lauryl betaine, cocobetaine, lauryl hydroxysultaine, cocamidopropyl hydroxysultaine; the nonionic surfactant may be one or more of the following group: cocamide DEA, cocamide MEA, cocamide methyl MEA, cocamide MIPA, cocamide AMP, lauryl glucoside, octyl/decyl glucoside, lauryl/myristyl glucoside, octyl/myristyl glucoside, lauryl amine oxide, coco glucoside.
In the selenium disulfide shampoo of the invention, the polyol used can be one or more than one of the following groups: glycerol, propylene glycol, 1, 3-propanediol, polyethylene glycol-8, butanediol, methylpropanediol, sorbitol, diglycerol, dipropylene glycol, 1, 2-pentanediol.
The selenium sulphide shampoo according to the invention preferably contains an appropriate amount of an antioxidant, for example 0.01-0.2%. The antioxidant can be one or more than one of the following substances: butylated hydroxytoluene, tocopherol (vitamin E), ciba-H, gersten M, tert-butylhydroquinone, pentaerythritol tetrakis (bis-tert-butylhydroxyhydrocinnamate).
In addition, the selenium disulfide shampoo can be added with:
cationic conditioners (cationic conditioners are effective for both wet and dry combing), for example, one or more of polyquaternium-10, polyquaternium-6, polyquaternium-7, polyquaternium-22, polyquaternium-39, polyquaternium-67, guar hydroxypropyltrimonium chloride, hydroxypropylguar hydroxypropyltrimonium chloride, stearamidopropyldimethylamine, behenoyloxy PG-trimonium chloride, and the like;
hair conditioners such as one or more of PPG-3 octyl ether, polyester-11, PEG-75 lanolin, phytosterol/octyldodecanol lauroyl glutamate, PEG-12 polydimethylsiloxane, silicone emulsion, silicone amino-terminated emulsion, hydrolyzed keratin, hydrolyzed silk, hydrolyzed collagen, etc.;
soothing components such as one or more of allantoin, bisabolol, herba Portulacae extract, herba Centellae extract, radix et caulis Opuntiae Dillenii extract, cortex moutan extract, radix Gentianae extract, and radix Stephaniae Japonicae extract;
pH regulators such as one or more of citric acid, lactic acid, glycolic acid, mandelic acid, lactobionic acid, phytic acid, tartaric acid, gluconolactone, and the like;
preservatives, for example, phenoxyethanol, dichlorobenzyl alcohol, o-cymene-5-ol, piroctone olamine, polyaminopropyl biguanide, sodium benzoate, potassium sorbate, benzoic acid, benzyl alcohol, chlorphenesin, methylparaben, propylparaben, bis (hydroxymethyl) imidazolidinyl urea, DMDM hydantoin, methylisothiazolinone, methylchloroisothiazolinone, and the like;
essence, pigment, etc.
On the other hand, in order to achieve the purpose of the invention, the invention also provides a method for preparing the selenium disulfide shampoo, which comprises the following steps:
step 1: dispersing the high molecular polymer capable of suspending the selenium disulfide particles uniformly by using a proper amount of water to obtain a high molecular polymer aqueous solution;
step 2: dissolving a sulfur protective agent into a transparent aqueous solution by using water, then uniformly mixing the solution with polyhydric alcohol, then adding selenium sulfide powder, mixing and stirring the mixture, grinding the mixture by using a three-roll grinder to enable the particle size of the selenium sulfide powder to be 1-5 mu m, adding the high molecular polymer aqueous solution obtained in the step 1, and uniformly stirring the mixture to obtain a selenium sulfide dispersion liquid;
and step 3: adding water into an emulsifying pot, adding the selected surfactant, stirring, heating to 72-78 ℃, uniformly stirring, and keeping the temperature;
and 4, step 4: cooling the mixture obtained in the step (3) to 65 ℃, and adding the selected chelating agent and the opacifier;
and 5: continuously cooling the mixture obtained in the step (4) to 45 ℃, adding other auxiliary agent components, uniformly stirring, and adjusting the pH value to 4.5-5.5;
step 6: continuously cooling the mixture obtained in the step 5 to 35 ℃, adding the selenium disulfide dispersion liquid obtained in the step 2, and uniformly stirring;
and 7: and (4) adding zinc salt into the mixture obtained in the step (6), and uniformly stirring to obtain the selenium disulfide shampoo.
