CN111973517A - A moisture keeping facial mask containing Saviae Miltiorrhizae radix extract with high water locking effect, and its preparation method - Google Patents

A moisture keeping facial mask containing Saviae Miltiorrhizae radix extract with high water locking effect, and its preparation method Download PDF

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CN111973517A
CN111973517A CN202010924900.0A CN202010924900A CN111973517A CN 111973517 A CN111973517 A CN 111973517A CN 202010924900 A CN202010924900 A CN 202010924900A CN 111973517 A CN111973517 A CN 111973517A
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mask
salvia miltiorrhiza
solution
stirring
water
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杜涛
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
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Abstract

The invention relates to the technical field of cosmetics and discloses a high-water-locking moisturizing mask containing a salvia miltiorrhiza extract and a preparation method thereof. The mask liquid comprises a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: glycerol, sodium hyaluronate, 1, 3-butanediol, a salvia miltiorrhiza extract, palmitoyl tetrapeptide-7, xanthan gum, potassium sorbate and the balance of deionized water; the preparation method comprises the steps of mixing deionized water, glycerol, 1, 3-butanediol and sodium hyaluronate, stirring and dispersing until the materials are completely dissolved, heating and preserving heat, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing, cooling to below 45 ℃, adding a red sage root extract and potassium sorbate, continuously stirring and dispersing to obtain a mask liquid, performing irradiation sterilization on the mask liquid, immersing a mask base film in the sterilized mask liquid, taking out and performing vacuum packaging. The mask prepared by the invention has excellent oxidation resistance and water locking performance.

Description

A moisture keeping facial mask containing Saviae Miltiorrhizae radix extract with high water locking effect, and its preparation method
Technical Field
The invention relates to the technical field of cosmetics, in particular to a high-water-locking moisturizing facial mask containing a salvia miltiorrhiza extract and a preparation method thereof.
Background
With the progress of the times and the development of economy, more and more people are focusing on the care of personal skin, and among them, facial masks are gaining more and more acceptance as cosmetics for cleaning, caring and nourishing facial skin. The facial mask has the advantages of convenient carrying, obvious effect and the like, and becomes a skin care product which is popular with people who love beauty. The action mechanism of the mask comprises the following three aspects: 1. the facial mask keeps sufficient nutrition and moisture of facial skin and enhances the elasticity and vitality of the skin by preventing the skin from contacting with air and inhibiting water evaporation; 2. a large amount of water in the mask can fully moisten the skin cuticle, so that the penetration capacity of the cuticle is enhanced, nutrient substances in the mask can effectively infiltrate into the skin, and the metabolism of epithelial tissue cells is promoted; 3. the facial mask has adhesion effect, and when the facial mask is removed, skin dirt is adhered to the facial mask, so that hair follicles of the skin are unobstructed, and sebum is smoothly discharged. General masks can be classified into a peeling type mask, a powder type mask, a clay type mask, a foam type mask, a molding type mask, and the like.
Chinese patent publication No. CN110464680 discloses a Auricularia fuscosuccinea moisturizing mask and a preparation method thereof, which comprises the steps of mixing Auricularia fuscosuccinea moisturizing components with sodium hyaluronate, betaine, trehalose, butanediol, propylene glycol, dipotassium glycyrrhizinate, a preservative, xanthan gum, allantoin, carbomer, triethanolamine and deionized water, homogenizing, stirring, sterilizing, correcting the pH value to prepare mask essence, and soaking a silk mask in the essence to obtain the Auricularia fuscosuccinea moisturizing mask. The mask prepared by the technical scheme has excellent moisturizing performance, but has general oxidation resistance and cannot meet the requirements of people.
Chinese patent publication No. CN204589515 discloses a micro-bubble mask non-woven fabric which is prepared by spunlace compounding of cellulose and a polypropylene hydrophobic layer, and has one water absorption surface and one water prevention and locking surface; chinese patent publication No. CN206183677 discloses a high water-locking moisture mask, which comprises a skin-friendly layer, a water-locking layer and a water-retaining layer which are stacked in sequence, wherein the skin-friendly layer, the water-locking layer and the water-retaining layer are compounded into a mask body through hot pressing. The water-locking mask disclosed in the technical scheme of the patent is formed by compounding multiple layers of base film materials, and the base film of the mask is thick, so that the air permeability of the mask is influenced.
Chinese patent publication No. CN108030702 discloses a water-locking moisture-preserving mask cloth and a preparation method and application thereof, wherein hydrophobic polymer is sprayed on one surface of a non-woven fabric, so that a hydrophobic coating is prepared on the surface of the hydrophilic non-woven fabric, and the hydrophobic coating can prevent evaporation of mask liquid, so that the mask liquid is continuously absorbed by skin. However, it is difficult to uniformly spray the hydrophobic polymer on the surface of the non-woven fabric by the spraying method, and the hydrophobic polymer sprayed on the surface of the non-woven fabric is bonded on the outer side (the surface of the non-woven fabric) of the fiber surface, so that one surface of the fiber on the surface of the non-woven fabric is hydrophilic and the other surface of the fiber is hydrophobic, and the moisture infiltrated in the non-woven fabric can still be diffused to the fiber on the surface of the non-woven fabric, thereby affecting the.
Disclosure of Invention
The invention aims to overcome the problems of the prior art and provides a high water-locking moisture-keeping facial mask containing a salvia miltiorrhiza extract and a preparation method thereof. The mask prepared by the invention has excellent oxidation resistance and water locking performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: 5-10% of glycerol, 1-3% of sodium hyaluronate, 1-2% of 1, 3-butanediol, 3-5% of salvia miltiorrhiza extract, 70.3-0.6% of palmitoyl tetrapeptide, 1-3% of xanthan gum, 0.05-0.3% of potassium sorbate and the balance of deionized water.
