CN108085973A - A kind of nti-freckle silk mask of high-moisture-retention - Google Patents

A kind of nti-freckle silk mask of high-moisture-retention Download PDF

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CN108085973A
CN108085973A CN201810032889.XA CN201810032889A CN108085973A CN 108085973 A CN108085973 A CN 108085973A CN 201810032889 A CN201810032889 A CN 201810032889A CN 108085973 A CN108085973 A CN 108085973A
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silk
freckle
nti
mulberry silk
moisture
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CN108085973B (en
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成光耀
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Guangzhou Zhenmeiyan Biotechnology Co ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • 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
    • D06M13/144—Alcohols; Metal alcoholates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212—Face masks
    • 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
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • 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
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08—Organic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—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
    • 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
    • D06M11/11—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 with halogen acids or salts thereof
    • D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic System
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • 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
    • D06M13/322—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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • 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
    • D06M13/322—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
    • D06M13/335—Amines having an amino group bound to a carbon atom of a six-membered aromatic ring
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • 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
    • D06M13/322—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
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/418—Cyclic amides, e.g. lactams; Amides of oxalic acid
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/10—Animal fibres

Abstract

The invention belongs to cosmetic technical fields, and in particular to a kind of nti-freckle silk mask of high-moisture-retention.The present invention to traditional mulberry silk be preced with etherification modified, the shortcomings that its water imbibition of mulberry silk mask matrix and water-retaining property prepared greatly improve, overcome easy conductive in traditional mulberry silk poor water retention property, carding process using amino crown ether as modifying agent；Etherification modified mulberry silk mask matrix will be preced with, the nti-freckle silk mask prepared with water retention property is combined with nti-freckle Essence.

Description

A kind of nti-freckle silk mask of high-moisture-retention
Technical field
The invention belongs to cosmetic technical fields, and in particular to a kind of nti-freckle silk mask of high-moisture-retention.
Background technology
In recent years, beauty industry is constantly in the state of high speed development, and market prospects are quite wide.Facial mask is as a kind of fast Disappear product, is stepped up in the status of beauty industry.Silk has with human skin the most as a kind of natural protein fibre Close amino acid structure.
Since silk fiber is arranged by many nanofibers, gas permeability and adsorptivity are fine；Due to sericin The presence of hydrophilic side group causes silk to have natural moisture-keeping efficacy on chain；Silk is very good to the refraction of light and reflecting properties, And aromatic amino acid can absorb ultraviolet light in silk so that silk has ability of the reduction ultraviolet light to skin injury； Protein containing many activity in silk, for example can effectively to remove in vivo oxygen free for oxidoreducing enzyme in silk Base, antibacterial protein can inhibit the growth of dermatophyte, and the carrier proteins such as sugar, fat can provide a variety of nutriments for skin. There are three types of " silk masks " currently on the market：One kind is that mask substrate is mixed using silk and other materials；Second It is the addition fibroin ingredient in facial mask essence, facial mask is not silk material in itself；The third is using imitated silk fibroin The mask substrate of the structure production of dimension net, generally copper ammonia fiber, entirely without fibroin.
103690393 B of CN disclose a kind of skin-whitening anti-wrinkle biological silk mask, with natural biological extract Goat Placenta water It is active ingredient raw materials to solve albumen object, hirudin, lotus root albumen, milk protein object, but not publicly any content in relation to silk； 102357070 B of CN disclose a kind of hydrolysis fibroin/rhEGF composition skin-care facial masks, to hydrolyze fibroin as original Material, the facial mask prepared have oxidation resistance, and energy slowing down skin aging has prevention and subtracts light facial lines, the uniqueness of color spot Effect；But any clinical or in vitro study data are not provided to prove that it has the effect declared.
The appearance of rarer real silk mask currently on the market, also has certain technical barrier.As silk is protected in itself It is aqueous bad, be made facial mask after base fabric retain Essence ability it is poor, can not be with skin attachement.Secondly, processing technology is Difficult point, traditional silk mask base fabric are processed mostly using spun lacing without spinning process.Since silk fiber electric conductivity is bad, combing It is easy to produce static electricity during reason, collaring occurs, it is difficult to normally comb.
