CN108085973B - Freckle-removing silk mask with high water retention property - Google Patents

Freckle-removing silk mask with high water retention property Download PDF

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CN108085973B
CN108085973B CN201810032889.XA CN201810032889A CN108085973B CN 108085973 B CN108085973 B CN 108085973B CN 201810032889 A CN201810032889 A CN 201810032889A CN 108085973 B CN108085973 B CN 108085973B
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silk
freckle
mulberry silk
water
mask
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CN108085973A (en
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成光耀
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Guangzhou Zhenmeiyan Biotechnology Co ltd
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Guangzhou Duomei Biotechnology Co Ltd
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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    • D06M11/07—Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
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    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
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    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
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Abstract

The invention belongs to the technical field of cosmetics, and particularly relates to a freckle-removing silk mask with high water-retaining property. According to the invention, the amino crown ether is used as a modifier to carry out crown etherification modification on the traditional mulberry silk, so that the water absorption and water retention of the prepared mulberry silk mask matrix are greatly improved, and the defects of poor water retention and easy conductivity in the carding process of the traditional mulberry silk are overcome; the coronary etherification modified mulberry silk mask matrix and the freckle removing essence are combined to prepare the freckle removing silk mask with the water retention property.

Description

Freckle-removing silk mask with high water retention property
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a freckle-removing silk mask with high water-retaining property.
Background
In recent years, the beauty industry is in a state of high-speed development, and the market prospect is quite wide. The facial mask is a fast-digestion product, and the position of the facial mask in the beauty industry is gradually improved. Silk, a natural protein fiber, has an amino acid structure closest to human skin.
Because the silk fiber is formed by arranging a plurality of nano fibers, the air permeability and the adsorbability are good; the silk has natural moisturizing effect due to the existence of hydrophilic side groups on sericin chains; the silk has very good refraction and reflection performance on light, and aromatic amino acid in the silk can absorb ultraviolet rays, so that the silk has the capability of reducing the damage of the ultraviolet rays to skin; silk contains many active proteins, such as oxidoreductase in silk, which can effectively remove oxygen free radicals in vivo, antimicrobial protein which can inhibit the growth of dermatophytes, and carrier proteins such as sugar and lipid which can provide various nutrients for skin. There are three types of silk masks in the current market: one is that the facial mask base cloth is made by mixing silk and other materials; secondly, fibroin components are added into facial mask essence, and the facial mask is not a silk material; the third is a mask base cloth produced by adopting a structure of a simulated silk fiber net, which is generally made of cuprammonium fibers and completely free of silk protein.
CN 103690393B discloses a whitening anti-wrinkle biological silk mask, which takes natural biological extracts of sheep placenta protein hydrolysate, hirudin, lotus root protein and milk protein as active ingredient raw materials, but does not disclose any content related to silk; CN 102357070B discloses a hydrolyzed fibroin/rhEGF composition skin-care facial mask, which takes hydrolyzed fibroin as a raw material, and the prepared facial mask has the unique effects of oxidation resistance, skin aging alleviation, face fine lines prevention and face fine lines reduction and color spots prevention and reduction; but does not give any clinical or in vitro data to demonstrate its claimed effect.
At present, the appearance of real silk masks is less in the market, and certain technical problems exist. If silk has poor water retention, the facial mask has poor capability of retaining essence after being made into base cloth, and cannot be attached to skin. Secondly, the processing technology is difficult, and most of the traditional silk mask base cloth is processed by a spunlace nonwoven process. Because silk fiber has poor conductivity, static electricity is easy to generate in the carding process, the roller winding phenomenon occurs, and normal carding is difficult.
Therefore, the development of a process capable of improving the water retention of the silk for preparing the modified silk mask has important significance.
Disclosure of Invention
The invention aims to overcome the defects that silk in a silk mask matrix in the prior art is poor in water retention and easy to conduct electricity in a carding process, provides a mulberry silk mask matrix modified by crown etherification to improve the water absorption and water retention of traditional mulberry silk, and then prepares a novel mulberry silk mask with a freckle removing effect by matching with freckle removing essence.
