CN113633559A - Preparation method of dandruff-removing and itching-relieving shampoo - Google Patents
Preparation method of dandruff-removing and itching-relieving shampoo Download PDFInfo
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- CN113633559A CN113633559A CN202110797709.9A CN202110797709A CN113633559A CN 113633559 A CN113633559 A CN 113633559A CN 202110797709 A CN202110797709 A CN 202110797709A CN 113633559 A CN113633559 A CN 113633559A
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- selenium
- selenium sulfide
- shampoo
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- carbon
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- 238000002360 preparation method Methods 0.000 title claims description 15
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- FAGMGMRSURYROS-UHFFFAOYSA-M trihexadecyl(methyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCC)CCCCCCCCCCCCCCCC FAGMGMRSURYROS-UHFFFAOYSA-M 0.000 claims abstract description 21
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- 238000004073 vulcanization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
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Abstract
The shampoo has stable composition, comfortable viscosity touch, quick foaming and rich foam, has rich foam through the compound use of fatty alcohol polyoxyethylene ether sodium sulfate, cocamidopropyl betaine and coconut oil fatty acid diethanolamide, has dry and wet combing properties through tri (hexadecyl) methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride and polyquaternary ammonium salt-10, effectively improves the suspension property of inorganic micro carbon spheres in the shampoo by adding the poloxamer 940, and can maintain long-term stability.
Description
Technical Field
The invention belongs to the technical field of daily chemical products, and particularly relates to a preparation method of an anti-dandruff and anti-itching shampoo.
Background
In daily life, under the influence of pressure and environmental pollution, more and more people are troubled by the problems of scurf, scalp itch, scalp inflammation and the like, most of the existing scurf removing products on the market adopt pyridine sulfate as the scurf removing agent, but the existing scurf removing agent has the defects that the pyridine sulfate is strong in irritation, insoluble in water and organic solvent, and is easy to appear poor in compatibility with other components, difficult to disperse, easy to precipitate and agglomerate when being applied to shampoo, so that the scurf removing effect is unstable. In the prior art, the plant extract is used as the anti-dandruff agent, and the anti-dandruff agent has the characteristics of mildness and no stimulation, but the plant extract has complex components, unclear effective components and beneficial effects, unobvious effects or even no claimed effect of a product, the effective components of the plant extract are easily influenced by an extraction process, and other components and shelf life in a system also easily influence the stability of the plant extract and the high activity of active substances, so that the anti-dandruff effect is unstable. The therapeutic agent for dandruff mainly comprises topical keratolytic agent such as sulfur and salicylic acid, broad-spectrum antifungal agent such as ketoconazole, selenium disulfide, zinc pyrithione and piroctone olamine, wherein the antifungal medicine has better clinical use effect, and is often prepared into shampoo for convenient use, and the external selenium disulfide, zinc pyrithione and piroctone olamine are three common anti-dandruff medicines, has good effect in clinical use for decades, although the antifungal medicine is a broad-spectrum antifungal medicine, the action mechanisms of the three medicines are different, the piroctone olamine is a salt consisting of piroctone and ethanolamine, can form a chelate with iron to interfere the metabolism of microorganisms, simultaneously, the antibacterial agent also has the function of killing fungi, has a wide antibacterial spectrum, and has the functions of resisting oxidation, decomposing oxides and the like so as to relieve local inflammatory reaction; zinc pyrithione is a heterocyclic compound, is used as a transport inhibitor of fungal cell membranes, can cause depolarization of membranes to kill fungi, can wrap the fungi after being dissolved so as to inhibit growth of the fungi, and has the function of inhibiting epidermal proliferation; selenium disulfide is an inorganic compound, has the effects of resisting fungi and inhibiting epidermal proliferation, is a medical lotion on the market, has the general content of 2.5 percent, has good curative effect on bacteria and seborrheic dermatitis on scalp, is mainly externally used in a shampoo mode, is generally and mainly externally used on scalp parts and hair parts, has the main effects of resisting fungi and relieving itching and has a certain function of controlling grease, so the lotion is generally and mostly used for scalp seborrheic dermatitis, pityriasis capitis and the like on scalp in clinic, can play a certain role of removing fat, diminishing inflammation and relieving itching after being generally washed for 1 time in 3 to 4 days, but has strong irritation on skin, and has overhigh solid content in the lotion, and cannot be used for a long time. In addition, the selenium disulfide has strong effect of inhibiting sebaceous gland secretion, and the high-content dosage form easily causes excessive dryness of scalp, and causes the problems of dandruff increase and scalp itching. Moreover, the selenium sulfide lotion has poor cleaning capability and needs to be matched with shampoo for use, which brings inconvenience to users.
In addition, medicinal selenium sulfide and shampoo in the market are usually purchased separately, and a user uses the shampoo and the selenium sulfide in a matched mode according to the ratio of 1:1 or 2:1 in the using process, mainly because the selenium sulfide is high in density, insoluble in water and oil and difficult to suspend in a shampoo system, the shampoo and the selenium sulfide are easily separated, the selenium sulfide is difficult to uniformly apply to the head of a human body, and the dandruff removing and itching relieving effects are poor.
At present, two main methods for preparing selenium disulfide are available.
The first method is a wet synthesis method: under the acidic condition, adding sodium sulfide (or ammonium sulfide, ammonium hydrogen sulfide) solution into selenious acid solution (selenium dioxide solution in water) to react with glacial acetic acid solution to generate selenium sulfide, and filtering, washing and drying to obtain the selenium sulfide product. The disadvantages are that: the purity of the selenium disulfide prepared by the method is low. Acetic acid is used in the synthesis process, so the production environment is relatively poor, and the requirement on equipment is high; and a large amount of sewage is generated in the synthesis and washing processes, so that the comprehensive production cost is high.