So a kind of technique that can improve silk water-retaining property of exploitation is used for preparing modified silk facial mask with important meaning Justice.
The content of the invention
The purpose of the present invention is overcome in silk mask matrix in the prior art in silk poor water retention property itself, carding process The shortcomings that easy conductive, provide a kind of amino be preced with etherification modified mulberry silk mask matrix improve the water imbibition of traditional mulberry silk and Then water-retaining property prepares out the new mulberry silk facial mask with effect of dispelling spots with nti-freckle Essence.
According to an aspect of the present invention, the present invention provides a kind of nti-freckle silk mask of high-moisture-retention, the high guarantors Aqueous nti-freckle silk mask is by silk matrix impregnation in nti-freckle Essence；The silk matrix is included by following preparation methods Following steps：
1）Mulberry silk is swollen：Mulberry silk of the sericin content less than 3%wt is taken to be placed in the ethanol water of lithium bromide to impregnate 20-40min then takes out the mulberry silk after swelling and be washed to filtrate without bromide ion detection, is then placed into being dried in vacuo It is dried in device to constant weight and obtains bulk shape mulberry silk；In the ethanol water of the lithium bromide count by weight percentage：Lithium bromide For 20%wt, ethyl alcohol 60%wt, water 20%wt, lithium bromide can fully make mulberry silk swelling fluffy, beneficial to the modification of next step, and And enhance the silk matrix flexibility prepared, the stickiness of face and facial mask can be improved；Ag may be employed in this step+Into Whether row detection bromide ion removes totally；
2）The modification of mulberry silk：Bulk shape mulberry silk is placed in the ethanol water of the activator containing 2-4%wt at 30-50 DEG C Lower ultrasonic immersing activates 6-8h；Then add in amino crown ether and ammoxidation is carried out under ultrasound condition, filtered after reacting 2h, water Crown ether mulberry silk is dried to obtain after washing；The amino crown ether is 2- aminomethyl-1,2 5- crown-s 5,4'- amino Benzo-18-crown-6-6 Or 4'- amino benzo -15- crown ethers -5；
The characteristics of present invention is using carboxyl is contained on silk fiber, its carboxyl is first activated, then again with amino crown ether into Row ammoxidation prepares the mulberry silk with crown ether structures, and mulberry silk substantially increases mulberry silk after being preced with etherification process Water imbibition and water-retaining property；Due to the increase of mulberry silk water imbibition, overcome and easily trigger Electrostatic Absorption in later stage carding step, The phenomenon that should not being combed.
3）Comb lapping：Gained crown ether mulberry silk is carried out being combed into single fiber mulberry silk using roller and clearer card, Then lapping is carried out by the way of cross lapping, silk non-woven fabric is prepared finally by spun lacing moulding process, by silk without Woven fabric mould punching is into types of facial makeup in Beijing operas shape up to silk matrix.
Preferably, step 2）The activator is N- hydroxy thiosuccinimides and 1- (3- dimethylamino-propyls) -3- The mixture of ethyl-carbodiimide hydrochloride, for calculation in the molar ratio：N- hydroxy thiosuccinimides：1- (3- dimethylaminos third Base) -3- ethyl-carbodiimide hydrochloride=1:2-3；The mole dosage of the amino crown ether is rubbed with N- hydroxy thiosuccinimides Your amount is equal；
Preferably, step 2）The amino crown ether is 4'- amino Benzo-18-crown-6-6, experiments have shown that when amino crown ether uses carbon Its water-retaining property of crown ether mulberry silk and water imbibition obtained during more 4'- amino Benzo-18-crown-6-6 of atomicity is the most excellent It is different.
Preferably, gained crown ether mulberry silk is handled before combing lapping is carried out by Cross-linked, and processing procedure is as follows：It will Crown ether mulberry silk is impregnated in room temperature ultrasound in crosslinked fluid and is filtered after carrying out Cross-linked 2-3h, and Cross-linked silkworm is dried to obtain in washing Silk, glutaraldehyde of the crosslinked fluid containing 5%wt, the guar gum of 3%wt, surplus is water.It is combed again after Cross-linked is handled Lapping process can make the silk matrix prepared have excellent mechanical performance, and the ability of stretch-proof deformation greatly enhances, side The phase combs the processing of the following process such as lapping after an action of the bowels.