According to one aspect of the invention, the freckle-removing silk mask with high water-retaining property is prepared by soaking a silk substrate in freckle-removing essence; the silk matrix is prepared by the following steps:
1) swelling mulberry silk: soaking mulberry silk with sericin content less than 3wt% in lithium bromide ethanol water solution for 20-40min, taking out the swollen mulberry silk, washing with water until no bromide ion is detected in the filtrate, and drying in a vacuum drier to constant weight to obtain bulked mulberry silk; the lithium bromide ethanol water solution comprises the following components in percentage by weight: the weight of lithium bromide is 20%, the weight of ethanol is 60%, the weight of water is 20%, the mulberry silk can be fully swelled and fluffed by the lithium bromide, the next modification is facilitated, the softness of the prepared silk matrix is enhanced, and the fitting property of the face and the facial mask can be improved; ag may be used in this step+Detecting whether the bromide ions are removed completely;
2) modification of mulberry silk: placing bulked mulberry silk into an ethanol water solution containing 2-4wt% of an activating agent, and performing ultrasonic immersion activation for 6-8h at the temperature of 30-50 ℃; then adding amino crown ether to carry out amination reaction under the ultrasonic condition, filtering after reacting for 2h, washing with water and drying to obtain crown ether mulberry silk; the amino crown ether is 2-aminomethyl-15-crown-5, 4 '-aminobenzo-18-crown ether-6 or 4' -aminobenzo-15-crown ether-5;
according to the invention, the mulberry silk with a crown ether structure is prepared by utilizing the characteristic that the silk fiber contains carboxyl, activating the carboxyl, and then carrying out amination reaction on the activated carboxyl and amino crown ether, and the water absorption and water retention of the mulberry silk are greatly improved after crown ether treatment; due to the increase of the water absorption of the mulberry silk, the phenomena that electrostatic adsorption is easily caused in a later carding process and carding is not suitable are overcome.
3) Carding and lapping: carding the obtained crown etherified mulberry silk into single fiber mulberry silk by a roller type carding machine, then lapping by adopting a cross lapping mode, finally preparing silk non-woven fabric by a spunlace forming process, and stamping the silk non-woven fabric into a facial mask shape by using a mould to obtain the silk substrate.
Preferably, the activating agent in the step 2) is a mixture of N-hydroxy thiosuccinimide and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, and the molar ratio is as follows: n-hydroxy thiosuccinimide: 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride =1: 2-3; the molar amount of the amino crown ether is equal to the molar amount of the N-hydroxyl thiosuccinimide;
preferably, the amino crown ether in the step 2) is 4 '-aminobenzo-18-crown ether-6, and tests show that the crown etherified mulberry silk obtained when the amino crown ether is 4' -aminobenzo-18-crown ether-6 with more carbon atoms has the most excellent water retention and water absorption.
Preferably, the obtained crown ether mulberry silk is subjected to crosslinking treatment before carding and lapping, and the treatment process is as follows: immersing the crown etherified mulberry silk in a crosslinking solution, performing ultrasonic crosslinking for 2-3h at room temperature, filtering, washing with water, and drying to obtain the crosslinked mulberry silk, wherein the crosslinking solution contains 5wt% of glutaraldehyde, 3wt% of guar gum and the balance of water. The silk substrate prepared by the carding and lapping process after the crosslinking treatment has excellent mechanical property, the tensile deformation resistance is greatly enhanced, and the subsequent processing treatments such as carding and lapping at the later stage are facilitated.
The freckle removing essence can be selected from essences with freckle removing effects in the prior art, and preferably comprises, by weight, 0.1-0.3% of hydrolyzed jojoba protein, 3.2-4.0% of lecithin, 1.0-1.5% of a thickening agent, 4.2-5.2% of glycerol, 2.2-2.6% of sorbitol, 1.1-1.3% of licoflavone, 0.2-0.3% of sodium citrate, 1.3-1.6% of sodium hyaluronate, 0.22-0.30% of human oligopeptide-1, 0.6-0.8% of steareth-20, 2.0-2.4% of n-octyltriethoxysilane, 0.6-0.9% of oat- β -glucan, and purified water which is added to 100%;
preferably, the thickener is xanthan gum, carboxymethyl hydroxyethyl cellulose or carbomer, more preferably carboxymethyl hydroxyethyl cellulose; the appropriate thickening agent can improve the viscosity of the mask essence, avoid the phenomenon of dropping liquid easily caused by too low viscosity and avoid the loss and waste of the freckle-removing essence; in addition, when carboxymethyl hydroxyethyl cellulose is selected as a thickening agent, the prepared freckle-removing silk mask with high water retention can be well attached to the face.