The second method comprises the following steps of pyrogenic synthesis: adding selenium and sulfur into a quartz tube according to a certain proportion, vacuumizing, sealing the tube, synthesizing at high temperature, and finally cooling, crushing the tube and sampling. The disadvantages are that: and (3) vacuumizing to seal the tube, wherein the quartz tube needs to be vacuumized to below 10-5Pa and then calcined and sealed, and the requirement on equipment is high. The quartz tube has small charging amount and low single-batch productivity; the quartz tube is a consumable, the produced quartz waste is more, and the comprehensive production cost is higher.
Disclosure of Invention
Based on the problems, the invention provides a preparation method of the anti-dandruff and itching-relieving shampoo, the shampoo has excellent anti-dandruff and itching-relieving effects, the composition of the shampoo is stable, the viscosity and touch feeling are comfortable, the shampoo is quickly soaked, and the foam is rich, and the specific preparation method is as follows:
(1) preparing selenium sulfide composite powder, putting the selenium sulfide composite powder into deionized water solution, stirring to obtain selenium sulfide composite powder suspension, and ultrasonically heating to 65-70%oC；
(2) Adding coconut oil fatty acid diethanolamide, tricetyl methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride, polyquaternium-10, and dimethylolhydantoin into the suspension in sequence, stirring for 30-40min, and cooling to 40-50%oC, slowly adding the Baphicam 940 powder, stirring for 1-2h, and standing for 12-15h at normal temperature;
(3) then heating and placing at 60-65 deg.CoC, adding fatty alcohol-polyoxyethylene ether sodium sulfate and cocamidopropyl betaine, stirring for 1-2h, and cooling to room temperature;
(4) adding the dianngkang 1491, the ethylenediamine tetraacetic acid and the essence, and stirring for 1-2 h;
(5) adding citric acid aqueous solution, adjusting pH =5 + -0.2, and viscosity 6-7Pa.s
(6) And (6) detecting, packaging and warehousing.
In some embodiments, the amount of the selenium sulfide composite powder is 5 to 15wt.%, the selenium sulfide composite powder is carbon nanospheres with nano selenium sulfide loaded on the surface, wherein the micro carbon spheres prepared by a hydrothermal method are used as a carrier, nano selenium sulfide is prepared on the surface of the micro carbon spheres through electrochemical cathodic reduction and gas phase reaction, the loading amount of the selenium sulfide on the surface of the carbon microsphere carrier is 1 to 3wt.%, the purity of the selenium sulfide is greater than or equal to 95wt.%, and the size of the selenium sulfide is 200-300 nm.
In certain embodiments, the coconut oil fatty acid diethanolamide is used in an amount of 2.5 to 3.5 wt.%; the amount of tris (hexadecyl) methylammonium chloride is 0.5-0.7 wt.%; guar hydroxypropyltrimonium chloride in an amount of 0.2-0.3 wt.%; the polyquaternium-10 is used in an amount of 0.1-0.15 wt.%; the dimethylol hydantoin is used in an amount of 0.15-0.25 wt.%; the amount of the poloxamer is 9400.3-0.4 wt.%.
In certain embodiments, the sodium fatty alcohol polyoxyethylene ether sulfate is present in an amount of 10-12 wt.%; the amount of cocamidopropyl betaine is 9-11 wt.%.
In certain embodiments, the dianhydrongkang 1491 is present in an amount of 1.5 to 2 wt.%; the amount of essence is 0.7-0.8 wt.%; the content of ethylenediamine tetraacetic acid is 0.1-0.15 wt%
In certain embodiments, the hydrothermal method produces carbon spheres as follows: dissolving 10-15g of glucose in 100ml of deionized water, adding 1-1.5g of formaldehyde, adjusting the pH concentration to 8-8.5 by using sodium hydroxide, stirring, transferring to a hydrothermal reaction kettle, adding 220 percent of formaldehyde in 200-220 percent of sodium hydroxideoAnd C, carrying out hydrothermal treatment for 12-16h to obtain a tan suspension, filtering, washing and drying.
In some embodiments, the electrolyte used in the electrochemical cathodic reduction is composed of sodium selenite, sodium chloride, boric acid, a surfactant, carbon sphere particles and deionized water.
In certain embodiments, the sodium selenite is 17.3-51.9g/L, the sodium chloride is 10-12 g/L, the boric acid is 20-25 g/L, the surfactant is 0.05-0.1 g/L, and the carbon sphere particles are 15-25 g/L.
In certain embodiments, the parameters of the electrochemical cathodic reduction are: the current density is 0.2-0.4 mA/cm2The electrochemical treatment time is 50-90 min.
In certain embodiments, the gas phase reaction: placing the microsphere carbon with the surface loaded with the selenium nano-particles in a reaction furnace, introducing sublimed sulfur powder gas, continuously rotating and rolling the reaction furnace in 140-oC, fully reacting for 5-8h, naturally cooling to form sulfur-doped selenium sulfide carbon sphere particles, placing the sulfur-doped selenium sulfide carbon sphere particles in a flowing gas drying furnace, wherein the flowing gas is nitrogen, and the drying temperature is 110-120-oC, drying for 2-3 h.
The shampoo composition comprises the following components: 10-12wt.% of sodium fatty alcohol polyoxyethylene ether sulfate; 9-11wt.% cocamidopropyl betaine; coconut oil fatty acid diethanolamide 2.5-3.5 wt.%; danningkang 14911.5-2 wt.%; 0.7-0.8 wt.% of perfume; 0.5-0.7 wt.% tri (hexadecyl) methylammonium chloride; bocam 9400.3-0.4 wt.%; dimethylol hydantoin 0.15-0.25 wt.%; guar hydroxypropyltrimonium chloride 0.2-0.3 wt.%; polyquaternium-100.1-0.15 wt.%; 0.1-0.15 wt.% ethylenediaminetetraacetic acid; 5-15 wt.% of selenium sulfide composite powder; citric acid adjusted pH =5 ± 0.2; the balance being deionized water.