Heretofore described nti-freckle Essence can be selected from the Essence in the prior art with freckle effect；It is preferred that , the nti-freckle Essence count by weight percentage, consists of the following compositions：The hydrolysis Jojoba albumen of 0.1-0.3%, The lecithin of 3.2-4.0%, the thickener of 1.0-1.5%, the glycerine of 4.2-5.2%, the sorbierite of 2.2-2.6%, 1.1-1.3%'s Licoflavone, the sodium citrate of 0.2-0.3%, the Sodium Hyaluronate of 1.3-1.6%, people's oligopeptides -1,0.6- of 0.22-0.30% The n-octytriethoxysilane of 0.8% stereth -20,2.0-2.4%, oat-beta glucan of 0.6-0.9%, purifying Water complements to 100%；
Preferably, the thickener xanthan gum, carboxymethyl hydroxyethyl cellulose or carbomer, more preferably carboxy methyl hydroxyethyl are fine Dimension element；Suitable thickener can improve the viscosity of facial mask essence, avoid viscosity is too low from being susceptible to dropping liquid phenomenon, avoid nti-freckle Essence is lost in waste；In addition when selecting carboxymethyl hydroxyethyl cellulose as thickener, the high-moisture-retention prepared is made Good be bonded can be realized between nti-freckle silk mask and face.
Instant and long-acting moistening effect can be provided using glycerine, oat-beta glucan and Sodium Hyaluronate in Essence, Since oat-beta glucan is by monomer β-D- glucopyranoses, got up shape by β-(1 → 3) and β-(1 → 4) glucosides key connection Into a kind of high molecular polymer, there is unique straight-chain molecular structure, impart good Transdermal absorption performance；Promote into fibre Smooth muscle cells collagen synthesis albumen is tieed up, promotes wound healing, repairs impaired skin, skin is given and smooth sense of touch is moistened such as silk.
People's oligopeptides -1 also known as EGF (recombinant human epidermal growth factor) in Essence have whitening spot-removing, reduce Skin Cell The content of middle melanin and coloured corpuscle accelerates melanocyte metabolism and comes off.Licoflavone is extracted from certain species Radix Glycyrrhizae Natural whitening agent, it can inhibit the activity of tyrosinase, and can inhibit the activity of dopachrome change and DHICA oxidizing ferment, It is a kind of quick, efficiently, green whitening cosmetics additive.
Compared with prior art, the invention has the advantages that：
1）The present invention carries out pre-treatment using the ethanol water of lithium bromide to mulberry silk to it, makes the silk matrix prepared more Add softness, it is more preferable to the stickiness of skin；
2）The present invention is modified mulberry silk using amino crown ether, makes the silk matrix water retention property and water absorbing properties prepared It greatly improves, while solves easy to produce static electricity in follow-up mulberry silk carding process, generation collaring；
3）The present invention carries out Cross-linked processing after etherification process is preced with, to mulberry silk, greatly strengthens its mechanical performance, is provided with The ability of excellent stretch-proof deformation, facilitates the later stage to comb the processing of the following process such as lapping；
4）The present invention as additive, greatly strengthens the stability of nti-freckle Essence, Ke Yiyan using glyceryl monostearate Its long shelf life.
Description of the drawings
Fig. 1 is the plot of water cut that different modified conditions obtain mulberry silk；
Fig. 2 is the stress-strain curve of different silk matrix.