The essence adopts glycerin, oat- β -glucan and sodium hyaluronate to provide instant and long-acting moisturizing effect, and oat- β -glucan is a high molecular polymer formed by connecting monomer β -D-glucopyranose through β - (1 → 3) and β - (1 → 4) glycosidic bonds, has a unique linear chain molecular structure, is endowed with good transdermal absorption performance, promotes fibroblasts to synthesize collagen, promotes wound healing, repairs damaged skin, and gives the skin a moist and smooth touch feeling like silk.
The human oligopeptide-1, also called EGF (recombinant human epidermal growth factor), in the essence has the effects of whitening skin, removing freckles, reducing the content of melanin and pigmented cells in skin cells and accelerating the metabolic shedding of the melanocytes. Licoflavone is a natural whitening agent extracted from specific variety of licorice, can inhibit the activity of tyrosinase, inhibit the activity of dopachrome interconversion and DHICA oxidase, and is a fast, efficient and green cosmetic additive for whitening and removing spots.
Compared with the prior art, the invention has the following advantages:
1) according to the invention, mulberry silk is pretreated by adopting an ethanol aqueous solution of lithium bromide, so that the prepared silk matrix is softer and has better skin adhesiveness;
2) according to the invention, the mulberry silk is modified by the amino crown ether, so that the water retention performance and the water absorption performance of the prepared silk matrix are greatly improved, and the problems that static electricity is easily generated and a roller winding phenomenon occurs in the subsequent mulberry silk carding process are solved;
3) according to the invention, after crown etherification, mulberry silk is subjected to crosslinking treatment, so that the mechanical property of the mulberry silk is greatly enhanced, the mulberry silk has excellent tensile deformation resistance, and the subsequent processing treatments such as later carding and lapping are facilitated;
4) the invention adopts the glycerol monostearate as the additive, greatly enhances the stability of the freckle-removing essence and can prolong the shelf life of the freckle-removing essence.
Drawings
FIG. 1 is a graph of water content of mulberry silk obtained under different modification conditions;
fig. 2 is a stress-strain graph of different silk matrices.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention.
The raw material mulberry silk used by the invention is from Tongxiang Zhixin home textile company Limited, the grade is A grade, and the sericin content is 0.2 wt%; the specific gravity of the silk is 1.35g/cm3。
Example 1
Preparing a silk matrix:
1) swelling mulberry silk: soaking 100g mulberry silk with sericin content less than 3wt% in 2L ethanol water solution of lithium bromide for 20-40min, taking out the swollen mulberry silk, and washing with water until no bromide ion is detected in the filtrate (using Ag)+Detecting), and then placing the mulberry silk in a vacuum drier for drying at 40 ℃ to constant weight to obtain bulked mulberry silk; the lithium bromide ethanol water solution comprises the following components in percentage by weight: 20% wt of lithium bromide, 60% wt of ethanol and 20% wt of water;
2) modification of mulberry silk: placing 100g of bulked mulberry silk in 1L of ethanol aqueous solution containing 2-4wt% of activating agent (the activating agent is a mixture of N-hydroxy thiosuccinimide and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride, and the molar ratio is calculated that the N-hydroxy thiosuccinimide is 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride =1: 2) and performing ultrasonic immersion activation for 6-8h at the temperature of 30-50 ℃; then adding amino crown ether (the adding molar amount of the amino crown ether is equal to the molar amount of the N-hydroxy thiosuccinimide in the activator) to carry out amination reaction under ultrasonic conditions, filtering after reacting for 2 hours, washing with water and drying to obtain crown etherified mulberry silk; the amino crown ether is 2-aminomethyl-15-crown-5, 4 '-aminobenzo-18-crown-6 or 4' -aminobenzo-15-crown-5;
3) carding and lapping: carding the obtained crown etherified mulberry silk into single fiber mulberry silk by a roller type carding machine, then lapping by adopting a cross lapping mode, finally preparing silk non-woven fabric by a spunlace forming process, and stamping the silk non-woven fabric into a facial mask shape by using a mould to obtain the silk substrate.
The water retention performance of the silk matrix prepared from different amino crown ethers in example 1 and the raw material mulberry silk were tested according to the following method: 1) about 10g of the sample was placed in an oven to dry to a constant weight and its weight m after constant weight was recorded to the nearest 0.01 g; 2) placing the sample with constant weight in 100ml of water, and soaking for 24h to ensure that the silk fiber achieves moisture absorption balance; 3) taking out after 24h, placing on a metal net with the aperture of 3mm, weighing until no water drops, and recording the weight m0(to the nearest 0.01 g). Then weighing every 10min, and recording as mn（m1、m2…..m9) And stopping after 90 min. Calculated Water cut (m)n-m）/mnX100%, and the water content curve is shown in FIG. 1.
