CN111956590A - Slow-release long-acting whitening sunscreen cream and preparation method thereof - Google Patents
Slow-release long-acting whitening sunscreen cream and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a slow-release long-acting whitening sunscreen cream and a preparation method thereof, belonging to the technical field of cosmetic preparation. The slow-release long-acting whitening sunscreen cream is prepared by mixing and reacting a prefabricated material, a hyaluronic acid aqueous solution and a chitosan acetic acid solution; the prefabricated material is prepared from the following raw materials in parts by weight: composite nano-oxide microspheres; acid-etched porous pearl powder; fibroin solution; dimethyl silicone oil; caprylic capric triglyceride; a vitamin E; aloe powder; deionized water; the composite oxide microspheres are prepared by reacting titanium tetrachloride, deionized water, hydrogen peroxide, water glass, sodium dodecyl benzene sulfonate, hydrochloric acid and hexadecyl trimethoxy silane; acid etched porous pearl powder is prepared from pearl, castor oil, absolute ethyl alcohol and deionized water through reaction. The slow-release long-acting whitening sunscreen cream disclosed by the invention has the advantages that the effective sunscreen time is effectively prolonged, the whitening effect is enhanced, the irritation is small, the broad spectrum is strong, and the application prospect is wide.
Description
Technical Field
The invention relates to a slow-release long-acting whitening sunscreen cream and a preparation method thereof, belonging to the technical field of cosmetic preparation.
Background
Along with the increasing living standard, the requirements of people on living quality are higher and higher, cosmetics become indispensable living goods for people, and the requirements of people on cosmetics tend to be natural, low-carbon, environment-friendly, nutritional, low-irritation or non-irritation and the like.
Ultraviolet rays are invisible rays in a high-energy sunlight area and cannot be seen by naked eyes of human beings, the harm to human health caused by excessive ultraviolet ray irradiation is increasingly serious, and the protection of the ultraviolet rays is an extremely urgent problem. Therefore, sun protection is very important in female cosmetics. The development of safe and effective sunscreen products is a potential branch of the modern fine chemical industry.
However, most of the existing common sunscreen creams are prepared from chemically synthesized raw materials, so that the skin is easily stimulated, active ingredients in the sunscreen cream can be completely released in a short time, the sunscreen effective time is short, and the sunscreen effect is not ideal.
In view of the above-mentioned drawbacks, the present designer actively makes research and innovation to create a slow-release long-acting whitening sunscreen cream and a preparation method thereof, so that the sunscreen cream has industrial utility value.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a slow-release long-acting whitening sunscreen cream and a preparation method thereof.
The slow-release long-acting whitening sunscreen cream is prepared by mixing and reacting a preformed material, a hyaluronic acid aqueous solution and a chitosan acetic acid solution;
the prefabricated material is prepared from the following raw materials in parts by weight:
8-10 parts of composite nano oxide microspheres;
8-10 parts of acid-etched porous pearl powder;
5-10 parts of a fibroin solution;
0.5-0.8 part of dimethyl silicone oil;
1.5-2.0 parts of caprylic capric triglyceride;
0.5-1.0 part of vitamin E;
0.2-0.4 parts of aloe powder;
10-15 parts of deionized water;
the composite oxide microspheres are prepared by reacting titanium tetrachloride, deionized water, hydrogen peroxide, water glass, sodium dodecyl benzene sulfonate, hydrochloric acid and hexadecyl trimethoxy silane;
the acid etched porous pearl powder is prepared by reacting pearl, castor oil, absolute ethyl alcohol and deionized water.