Specific embodiment
Understand to make the object, technical solutions and advantages of the present invention clearer, With reference to embodiment, to this Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
The raw materials used in the present invention mulberry silk comes from Tongxiang Zhi Xin home textiles Co., Ltd, and grade is A grades, sericin content For 0.2%wt；Silk proportion is 1.35g/cm3。
Embodiment 1
Prepare silk matrix：
1）Mulberry silk is swollen：Mulberry silk of the 100g sericins content less than 3%wt is taken to be placed in the ethanol water of 2L lithium bromides 20-40min is impregnated, the mulberry silk after swelling is then taken out and be washed to filtrate without bromide ion detection（Using Ag+It is examined It surveys）, it is then placed into vacuum desiccator drying to constant weight at 40 DEG C and obtains bulk shape mulberry silk；In the ethanol water of lithium bromide Count by weight percentage：Lithium bromide is 20%wt, ethyl alcohol 60%wt, water 20%wt；
2）The modification of mulberry silk：The bulk shape mulberry silks of 100g are placed in the ethanol water of activators of the 1L containing 2-4%wt（It is living Agent is the mixture of N- hydroxy thiosuccinimides and 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, For calculation in the molar ratio：N- hydroxy thiosuccinimides：1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochloride=1: 2）Ultrasonic immersing activates 6-8h at 30-50 DEG C；Then amino crown ether is added in（The addition mole dosage and activator of amino crown ether Middle N- hydroxy thiosuccinimides mole is equal）Ammoxidation is carried out under ultrasound condition, is filtered after reacting 2h, is washed After dry to obtain crown ether mulberry silk；Amino crown ether is 2- aminomethyl-1,2 5- crown-s 5,4'- amino Benzo-18-crown-6-6 or 4'- Amino benzo -15- crown ethers -5；
3）Comb lapping：Gained crown ether mulberry silk is carried out being combed into single fiber mulberry silk using roller and clearer card, then Lapping is carried out by the way of cross lapping, silk non-woven fabric is prepared finally by spun lacing moulding process, by silk non-woven fabric With mould punching into types of facial makeup in Beijing operas shape up to silk matrix.
Water conservation is carried out by the following method to the silk matrix and raw material mulberry silk that in embodiment 1 prepared by different amino crown ethers Property performance test：1) sample about 10g is placed in baking oven and dried to constant weight, record the weight m after its constant weight（It is accurate to 0.01g）；2) sample after constant weight is placed in 100ml water, impregnates for 24 hours, silk fiber is made to reach moisture equilibrium at dry side；3）It takes out afterwards for 24 hours It is placed on the metal mesh that aperture is 3mm, until weighing under no water droplet, and records its weight m0（It is accurate to 0.01g）.Then it is every It weighs once every 10min, is recorded as m respectivelyn（m1、m2…..m9）, stop after 90min.Calculate moisture content（mn-m）/mnX100%, And it is as shown in Figure 1 to draw plot of water cut.
Plot of water cut can be seen that by amino crown etherization treated silk matrix than raw material mulberry silk from Fig. 1 Its water imbibition and water-retaining property greatly enhance, raw material（Unmodified mulberry silk）Moisture content after its 90min is only 45% or so, far Far below amino crown etherization treated silk matrix（It is more than 75%）, wherein 4'- amino Benzo-18-crown-6-6 be modified Water-retaining property and the property of water-bearing are the most excellent, it is possible to firmly lock nti-freckle Essence, avoid being lost in, increase skin and nti-freckle essence The action time of magnificent liquid, so as to which skin be promoted to absorb.
Embodiment 2
Prepare silk matrix：
1）Mulberry silk is swollen：Mulberry silk of the 100g sericins content less than 3%wt is taken to be placed in the ethanol water of 2L lithium bromides 20-40min is impregnated, the mulberry silk after swelling is then taken out and be washed to filtrate without bromide ion detection（Using Ag+It is examined It surveys）, it is then placed into vacuum desiccator drying to constant weight at 40 DEG C and obtains bulk shape mulberry silk；In the ethanol water of lithium bromide Count by weight percentage：Lithium bromide is 20%wt, ethyl alcohol 60%wt, water 20%wt；
2）The modification of mulberry silk：The bulk shape mulberry silks of 100g are placed in the ethanol water of activators of the 1L containing 2-4%wt（It is living Agent is the mixture of N- hydroxy thiosuccinimides and 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, For calculation in the molar ratio：N- hydroxy thiosuccinimides：1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochloride=1: 2）Ultrasonic immersing activates 6-8h at 30-50 DEG C；Then amino crown ether 4'- amino Benzo-18-crown-6-6 is added in（Amino crown ether Addition mole dosage it is equal with N- hydroxy thiosuccinimides mole in activator）Amination is carried out under ultrasound condition Reaction filters after reacting 2h, crown ether mulberry silk is dried to obtain after washing；
3）Crown ether mulberry silk 10g is impregnated in 300mL crosslinked fluids（Glutaraldehyde of the crosslinked fluid containing 5%wt, the guar gum of 3%wt, The water of 92%wt）Middle room temperature ultrasound filters after carrying out Cross-linked 2-3h, dries to obtain Cross-linked mulberry silk after washing at 50 DEG C, described.