As can be seen from the water content curve in fig. 1, the water absorption and water retention of the silk substrate subjected to the amino crown etherification treatment are greatly enhanced compared with those of the raw material mulberry silk, the water content of the raw material (unmodified mulberry silk) after 90min is only about 45%, and the water content of the raw material (unmodified mulberry silk) is far lower than that of the silk substrate subjected to the amino crown etherification treatment (more than 75%), wherein the water retention and water retention of the modification of 4' -aminobenzo-18-crown ether-6 are the most excellent, so that the freckle-removing essence can be firmly locked, the loss is avoided, the action time of the skin and the freckle-removing essence is prolonged, and the skin absorption is promoted.
Example 2
Preparing a silk matrix:
1) swelling mulberry silk: soaking 100g mulberry silk with sericin content less than 3wt% in 2L ethanol water solution of lithium bromide for 20-40min, taking out the swollen mulberry silk, and washing with water until no bromide ion is detected in the filtrate (using Ag)+Detecting), and then placing the mulberry silk in a vacuum drier for drying at 40 ℃ to constant weight to obtain bulked mulberry silk; the lithium bromide ethanol water solution comprises the following components in percentage by weight: 20% wt of lithium bromide, 60% wt of ethanol and 20% wt of water;
2) modification of mulberry silk: placing 100g of bulked mulberry silk in 1L of ethanol aqueous solution containing 2-4wt% of activating agent (the activating agent is a mixture of N-hydroxy thiosuccinimide and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride, and the molar ratio is calculated that the N-hydroxy thiosuccinimide is 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride =1: 2) and performing ultrasonic immersion activation for 6-8h at the temperature of 30-50 ℃; then adding amino crown ether 4' -aminobenzo-18-crown ether-6 (the molar amount of the added amino crown ether is equal to the molar amount of N-hydroxy thiosuccinimide in the activating agent) to carry out amination reaction under the ultrasonic condition, filtering after 2h of reaction, washing with water and drying to obtain crown etherified mulberry silk;
3) immersing 10g of crown etherified mulberry silk in 300mL of cross-linking solution (the cross-linking solution contains 5% wt of glutaraldehyde, 3% wt of guar gum and 92% wt of water) for cross-linking for 2-3h by ultrasonic treatment at room temperature, filtering, washing with water, and drying at 50 ℃ to obtain the cross-linked mulberry silk.
4) Carding and lapping: carding the crosslinked mulberry silk into single-fiber mulberry silk by a roller card, lapping by adopting a cross lapping mode, preparing silk non-woven fabric by a spunlace forming process, and stamping the silk non-woven fabric into a facial makeup shape by using a die to obtain the silk substrate.
The silk substrate prepared by modifying 4' -aminobenzo-18-crown ether-6 in example 1 (abbreviated as 18-6 crown etherification, curve b) and the substrate prepared in example 2 (abbreviated as 18-6 crown etherification/crosslinking modification, curve c) and the raw material mulberry silk (curve a) were tested for their stress-strain curves in the dry state using a universal material testing machine (Instron 3365, usa) as shown in fig. 2.
The result shows that the mulberry silk (curve a) adopted as the raw material has smaller tensile failure stress which is about 2.0MPa and tensile failure strain which is about 60 percent; the tensile failure stress of the silk substrate (abbreviated as 18-6 crown etherification, curve b) prepared by modifying 4' -aminobenzo-18-crown ether-6 is about 2.2MPa, and the tensile failure is increased to 100 percent; after crosslinking modification (abbreviated as 18-6 crown etherification/crosslinking modification, curve c), the tensile failure stress is about 2.4MPa, the tensile failure is increased to 140 percent, and the mechanical property is obviously greatly enhanced compared with that before crosslinking modification, especially the tensile failure force.
Example 3
Preparing the freckle-removing essence:
weighing 0.2kg of hydrolyzed jojoba protein, 3.6kg of lecithin, 1.2kg of thickening agent, 4.3kg of glycerin, 2.4kg of sorbitol, 1.2kg of licoflavone, 0.2kg of sodium citrate, 1.4kg of sodium hyaluronate, 0.25kg of human oligopeptide-1, 0.7kg of steareth-20, 2.2kg of n-octyltriethoxysilane, 0.8kg of oat- β -glucan and purified water, supplementing to 100kg to obtain a mixed solution, placing the mixed solution into a homogenizer, homogenizing at 60-70 ℃ for 6-8h, then cooling to room temperature to obtain a white spot-removing essence solution with the pH of 7.3-7.5, filling the spot-removing essence solution into an aluminum foil bag, and then adding the silk substrate prepared in example 1 to obtain the final mulberry silk spot-removing facial mask.