In the above-described method of the present invention, an antioxidant may be further added during or after the milling in step 2.
In the method of the present invention, after step 3 and before step 4, the method further includes the following steps: dispersing the selected cationic conditioner in water, adding into an emulsifying pot, and stirring at 72-78 deg.C for 10-60 min.
In the above-described method of the present invention, the other auxiliary agents added in step 5 include hair conditioners, soothing components, preservatives, perfumes, pigments, PH adjusters, and the like.
The selenium disulfide particles in the selenium disulfide shampoo are small in particle size, the specific surface area is increased, the adhesion with the skin and the hair surface is also increased, and therefore the contact surface area and the contact time of the selenium disulfide and the skin are increased, and the selenium disulfide can fully and effectively exert the drug effect even under the condition of low content of the selenium disulfide. The invention prevents the selenium disulfide particles from agglomerating into larger particles again by using the high molecular polymer capable of suspending the selenium disulfide, and further improves the stability of the selenium disulfide by using a sulfur protective agent, an opacifier, a chelating agent and a zinc salt. The selenium disulfide shampoo has low content of selenium disulfide, thereby having low irritation, good anti-dandruff effect and good washing feeling.
The present invention will be further described with reference to the following detailed description and the accompanying drawings, which are provided for illustration of specific embodiments of the invention and are not intended to limit the invention.
Drawings
FIG. 1 is a graph of the particle size distribution of selenium disulfide particles of a selenium disulfide dispersion obtained in the preparation of example 1.
Detailed description of the preferred embodiments
Examples 1 to 3 and comparative examples 1 to 3
In the preparation of the selenium disulfide shampoos of examples 1-3 and comparative examples 1-3, the following general procedure was followed, but the specific procedure and the specific operation in each step can be slightly modified for different formulations according to the raw materials in the formulation:
step 1: dispersing the selected high molecular polymer with proper amount of water uniformly for later use;
step 2: dissolving the selected sulfur protective agent into a transparent aqueous solution by using water, then uniformly mixing the transparent aqueous solution with the selected polyhydric alcohol, then adding selenium sulfide powder, mixing and stirring the mixture until the mixture is completely wetted, processing the mixture by using a three-roll grinder to obtain a suspension, adding the suspension into the high molecular polymer aqueous solution obtained in the step (1), uniformly stirring the suspension, and adding an antioxidant to prepare a selenium sulfide dispersion for later use;
and step 3: adding water into an emulsifying pot, adding the selected anionic surfactant, amphoteric surfactant and nonionic surfactant, stirring, heating to 72-78 deg.C, stirring, and keeping the temperature;
and 4, step 4: dispersing the selected cationic conditioner in water, adding the cationic conditioner into an emulsifying pot, and stirring for 30 minutes at the temperature of 72-78 ℃;
and 5: cooling to 65 deg.C, adding selected chelating agent and opacifier;
step 6: cooling to 45 deg.C, adding selected hair conditioner, soothing components, antiseptic, essence, pigment, etc., stirring, and adjusting pH to 4.5-5.5 with pH regulator;
and 7: cooling to 35 ℃, adding the selenium disulfide dispersion liquid prepared in the step 2, and uniformly stirring;
and 8: adding the compound zinc salt, and uniformly stirring to obtain the selenium disulfide shampoo.
According to the preparation method and the formula shown in the following table 1, the selenium disulfide shampoos of examples 1-3 and comparative examples 1-3 are prepared.
And (3) measuring the particle size distribution of the selenium disulfide (polyalcohol) dispersion liquid obtained by the three-roll grinding treatment in the step (2) by using a Malvern nanometer particle size analyzer. Wherein, the particle size distribution of the selenium disulfide dispersion obtained in step 2 of example 1 is shown in fig. 1. The particle size distributions of the selenium disulfide dispersions obtained in examples 2-3 and comparative examples 1-3 are also substantially as shown in figure 1.
As can be seen from fig. 1, after the selenium disulfide powder is diluted by polyol, three-roll milled, and added with a high molecular substance capable of suspending selenium disulfide particles, in the obtained selenium disulfide polyol dispersion, almost all selenium disulfide particles have a particle size stabilized within a range of 1-5 μm for a period of time. This indicates that the polymer material capable of suspending the selenium sulfide particles can better prevent the selenium sulfide particles from re-agglomerating.