4）Comb lapping：Cross-linked mulberry silk is carried out being combed into single fiber mulberry silk using roller and clearer card, then Lapping is carried out by the way of cross lapping, silk non-woven fabric is prepared finally by spun lacing moulding process, by silk non-woven fabric With mould punching into types of facial makeup in Beijing operas shape up to silk matrix.
4'- amino Benzo-18-crown-6-6 in embodiment 1 is modified and prepares gained silk matrix（It is abbreviated as 18-6 crown ethers Change, curve b）Gained matrix is prepared with embodiment 2（It is abbreviated as 18-6 crown ethers/Cross-linked to be modified, curve c）With raw material mulberry silk （Curve a）The load-deformation curve under its drying regime is tested using universal testing machine (Instron3365, the U.S.), As shown in Figure 2.
The result shows that using raw material mulberry silk（Curve a）Tensile failure stress is smaller, about 2.0MPa, and tensile failure should Become about 60%；4'- amino Benzo-18-crown-6-6, which is modified, prepares gained silk matrix（It is abbreviated as 18-6 crown ethers, curve b）It draws It is about 2.2MPa to stretch bursting stress, and tensile failure should increase to 100%；Crosslinkedization is modified（It is abbreviated as 18-6 crown ethers/friendship Connectionization is modified, curve c）Tensile failure stress is about 2.4MPa, and tensile failure should increase to 140%, hence it is evident that more cross-linking modified preceding power The property learned greatly enhances, especially tensile failure power.
Embodiment 3
Prepare nti-freckle Essence：
Weigh 0.2kg hydrolysis Jojoba albumen, the lecithin of 3.6kg, the thickener of 1.2kg, the glycerine of 4.3kg, the mountain of 2.4kg Pears alcohol, 1.2kg licoflavones, the sodium citrate of 0.2kg, the Sodium Hyaluronate of 1.4kg, people's oligopeptides -1,0.7kg of 0.25kg The n-octytriethoxysilane of stereth -20,2.2kg, oat-beta glucan of 0.8kg, purified water complement to 100kg obtains mixed liquor；Mixed liquor is placed into homogenizer the progress homogeneous 6-8h at 60-70 DEG C, room temperature is then cooled to and obtains Off-white color nti-freckle Essence, pH 7.3-7.5；Nti-freckle Essence is filling in aluminium foil bag, then add in prepared by embodiment 1 Silk matrix obtains final mulberry silk freckle-removing mask.
Comparative example 3
It is natural using commercially available evil spirit（Japanese 384 silk mask paper）For mask matrix, using the off-white color nti-freckle elite in embodiment 3 Liquid self-made face pack, that is, change mask matrix.
Clinical verification is carried out using the freckle-removing mask of comparative example 3 and embodiment 3（20-30 Sui female volunteers are slight Chloasma）, each 20 people of two groups of A groups, B groups is randomly divided into, A groups use mulberry silk freckle-removing mask product prepared by embodiment 3, B groups The mask product prepared using comparative example 3, ocular estimate carry out statistical classification to freckle effect daily（A represents spot substantially completely It disappears, b, which represents spot, substantially to desalinate, and c, which represents spot, slightly to desalinate, and d represents spot substantially without significant change）, as a result such as 1 institute of table Show：
1 freckle effect statistical form of table
10 days 15 days 20 days 30 days 40 days
A groups 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)
B groups 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）Representing a grades has 10 people.