The preparation method of the slow-release long-acting whitening sunscreen cream provided by the embodiment of the invention comprises the following specific preparation steps:
(1) weighing Margarita, pulverizing to obtain Margarita powder, mixing with oleum ricini, and rancidity treating;
(2) washing the rancidity product, and drying to obtain acid etched porous pearl powder;
(3) mixing the mixed silk raw material with a sodium carbonate solution, degumming, cleaning, and drying to obtain degummed silk fiber;
(4) mixing the degummed silk fiber with lithium bromide, hydrolyzing and dialyzing to obtain a silk protein solution;
(5) mixing titanium tetrachloride and deionized water for hydrolysis, adding hydrogen peroxide into the hydrolysate, and performing ultrasonic hydrolysis to obtain titanium dioxide hydrosol;
(6) mixing and stirring titanium dioxide hydrosol, water glass, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid to obtain emulsion, adding hexadecyl trimethoxy silane into the emulsion, reacting, filtering to obtain filter residue, washing and drying to obtain the composite nano oxide microspheres;
(7) weighing composite nano oxide microspheres, acid-etched porous pearl powder, fibroin solution, simethicone, caprylic/capric triglyceride, vitamin E, aloe powder and deionized water, mixing and stirring to obtain a prefabricated material;
(8) mixing the prefabricated material and the hyaluronic acid aqueous solution to obtain a base solution, then dropwise adding the chitosan acetic acid solution into the base solution to obtain a mixture, heating, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Further, the preparation method comprises the following specific steps:
(1) weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder with castor oil, paving the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse, and standing for rancidity treatment;
(2) after the rancidity treatment is finished, repeatedly washing the rancidity product for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, after washing is finished, putting the rancidity product into an oven, heating, and drying to obtain the rancid porous pearl powder for later use;
(3) mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L, degumming, and after degumming is finished, cleaning the silk fiber with water and drying to obtain degummed silk fiber;
(4) mixing the degummed silk fiber with lithium bromide, hydrolyzing, obtaining a silk protein lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a silk protein solution for later use;
(5) mixing titanium tetrachloride and deionized water, carrying out hydrolysis reaction to obtain a hydrolysate, adding hydrogen peroxide with the mass concentration of 50% such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis to obtain titanium dioxide hydrosol;
(6) mixing and stirring the titanium dioxide hydrosol, 0.5mol/L sodium silicate, deionized water, sodium dodecyl benzene sulfonate and 0.1mol/L hydrochloric acid to obtain emulsion, adding 10% hexadecyl trimethoxy silane by mass of the sodium silicate into the emulsion, reacting, filtering and separating to obtain filter residue, washing the filter residue, and drying to obtain the composite nano oxide microspheres;
(7) weighing composite nano oxide microspheres, acid-etched porous pearl powder, fibroin solution, simethicone, caprylic/capric triglyceride, vitamin E, aloe powder and deionized water, mixing and stirring to obtain a prefabricated material;
(8) mixing the prefabricated material and a hyaluronic acid aqueous solution to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.8-7.2 to obtain a mixture, putting the obtained mixture into an oven, heating, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Further, the preparation method comprises the following specific steps:
(1) weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse, and standing for rancidity treatment for 7-10 days;
(2) after the rancidity treatment is finished, repeatedly washing the rancidity product for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, after washing is finished, putting the rancidity product into an oven, heating to 60-70 ℃, and drying for 1-2 hours to obtain the rancid porous pearl powder for later use;
(3) mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming, and after degumming is finished, washing silk fibers with water and drying to obtain degummed silk fibers;
(4) mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 5-6 hours at 35-40 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use;
(5) mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 3-5 h to obtain a hydrolysate, adding hydrogen peroxide with the mass concentration of 50% such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis to obtain titanium dioxide hydrosol;
(6) mixing and stirring the titanium dioxide hydrosol, 0.5mol/L sodium silicate, deionized water, sodium dodecyl benzene sulfonate and 0.1mol/L hydrochloric acid to obtain emulsion, adding hexadecyl trimethoxy silane accounting for 10% of the mass of the sodium silicate into the emulsion, heating to 30-70 ℃, reacting for 3-5 h, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres;
(7) weighing 8-10 parts of the composite nano oxide microspheres, 8-10 parts of acid-etched porous pearl powder, 5-10 parts of fibroin solution, 0.5-0.8 part of simethicone, 1.5-2.0 parts of caprylic/capric triglyceride, 0.5-1.0 part of vitamin E, 0.2-0.4 part of aloe powder and 10-15 parts of deionized water, mixing and stirring to obtain a prefabricated material;
(8) mixing the prefabricated material and a hyaluronic acid aqueous solution to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.8-7.2 to obtain a mixture, putting the obtained mixture into an oven, heating, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Further, the temperature of the greenhouse in the step (1) is 45-55 ℃, and the relative humidity of air is 60-70%.
Further, the degumming temperature in the step (3) is 70-80 ℃, and the degumming time is 1-2 hours.
Further, the frequency of ultrasonic hydrolysis in the step (5) is 20-40 kHz, and the time of ultrasonic hydrolysis is 20-30 min.
Further, the mass ratio of the titanium dioxide hydrosol and the water glass with the concentration of 0.5mol/L, the deionized water, the sodium dodecyl benzene sulfonate and the hydrochloric acid with the concentration of 0.1mol/L in the step (6) is 1:1: 10: 1:3.
Further, the mass ratio of the prefabricated material and the hyaluronic acid aqueous solution in the step (8) is 1: 1.
Further, the temperature for heating and raising the temperature in the step (8) is 37-40 ℃.