Preferably, the preparation method of the salvia miltiorrhiza extract comprises the following steps:
drying and crushing roots and stems of salvia miltiorrhiza to obtain salvia miltiorrhiza powder, adding the salvia miltiorrhiza powder into ethanol water solution with the mass concentration of 70-85%, uniformly stirring and mixing, adding alkali to adjust the pH value of the system to 10-11, heating in water bath to 80-90 ℃, carrying out heat preservation reflux extraction, filtering and separating to obtain primary extract, adding acid to the primary extract to adjust the pH value to 6-7, standing for 10-15h, filtering to remove precipitates, and then carrying out secondary filtration through an ultrafiltration membrane to obtain the salvia miltiorrhiza extract.
Preferably, the mass volume ratio of the salvia miltiorrhiza powder to the ethanol water solution is 1g/25-30 mL.
Preferably, the heat-preservation reflux extraction time is 3-6 h.
Preferably, the ultrafiltration membrane has a molecular weight cut-off of 5000Da to 8000 Da.
Preferably, the preparation method of the mask base film comprises the following steps:
1) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate solution, immersing the viscose non-woven fabric into the sodium alginate solution, dropwise adding a glutaraldehyde crosslinking agent, heating to 40-50 ℃, preserving heat, reacting for 1-2h, taking out the non-woven fabric, and drying to obtain a pretreated non-woven fabric;
2) uniformly mixing deionized water and ethanol according to the volume ratio of 1:20-30 to obtain a mixed solution, adding nano titanium dioxide into the mixed solution, uniformly dispersing by ultrasonic oscillation to obtain a suspension, dropwise adding a sodium hydroxide solution into the suspension to adjust the pH value to 7.5-8.0, then adding tridecafluorooctyl trimethoxysilane and gamma-glycidyl ether oxypropyl trimethoxysilane, heating in a water bath to 50-60 ℃, stirring for reaction for 2-5h, and performing suction filtration, washing and drying to obtain coupling agent surface modified titanium dioxide;
3) uniformly mixing deionized water and ethanol according to the volume ratio of 1:1-2 to obtain a mixed solution, adding bis (2-hydroxyethyl) dimethylammonium chloride into the mixed solution, stirring and dissolving to obtain a bis (2-hydroxyethyl) dimethylammonium chloride solution, adding coupling agent surface modified titanium dioxide into the bis (2-hydroxyethyl) dimethylammonium chloride solution, uniformly dispersing by ultrasonic oscillation, dropwise adding a hydrochloric acid solution to adjust the pH value of the system to 5.0-6.0, adding a tin tetrachloride catalyst, heating in a water bath to 70-80 ℃, stirring to perform a ring-opening reaction, and performing suction filtration, washing and drying to obtain modified nano titanium dioxide particles;
4) putting the pretreated non-woven fabric in the step 1) into a flat-bottom glass container and keeping one surface of the pretreated non-woven fabric tightly attached to the bottom surface of the flat-bottom glass container; adding the modified nano titanium dioxide particles into a mixed solution of ethanol and water, uniformly dispersing by ultrasonic oscillation to obtain a dispersion liquid, pouring the dispersion liquid into a flat-bottomed glass container, standing, taking out the pretreated non-woven fabric, and placing the non-woven fabric in an oven for drying treatment to obtain the modified nano titanium dioxide particles.
Preferably, the mass ratio of the tridecafluorooctyltrimethoxysilane to the gamma-glycidoxypropyltrimethoxysilane in the step 2) is 1: 0.15-0.3.
Preferably, the mass ratio of the nano titanium dioxide to the tridecafluorooctyltrimethoxysilane in the step 2) is 1: 0.3-0.6.
The preparation method of the high water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises the following steps: mixing deionized water, glycerol, 1, 3-butanediol, and sodium hyaluronate, stirring and dispersing until completely dissolved, heating to 75-80 deg.C, and keeping the temperature for 10-20 min; cooling to 50-60 deg.C, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing for 20-30min, cooling to below 45 deg.C, adding Saviae Miltiorrhizae radix extract and potassium sorbate, stirring and dispersing for 15-30min to obtain facial mask solution, sterilizing by irradiation, soaking the facial mask base membrane in sterilized facial mask solution, taking out, and vacuum packaging.
Preferably, the mask basement membrane is soaked in the sterilized mask liquid for 10-20 min.
The facial mask liquid is prepared by compounding glycerin, sodium hyaluronate and 1, 3-butanediol as moisturizing ingredients of the facial mask liquid and is used for keeping skin wet for a long time; palmitoyl tetrapeptide-7 is used as a skin conditioner for shrinking pores and tightening skin; xanthan gum is used as a thickening agent to increase the viscosity of the mask liquid; potassium sorbate is used as an antibacterial agent, so that the preservative effect is achieved, and the shelf life of the mask is prolonged; the red sage root extract is used as an antioxidant, can effectively remove oxygen free radicals in skin cells of a human body, and inhibit lipid peroxidation, thereby delaying skin aging.