A shows that nti-freckle elite breast of the present invention plays certain freckle effect, A and B comparing results with two groups of result of the tests of B Showing to play using mask matrix prepared by the present invention preferably makes nti-freckle elite breast interact with skin, desalinates and goes Except color spot, this is because the shortcomings that mask matrix prepared by the present invention overcomes traditional mulberry silk facial mask poor water retention property, improves Its water-retaining property can carry more nti-freckle Essences and skin contact, and the uptake of Essence is played so as to increase skin The effect of quick-acting nti-freckles.
Embodiment 4
Although mulberry silk freckle-removing mask prepared by the embodiment of the present invention 3 is provided with good freckle effect, although being placed in aluminium foil bag In be sealed but its stability is poor, its color that is placed at room temperature for 12 months starts to turn yellow, viscosity declines, part oil water stratification shows As.
In order to enhance its stability, the present invention again studies its stability, white in the class of the preparation of embodiment 3 respectively 0.1%wt is added in color nti-freckle Essence（Using Essence weight as calculating basis）Different type stabilizer carry out high speed homogenization It is placed again after 30min, investigates its stability, to which suitable stabilizer can be found out.The stabilizer of investigation is respectively anti- Oxidant vitamin C, Macrogol 4000, glyceryl monostearate, aluminium-magnesium silicate, Tween 80, Polyethylene Glycol Oleate.
Result of the test shows that only glyceryl monostearate can play the role of apparent stabilizer, after being placed at room temperature for 12 months Without apparent color change and without apparent lamination, remaining stabilizer fails to increase its effect phase；It is sweet in order to further verify The effect that oily monostearate is stablized, the Essence prepared as additive（Concrete component is：0.2g hydrolyzes Jojoba Albumen, the lecithin of 3.6g, the thickener of 1.2g, the glycerine of 4.3g, the sorbierite of 2.4g, 1.2g licoflavones, the lemon of 0.2g Lemon acid sodium, the Sodium Hyaluronate of 1.4g, three second of n-octyl of stereth -20,2.2g of people's oligopeptides -1,0.7g of 0.25g Oxysilane, oat-beta glucan of 0.8g, purified water complement to 100g and obtain mixed liquor, then add the glycerine list of 0.1g again Stearate）It is placed 30 days respectively at 0 DEG C and 45 DEG C, has no apparent water-oil separating and color change, illustrate it in accelerated test Under can also be stabilized, hence it is evident that improve the stability of Essence, its shelf life can be extended.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's In the case of spirit and scope, can embodiments of the present invention be made with various changes, replacement and change.

Claims (8)

1. a kind of nti-freckle silk mask of high-moisture-retention, the nti-freckle silk mask of the high-moisture-retention is being dispelled by silk matrix impregnation In spot Essence；It is characterized in that：The silk matrix is prepared by following preparation methods：
1）Mulberry silk is swollen：Mulberry silk of the sericin content less than 3%wt is taken to be placed in the ethanol water of lithium bromide to impregnate 20-40min then takes out the mulberry silk after swelling and be washed to filtrate without bromide ion detection, is then placed into being dried in vacuo It is dried in device to constant weight and obtains bulk shape mulberry silk；In the ethanol water of the lithium bromide count by weight percentage：Lithium bromide For 20%wt, ethyl alcohol 60%wt, water 20%wt；
2）The modification of mulberry silk：Bulk shape mulberry silk is placed in the ethanol water of the activator containing 2-4%wt at 30-50 DEG C Lower ultrasonic immersing activates 6-8h；Then add in amino crown ether and ammoxidation is carried out under ultrasound condition, filtered after reacting 2h, water Crown ether mulberry silk is dried to obtain after washing；The amino crown ether is 2- aminomethyl-1,2 5- crown-s 5,4'- amino Benzo-18-crown-6-6 Or 4'- amino benzo -15- crown ethers -5；
3）Comb lapping：Gained crown ether mulberry silk is carried out being combed into single fiber mulberry silk using roller and clearer card, then Lapping is carried out by the way of cross lapping, silk non-woven fabric is prepared finally by spun lacing moulding process, by silk non-woven fabric With mould punching into types of facial makeup in Beijing operas shape up to silk matrix.