Comparative example 3
The mask is prepared by adopting commercially available magical natural (Japanese 384 silk mask paper) as a mask substrate and adopting the white-like freckle removing essence in the example 3, namely the mask substrate is changed.
Clinical verification is carried out by adopting the freckle removing facial mask of the comparative example 3 and the freckle removing facial mask of the example 3 (20-30 years old female volunteers, all mild chloasma), the facial mask is randomly divided into two groups of A group and B group of 20 persons, the A group adopts the mulberry silk freckle removing facial mask product prepared in the example 3, the B group adopts the facial mask product prepared in the comparative example 3, the freckle removing effect is statistically classified every day by a visual method (a represents that the speckles basically disappear, B represents that the speckles are obviously faded, c represents that the speckles are slightly faded, d represents that the speckles basically do not change), and the results are shown in a table:
TABLE 1 speckle-removing effect statistics table
10 days 15 days 20 days 30 days 40 days
Group A a(0),b(3),c(7),d (10) a(1),b(5),c(11), d(3) a(4),b(8),c (6),d(2) a(7),b(6),c (6),d(1) a(14),b(4),c (1),d(1)
Group B a(0),b(1),c(4), d(15) a(0),b(3),c(7), d(12) a(1),b(5),c (6),d(8) a(3),b(7),c (4),d(6) a(10),b(3),c (4),d(3)
Note: a (10) represents 10 persons in class a.
The two groups of test results of A and B show that the freckle-removing essence lotion plays a certain freckle removing effect, and the comparison result of A and B shows that the mask substrate prepared by the invention can better enable the freckle-removing essence lotion to interact with skin, and fade and remove freckles.
Example 4
Although the mulberry silk freckle-removing mask prepared in the embodiment 3 of the invention has a good freckle removing effect, the mulberry silk freckle-removing mask is poor in stability even if the mulberry silk freckle-removing mask is placed in an aluminum foil bag for sealing, and the mulberry silk freckle-removing mask begins to turn yellow, has reduced viscosity and is partially oil-water layered after being placed at room temperature for 12 months.
In order to enhance the stability of the essence, the invention researches the stability of the essence, and respectively adds 0.1 wt% (based on the weight of the essence) of different types of stabilizers into the white freckle-removing essence prepared in example 3, homogenizes the mixture at a high speed for 30min, and then stands the mixture to examine the stability of the mixture so as to find out a proper stabilizer. The stabilizers examined are respectively antioxidant vitamin C, polyethylene glycol 4000, glycerol monostearate, magnesium aluminum silicate, Tween 80 and polyethylene glycol oleate.
In order to further verify the stabilizing effect of the glycerol monostearate, the essence prepared by using the glycerol monostearate as an additive (specifically comprising 0.2g of hydrolyzed jojoba protein, 3.6g of lecithin, 1.2g of a thickening agent, 4.3g of glycerol, 2.4g of sorbitol, 1.2g of licoflavone, 0.2g of sodium citrate, 1.4g of sodium hyaluronate, 0.25g of human oligopeptide-1, 0.7g of steareth-20, 2.2g of n-octyltriethoxysilane, 0.8g of oat- β -glucan, purified water is supplemented to 100g, and then 0.1g of glycerol monostearate is added to be respectively placed at 0 ℃ and 45 ℃ for 30 days, so that separation and color change are not obvious, and the existence of the oil-water stabilizing effect of the essence can be obviously improved under the test.
Although the embodiments of the present invention have been described in detail, it should be understood that various changes, substitutions, and alterations can be made hereto without departing from the spirit and scope of the invention.