By adopting the scheme, the invention at least has the following advantages:
due to the addition of the acid etched porous pearl powder and the composite nano oxide microspheres, the slow-release long-acting whitening sun cream has the advantages that the effective sun-screening time is effectively prolonged, the whitening effect is enhanced, the irritation of the used sun-screening whitening raw materials to skin is small, the broad spectrum is strong, and the slow-release long-acting whitening sun cream has a wide application prospect.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
(1) Weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to a mass ratio of 2:1, paving the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse with the temperature of 45-55 ℃ and the relative air humidity of 60-70%, and standing and rancidity for 7-10 days;
(2) after the rancidity treatment is finished, repeatedly washing the rancidity product for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, after washing is finished, putting the rancidity product into an oven, heating to 60-70 ℃, and drying for 1-2 hours to obtain the rancid porous pearl powder for later use; firstly, pearl powder with whitening effect and vegetable oil are mixed and then put in a high-temperature and high-humidity environment for rancidity treatment, the vegetable oil is used for rancidity to generate an acid substance, the acid-soluble ingredients in the pearl powder are corroded and removed through the acid substance, so that the slightly rotten pearl powder with the surface is obtained, the porosity of the surface of the pearl powder is increased, the light incident to the surface of the sun cream is reflected or refracted for multiple times through the rough and porous surface of the acid-etched pearl powder to be reduced, and therefore the ultraviolet-proof effect is achieved;
(3) mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming at the temperature of 70-80 ℃ for 1-2 h, after degumming, washing the silk fibers with water, and drying to obtain degummed silk fibers; firstly, degumming a silk raw material to remove non-silk protein components, thereby having the function of removing impurities;
(4) mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 5-6 hours at 35-40 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use; fibroin with excellent whitening effect is prepared from silk and is used as a biological whitening component, so that the problems of poor skin affinity and easy skin irritation of the traditional chemical substance sunscreen cream are solved;
(5) mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 3-5 h to obtain a hydrolysate, adding hydrogen peroxide with the mass concentration of 50% such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis for 20-30 min at the frequency of 20-40 kHz to obtain titanium dioxide hydrosol;
(6) according to the mass ratio of 1:1: 10: 1:3, mixing and stirring the titanium dioxide hydrosol, 0.5mol/L sodium silicate, deionized water, sodium dodecyl benzene sulfonate and 0.1mol/L hydrochloric acid to obtain emulsion, adding hexadecyl trimethoxy silane accounting for 10% of the mass of the sodium silicate into the emulsion, heating to 30-70 ℃, reacting for 3-5 h, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres; active titanium dioxide hydrosol and water glass are mixed, active titanium dioxide is directly compounded into a system in the process of preparing nano porous silicon dioxide, and under the action of a surfactant, a composite oxide with a porous structure is finally prepared, wherein the titanium dioxide and the silicon dioxide in the composite oxide are excellent ultraviolet light screening agents, the sun-screening effect of the sunscreen cream is effectively improved by adding the titanium dioxide and the silicon dioxide, in addition, the light incident to the surface of the sunscreen cream is reflected or refracted for multiple times to be reduced by the composite nano oxide microspheres, so that the ultraviolet light screening effect is achieved, the incident ultraviolet light is partially absorbed by pores in a molecular motion mode, so that the sunscreen effect is achieved, other sun-screening effective components can be fixedly loaded due to the same porous structure, a slow release effect is achieved, and the sun-screening effective time of the sunscreen cream is prolonged;
(7) weighing 8-10 parts of the composite nano oxide microspheres, 8-10 parts of acid-etched porous pearl powder, 5-10 parts of fibroin solution, 0.5-0.8 part of simethicone, 1.5-2.0 parts of caprylic/capric triglyceride, 0.5-1.0 part of vitamin E, 0.2-0.4 part of aloe powder and 10-15 parts of deionized water, mixing and stirring to obtain a prefabricated material; mixing the sun cream auxiliary material and the functional material with the porous structure to obtain a prefabricated material;
(8) mixing the prefabricated material and a hyaluronic acid aqueous solution according to the mass ratio of 1:1 to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.8-7.2 to obtain a mixture, putting the obtained mixture into an oven, heating to 37-40 ℃, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream. The prefabricated material, the chitosan acetic acid solution and the hyaluronic acid solution are mixed for gelation, so that the effective components for sunscreen and whitening are locked and fixed, and the gel structure can enable the effective components to have a slow release effect, so that the effective acting time of the sunscreen cream is prolonged.