According to the invention, the nano titanium dioxide particles with hydrophobic property are combined on one surface of the non-woven fabric, so that one side of the non-woven fabric is hydrophilic, the other side of the non-woven fabric is hydrophilic, and the side with hydrophobic property of the non-woven fabric can prevent moisture in the non-woven fabric from evaporating, thereby increasing the water locking performance of the mask non-woven fabric base film and enabling the mask liquid to be fully absorbed by skin. According to the invention, glutaraldehyde is used for performing cross-linking treatment on sodium alginate in the specific preparation process of the non-woven fabric base film, so that the surface of the non-woven fabric fiber is coated with a layer of anionic sodium alginate polymer, the hydrophilic water retention performance of the non-woven fabric fiber is improved, and the surface of the fiber is negatively charged. The method comprises the steps of modifying the surface of nano titanium dioxide by using tridecafluorooctyl trimethoxysilane and gamma-glycidoxypropyltrimethoxysilane, grafting the tridecafluorooctyl trimethoxysilane and the gamma-glycidoxypropyltrimethoxysilane on the surface of the nano titanium dioxide, loading C-F bonds and epoxy groups with super-hydrophobic properties on the surface of the nano titanium dioxide to prepare super-hydrophobic nano titanium dioxide particles loaded with epoxy groups on the surface, then utilizing the epoxy groups on the surface of the hydrophobic nano titanium dioxide particles to perform ring-opening reaction with hydroxyl groups on (2-hydroxyethyl) dimethyl ammonium chloride, grafting cationic compound (2-hydroxyethyl) dimethyl ammonium chloride on the surface of the hydrophobic nano titanium dioxide particles, enabling the surface of the hydrophobic nano titanium dioxide particles to be positively charged, and enabling the surface of non-woven fabric fibers to be negatively charged, the hydrophobic nano titanium dioxide particles are combined on the surface of the non-woven fabric fiber under the action of electrostatic attraction and sedimentation, so that the hydrophobic nano titanium dioxide particles are uniformly dispersed on the upper surface of the non-woven fabric, and one surface of the non-woven fabric has hydrophobic performance. Compared with the traditional method, the method for directly spraying the hydrophobic polymer on the surface of the non-woven fabric has the advantages that: 1. the hydrophobic nano titanium dioxide particles can be uniformly combined on the surface of the non-woven fabric fiber under the action of electrostatic attraction and free sedimentation, so that the hydrophobic properties of all areas on the surface of the non-woven fabric are similar, and the water locking performance of the non-woven fabric is improved; 2. the hydrophobic substance is combined on the surface of the non-woven fabric by adopting a traditional hydrophobic polymer spraying mode, so that the effect that one side wall of the surface layer fiber of the non-woven fabric is hydrophilic and the other side wall of the surface layer fiber of the non-woven fabric is hydrophobic can only be achieved, and the surface of the non-woven fabric can not be completely covered and combined, and the hydrophobic nano titanium dioxide particles can be completely combined on the surface of the non-woven fabric, so that the whole surface of the fiber is hydrophobic.
Drawings
FIG. 1 is a graph showing the relationship between DPPH radical scavenging rate and the concentration of Salvia miltiorrhiza Bunge extract.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. In the present invention, unless otherwise specified, raw materials, equipment, and the like used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
The non-woven fabric used in the specific embodiment is viscose spunlace non-woven fabric with the gram weight of 34.15g/m2The linear density of the viscose is 1 dtex; sodium alginate: viscosity of 100-200mPa.s, water content less than or equal to 15 percent, pH value of 6.0-8.0, water-insoluble substance less than or equal to 0.6 percent, viscosity reduction rate less than or equal to 20 percent, produced by Qingdao double-formed seaweed Limited company; nano titanium dioxide: model VK-T25F, particle size 20-30nm, specific surface area 100-200m2The pH value is 6-8, and the Hangzhou Wanjing new material is produced by the company Limited.
Example 1
The preparation method of the salvia miltiorrhiza extract comprises the following steps:
drying and crushing roots and stems of salvia miltiorrhiza to obtain salvia miltiorrhiza powder, adding the salvia miltiorrhiza powder into an ethanol aqueous solution with the mass concentration of 85%, stirring and mixing uniformly, wherein the mass volume ratio of the salvia miltiorrhiza powder to the ethanol aqueous solution is 1g/25mL, adding alkali to adjust the pH value of a system to 11, heating in a water bath to 90 ℃, preserving heat, performing reflux extraction for 5h, filtering and separating to obtain a primary extract, adding acid to the primary extract to adjust the pH value to 6, standing for 13h, filtering to remove precipitates, and performing secondary filtration through an ultrafiltration membrane with the molecular weight cutoff of 8000Da to obtain the salvia miltiorrhiza extract.
The high-water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: 8% of glycerin, 2.5% of sodium hyaluronate, 1.5% of 1, 3-butanediol, 4% of salvia miltiorrhiza extract, 70.5% of palmitoyl tetrapeptide, 2.5% of xanthan gum, 0.15% of potassium sorbate and the balance of deionized water.