The sodium fatty alcohol-polyoxyethylene ether sulfate is easily soluble in water and an anionic surfactant, but the structural formula of the sodium fatty alcohol-polyoxyethylene ether sulfate can obviously show that the sodium fatty alcohol-polyoxyethylene ether sulfate has the characteristics of anions and non-ions at the same time, so that the sodium fatty alcohol-polyoxyethylene ether sulfate is endowed with excellent decontamination, emulsification and foaming performances, but the action of the surfactant depends on the pH value of a solution, namely the stability is poor under the condition of over-acid or over-alkali, generally, the pH application range of the sodium fatty alcohol-polyoxyethylene ether sulfate is controlled to be more than 4, the sodium fatty alcohol-polyoxyethylene ether sulfate is limited to be an acidic shampoo by considering the hair quality requirement, and the pH =5 +/-0.2
The cocamidopropyl betaine is a zwitterionic surfactant, presents anion and cation properties, can show excellent synergistic performance when being compounded with a nonionic surfactant such as coconut oil fatty acid diethanolamide, is easy to dissolve in water, has much foam, high viscosity, small irritation to skin and certain bactericidal property.
Coconut oil fatty acid diethanolamide is a nonionic surfactant, is easy to dissolve in water, and can remarkably improve the thickening effect of a solution when an anionic surfactant fatty alcohol polyoxyethylene ether sodium sulfate is compounded for use.
The Douning 1491 is large-particle-size polymer emulsified silicone oil, is an additive of shampoo, is low in addition amount, mainly improves the combing property of hair after the shampoo is used, and provides smooth silk touch.
Although the proportion of the essence in the formula of the shampoo is small, the sensory characteristics of the shampoo are affected, the acceptance degree of consumers is directly affected, the stability and the fragrance of the essence in a product are considered when the essence is selected, the fragrance during and after the shampoo is matched with the brand declaration, and the viscosity and the stability of the shampoo are not affected when the essence is selected.
The tricetyl methyl ammonium chloride is a macromolecular quaternary ammonium salt, particularly, the molecular structure can obviously show that the tricetyl methyl ammonium chloride contains three cetyl groups, and in the use process of the tricetyl methyl ammonium chloride as shampoo, the performance of the tricetyl methyl ammonium chloride is that the steric hindrance of the three cetyl groups can prevent the cation of the tricetyl methyl ammonium chloride from reacting with an anionic surfactant to a certain extent due to the mono-alkyl quaternary ammonium salt and the dialkyl quaternary ammonium salt, so that the additive effect of the tricetyl methyl ammonium chloride can be effectively exerted, and the combing effect of dry combing and wet combing can be obviously improved in the use process of the shampoo.
The poloxamer 940 is a stabilizer or a thickener for the hair washing liquid to be scorched, the main effect of the invention is a stabilizing effect, the addition of the poloxamer 940 can effectively integrate various components to enable the components to be in a proper state, the inorganic components obviously added in the invention can cause the stability of the poloxamer 940 in the hair washing liquid to be important and can effectively suspend particulate matters, so that some documents also refer to the poloxamer 940 as a suspension stabilizer, but the cations of the poloxamer 940 are particularly nameful, such as calcium, magnesium and the like, so that at least a small amount of ethylenediamine tetraacetic acid complexing agent is added into the hair washing liquid to chelate and shield the metal cations.
The dimethylol hydantoin is a commonly used bactericide for washing and protecting compositions, has obvious inhibiting and killing effects on pathogenic bacteria such as escherichia coli, staphylococcus aureus and the like, is a mild antiseptic bactericide, has no influence on use within the range of 0.15-0.25 wt.%, and can obviously improve the shelf life of products.
Guar hydroxypropyl trimethyl ammonium chloride is a high molecular polymer with excellent water solubility, when used as a washing and protecting additive, the guar hydroxypropyl trimethyl ammonium chloride has good sizing and protecting functions on hair, shows excellent antistatic property and conditioning effect after being adsorbed on the hair, changes the wet combing property and dry combing property of the hair, enables the hair to keep luster and softness for a long time, has good elasticity, can achieve better conditioning effect when being matched with polyquaternium series for use, provides good dry and wet combing performance, enables the hair to be fresh and elegant, is polyquaternium-10 which is dissolved in water, can be compounded with various surfactants, has multiple functions of thickening, water retention, antistatic property, wetting property, smoothness and the like, has the capability of protecting damaged protein matrixes, repairs hair tips to split, and endows the hair with excellent wetting property and combing property, the hair is bright and smooth.
The selenium sulfide composite powder is a key component for removing dandruff and relieving itching of shampoo, has the effects of resisting fungi and inhibiting epidermal proliferation, and the preparation method of the selenium sulfide composite powder mainly comprises the following steps:
(1) preparing carbon spheres by a hydrothermal method;
(2) preparing electrolyte, and depositing nano selenium carbon sphere particles on the cathode of the surface of the carbon sphere through electrochemical treatment;
(3) vacuum drying the obtained nano selenium carbon sphere particles,
(4) preparing sulfur-doped selenium sulfide carbon sphere particles through vulcanization;
(5) purifying the selenium sulfide carbon sphere particles to obtain the selenium sulfide composite powder for washing and protecting.
(a) Preparation of carbon spheres by hydrothermal method: what is needed isThe process for preparing the carbon spheres by the hydrothermal method comprises the following steps: dissolving 10-15g of glucose in 100ml of deionized water, adding 1-1.5g of formaldehyde, adjusting the pH concentration to 8-8.5 by using sodium hydroxide, stirring, transferring to a hydrothermal reaction kettle, adding 220 percent of formaldehyde in 200-220 percent of sodium hydroxideoAnd C, carrying out hydrothermal treatment for 12-16h to obtain a tan suspension, and filtering, washing and drying to obtain carbon sphere particles.