Example 1
Weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse with the temperature of 45 ℃ and the relative air humidity of 60%, and standing and rancidity treatment for 7 days; after the rancidity treatment is finished, repeatedly washing the rancidity product for 3 times by using absolute ethyl alcohol and deionized water in sequence, after the washing is finished, putting the rancidity product into a drying oven, heating to 60 ℃, and drying for 1h to obtain the acidic corrosion porous pearl powder for later use; mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming at the temperature of 70 ℃ for 1h, after degumming is finished, washing the silk fiber with water, and drying to obtain degummed silk fiber; mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 5 hours at 35 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use; mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 3h to obtain a hydrolysate, adding 50% hydrogen peroxide by mass concentration such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis for 20min at the frequency of 20kHz to obtain titanium dioxide hydrosol; according to the mass ratio of 1:1: 10: 1:3, mixing and stirring the titanium dioxide hydrosol, water glass with the concentration of 0.5mol/L, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid with the concentration of 0.1mol/L to obtain emulsion, adding hexadecyl trimethoxy silane with the mass of 10% of the water glass into the emulsion, heating to 30 ℃, reacting for 3hh, filtering and separating to obtain filter residue, washing the filter residue, and drying to obtain the composite nano oxide microspheres; weighing 8 parts of the composite nano oxide microspheres, 8 parts of acid-etched porous pearl powder, 5 parts of fibroin solution, 0.5 part of simethicone, 1.5 parts of caprylic/capric triglyceride, 0.5 part of vitamin E, 0.2 part of aloe powder and 10 parts of deionized water, mixing and stirring to obtain a prefabricated material; mixing the prefabricated material and a hyaluronic acid aqueous solution according to the mass ratio of 1:1 to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.8 to obtain a mixture, putting the obtained mixture into an oven, heating to 37 ℃, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Example 2
Weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse with the temperature of 48 ℃ and the relative air humidity of 62%, and standing and rancidizing for 8 days; after the rancidity treatment is finished, repeatedly washing the rancidity product for 3 times by using absolute ethyl alcohol and deionized water in sequence, after the washing is finished, putting the rancidity product into a drying oven, heating to 62 ℃, and drying for 2 hours to obtain the acidic corrosion porous pearl powder for later use; mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming at the temperature of 72 ℃ for 1h, after degumming is finished, washing the silk fiber with water, and drying to obtain degummed silk fiber; mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 5 hours at 36 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use; mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 3h to obtain a hydrolysate, adding hydrogen peroxide with the mass concentration of 50% such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis for 21min at the frequency of 22kHz to obtain titanium dioxide hydrosol; according to the mass ratio of 1:1: 10: 1:3, mixing and stirring the titanium dioxide hydrosol, water glass with the concentration of 0.5mol/L, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid with the concentration of 0.1mol/L to obtain emulsion, adding hexadecyl trimethoxy silane with the mass of 10% of the water glass into the emulsion, heating to 35 ℃, reacting for 3 hours, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres; weighing 9 parts of the composite nano oxide microspheres, 9 parts of acid-etched porous pearl powder, 6 parts of fibroin solution, 0.6 part of simethicone, 1.6 parts of caprylic/capric triglyceride, 0.6 part of vitamin E, 0.2 part of aloe powder and 11 parts of deionized water, mixing and stirring to obtain a prefabricated material; mixing the prefabricated material and a hyaluronic acid aqueous solution according to the mass ratio of 1:1 to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.9 to obtain a mixture, putting the obtained mixture into an oven, heating to 37 ℃, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Example 3
Weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse with the temperature of 49 ℃ and the relative air humidity of 65%, and standing and rancidizing for 8 days; after the rancidity treatment is finished, repeatedly washing the rancidity product for 4 times by using absolute ethyl alcohol and deionized water in sequence, after the washing is finished, putting the rancidity product into a drying oven, heating to 63 ℃, and drying for 1h to obtain the acidic corrosion porous pearl powder for later use; mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming at the temperature of 73 ℃ for 1h, after degumming is finished, washing the silk fiber with water, and drying to obtain degummed silk fiber; mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 5 hours at 36 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use; mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 3h to obtain a hydrolysate, adding 50% hydrogen peroxide by mass concentration such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis for 25min at the frequency of 25kHz to obtain titanium dioxide hydrosol; according to the mass ratio of 1:1: 10: 1:3, mixing and stirring the titanium dioxide hydrosol, water glass with the concentration of 0.5mol/L, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid with the concentration of 0.1mol/L to obtain emulsion, adding hexadecyl trimethoxy silane with the mass of 10% of the water glass into the emulsion, heating to 40 ℃, reacting for 4 hours, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres; weighing 9 parts of the composite nano oxide microspheres, 9 parts of acid-etched porous pearl powder, 8 parts of fibroin solution, 0.7 part of simethicone, 1.7 parts of caprylic/capric triglyceride, 0.7 part of vitamin E, 0.3 part of aloe powder and 13 parts of deionized water, mixing and stirring to obtain a prefabricated material; mixing the prefabricated material and a hyaluronic acid aqueous solution according to the mass ratio of 1:1 to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 7.0 to obtain a mixture, putting the obtained mixture into an oven, heating to 39 ℃, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Example 4
Weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse with the temperature of 52 ℃ and the relative air humidity of 68%, and standing and rancidity treatment for 8 days; after the rancidity treatment is finished, repeatedly washing the rancidity product for 4 times by using absolute ethyl alcohol and deionized water in sequence, after the washing is finished, putting the rancidity product into a drying oven, heating to 68 ℃, and drying for 2 hours to obtain the acidic corrosion porous pearl powder for later use; mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming at the temperature of 78 ℃ for 2h, after degumming is finished, washing the silk fiber with water, and drying to obtain degummed silk fiber; mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 6 hours at 38 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use; mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 5 hours to obtain a hydrolysate, adding 50% hydrogen peroxide by mass concentration such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis for 28 minutes at the frequency of 20-40 kHz to obtain titanium dioxide hydrosol; according to the mass ratio of 1:1: 10: 1:3, mixing and stirring the titanium dioxide hydrosol, water glass with the concentration of 0.5mol/L, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid with the concentration of 0.1mol/L to obtain emulsion, adding hexadecyl trimethoxy silane with the mass of 10% of the water glass into the emulsion, heating to 60 ℃, reacting for 5 hours, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres; weighing 9 parts of the composite nano oxide microspheres, 9 parts of acid-etched porous pearl powder, 9 parts of fibroin solution, 0.7 part of simethicone, 1.8 parts of caprylic/capric triglyceride, 0.8 part of vitamin E, 0.3 part of aloe powder and 14 parts of deionized water, mixing and stirring to obtain a prefabricated material; mixing the prefabricated material and a hyaluronic acid aqueous solution according to the mass ratio of 1:1 to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 7.1 to obtain a mixture, putting the obtained mixture into an oven, heating to 39 ℃, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Example 5
Weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse with the temperature of 55 ℃ and the relative air humidity of 70%, and standing and rancidity treatment for 10 days; after the rancidity treatment is finished, repeatedly washing the rancidity product for 5 times by using absolute ethyl alcohol and deionized water in sequence, after the washing is finished, putting the rancidity product into a drying oven, heating to 70 ℃, and drying for 2 hours to obtain the acidic corrosion porous pearl powder for later use; mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming at the temperature of 80 ℃ for 2h, after degumming is finished, washing the silk fiber with water, and drying to obtain degummed silk fiber; mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 6 hours at 40 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use; mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 5h to obtain a hydrolysate, adding 50% hydrogen peroxide by mass concentration such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis for 30min at the frequency of 40kHz to obtain titanium dioxide hydrosol; according to the mass ratio of 1:1: 10: 1:3, mixing and stirring the titanium dioxide hydrosol, water glass with the concentration of 0.5mol/L, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid with the concentration of 0.1mol/L to obtain emulsion, adding hexadecyl trimethoxy silane with the mass of 10% of the water glass into the emulsion, heating to 70 ℃, reacting for 3-5 h, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres; weighing 10 parts of the composite nano oxide microspheres, 10 parts of acid-etched porous pearl powder, 10 parts of fibroin solution, 0.8 part of simethicone, 2.0 parts of caprylic/capric triglyceride, 1.0 part of vitamin E, 0.4 part of aloe powder and 15 parts of deionized water, mixing and stirring to obtain a prefabricated material; mixing the prefabricated material and a hyaluronic acid aqueous solution according to the mass ratio of 1:1 to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 7.2 to obtain a mixture, putting the obtained mixture into an oven, heating to 40 ℃, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
Performance detection test:
the sunscreen creams of examples 1-5 were tested for performance, and the results are shown in Table 1:
the detection method comprises the following steps:
irritation test: taking 5 healthy rabbits with weight of 2.5-3.0kg, and shaving off hair of about 3cm on both sides of back2Uniformly coating 0.5g of sunscreen cream on the shaved part of one side 3 times a day, observing the skin of the rabbit at the application side and the skin at the non-application side for 2, 4, 6, 12, 24, 48 and 72 hours after application, and observing the skin at the application side without erythema, hyperemia and other abnormal changes.