The preparation method of the mask base film comprises the following steps:
1) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate solution with the mass concentration of 3.0%, immersing the non-woven fabric into the sodium alginate solution according to the bath ratio of 1:30, dropwise adding glutaraldehyde crosslinking agent, wherein the addition amount of the glutaraldehyde crosslinking agent is 4.5 wt% of the sodium alginate, heating to 50 ℃, carrying out heat preservation reaction for 1h, taking out the non-woven fabric, and drying to obtain a pretreated non-woven fabric;
2) uniformly mixing deionized water and ethanol according to the volume ratio of 1:30 to obtain a mixed solution, adding nano titanium dioxide into the mixed solution according to the mass-to-volume ratio of 1g/80mL, uniformly dispersing by ultrasonic oscillation to obtain a suspension, dropwise adding a sodium hydroxide solution with the mass concentration of 1.0% into the suspension to adjust the pH value to 7.5, then adding tridecafluorooctyltrimethoxysilane and gamma-glycidyl ether oxypropyltrimethoxysilane, wherein the mass ratio of the tridecafluorooctyltrimethoxysilane to the gamma-glycidyl ether oxypropyltrimethoxysilane is 1:0.2, the mass ratio of the nano titanium dioxide to the tridecafluorooctyltrimethoxysilane is 1:0.5, heating in a water bath to 50 ℃, stirring for reaction for 4 hours, and obtaining the coupling agent surface modified titanium dioxide through suction filtration, washing and drying;
3) uniformly mixing deionized water and ethanol according to the volume ratio of 1:1 to obtain a mixed solution, adding bis (2-hydroxyethyl) dimethylammonium chloride into the mixed solution, stirring and dissolving to prepare a bis (2-hydroxyethyl) dimethylammonium chloride solution with the mass concentration of 5.0%, adding coupling agent surface modified titanium dioxide into the bis (2-hydroxyethyl) dimethylammonium chloride solution, wherein the mass ratio of the coupling agent surface modified titanium dioxide to the bis (2-hydroxyethyl) dimethylammonium chloride is 1:0.4, uniformly dispersing by ultrasonic oscillation, dropwise adding a hydrochloric acid solution with the mass concentration of 0.5mol/L to adjust the pH of the system to 6.0, adding a tin tetrachloride catalyst, wherein the addition amount of the tin tetrachloride catalyst is 3.0 wt% of the bis (2-hydroxyethyl) dimethylammonium chloride, heating in a water bath to 70 ℃, stirring to carry out a ring-opening reaction for 4 hours, carrying out suction filtration, washing and drying to obtain modified nano titanium dioxide particles;
4) putting the pretreated non-woven fabric in the step 1) into a flat-bottom glass container and keeping one surface of the pretreated non-woven fabric tightly attached to the bottom surface of the flat-bottom glass container; mixing ethanol and water according to the volume ratio of 1:1, then adding modified nano titanium dioxide particles into a mixed solution of the ethanol and the water according to the mass-volume ratio of 1g/60mL, uniformly dispersing by ultrasonic oscillation to obtain a dispersion liquid, pouring the dispersion liquid into a flat-bottomed glass container, keeping the mass ratio of the pretreated non-woven fabric to the dispersion liquid at 1:50, standing for 13h, taking out the pretreated non-woven fabric, and drying in an oven at 70 ℃ for 2h to obtain the modified nano titanium dioxide particles.
The preparation method of the high water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises the following steps:
mixing deionized water, glycerol, 1, 3-butanediol and sodium hyaluronate, stirring and dispersing until completely dissolved, heating to 80 ℃, and keeping the temperature for 10 min; cooling to 60 deg.C, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing for 30min, cooling to below 45 deg.C, adding Saviae Miltiorrhizae radix extract and potassium sorbate, stirring and dispersing for 30min to obtain facial mask solution, sterilizing by irradiation, soaking the facial mask base membrane in sterilized facial mask solution for 20min, taking out, and vacuum packaging.
Example 2
The preparation method of the salvia miltiorrhiza extract comprises the following steps:
drying and crushing roots and stems of salvia miltiorrhiza to obtain salvia miltiorrhiza powder, adding the salvia miltiorrhiza powder into 70% ethanol aqueous solution by mass concentration, stirring and mixing uniformly, wherein the mass volume ratio of the salvia miltiorrhiza powder to the ethanol aqueous solution is 1g/30mL, adding alkali to adjust the pH value of the system to 10, heating in a water bath to 80 ℃, performing heat preservation and reflux extraction for 4h, filtering and separating to obtain a primary extract, adding acid to the primary extract to adjust the pH value to 7, standing for 12h, filtering to remove precipitates, and performing secondary filtration through an ultrafiltration membrane with the molecular weight cutoff of 5000Da to obtain the salvia miltiorrhiza extract.
The high-water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: 6% of glycerin, 1.5% of sodium hyaluronate, 1.5% of 1, 3-butanediol, 3.5% of salvia miltiorrhiza extract, 70.4% of palmitoyl tetrapeptide, 1.5% of xanthan gum, 0.1% of potassium sorbate and the balance of deionized water.
The preparation method of the mask base film comprises the following steps:
1) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate solution with the mass concentration of 3.0%, immersing the non-woven fabric into the sodium alginate solution according to the bath ratio of 1:30, dropwise adding glutaraldehyde crosslinking agent, wherein the addition amount of the glutaraldehyde crosslinking agent is 3.5 wt% of the sodium alginate, heating to 40 ℃, carrying out heat preservation reaction for 2 hours, taking out the non-woven fabric, and drying to obtain a pretreated non-woven fabric;
2) uniformly mixing deionized water and ethanol according to the volume ratio of 1:20 to obtain a mixed solution, adding nano titanium dioxide into the mixed solution according to the mass-to-volume ratio of 1g/80mL, uniformly dispersing by ultrasonic oscillation to obtain a suspension, dropwise adding a sodium hydroxide solution with the mass concentration of 1.0% into the suspension to adjust the pH value to 8.0, then adding tridecafluorooctyltrimethoxysilane and gamma-glycidyl ether oxypropyltrimethoxysilane, wherein the mass ratio of the tridecafluorooctyltrimethoxysilane to the gamma-glycidyl ether oxypropyltrimethoxysilane is 1:0.25, the mass ratio of the nano titanium dioxide to the tridecafluorooctyltrimethoxysilane is 1:0.4, heating in a water bath to 60 ℃, stirring for reaction for 3 hours, and obtaining the coupling agent surface modified titanium dioxide through suction filtration, washing and drying;
3) uniformly mixing deionized water and ethanol according to the volume ratio of 1:2 to obtain a mixed solution, adding bis (2-hydroxyethyl) dimethylammonium chloride into the mixed solution, stirring and dissolving to prepare a bis (2-hydroxyethyl) dimethylammonium chloride solution with the mass concentration of 5.0%, adding coupling agent surface modified titanium dioxide into the bis (2-hydroxyethyl) dimethylammonium chloride solution, wherein the mass ratio of the coupling agent surface modified titanium dioxide to the bis (2-hydroxyethyl) dimethylammonium chloride is 1:0.3, uniformly dispersing by ultrasonic oscillation, dropwise adding a hydrochloric acid solution with the mass concentration of 0.5mol/L to adjust the pH of the system to 5.0, adding a tin tetrachloride catalyst, wherein the adding amount of the tin tetrachloride catalyst is 3.0 wt% of the bis (2-hydroxyethyl) dimethylammonium chloride, heating in a water bath to 80 ℃, stirring to carry out a ring-opening reaction for 3.5 hours, carrying out suction filtration, washing and drying to obtain modified nano titanium dioxide particles;
4) putting the pretreated non-woven fabric in the step 1) into a flat-bottom glass container and keeping one surface of the pretreated non-woven fabric tightly attached to the bottom surface of the flat-bottom glass container; mixing ethanol and water according to the volume ratio of 1:1, then adding modified nano titanium dioxide particles into a mixed solution of the ethanol and the water according to the mass-volume ratio of 1g/60mL, uniformly dispersing by ultrasonic oscillation to obtain a dispersion liquid, pouring the dispersion liquid into a flat-bottomed glass container, keeping the mass ratio of the pretreated non-woven fabric to the dispersion liquid at 1:50, standing for 12h, taking out the pretreated non-woven fabric, and drying in an oven at 50 ℃ for 3h to obtain the modified nano titanium dioxide particles.