The micron-sized carbon spheres are prepared by a hydrothermal method, the micron-sized carbon spheres are low in density and high in specific surface area, the most main reason is that the carbon spheres obtained through hydrothermal treatment contain a large number of polar functional groups, mainly a large number of oxygen-containing functional groups such as hydroxyl and carbonyl, when the carbon spheres are used as electrolyte additives, the carbon spheres can be uniformly distributed in electrolyte, a hydrothermal solution comprises glucose, formaldehyde and a pH regulator, wherein the glucose is a carbon source, the size of the prepared carbon spheres is intensively distributed in a range of 2-4 mu m, and when the particle size of the carbon spheres is closely related to the concentration of the glucose, the concentration of the glucose is increased within a certain range, and the size of the obtained carbon spheres is obviously increased; formaldehyde is an auxiliary agent or a stabilizing agent, wherein carbonyl can effectively react with hydroxyl or carbonyl on the surface of the carbon sphere, so that the polarity of the carbon sphere can be enhanced, and the stability of the carbon sphere in water can be improved; in addition, in addition to concentration and time, the key factors for hydrothermal process are temperature, when the hydrothermal temperature is low, the particles are small, the dispersion degree is high, but the uniformity of the particle size is low, carbon microspheres with uniform particle size cannot be effectively obtained, when the hydrothermal temperature is high, the particles are large, and are easy to agglomerate, so that the dispersion degree is low, and the hydrothermal temperature is limited to 200-oC, the temperature section can obtain 2-4 mu m big balls, and the dispersity is good, thereby being beneficial to process production and control.
(b) Preparing electrolyte, and depositing nano selenium carbon sphere particles on the cathode of the surface of the carbon sphere through electrochemical treatment;
the invention does not put forward the means of electrodeposition for the first time, electrochemical reduction obtains nano-selenium particles, for example, CN102776524A discloses a preparation method of nano-selenium, comprising: a) adding electrolyte containing a selenium source and inorganic inert particles into an electrolytic cell, and introducing direct current into the electrolytic cell under the stirring state; b) and sequentially filtering, washing and drying the mixture in the electrolytic cell to obtain a mixture of selenium particles and inorganic inert particles.
In said patent, the following explanations are made:
as the reduction reaction proceeds, selenium is continuously formed on the cathode surface. In order to avoid that selenium particles are deposited on the surface of a cathode in a large quantity to form crystalline selenium and avoid that an excessively high polarization potential increases energy consumption in a reaction process, inorganic inert particles are added into an electrolytic cell and are electrolyzed in a stirring state, the inorganic inert particles continuously collide with the cathode under the driving of stirring force, the inorganic inert particles rub with the surface of the cathode and simultaneously drive selenium particles on the surface of the cathode to be separated from the surface of the cathode to enter an electrolyte system, then a mixture in the electrolytic cell is filtered, and solid particles obtained by filtering are sequentially washed and dried to obtain a mixture of amorphous selenium particles and inorganic inert particles.
The patent presents the following obvious problems:
(1) the patent precipitates selenium material on the surface of a cathode through electrochemical reduction treatment, and then physically collides and scrapes the selenium material on the surface of the cathode through the grinding action of inorganic inert particles to finally obtain a mixture of selenium and inorganic particles, and the surface of the inorganic particles cannot be electrodeposited with selenium particles due to the non-conductivity of the inorganic inert particles.
(2) The selenium finally prepared by the patent is in a nanometer scale, which represents a doubtful attitude of the present invention, and the skilled person knows that the particle size of the inorganic inert particles is 150-200 meshes, and the use of inert particles close to 70 microns cannot scrape the selenium particles in the nanometer scale on the surface of the cathode.
However, the electrochemical treatment provided by the patent is feasible to deposit nano-scale selenium on the surface of the cathode, and based on the above principle, the invention adopts the conductive carbon spheres and deposits the selenium nano-particles on the surface of the conductive carbon spheres, i.e. micron carbon spheres with selenium nano-particles attached to the surface can be obtained, which is specifically explained as follows:
firstly, preparing electrolyte, wherein the electrolyte consists of 17.3-51.9g/L of sodium selenite, 10-12 g/L of sodium chloride, 20-25 g/L of boric acid, 0.05-0.1 g/L of surfactant and 15-25g/L of carbon sphere particles, and the boric acid is boric acid, and the deionized water.
Wherein the sodium selenite is a selenium source and reacts with 6H under the acidic electrochemical condition++SeO3 2-+4e-→3H2O + Se; the sodium chloride is conductive salt, so that the conductivity of the electrolyte is improved, and in addition, sodium sulfate and magnesium sulfate can also be used as conductive salt;
boric acid is used as a pH stabilizer, so that the pH stability of the electrolyte is effectively maintained; the surfactant is used for improving the dispersibility of the inorganic particles in the plating solution, and can be any surfactant in the prior art, such as sodium dodecyl sulfate, a nonionic surfactant P123, or a Tween surfactant.