And (3) detecting the sun protection coefficient:
a blank background curve of the carrier was first plotted on the SPF-290 assay system. Then evenly spotting 2mg/cm on the transparent film by using a spotter2After being dried, the samples are randomly selected by an SPF-290 analysis system to be tested at 5 points on a transparent film, 5 optical wavelengths, namely monochromatic light protection index curves, are drawn, the test results are calculated to obtain SPF values and standard deviations, and each sample is repeatedly analyzed for 5 times to obtain the sun protection coefficient value;
effective sunscreen time:
measuring the effective sun-screening time by a sun-screening coefficient analyzer;
TABLE 1 Performance test results
Comparative examples 1 to 5:
compared with example 1, in comparative examples 1-5, acid etched porous Margarita powder is replaced with common Margarita powder with weight gradually increased by 10% compared with acid etched porous Margarita powder, and the rest is the same as the preparation method of example 1;
comparative examples 6 to 10:
compared with the example 1, in the comparative examples 6 to 10, the composite nano-oxide microspheres are replaced by the common nano-titanium dioxide particles with the weight gradually increased by 10 percent compared with the composite nano-oxide microspheres, and the rest is the same as the preparation steps of the example 1;
performance detection test:
the performance of the sunscreen creams in the control examples 1 to 10 was measured, and the results are shown in table 2:
the detection method comprises the following steps:
irritation test: taking 5 healthy rabbits with weight of 2.5-3.0kg, and shaving off hair of about 3cm on both sides of back2Uniformly coating 0.5g of sunscreen cream on the shaved part of one side 3 times a day, observing the skin of the rabbit at the application side and the skin at the non-application side for 2, 4, 6, 12, 24, 48 and 72 hours after application, and observing the skin at the application side without erythema, hyperemia and other abnormal changes.
And (3) detecting the sun protection coefficient:
a blank background curve of the carrier was first plotted on the SPF-290 assay system. Then evenly spotting 2mg/cm on the transparent film by using a spotter2After being dried, the samples are randomly selected by an SPF-290 analysis system to be tested at 5 points on a transparent film, 5 optical wavelengths, namely monochromatic light protection index curves, are drawn, the test results are calculated to obtain SPF values and standard deviations, and each sample is repeatedly analyzed for 5 times to obtain the sun protection coefficient value;
effective sunscreen time:
measuring the effective sun-screening time by a sun-screening coefficient analyzer;
TABLE 2 Performance test results
Comparing the comparison examples 1-5 with the comparison examples 1-5, it can be seen that the sun protection factor and the effective sun protection time in the comparison examples 1-5 are both significantly reduced, therefore, the pearl powder with whitening effect and the vegetable oil are mixed and put in the environment of high temperature and high humidity for rancidity treatment, the vegetable oil is used for rancidity treatment, acid substances are generated by rancidity of the vegetable oil, the acid soluble components in the pearl powder are corroded and removed by the acid substances, so that the slightly rotten pearl powder with the surface is obtained, the porosity of the pearl powder is increased, the light incident on the surface of the sun cream is reflected or refracted for many times by the acid corrosion of the rough and porous surface of the pearl powder, so that the effect of preventing ultraviolet rays and sun is achieved, meanwhile, the porous pearl powder is arranged, the incident ultraviolet light is absorbed in the form of molecular motion through the pores of the pearl powder, so that the sun protection effect is achieved, and in addition, the other, the sunscreen cream has a slow release effect, and the sunscreen effective time of the sunscreen cream is prolonged;
comparing the comparison examples 6-10 with the examples 1-5, it can be seen that the sun protection factor and the effective sun protection time in the comparison examples 6-10 are both significantly reduced, therefore, the invention mixes the active titanium dioxide hydrosol and the water glass, directly compounds the active titanium dioxide into the system in the process of preparing the nano porous silicon dioxide, and finally prepares the composite oxide with the porous structure under the action of the surfactant, wherein the titanium dioxide and the silicon dioxide in the composite oxide are both excellent ultraviolet light shielding agents, the addition of the titanium dioxide and the silicon dioxide effectively improves the sun protection effect of the sun protection cream, in addition, the light incident to the surface of the sun protection cream is reflected or refracted for many times to reduce, thereby the ultraviolet protection and sun protection effects are achieved, and the incident ultraviolet light part is absorbed by pores in the form of molecular motion, therefore, the sunscreen cream has a sunscreen effect, and other sunscreen active ingredients can be fixedly loaded due to the same porous structure, so that the sunscreen cream has a slow release effect, and the sunscreen effective time of the sunscreen cream is prolonged.