2. the nti-freckle silk mask of high-moisture-retention according to claim 1, it is characterised in that：Step 2）The activator is The mixture of N- hydroxy thiosuccinimides and 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, by mole Than calculating：N- hydroxy thiosuccinimides：1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochloride=1:2-3；Institute The mole dosage for stating amino crown ether is equal with N- hydroxy thiosuccinimide moles.
3. the nti-freckle silk mask of high-moisture-retention according to claim 1, it is characterised in that：The amino crown ether is 4'- Amino Benzo-18-crown-6-6.
4. the nti-freckle silk mask of high-moisture-retention according to claim 1, it is characterised in that：Gained crown ether mulberry silk exists It is handled before carrying out combing lapping by Cross-linked, processing procedure is as follows：Crown ether mulberry silk is impregnated in room temperature in crosslinked fluid to surpass Sound filters after carrying out Cross-linked 2-3h, washes and dries to obtain Cross-linked mulberry silk, glutaraldehyde of the crosslinked fluid containing 5%wt, 3%wt's Guar gum, surplus are water.
5. the nti-freckle silk mask of high-moisture-retention according to claim 1, it is characterised in that：The nti-freckle Essence is by weight Percentage calculation is measured, is consisted of the following compositions：
The hydrolysis Jojoba albumen of 0.1-0.3%, the lecithin of 3.2-4.0%, the thickener of 1.0-1.5%, 4.2-5.2%'s is sweet Oil, the sorbierite of 2.2-2.6%, the licoflavone of 1.1-1.3%, the sodium citrate of 0.2-0.3%, the hyaluronic acid of 1.3-1.6% Sodium, the n-octytriethoxysilane of stereth -20,2.0-2.4% of people's oligopeptides -1,0.6-0.8% of 0.22-0.30%, Oat-beta glucan of 0.6-0.9%, purified water complement to 100%.
6. the nti-freckle silk mask of high-moisture-retention according to claim 5, it is characterised in that：The thickener is given birth to for the Chinese Glue, carboxymethyl hydroxyethyl cellulose or carbomer.
7. the nti-freckle silk mask of high-moisture-retention according to claim 6, it is characterised in that：The thickener is carboxymethyl Hydroxyethyl cellulose.
8. the nti-freckle silk mask of high-moisture-retention according to claim 5, it is characterised in that：Add in the nti-freckle Essence Add stabilizer, the stabilizer is glyceryl monostearate.
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CN109008499A (en) * 2018-08-28 2018-12-18 江苏鑫缘丝绸科技有限公司 A kind of expansion silk floss sheet and preparation method thereof
CN109730497A (en) * 2018-11-29 2019-05-10 江苏鑫缘丝绸科技有限公司 Expansion silk wadding quilt based on mulberry silk and preparation method thereof
CN111374933A (en) * 2020-04-06 2020-07-07 陕西斯戴木生物科技有限公司 Improved silk mask with high water retention and high freckle removing activity
CN112043620A (en) * 2020-08-28 2020-12-08 张永梅 Silk mask
CN112251918A (en) * 2020-10-12 2021-01-22 惠州市好好爱日化用品有限公司 Silk mask base cloth, preparation method thereof and silk mask

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CN109008499A (en) * 2018-08-28 2018-12-18 江苏鑫缘丝绸科技有限公司 A kind of expansion silk floss sheet and preparation method thereof
CN109730497A (en) * 2018-11-29 2019-05-10 江苏鑫缘丝绸科技有限公司 Expansion silk wadding quilt based on mulberry silk and preparation method thereof
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CN112043620A (en) * 2020-08-28 2020-12-08 张永梅 Silk mask
CN112251918A (en) * 2020-10-12 2021-01-22 惠州市好好爱日化用品有限公司 Silk mask base cloth, preparation method thereof and silk mask

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