In addition, because a large number of oxygen-containing polar groups exist on the surface of the carbon sphere, the groups can obviously adsorb SeO3 2-Ions to form C-SeO3 2-The carbon spheres strongly impact the surface of the cathode material in a disordered state under the stirring condition, and when the conductive carbon spheres are contacted with the cathode, the SeO on the surface of the carbon spheres3 2-Electrochemical reduction on carbon spheres to form nano-selenium, and furthermore, if free SeO3 2-Free SeO upon contact with conductive carbon spheres3 2-Nano-selenium is deposited on the surface of the cathode, and in addition, the carbon spheres are likely to contact with the cathode under stirring to conduct electricity, which indicates that a part of free SeO exists3 2-Cannot be contacted with the conductive carbon spheres, i.e. SeO inevitably occurs on the cathode surface3 2-Electrochemically, so that after a long time of electrochemical reduction treatment, selenium particles are formed on the cathode surface, namely at least three types of selenium are present in the electrolysis, one is selenium A attached to the surface of the carbon sphere, one is selenium B attached to the surface of the cathode, and one is selenium C falling from the cathode surface into the electrolysis due to stirring or friction, wherein nano-selenium carbon sphere particles are recoveredWhen the selenium-containing carbon spheres are used, the particles comprise selenium A and selenium C which are mixtures, but the selenium A and the selenium C are obviously different in morphology, the selenium A is nanoscale selenium particles attached to the surfaces of the carbon spheres, the size of the selenium A is 50-200nm, the selenium C is macroscopic particle selenium obtained through physical collision friction and is a micrometer or millimeter-sized selenium simple substance, the selenium C needs to be recovered, due to the obvious difference in morphology and size of the selenium A and the selenium C, the selenium A is micrometer-sized carbon sphere-nano selenium particles, is good in water solubility and low in density, can be suspended in an aqueous solution for a long time and does not precipitate, the selenium C is micrometer and millimeter-sized amorphous simple substance particles which are poor in water solubility and high in density and are easy to precipitate, and therefore the selenium A and the selenium C can be separated through a simple suspension separation method or a centrifugal separation method, carrying out step (3) treatment on the obtained selenium A, namely drying the obtained nano selenium carbon sphere particles in vacuum; soaking the obtained selenium C in alkali liquor, and recovering for the second time to prepare sodium selenite, wherein the reaction formula is as follows:
3Se+6NaOH=Na2SeO3+2Na2Se+2H2O。
in addition, inert conductive materials are used as a cathode and an anode in the electrochemical process, the cathode is detachably attached to the inside of the electrolytic cell and arranged around the anode, and the anode is arranged in the center of the electrolytic cell and is stirred in the electrochemical reduction process of selenium. And a large amount of selenium B is deposited on the surface of the cathode, and the selenium B and the selenium C are treated in the same way for secondary recovery, so that the detachable cathode needs to be cleaned regularly, the conductivity of the cathode can be improved, and the selenium C on the surface of the cathode can be recovered.
(c) And (3) drying the obtained nano selenium carbon sphere particles in vacuum: the temperature of the vacuum drying is 100-120 DEG CoAnd C, the time is 1-2h, the vacuum drying is mainly aimed at removing liquid on the surface of the nano selenium carbon microsphere, and the nano selenium is required to be dried in vacuum due to high activity of the nano selenium, so that the drying temperature is not easy to be too high, and the phenomenon that the bonding force of the nano selenium and the micro carbon sphere is reduced due to too high temperature, so that heat transfer occurs and the particle size is increased finally is avoided.
(d) Preparation of sulfur-doped selenium sulfide by vulcanizationCarbon sphere particles; placing the selenium sulfide carbon sphere particles obtained by drying in the step (3) in a reaction furnace, introducing sublimed sulfur powder gas, continuously rotating and rolling the reaction furnace in 140-oAnd C, fully reacting for 5-8h, and naturally cooling to form sulfur-doped selenium sulfide carbon sphere particles.
As mentioned above, in the invention, by a mode similar to barrel plating, the conductive carbon microspheres are contacted with the cathode, so that the carbon microspheres are used as the cathode, selenium is electrochemically reduced on the surface of the carbon microspheres, the size of the obtained selenium A is 50-200nm, the particle size is small, the activity is higher, the distribution is uniform, and the reaction of sulfur gas and selenium nanoparticles can be realized at a certain temperature by a simple sulfur sublimation method to form selenium sulfide nanoparticles.
(e) Purifying the selenium sulfide carbon sphere particles to obtain selenium sulfide composite powder for washing and protecting: placing the sulfur-doped selenium sulfide carbon sphere particles prepared in the step (5) into a flowing gas drying furnace, wherein the flowing gas is nitrogen, and the drying temperature is 110-oAnd C, drying for 2-3h, wherein the sublimed sulfur powder gas comprises 95-98vol.% nitrogen.
As mentioned above, because the loading of nano-selenium is limited, and the nano-selenium can react with the sulfur powder completely, the excess sulfur powder can exist in the following two forms: (1) sublimed sulfur does not deposit on the surface of the microsphere, moves along with the nitrogen gas and does not stay; (2) and (2) blocking sulfur, wherein the microporous spheres have a certain specific surface area and can be blocked by micropores or nanopores, sulfur powder is formed in the cooling process, based on the above content, in order to improve the purity of the selenium sulfide on the surfaces of the microporous carbon spheres, the sulfur-doped selenium sulfide carbon sphere particles obtained in the step (4) need to be subjected to surface treatment in a way of performing circulating heating by inert gas, and then blocking sulfur to perform secondary sublimation, so as to leave the surfaces of the carriers, thereby finally obtaining the high-purity selenium sulfide composite powder for washing and protecting, wherein the loading amount of the selenium sulfide on the surfaces of the carbon microsphere carriers is 1-3wt.%, the purity of the selenium sulfide is greater than or equal to 95wt.%, and the size of the selenium sulfide is 200-300 nm. As shown in fig. 1 and fig. 2, the selenium sulfide nanoparticles are located in the dashed boxes.
Advantageous technical effects
(1) According to the selenium sulfide composite powder for hair washing, the selenium sulfide is uniformly dispersed on the surface of the carbon nanospheres in a nano form, the carbon nanospheres have good water solubility, the carbon microsphere particles can be used as an activated carbon hair washing additive, the generation of dandruff can be reduced, the secretion of grease can be reduced, and the malassezia can be obviously inhibited, namely the carbon nanospheres and the selenium sulfide are used as additives, so that the hair washing has multiple functions.
(2) The shampoo has rich foam through the compound use of the sodium fatty alcohol polyoxyethylene ether sulfate, the cocamidopropyl betaine and the coconut fatty acid diethanolamide, the dry and wet combing properties are achieved through the tri (hexadecyl) methyl ammonium chloride, the guar gum hydroxypropyl trimethyl ammonium chloride and the polyquaternium-10, the suspension property of the inorganic micro-carbon spheres in the shampoo is effectively improved through adding the poloxamer 940, and the obtained shampoo can maintain long-term stability.
(3) The shampoo has proper viscosity, is comfortable to use and has good overall use feeling.
Drawings
FIG. 1: SEM picture of the selenium sulfide composite powder prepared by the invention.
FIG. 2 is a drawing: SEM enlarged view of the selenium sulfide composite powder prepared by the invention.
FIG. 3: the shampoo of the invention is used for treating scalp states after 0 week, four weeks and 2 weeks.