The preparation method of the high water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises the following steps:
mixing deionized water, glycerol, 1, 3-butanediol and sodium hyaluronate, stirring and dispersing until completely dissolved, heating to 75 ℃, and keeping the temperature for 20 min; cooling to 50 deg.C, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing for 20min, cooling to below 45 deg.C, adding Saviae Miltiorrhizae radix extract and potassium sorbate, stirring and dispersing for 15min to obtain facial mask solution, sterilizing by irradiation, soaking the facial mask base membrane in sterilized facial mask solution for 10min, taking out, and vacuum packaging.
Example 3
The preparation method of the salvia miltiorrhiza extract comprises the following steps:
drying and crushing root and stem of salvia miltiorrhiza to obtain salvia miltiorrhiza powder, adding the salvia miltiorrhiza powder into an ethanol aqueous solution with the mass concentration of 80%, stirring and mixing uniformly, wherein the mass volume ratio of the salvia miltiorrhiza powder to the ethanol aqueous solution is 1g/28mL, adding alkali to adjust the pH of the system to 10.5, heating in a water bath to 85 ℃, preserving heat, refluxing and extracting for 6h, filtering and separating to obtain a primary extract, adding acid to the primary extract to adjust the pH to 6.5, standing for 15h, filtering to remove precipitates, and then performing secondary filtration through an ultrafiltration membrane with the molecular weight cutoff of 6000Da to obtain the salvia miltiorrhiza extract.
The high-water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: 10% of glycerin, 3% of sodium hyaluronate, 2% of 1, 3-butanediol, 5% of salvia miltiorrhiza extract, 70.6% of palmitoyl tetrapeptide, 3% of xanthan gum, 0.3% of potassium sorbate and the balance of deionized water.
The preparation method of the mask base film comprises the following steps:
1) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate solution with the mass concentration of 3.0%, immersing the non-woven fabric into the sodium alginate solution according to the bath ratio of 1:30, dropwise adding glutaraldehyde crosslinking agent, wherein the addition amount of the glutaraldehyde crosslinking agent is 5.0 wt% of the sodium alginate, heating to 45 ℃, keeping the temperature and reacting for 1.5h, taking out the non-woven fabric, and drying to obtain a pretreated non-woven fabric;
2) uniformly mixing deionized water and ethanol according to the volume ratio of 1:25 to obtain a mixed solution, adding nano titanium dioxide into the mixed solution according to the mass-to-volume ratio of 1g/80mL, uniformly dispersing by ultrasonic oscillation to obtain a suspension, dropwise adding a sodium hydroxide solution with the mass concentration of 1.0% into the suspension to adjust the pH value to 7.5, then adding tridecafluorooctyltrimethoxysilane and gamma-glycidyl ether oxypropyltrimethoxysilane, wherein the mass ratio of the tridecafluorooctyltrimethoxysilane to the gamma-glycidyl ether oxypropyltrimethoxysilane is 1:0.15, the mass ratio of the nano titanium dioxide to the tridecafluorooctyltrimethoxysilane is 1:0.6, heating in a water bath to 55 ℃, stirring and reacting for 5 hours, and obtaining the coupling agent surface modified titanium dioxide after suction filtration, washing and drying;
3) uniformly mixing deionized water and ethanol according to the volume ratio of 1:1.5 to obtain a mixed solution, adding bis (2-hydroxyethyl) dimethylammonium chloride into the mixed solution, stirring and dissolving to prepare a bis (2-hydroxyethyl) dimethylammonium chloride solution with the mass concentration of 5.0%, adding coupling agent surface modified titanium dioxide into the bis (2-hydroxyethyl) dimethylammonium chloride solution, wherein the mass ratio of the coupling agent surface modified titanium dioxide to the bis (2-hydroxyethyl) dimethylammonium chloride is 1:0.5, performing ultrasonic oscillation and uniform dispersion, dropwise adding a hydrochloric acid solution with the mass concentration of 0.5mol/L to adjust the pH of the system to 5.5, adding a tin tetrachloride catalyst, wherein the addition amount of the tin tetrachloride catalyst is 3.0 wt% of the bis (2-hydroxyethyl) dimethylammonium chloride, heating in a water bath to 75 ℃, stirring to perform ring-opening reaction for 5 hours, carrying out suction filtration, washing and drying to obtain modified nano titanium dioxide particles;
4) putting the pretreated non-woven fabric in the step 1) into a flat-bottom glass container and keeping one surface of the pretreated non-woven fabric tightly attached to the bottom surface of the flat-bottom glass container; mixing ethanol and water according to the volume ratio of 1:1, then adding modified nano titanium dioxide particles into a mixed solution of the ethanol and the water according to the mass-volume ratio of 1g/60mL, uniformly dispersing by ultrasonic oscillation to obtain a dispersion liquid, pouring the dispersion liquid into a flat-bottomed glass container, keeping the mass ratio of the pretreated non-woven fabric to the dispersion liquid at 1:50, standing for 15h, taking out the pretreated non-woven fabric, and drying in an oven at 60 ℃ for 2.5h to obtain the modified nano titanium dioxide particles.