Claims (10)
1. A slow-release long-acting whitening sunscreen cream is characterized in that: prepared by mixing and reacting a prefabricated material, a hyaluronic acid aqueous solution and a chitosan acetic acid solution;
the prefabricated material is prepared from the following raw materials in parts by weight:
8-10 parts of composite nano oxide microspheres;
8-10 parts of acid-etched porous pearl powder;
5-10 parts of a fibroin solution;
0.5-0.8 part of dimethyl silicone oil;
1.5-2.0 parts of caprylic capric triglyceride;
0.5-1.0 part of vitamin E;
0.2-0.4 parts of aloe powder;
10-15 parts of deionized water;
the composite oxide microspheres are prepared by reacting titanium tetrachloride, deionized water, hydrogen peroxide, water glass, sodium dodecyl benzene sulfonate, hydrochloric acid and hexadecyl trimethoxy silane;
the acid etched porous pearl powder is prepared by reacting pearl, castor oil, absolute ethyl alcohol and deionized water.
2. A preparation method of a slow-release long-acting whitening sunscreen cream is characterized by comprising the following specific preparation steps:
(1) weighing Margarita, pulverizing to obtain Margarita powder, mixing with oleum ricini, and rancidity treating;
(2) washing the rancidity product, and drying to obtain acid etched porous pearl powder;
(3) mixing the mixed silk raw material with a sodium carbonate solution, degumming, cleaning, and drying to obtain degummed silk fiber;
(4) mixing the degummed silk fiber with lithium bromide, hydrolyzing and dialyzing to obtain a silk protein solution;
(5) mixing titanium tetrachloride and deionized water for hydrolysis, adding hydrogen peroxide into the hydrolysate, and performing ultrasonic hydrolysis to obtain titanium dioxide hydrosol;
(6) mixing and stirring titanium dioxide hydrosol, water glass, deionized water, sodium dodecyl benzene sulfonate and hydrochloric acid to obtain emulsion, adding hexadecyl trimethoxy silane into the emulsion, reacting, filtering to obtain filter residue, washing and drying to obtain the composite nano oxide microspheres;
(7) weighing composite nano oxide microspheres, acid-etched porous pearl powder, fibroin solution, simethicone, caprylic/capric triglyceride, vitamin E, aloe powder and deionized water, mixing and stirring to obtain a prefabricated material;
(8) mixing the prefabricated material and the hyaluronic acid aqueous solution to obtain a base solution, then dropwise adding the chitosan acetic acid solution into the base solution to obtain a mixture, heating, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
3. The preparation method of the slow-release long-acting whitening sunscreen cream according to claim 2 is characterized by comprising the following specific preparation steps:
(1) weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder with castor oil, paving the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse, and standing for rancidity treatment;
(2) after the rancidity treatment is finished, repeatedly washing the rancidity product for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, after washing is finished, putting the rancidity product into an oven, heating, and drying to obtain the rancid porous pearl powder for later use;
(3) mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L, degumming, and after degumming is finished, cleaning the silk fiber with water and drying to obtain degummed silk fiber;
(4) mixing the degummed silk fiber with lithium bromide, hydrolyzing, obtaining a silk protein lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a silk protein solution for later use;
(5) mixing titanium tetrachloride and deionized water, carrying out hydrolysis reaction to obtain a hydrolysate, adding hydrogen peroxide with the mass concentration of 50% such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis to obtain titanium dioxide hydrosol;
(6) mixing and stirring the titanium dioxide hydrosol, 0.5mol/L sodium silicate, deionized water, sodium dodecyl benzene sulfonate and 0.1mol/L hydrochloric acid to obtain emulsion, adding 10% hexadecyl trimethoxy silane by mass of the sodium silicate into the emulsion, reacting, filtering and separating to obtain filter residue, washing the filter residue, and drying to obtain the composite nano oxide microspheres;
(7) weighing composite nano oxide microspheres, acid-etched porous pearl powder, fibroin solution, simethicone, caprylic/capric triglyceride, vitamin E, aloe powder and deionized water, mixing and stirring to obtain a prefabricated material;
(8) mixing the prefabricated material and a hyaluronic acid aqueous solution to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.8-7.2 to obtain a mixture, putting the obtained mixture into an oven, heating, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
4. The preparation method of the slow-release long-acting whitening sunscreen cream according to claim 2 or 3, which is characterized by comprising the following specific preparation steps:
(1) weighing pearls, putting the pearls into a grinder, grinding the pearls, sieving the pearls with a 200-mesh sieve, collecting the pearl powder, mixing the pearl powder and castor oil according to the mass ratio of 2:1, spreading the mixture in a stainless steel tray, moving the stainless steel tray into a greenhouse, and standing for rancidity treatment for 7-10 days;
(2) after the rancidity treatment is finished, repeatedly washing the rancidity product for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, after washing is finished, putting the rancidity product into an oven, heating to 60-70 ℃, and drying for 1-2 hours to obtain the rancid porous pearl powder for later use;
(3) mixing the mixed silk raw material of the pupa lining and the cut cocoons with a sodium carbonate solution with the concentration of 0.5mol/L according to the mass ratio of 5:6, degumming, and after degumming is finished, washing silk fibers with water and drying to obtain degummed silk fibers;
(4) mixing the degummed silk fiber and lithium bromide according to the mass ratio of 2:1, hydrolyzing for 5-6 hours at 35-40 ℃, obtaining a fibroin lithium bromide solution after the hydrolysis is finished, continuously dialyzing, and removing the lithium bromide in the solution to obtain a fibroin solution for later use;
(5) mixing titanium tetrachloride and deionized water according to the mass ratio of 1:10, carrying out hydrolysis reaction for 3-5 h to obtain a hydrolysate, adding hydrogen peroxide with the mass concentration of 50% such as deionized water into the hydrolysate, and carrying out ultrasonic hydrolysis to obtain titanium dioxide hydrosol;
(6) mixing and stirring the titanium dioxide hydrosol, 0.5mol/L sodium silicate, deionized water, sodium dodecyl benzene sulfonate and 0.1mol/L hydrochloric acid to obtain emulsion, adding hexadecyl trimethoxy silane accounting for 10% of the mass of the sodium silicate into the emulsion, heating to 30-70 ℃, reacting for 3-5 h, filtering and separating to obtain filter residues, washing the filter residues, and drying to obtain the composite nano oxide microspheres;
(7) weighing 8-10 parts of the composite nano oxide microspheres, 8-10 parts of acid-etched porous pearl powder, 5-10 parts of fibroin solution, 0.5-0.8 part of simethicone, 1.5-2.0 parts of caprylic/capric triglyceride, 0.5-1.0 part of vitamin E, 0.2-0.4 part of aloe powder and 10-15 parts of deionized water, mixing and stirring to obtain a prefabricated material;
(8) mixing the prefabricated material and a hyaluronic acid aqueous solution to obtain a base solution, then dropwise adding a chitosan acetic acid solution with the mass fraction of 5% into the base solution until the pH value of the base solution reaches 6.8-7.2 to obtain a mixture, putting the obtained mixture into an oven, heating, standing for gelation, and bottling to obtain the slow-release long-acting whitening sunscreen cream.
5. The preparation method of the slow-release long-acting whitening sunscreen cream according to any one of claims 2 to 4, characterized in that: in the step (1), the temperature of the greenhouse is 45-55 ℃, and the relative humidity of air is 60-70%.
6. The preparation method of the slow-release long-acting whitening sunscreen cream according to any one of claims 2 to 4, characterized in that: the degumming temperature in the step (3) is 70-80 ℃, and the degumming time is 1-2 h.
7. The preparation method of the slow-release long-acting whitening sunscreen cream according to any one of claims 2 to 4, characterized in that: the frequency of ultrasonic hydrolysis in the step (5) is 20-40 kHz, and the time of ultrasonic hydrolysis is 20-30 min.
8. The preparation method of the slow-release long-acting whitening sunscreen cream according to any one of claims 2 to 4, characterized in that: the mass ratio of the titanium dioxide hydrosol and the water glass with the concentration of 0.5mol/L, the deionized water, the sodium dodecyl benzene sulfonate and the hydrochloric acid with the concentration of 0.1mol/L in the step (6) is 1:1: 10: 1:3.
9. The preparation method of the slow-release long-acting whitening sunscreen cream according to any one of claims 2 to 4, characterized in that: the mass ratio of the prefabricated material to the hyaluronic acid aqueous solution in the step (8) is 1: 1.
10. The preparation method of the slow-release long-acting whitening sunscreen cream according to any one of claims 2 to 4, characterized in that: the heating temperature in the step (8) is 37-40 ℃.
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| CN116919845A (en) * | 2023-08-30 | 2023-10-24 | 美尚(广州)化妆品股份有限公司 | Fibroin sun cream and preparation method thereof |
| CN116919845B (en) * | 2023-08-30 | 2024-06-18 | 美尚(广州)化妆品股份有限公司 | Fibroin sun cream |
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