TABLE 1
Component name Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2 Comparative example 3
Ammonium laureth sulfate 12.00 12.00 12.00 12.00 12.00 12.00
Ammonium lauryl sulfate 2.80 2.80 2.80 2.80 2.80 2.80
Cocoamidopropyl betaine 1.20 1.20 1.20 1.20 1.20 1.20
Cocoamide DEA 1.50 1.50 1.50 1.50 1.50 1.50
Polyquaternary ammonium salt-10 0.40 0.40 0.40 0.40 0.40 0.40
Titanium dioxide 1.00 1.00 1.00 1.00 1.00 1.00
Acrylic acid (ester) copolymer 3.00 3.00 3.00 3.00 3.00 3.00
Microcrystalline cellulose 0.50 0.50 0.50 0.50 0.50 0.50
Butylated hydroxytoluene 0.10 0.10 0.10 0.10 0.10 0.10
Etidronate tetrasodium salt 0.30 0.30 0.30 - 0.30 -
Hydroxyethylidene diphosphonic acid 0.30 0.30 0.30 - 0.30 -
Citric acid sodium salt 0.30 0.30 0.30 0.30 0.30 0.30
Citric acid Proper amount of Proper amount of Proper amount of Proper amount of Proper amount of Proper amount of
Selenium disulfide 0.30 0.60 1.00 0.60 0.60 0.60
Glycerol 2.00 2.00 2.00 2.00 2.00 2.00
Haimei ammonium chloride 0.15 0.15 0.15 - - 0.15
Phenoxyethanol 0.50 0.50 0.50 0.50 0.50 0.50
Sodium benzoate 0.30 0.30 0.30 0.30 0.30 0.30
Zinc lactate 0.05 0.05 0.05 - - 0.05
Pure water Supplement to 100 Supplement to 100 Supplement to 100 Supplement to 100 Supplement to 100 Supplement to 100
Note: the components in the table are parts by weight.
Stability test
Heat resistance stability test method:
the sample was put into a 100 g plastic bottle, put into a 50 ℃ oven, observed for 2 days, 1 week, 2 weeks, 3 weeks, and 4 weeks, respectively, and compared with the sample left to stand at room temperature.
Heat resistance stability test results:
after 4 weeks in examples 1,2 and 3, the color was slightly darker than normal temperature; comparative example 1, after 2 days, was clearly blackened; comparative example 2, after 1 week, was visibly black; comparative example 3, after 3 weeks, was clearly blackened.
Evaluation of anti-dandruff Effect
In a preliminary evaluation experiment in a laboratory, the shampoo containing 0.3% of selenium disulfide in a selenium disulfide dispersion liquid with a particle size of 1-5 μm in example 1 can achieve the anti-dandruff effect of the shampoo containing 1% of selenium disulfide homogeneous liquid in the prior art.

Claims (10)

1. The selenium sulfide shampoo comprises the following components in percentage by weight:
0.05-1% selenium sulphide particles;
0.5-6% of high molecular polymer capable of suspending selenium disulfide particles;
0.5-5% of a polyol;
0.05-1% of a sulfur protectant;
0.1-2% of a chelating agent;
0.02-0.2% of zinc salt;
0.1-3% of a sunscreen agent;
a surfactant; and
the balance of water.
2. The selenium sulfide shampoo according to claim 1, wherein the high molecular polymer is one or more selected from the following group: acrylic acid (ester) copolymer, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, acrylic acid (ester)/stearyl alcohol polyether-20 methacrylate copolymer, acrylic acid (ester)/palm oil alcohol polyether-25 acrylate copolymer, microcrystalline cellulose, magnesium aluminum silicate, modified corn starch, acrylamide copolymer and trihydroxy stearin.
3. The selenium sulfide shampoo of claim 1, wherein the selenium sulfide particles have a particle size of 1-5 μm.
4. The selenium disulfide shampoo of claim 1 wherein the sulfur protectant is nimonium chloride.
5. The selenium sulfide shampoo according to claim 1, wherein the zinc salt is one or more selected from the following group: zinc gluconate, zinc glycinate, zinc sulfate, zinc carbonate, zinc lactate, zinc PCA, and zinc laurate.
6. The selenium disulfide shampoo as claimed in claim 1, wherein the sunscreen agent is one or more selected from the following group: titanium dioxide, ethylene glycol distearate, mica, and synthetic fluorophlogopite.