The preparation method of the high water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises the following steps:
mixing deionized water, glycerol, 1, 3-butanediol and sodium hyaluronate, stirring and dispersing until completely dissolved, heating to 78 ℃, and keeping the temperature for 15 min; cooling to 55 deg.C, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing for 25min, cooling to below 45 deg.C, adding Saviae Miltiorrhizae radix extract and potassium sorbate, stirring and dispersing for 20min to obtain facial mask solution, sterilizing by irradiation, soaking the facial mask base membrane in sterilized facial mask solution for 15min, taking out, and vacuum packaging.
Example 4
The preparation method of the salvia miltiorrhiza extract comprises the following steps:
drying and crushing roots and stems of salvia miltiorrhiza to obtain salvia miltiorrhiza powder, adding the salvia miltiorrhiza powder into an ethanol aqueous solution with the mass concentration of 80%, stirring and mixing uniformly, wherein the mass volume ratio of the salvia miltiorrhiza powder to the ethanol aqueous solution is 1g/28mL, adding alkali to adjust the pH of the system to 10.5, heating in a water bath to 85 ℃, preserving heat, refluxing and extracting for 3h, filtering and separating to obtain a primary extract, adding acid to the primary extract to adjust the pH to 6.5, standing for 10h, filtering to remove precipitates, and then performing secondary filtration through an ultrafiltration membrane with the molecular weight cutoff of 7000Da to obtain the salvia miltiorrhiza extract.
The high-water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: 5% of glycerin, 1% of sodium hyaluronate, 1% of 1, 3-butanediol, 3% of salvia miltiorrhiza extract, 70.3% of palmitoyl tetrapeptide, 1% of xanthan gum, 0.05% of potassium sorbate and the balance of deionized water.
The preparation method of the mask base film comprises the following steps:
1) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate solution with the mass concentration of 3.0%, immersing the non-woven fabric into the sodium alginate solution according to the bath ratio of 1:30, dropwise adding glutaraldehyde crosslinking agent, wherein the addition amount of the glutaraldehyde crosslinking agent is 3.0 wt% of the sodium alginate, heating to 45 ℃, keeping the temperature and reacting for 1.5h, taking out the non-woven fabric, and drying to obtain a pretreated non-woven fabric;
2) uniformly mixing deionized water and ethanol according to the volume ratio of 1:25 to obtain a mixed solution, adding nano titanium dioxide into the mixed solution according to the mass-to-volume ratio of 1g/80mL, uniformly dispersing by ultrasonic oscillation to obtain a suspension, dropwise adding a sodium hydroxide solution with the mass concentration of 1.0% into the suspension to adjust the pH value to 8.0, then adding tridecafluorooctyltrimethoxysilane and gamma-glycidyl ether oxypropyltrimethoxysilane, wherein the mass ratio of the tridecafluorooctyltrimethoxysilane to the gamma-glycidyl ether oxypropyltrimethoxysilane is 1:0.3, the mass ratio of the nano titanium dioxide to the tridecafluorooctyltrimethoxysilane is 1:0.3, heating in a water bath to 55 ℃, stirring for reaction for 2h, and obtaining the coupling agent surface modified titanium dioxide through suction filtration, washing and drying;
3) uniformly mixing deionized water and ethanol according to the volume ratio of 1:1.5 to obtain a mixed solution, adding bis (2-hydroxyethyl) dimethylammonium chloride into the mixed solution, stirring and dissolving to prepare a bis (2-hydroxyethyl) dimethylammonium chloride solution with the mass concentration of 5.0%, adding coupling agent surface modified titanium dioxide into the bis (2-hydroxyethyl) dimethylammonium chloride solution, wherein the mass ratio of the coupling agent surface modified titanium dioxide to the bis (2-hydroxyethyl) dimethylammonium chloride is 1:0.2, performing ultrasonic oscillation and uniform dispersion, dropwise adding a hydrochloric acid solution with the mass concentration of 0.5mol/L to adjust the pH of the system to 5.5, adding a tin tetrachloride catalyst, wherein the addition amount of the tin tetrachloride catalyst is 3.0 wt% of the bis (2-hydroxyethyl) dimethylammonium chloride, heating in a water bath to 75 ℃, stirring to perform ring-opening reaction for 3 hours, carrying out suction filtration, washing and drying to obtain modified nano titanium dioxide particles;
4) putting the pretreated non-woven fabric in the step 1) into a flat-bottom glass container and keeping one surface of the pretreated non-woven fabric tightly attached to the bottom surface of the flat-bottom glass container; mixing ethanol and water according to the volume ratio of 1:1, then adding modified nano titanium dioxide particles into a mixed solution of the ethanol and the water according to the mass-volume ratio of 1g/60mL, uniformly dispersing by ultrasonic oscillation to obtain a dispersion liquid, pouring the dispersion liquid into a flat-bottomed glass container, keeping the mass ratio of the pretreated non-woven fabric to the dispersion liquid at 1:50, standing for 10h, taking out the pretreated non-woven fabric, and drying in an oven at 60 ℃ for 2.5h to obtain the modified nano titanium dioxide particles.