FIG. 4 is a drawing: the viscosity of the shampoo of the invention is tested with the stability of time.
The specific implementation mode is as follows:
the preparation process of all the selenium sulfide composite powder in the shampoo is unified as follows:
the selenium sulfide composite powder for hair washing is prepared by the following steps:
(1) the carbon spheres were prepared by a hydrothermal method.
Dissolving 12.5g of glucose in 100ml of deionized water, adding 1.25g of formaldehyde, adjusting the pH concentration to 8.25 by using sodium hydroxide, stirring, transferring to a hydrothermal reaction kettle, and performing reaction at 210oAnd C, carrying out hydrothermal treatment for 14h to obtain a tan suspension, and carrying out filtering, washing and drying treatment to obtain carbon sphere particles.
(2) Preparing electrolyte, and depositing nano selenium carbon sphere particles on the cathode of the surface of the carbon sphere through electrochemical treatment.
The prepared electrolyte consists of 34.6g/L of sodium selenite, 11g/L of sodium chloride, 22.5 g/L of boric acid, 0.075 g/L of surfactant and 20/L of carbon sphere particles, wherein the sodium selenite, the sodium chloride, the boric acid, the surfactant, the carbon sphere particles and the deionized water are mixed together.
Inert conductive materials are used as a cathode and an anode in the electrochemical process, the cathode is detachably attached to the inside of the electrolytic cell and arranged around the anode, and the anode is arranged at the central position of the electrolytic cell and is stirred in the electrochemical reduction process of selenium.
The current density of the electrochemical treatment is 0.3 mA/cm2The electrochemical treatment time is 70 min.
(3) And (4) drying the obtained nano selenium carbon sphere particles in vacuum.
The temperature of the vacuum drying is 110 DEG CoC, the time is 1.5 h.
(4) And (4) vulcanizing to prepare sulfur-doped selenium sulfide carbon sphere particles.
Placing the selenium sulfide carbon sphere particles obtained by drying in the step (3) in a reaction furnace, introducing sublimed sulfur powder gas, wherein the sublimed sulfur powder gas comprises 95-98vol.% of nitrogen, continuously rotating the reaction furnace, and turning at 155 DEGoAnd C, fully reacting for 6.5 hours, and naturally cooling to form sulfur-doped selenium sulfide carbon sphere particles.
(5) Purifying the selenium sulfide carbon sphere particles to obtain the selenium sulfide composite powder for washing and protecting.
Example 1
A preparation method of an anti-dandruff and anti-itching shampoo comprises the following steps:
(1) preparing selenium sulfide composite powder, putting the selenium sulfide composite powder into deionized water solution, stirring to obtain selenium sulfide composite powder suspension, and ultrasonically heating to 65%oC；
(2) Adding coconut oil fatty acid diethanolamide, tricetyl methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride, polyquaternium-10, and dimethylolhydantoin to the suspension in sequence, and stirring for 30minThen cooling to 40 deg.CoC, slowly adding the Baphicam 940 powder, stirring for 1h, and standing for 12h at normal temperature;
(3) then heating and placing at 60oC, adding fatty alcohol-polyoxyethylene ether sodium sulfate and cocamidopropyl betaine, stirring for 1h, and cooling to room temperature;
(4) adding the dianngkang 1491, the ethylenediamine tetraacetic acid and the essence, and stirring for 1 h;
(5) adding citric acid aqueous solution, adjusting pH =5 + -0.2, and viscosity 6-7Pa.s
(6) And (6) detecting, packaging and warehousing.
The obtained shampoo comprises the following components:
fatty alcohol polyoxyethylene ether sodium sulfate 10wt.%
Cocamidopropyl betaine 9wt. -%)
Coconut oil fatty acid diethanolamide 2.5 wt. -%)
Doanningkang 14911.5 wt. -%)
0.7wt.% of essence
0.5 wt.% of tricetyl methyl ammonium chloride
Becam 9400.3 wt. -%)
Dimethylol hydantoin 0.15wt. -%)
Guar hydroxypropyltrimonium chloride 0.2wt. -%)
Polyquaternium-100.1 wt. -%)
0.1 wt.% of ethylenediaminetetraacetic acid
5wt.% of selenium sulfide composite powder
Citric acid adjusted pH =5 ± 0.2
The balance being deionized water.
Example 2
A preparation method of an anti-dandruff and anti-itching shampoo comprises the following steps:
(1) preparing selenium sulfide composite powder, putting the selenium sulfide composite powder into deionized water solution, stirring to obtain selenium sulfide composite powder suspension, and ultrasonically heating to 67 DEGoC；
(2) Adding coconut oil fatty acid diethanolamide, tricetyl methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride, polyquaternium-10, and dimethylol sea water into the suspension in sequenceStirring for 35min, and cooling to 45%oC, slowly adding the Baphicam 940 powder, stirring for 1.5h, and standing for 13h at normal temperature;
(3) then heating and placing at 60-65 deg.CoC, adding fatty alcohol-polyoxyethylene ether sodium sulfate and cocamidopropyl betaine, stirring for 1.5h, and cooling to room temperature;
(4) adding the dianngkang 1491, the ethylenediamine tetraacetic acid and the essence into the mixture, and stirring for 1.5 hours;
(5) adding citric acid aqueous solution, adjusting pH =5 + -0.2, and viscosity 6-7Pa.s
(6) And (6) detecting, packaging and warehousing.
The obtained shampoo comprises the following components:
11wt.% of sodium fatty alcohol polyoxyethylene ether sulfate
10wt.% of cocamidopropyl betaine
Coconut oil fatty acid diethanolamide 3wt. -%)
Doanningkang 14911.75 wt. -%)
0.75 wt.% of essence
0.6 wt.% of tricetyl methyl ammonium chloride
Becam 9400.35 wt. -%)
Dimethylol hydantoin 0.2wt. -%)
Guar hydroxypropyltrimonium chloride 0.25wt. -%)
Polyquaternium-100.125 wt.%
0.125 wt.% of ethylenediaminetetraacetic acid
10wt.% of selenium sulfide composite powder
Citric acid adjusted pH =5 ± 0.2
The balance being deionized water.