7. The selenium sulfide shampoo as claimed in claim 1, wherein the surfactant is an anionic surfactant, and the anionic surfactant is one or more selected from the following group: sodium laureth sulfate, ammonium laureth sulfate, C 12-14 Olefin sulfonic acid sodium salt, C 14-16 Sodium olefin sulfonate, disodium laureth sulfosuccinate, potassium laureth phosphate, sodium lauroyl sarcosinate, sodium lauroyl glutamate, sodium methylcocoyl taurate, sodium cocoyl amidopropionate, sodium cocoyl glycinate, sodium cocoyl methyl taurate, sodium cocoyl malic amino acid, sodium cocoyl isethionate, sodium laureth-6 carboxylate, potassium cocoyl hydrolyzed oat protein, and sodium lauroyl oat amino acid.
8. The selenium sulfide shampoo of claim 7, wherein the surfactant further comprises an amphoteric surfactant and/or a nonionic surfactant.
9. A process for preparing a selenium sulphide shampoo according to any one of claims 1 to 8, wherein the process comprises the steps of:
step 1: dispersing the high molecular polymer capable of suspending the selenium disulfide particles uniformly by using a proper amount of water to obtain a high molecular polymer aqueous solution;
and 2, step: dissolving a sulfur protective agent into a transparent aqueous solution by using water, then uniformly mixing the solution with polyhydric alcohol, then adding selenium sulfide powder, mixing and stirring the mixture, grinding the mixture by using a three-roll grinder to enable the particle size of the selenium sulfide powder to be between 1 and 5 mu m, adding the high molecular polymer aqueous solution obtained in the step 1, and uniformly stirring the mixture to obtain a selenium sulfide dispersion liquid;
and 3, step 3: adding water into an emulsifying pot, adding the selected surfactant, stirring, heating to 72-78 ℃, uniformly stirring, and keeping the temperature;
and 4, step 4: cooling the mixture obtained in the step (3) to 65 ℃, and adding the selected chelating agent and the opacifier;
and 5: continuously cooling the mixture obtained in the step 4 to 45 ℃, adding other auxiliary agent components, uniformly stirring, and adjusting the pH value to 4.5-5.5;
step 6: continuously cooling the mixture obtained in the step 5 to 35 ℃, adding the selenium disulfide dispersion liquid obtained in the step 2, and uniformly stirring;
and 7: and (5) adding zinc salt into the mixture obtained in the step (6), and uniformly stirring to obtain the selenium disulfide shampoo.
10. The method of claim 9, further comprising, after step 3 and before step 4, the steps of: dispersing the selected cationic conditioner in water, adding into an emulsifying pot, and stirring at 72-78 deg.C for 10-60 min.
CN202211421051.2A 2022-11-14 2022-11-14 Selenium disulfide shampoo and preparation method thereof Pending CN115887294A (en)

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CN110709059A (en) * 2018-12-26 2020-01-17 拉芳家化股份有限公司 Dandruff-removing and itching-relieving shampoo composition containing multi-element zinc
CN113893189A (en) * 2015-11-09 2022-01-07 勃林格殷格翰动物保健美国公司 Pet care cleansing compositions
CN114010514A (en) * 2021-10-08 2022-02-08 大有药业扬州有限公司 Micronized selenium disulfide active antifungal lotion
CN114159322A (en) * 2021-12-09 2022-03-11 江苏知原药业股份有限公司 Selenium sulfide liquid shampoo and method for improving stability of selenium sulfide liquid shampoo
CN115068354A (en) * 2022-07-18 2022-09-20 远方舒霖(广东)生物制品有限公司 Selenium sulfide anti-dandruff shampoo formula

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103442567A (en) * 2011-03-23 2013-12-11 巴斯夫欧洲公司 Compositions containing polymeric, ionic compounds comprising imidazolium groups
CN105473125A (en) * 2013-08-21 2016-04-06 荷兰联合利华有限公司 Hair treatment compositions
CN113893189A (en) * 2015-11-09 2022-01-07 勃林格殷格翰动物保健美国公司 Pet care cleansing compositions
CN110709059A (en) * 2018-12-26 2020-01-17 拉芳家化股份有限公司 Dandruff-removing and itching-relieving shampoo composition containing multi-element zinc
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