Claims (5)

1. A freckle-removing silk mask with high water-retaining property is characterized in that a silk substrate is soaked in freckle-removing essence; the method is characterized in that: the silk matrix is prepared by the following preparation method:
1) swelling mulberry silk: soaking mulberry silk with sericin content less than 3wt% in lithium bromide ethanol water solution for 20-40min, taking out the swollen mulberry silk, washing with water until no bromide ion is detected in the filtrate, and drying in a vacuum drier to constant weight to obtain bulked mulberry silk; the lithium bromide ethanol water solution comprises the following components in percentage by weight: 20 wt% of lithium bromide, 60 wt% of ethanol and 20 wt% of water;
2) modification of mulberry silk: placing bulked mulberry silk into an ethanol water solution containing 2-4wt% of an activating agent, and performing ultrasonic immersion activation for 6-8h at the temperature of 30-50 ℃; then adding amino crown ether to carry out amination reaction under the ultrasonic condition, filtering after reacting for 2h, washing with water and drying to obtain crown ether mulberry silk; the amino crown ether is 4' -aminobenzo-18-crown ether-6; the activating agent is a mixture of N-hydroxy thiosuccinimide and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride, and the molar ratio is calculated as follows: n-hydroxy thiosuccinimide: 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride =1: 2-3; the molar amount of the amino crown ether is equal to the molar amount of the N-hydroxyl thiosuccinimide;
3) carding and lapping: carding the obtained crown etherified mulberry silk into single-fiber mulberry silk by a roller type carding machine, then lapping by adopting a cross lapping mode, finally preparing silk non-woven fabric by a spunlace forming process, and stamping the silk non-woven fabric into a facial mask shape by using a mould to obtain a silk substrate;
wherein: the obtained crown etherified mulberry silk is subjected to crosslinking treatment before carding and lapping, and the treatment process is as follows: immersing the crown etherified mulberry silk in a crosslinking solution, performing ultrasonic crosslinking for 2-3h at room temperature, filtering, washing with water, and drying to obtain the crosslinked mulberry silk, wherein the crosslinking solution contains 5wt% of glutaraldehyde, 3wt% of guar gum, and the balance of water.
2. The freckle-removing silk mask with high water retention property according to claim 1, is characterized in that: the freckle-removing essence consists of the following components in percentage by weight:
0.1-0.3% of hydrolyzed jojoba protein, 3.2-4.0% of lecithin, 1.0-1.5% of thickening agent, 4.2-5.2% of glycerin, 2.2-2.6% of sorbitol, 1.1-1.3% of licoflavone, 0.2-0.3% of sodium citrate, 1.3-1.6% of sodium hyaluronate, 0.22-0.30% of human oligopeptide-1, 0.6-0.8% of steareth-20, 2.0-2.4% of n-octyltriethoxysilane, 0.6-0.9% of oat- β -dextran, and purified water to make up to 100%.
3. The freckle-removing silk mask with high water retention property according to claim 2, is characterized in that: the thickener is xanthan gum, carboxymethyl hydroxyethyl cellulose or carbomer.
4. The freckle-removing silk mask with high water retention property according to claim 3, wherein: the thickening agent is carboxymethyl hydroxyethyl cellulose.
5. The freckle-removing silk mask with high water retention property according to claim 4, wherein: the freckle removing essence is added with a stabilizer, and the stabilizer is glycerol monostearate.
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CN111374933B (en) * 2020-04-06 2022-03-25 广州玥颜化妆品有限公司 Silk mask
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JPH0571072A (en) * 1991-04-10 1993-03-23 Kyoto Pref Gov Method for modifying and processing silk yarn product
US20140315828A1 (en) * 2013-04-22 2014-10-23 Allergan, Inc. Cross-linked silk-hyaluronic acid compositions
CN104593945B (en) * 2013-10-30 2017-08-25 唐懿 A kind of high water absorption silk non-woven fabric production technology
CN104306314A (en) * 2014-09-27 2015-01-28 青岛美嘉隆包装机械有限公司 Moisture-preserving oil-removing face mask
CN104631118B (en) * 2015-01-22 2016-08-24 浙江理工大学 A kind of absorbable antibacterial alginate fibre
CN104922024A (en) * 2015-06-20 2015-09-23 青岛拓联信息技术有限公司 Essence with skin-caring and whitening effects
CN105111447A (en) * 2015-09-24 2015-12-02 天津市利顺达粘合剂有限公司 Novel water-soluble amino silicone oil and preparation method thereof
CN105297440B (en) * 2015-11-11 2018-01-12 浙江理工大学 A kind of method to silk graft modification
CN106176282B (en) * 2016-08-19 2019-06-11 山西锦波生物医药股份有限公司 Protein powder film liquid and production method
CN107227622A (en) * 2017-06-15 2017-10-03 兴化市大地蓝绢纺有限公司 The preparation method of the super soft finishing agent of organic block silk

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