The preparation method of the high water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract comprises the following steps:
mixing deionized water, glycerol, 1, 3-butanediol and sodium hyaluronate, stirring and dispersing until completely dissolved, heating to 78 ℃, and keeping the temperature for 15 min; cooling to 55 deg.C, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing for 25min, cooling to below 45 deg.C, adding Saviae Miltiorrhizae radix extract and potassium sorbate, stirring and dispersing for 20min to obtain facial mask solution, sterilizing by irradiation, soaking the facial mask base membrane in sterilized facial mask solution for 15min, taking out, and vacuum packaging.
Comparative example
The viscose nonwoven fabric without any treatment was used as a control.
1. Testing the mechanical property of the mask base film:
the tensile breaking strength is an important index for evaluating the performance of the non-woven fabric, and the strength directly influences the performance and the application of the non-woven fabric. The mask base cloth is used as a material which is often held and applied to the face before use, and needs a certain heat-insulating and stable mechanical strength. The mask is applied to the face with slight adjustment of pulling, and therefore, the strength of the mask base cloth in a wet state needs to be detected. The base film material was cut into 5cm × 30 cm-sized samples according to GB/T24218.3-2010, and subjected to a tensile test in a YG065H electronic textile strength tester with a nip distance of 20 cm. For the strength test in a wet state, the sample is subjected to humidity adjustment according to GB/T6529-2008, the test in the wet state is carried out by soaking the sample in deionized distilled water for 1h, taking out the sample, filtering out excessive water and immediately carrying out the test.
Figure BDA0002668083350000091
2. Testing the water locking performance of the mask base film:
respectively soaking the base film materials in examples 1-4 and comparative example in deionized water for 30min, taking out, placing in air, draining until no water drops, and weighing the base film materials to obtain m1Adhering the hydrophilic surface of the base film material to a glass plate, respectively standing at 28 deg.C for 10min, 20min, 30min, and 40min, and weighing the base film material at the moment2The evaporation rate (%) of water in the base film material was calculated according to the following formula (m)1-m2)/m1×100%。
Figure BDA0002668083350000101
The wet strength of the base film material prepared by the invention can reach more than 17.21 in the transverse direction and 23.36 in the longitudinal direction respectively through the mechanical property test result of the base film material, and the daily use requirement of the mask can be met. Through the water locking performance test of the base film material, the water evaporation rates of 10min, 20min, 30min and 40min of the invention are obviously lower than those of the comparative example, and the water evaporation rate of 40min is controlled below 25% in the environment of 28 ℃, so that the base film material has a good water locking effect.
3. And (3) detecting the antioxidant effect of the mask liquid:
will DPreparing DPPH into 0.2mmmol/mL DPPH absolute ethanol solution in a volumetric flask, mixing 2mL absolute ethanol solutions (10mg/mL, 20mg/mL, 30mg/mL, 40mg/mL, 50mg/mL) of Saviae Miltiorrhizae radix extract with 2mL absolute ethanol solution, reacting for 30min in dark condition, measuring absorbance at 517nm, and recording as A1Uniformly mixing 2mL of absolute ethyl alcohol and 2mL of alcohol solution of LDPPH, testing the absorbance at 517nm, and recording as A02mL of absolute ethanol was mixed with 2mL of absolute ethanol solutions of the Salvia miltiorrhiza Bunge extracts at different concentrations, and the absorbance at 517nm was measured and recorded as A2.
DPPH radical scavenging ratio (%) - [1- (A)1-A2)/A0]X 100%, wherein A in the formula0Absorbance of blank control; a. the1Is the absorbance of the salvia extract solution; a. the2Is the absorbance of the liquid body to be detected.
The test structure is shown in figure 1, and the test result shows that the salvia miltiorrhiza bunge extract has good antioxidant activity, and the DPPH free radical clearance rate is improved along with the increase of the concentration of the salvia miltiorrhiza bunge extract.
The foregoing is directed to the preferred embodiment of the present invention and it is noted that various modifications and changes may be made by those skilled in the art without departing from the spirit of the invention and these modifications and changes are to be considered within the scope of the invention.

Claims (10)

1. The high-water-locking moisturizing mask containing the salvia miltiorrhiza bunge extract is characterized by comprising a mask base film and a mask liquid, wherein the mask liquid comprises the following components in parts by weight: 5-10% of glycerol, 1-3% of sodium hyaluronate, 1-2% of 1, 3-butanediol, 3-5% of salvia miltiorrhiza extract, 70.3-0.6% of palmitoyl tetrapeptide, 1-3% of xanthan gum, 0.05-0.3% of potassium sorbate and the balance of deionized water.
2. The mask as claimed in claim 1, wherein the method for preparing the salvia miltiorrhiza bunge extract comprises the following steps:
drying and crushing roots and stems of salvia miltiorrhiza to obtain salvia miltiorrhiza powder, adding the salvia miltiorrhiza powder into ethanol water solution with the mass concentration of 70-85%, uniformly stirring and mixing, adding alkali to adjust the pH value of the system to 10-11, heating in water bath to 80-90 ℃, carrying out heat preservation reflux extraction, filtering and separating to obtain primary extract, adding acid to the primary extract to adjust the pH value to 6-7, standing for 10-15h, filtering to remove precipitates, and then carrying out secondary filtration through an ultrafiltration membrane to obtain the salvia miltiorrhiza extract.