Example 3
A preparation method of an anti-dandruff and anti-itching shampoo comprises the following steps:
(1) preparing selenium sulfide composite powder, putting the selenium sulfide composite powder into deionized water solution, stirring to obtain selenium sulfide composite powder suspension, and ultrasonically heating to 70 DEGoC；
(2) Adding coconut fatty acid diethanolamide, tricetyl methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride, and water to the suspension,Stirring polyquaternium-10 and dimethylol hydantoin for 40min, and cooling to 50%oC, slowly adding the Baphicam 940 powder, stirring for 2h, and standing for 15h at normal temperature;
(3) then the temperature is increased and is placed at 65oC, adding fatty alcohol-polyoxyethylene ether sodium sulfate and cocamidopropyl betaine, stirring for 2 hours, and cooling to room temperature;
(4) adding the dianngkang 1491, the ethylenediamine tetraacetic acid and the essence, and stirring for 2 h;
(5) adding citric acid aqueous solution, adjusting pH =5 + -0.2, and viscosity 6-7Pa.s
(6) And (6) detecting, packaging and warehousing.
The obtained shampoo comprises the following components:
12wt.% of sodium fatty alcohol polyoxyethylene ether sulfate
11wt.% of cocamidopropyl betaine
Coconut oil fatty acid diethanolamide 3.5 wt. -%)
Doanningkang 14912 wt. -%)
0.8 wt.% of essence
0.7wt.% of tricetyl methyl ammonium chloride
Becam 9400.4 wt. -%)
Dimethylol hydantoin 0.25wt. -%)
Guar hydroxypropyltrimonium chloride 0.3wt. -%)
Polyquaternium-100.15 wt.%
0.15wt.% of ethylenediaminetetraacetic acid
15wt.% of selenium sulfide composite powder
Citric acid adjusted pH =5 ± 0.2
The balance being deionized water.
Comparative example 1
A preparation method of an anti-dandruff and anti-itching shampoo comprises the following steps:
(1) taking a proper amount of deionized water;
(2) sequentially adding coconut oil fatty acid diethanolamide, tri (hexadecyl) methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride, polyquaternium-10 and dimethylolhydantoin into the deionized water, stirring for 35min, and cooling to 45%oC, slowly adding the Baphicam 940 powder,stirring for 1.5h, and standing for 13h at normal temperature;
(3) then heating and placing at 60-65 deg.CoC, adding fatty alcohol-polyoxyethylene ether sodium sulfate and cocamidopropyl betaine, stirring for 1.5h, and cooling to room temperature;
(4) adding the dianngkang 1491, the ethylenediamine tetraacetic acid and the essence into the mixture, and stirring for 1.5 hours;
(5) adding citric acid aqueous solution, adjusting pH =5 + -0.2, and viscosity 6-7Pa.s
(6) And (6) detecting, packaging and warehousing.
The obtained shampoo comprises the following components:
11wt.% of sodium fatty alcohol polyoxyethylene ether sulfate
10wt.% of cocamidopropyl betaine
Coconut oil fatty acid diethanolamide 3wt. -%)
Doanningkang 14911.75 wt. -%)
0.75 wt.% of essence
0.6 wt.% of tricetyl methyl ammonium chloride
Becam 9400.35 wt. -%)
Dimethylol hydantoin 0.2wt. -%)
Guar hydroxypropyltrimonium chloride 0.25wt. -%)
Polyquaternium-100.125 wt.%
0.125 wt.% of ethylenediaminetetraacetic acid
10wt.% of selenium sulfide composite powder
Citric acid adjusted pH =5 ± 0.2
The balance being deionized water.
Comparative example 2
The hexosaminum scurf-removing and itching-relieving shampoo purchased in the existing market.
The shampoo obtained in example 2 was subjected to a viscosity test, as shown in fig. 4, and within a certain time range, the shampoo of the present invention had a small viscosity fluctuation range and good stability, and the viscosity of the shampoo of the present invention was 6 to 7Pa.s, if the viscosity is too low, the product stability is poor, the shelf stability of the product is affected, and the product is easy to flow away from the hands of consumers during use and gives a feeling of poor quality; the viscosity is too high for the consumer to easily apply to the hair during useThe smearing affects the use feeling of the product for the consumer.
The shampoo is applied to a tester for moistening hair by 30-50ml, the tester gently rubs the hair to ensure that the hair is in full contact with the scalp, after 2-5min, the hair is washed clean by clear water for 2 times a week and used for 4 weeks, the use of the shampoo is stopped, the common shampoo is used, namely the treatment is stopped for 2 weeks, during testing, the hair cannot be washed in the previous day, dandruff is collected, and the quantity of malassezia and grease is detected.
TABLE 1
TABLE 2
Dandruff, known as pityriasis capitis, is a skin disease caused by a fungus called malassezia spp. The mass propagation of malassezia on the scalp causes the hyperproliferation of the scalp stratum corneum, thereby promoting the abnormal falling of stratum corneum cells in the form of white or gray scales, namely the scales, which are dandruff, as can be obviously seen from figure 3, the patient has obvious dandruff and red swelling, the use passes the test, as shown in table 1, the average malassezia on the head of the patient is 125-2On the left and right, the usage of the shampoo and the Haifei of the invention has obvious malassezia reduction in the fourth week, in addition, the table 2 shows that the oil removal efficiency is higher, compared with the Haifei, the anti-dandruff and itching relieving effects are obvious, more obvious, compared with the Haifei, the selenium sulfide of the invention has obvious treatment effect, the malassezia and the grease of the patient are lower when the treatment is stopped for 1 week and 2 weeks.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the dandruff-removing and itching-relieving shampoo is characterized by comprising the following steps:
(1) preparing selenium sulfide composite powder, putting the selenium sulfide composite powder into deionized water solution, stirring to obtain selenium sulfide composite powder suspension, and ultrasonically heating to 65-70%oC；
(2) Adding coconut oil fatty acid diethanolamide, tricetyl methyl ammonium chloride, guar gum hydroxypropyl trimethyl ammonium chloride, polyquaternium-10, and dimethylolhydantoin into the suspension in sequence, stirring for 30-40min, and cooling to 40-50%oC, slowly adding the Baphicam 940 powder, stirring for 1-2h, and standing for 12-15h at normal temperature;
(3) then heating and placing at 60-65 deg.CoC, adding fatty alcohol-polyoxyethylene ether sodium sulfate and cocamidopropyl betaine, stirring for 1-2h, and cooling to room temperature;
(4) adding the dianngkang 1491, the ethylenediamine tetraacetic acid and the essence, and stirring for 1-2 h;
(5) adding citric acid aqueous solution, adjusting pH =5 + -0.2, and viscosity 6-7Pa.s
(6) And (6) detecting, packaging and warehousing.