3. The mask as claimed in claim 2, wherein the moisture-keeping mask containing the salvia miltiorrhiza bunge extract is characterized in that the mass-to-volume ratio of the salvia miltiorrhiza bunge powder to the ethanol aqueous solution is 1g/25-30 mL.
4. The mask as claimed in claim 2, wherein the extraction time of the heat-preserving reflux is 3-6 h.
5. The mask as claimed in claim 2, wherein the ultrafiltration membrane has a molecular weight cut-off of 5000Da to 8000 Da.
6. The mask with high water-locking and moisture-keeping function containing the salvia miltiorrhiza bunge extract as claimed in claim 1, wherein the preparation method of the mask base film comprises the following steps:
1) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate solution, immersing the viscose non-woven fabric into the sodium alginate solution, dropwise adding a glutaraldehyde crosslinking agent, heating to 40-50 ℃, preserving heat, reacting for 1-2h, taking out the non-woven fabric, and drying to obtain a pretreated non-woven fabric;
2) uniformly mixing deionized water and ethanol according to the volume ratio of 1:20-30 to obtain a mixed solution, adding nano titanium dioxide into the mixed solution, uniformly dispersing by ultrasonic oscillation to obtain a suspension, dropwise adding a sodium hydroxide solution into the suspension to adjust the pH value to 7.5-8.0, then adding tridecafluorooctyl trimethoxysilane and gamma-glycidyl ether oxypropyl trimethoxysilane, heating in a water bath to 50-60 ℃, stirring for reaction for 2-5h, and performing suction filtration, washing and drying to obtain coupling agent surface modified titanium dioxide;
3) uniformly mixing deionized water and ethanol according to the volume ratio of 1:1-2 to obtain a mixed solution, adding bis (2-hydroxyethyl) dimethylammonium chloride into the mixed solution, stirring and dissolving to obtain a bis (2-hydroxyethyl) dimethylammonium chloride solution, adding coupling agent surface modified titanium dioxide into the bis (2-hydroxyethyl) dimethylammonium chloride solution, uniformly dispersing by ultrasonic oscillation, dropwise adding a hydrochloric acid solution to adjust the pH value of the system to 5.0-6.0, adding a tin tetrachloride catalyst, heating in a water bath to 70-80 ℃, stirring to perform a ring-opening reaction, and performing suction filtration, washing and drying to obtain modified nano titanium dioxide particles;
4) putting the pretreated non-woven fabric in the step 1) into a flat-bottom glass container and keeping one surface of the pretreated non-woven fabric tightly attached to the bottom surface of the flat-bottom glass container; adding the modified nano titanium dioxide particles into a mixed solution of ethanol and water, uniformly dispersing by ultrasonic oscillation to obtain a dispersion liquid, pouring the dispersion liquid into a flat-bottomed glass container, standing, taking out the pretreated non-woven fabric, and placing the non-woven fabric in an oven for drying treatment to obtain the modified nano titanium dioxide particles.
7. The mask as claimed in claim 6, wherein the weight ratio of tridecafluorooctyltrimethoxysilane to gamma-glycidoxypropyltrimethoxysilane in step 2) is 1: 0.15-0.3.
8. The mask as claimed in claim 6, wherein the ratio of the nano titanium dioxide to the tridecafluorooctyltrimethoxysilane in step 2) is 1: 0.3-0.6.
9. The method for preparing a moisture-retaining mask with high water retention containing salvia miltiorrhiza bunge extract as claimed in any one of claims 1 to 8, comprising the steps of: mixing deionized water, glycerol, 1, 3-butanediol, and sodium hyaluronate, stirring and dispersing until completely dissolved, heating to 75-80 deg.C, and keeping the temperature for 10-20 min; cooling to 50-60 deg.C, adding palmitoyl tetrapeptide-7 and xanthan gum, stirring and dispersing for 20-30min, cooling to below 45 deg.C, adding Saviae Miltiorrhizae radix extract and potassium sorbate, stirring and dispersing for 15-30min to obtain facial mask solution, sterilizing by irradiation, soaking the facial mask base membrane in sterilized facial mask solution, taking out, and vacuum packaging.
10. The method for preparing a moisture-preserving mask with high water-locking capacity comprising salvia miltiorrhiza bunge extract as claimed in claim 9, wherein the mask basement membrane is soaked in the sterilized mask solution for 10-20 min.
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CN112535654A (en) * 2020-12-02 2021-03-23 罗亚文 Preparation method of mask with water locking effect
CN112870088A (en) * 2021-01-27 2021-06-01 佛山市优特医疗科技有限公司 Moisture-absorbing gel-forming transparent mask
CN112870088B (en) * 2021-01-27 2022-05-17 佛山市优特医疗科技有限公司 Moisture-absorbing gel-forming transparent mask
CN113750006A (en) * 2021-08-27 2021-12-07 植然天成(北京)生物科技有限公司 Salvia miltiorrhiza mud-shaped mask and preparation method and use method thereof
CN113750006B (en) * 2021-08-27 2022-10-28 植然天成(北京)生物科技有限公司 Salvia miltiorrhiza mud-shaped mask and preparation method and use method thereof
CN115364030A (en) * 2022-09-23 2022-11-22 西南林业大学 Paris polyphylla product and preparation method and application thereof
CN115364030B (en) * 2022-09-23 2023-06-20 西南林业大学 Paris polyphylla product and preparation method and application thereof

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Application publication date: 20201124