2. The method for preparing the anti-dandruff and anti-itching shampoo as claimed in claim 1, wherein the amount of the selenium sulfide composite powder is 5-15 wt.%, the selenium sulfide composite powder is carbon nanospheres loaded with nano selenium sulfide on the surface, wherein micron carbon spheres prepared by a hydrothermal method are used as a carrier, the nano selenium sulfide is prepared on the surface of the micron carbon spheres through electrochemical cathodic reduction and gas phase reaction, the loading amount of the selenium sulfide on the surface of the carbon microsphere carrier is 1-3wt.%, the purity of the selenium sulfide is greater than or equal to 95wt.%, and the size of the selenium sulfide is 200-300 nm.
3. The method for preparing an antidandruff and antipruritic shampoo according to claim 1, wherein the coconut oil fatty acid diethanolamide is used in an amount of 2.5 to 3.5 wt.%; the amount of tris (hexadecyl) methylammonium chloride is 0.5-0.7 wt.%; guar hydroxypropyltrimonium chloride in an amount of 0.2-0.3 wt.%; the polyquaternium-10 is used in an amount of 0.1-0.15 wt.%; the dimethylol hydantoin is used in an amount of 0.15-0.25 wt.%; the amount of the poloxamer is 9400.3-0.4 wt.%.
4. The method for preparing an anti-dandruff and antipruritic shampoo according to claim 1, wherein the amount of the sodium fatty alcohol polyoxyethylene ether sulfate is 10 to 12 wt.%; the amount of cocamidopropyl betaine is 9-11 wt.%.
5. The method for preparing an anti-dandruff and anti-itching shampoo according to claim 1, wherein the amount of the dianngkang 1491 is 1.5 to 2 wt.%; the amount of essence is 0.7-0.8 wt.%; the amount of EDTA is 0.1-0.15 wt.%.
6. The method for preparing the dandruff-removing and itching-relieving shampoo as claimed in claim 2, wherein the process for preparing the carbon spheres by the hydrothermal method is as follows: dissolving 10-15g of glucose in 100ml of deionized water, adding 1-1.5g of formaldehyde, adjusting the pH concentration to 8-8.5 by using sodium hydroxide, stirring, transferring to a hydrothermal reaction kettle, adding 220 percent of formaldehyde in 200-220 percent of sodium hydroxideoAnd C, carrying out hydrothermal treatment for 12-16h to obtain a tan suspension, filtering, washing and drying.
7. The method for preparing an antidandruff and antipruritic shampoo according to claim 2, wherein the electrolyte used in the electrochemical cathodic reduction is composed of sodium selenite, sodium chloride, boric acid, a surfactant, carbon sphere particles and deionized water.
8. The method for preparing an antidandruff and antipruritic shampoo according to claim 2, wherein the sodium selenite is 17.3 to 51.9g/L, the sodium chloride is 10 to 12 g/L, the boric acid is 20 to 25g/L, the surfactant is 0.05 to 0.1 g/L, and the carbon sphere particles are 15 to 25 g/L.
9. The method for preparing the dandruff-removing and itching-relieving shampoo as claimed in claim 2, wherein the parameters of the electrochemical cathodic reduction are as follows: the current density is 0.2-0.4 mA/cm2The electrochemical treatment time is 50-90 min.
10. The method for preparing the dandruff-removing and itching-relieving shampoo as claimed in claim 2, wherein the gas phase reaction: placing the microsphere carbon with the surface loaded with the selenium nano-particles in a reaction furnace, introducing sublimed sulfur powder gas, continuously rotating and rolling the reaction furnace in 140-oC, fully reacting for 5-8h, naturally cooling to form sulfur-doped selenium sulfide carbon sphere particles, placing the sulfur-doped selenium sulfide carbon sphere particles in a flowing gas drying furnace, wherein the flowing gas is nitrogen, and the drying temperature is 110-120-oC, drying for 2-3 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114557896A (en) * | 2022-04-16 | 2022-05-31 | 梁小龙 | Preparation method of anti-dandruff shampoo |
| CN114569493A (en) * | 2022-04-16 | 2022-06-03 | 梁小龙 | Anti-dandruff shampoo composition |
| CN114601741A (en) * | 2022-04-16 | 2022-06-10 | 梁小龙 | Selenium sulfide shampoo composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114557896A (en) * | 2022-04-16 | 2022-05-31 | 梁小龙 | Preparation method of anti-dandruff shampoo |
| CN114569493A (en) * | 2022-04-16 | 2022-06-03 | 梁小龙 | Anti-dandruff shampoo composition |
| CN114601741A (en) * | 2022-04-16 | 2022-06-10 | 梁小龙 | Selenium sulfide shampoo composition |
| CN114601741B (en) * | 2022-04-16 | 2023-12-12 | 浙江领康企业管理有限公司 | Selenium sulfide shampoo composition |
| CN114557896B (en) * | 2022-04-16 | 2024-01-23 | 前研化妆品科技(上海)有限公司 | Preparation method of anti-dandruff shampoo |
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Application publication date: 20211112 |