CN110438665A - A kind of preparation method of self-supporting solid-state multicomponent facial mask - Google Patents
A kind of preparation method of self-supporting solid-state multicomponent facial mask Download PDFInfo
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- CN110438665A CN110438665A CN201910724838.8A CN201910724838A CN110438665A CN 110438665 A CN110438665 A CN 110438665A CN 201910724838 A CN201910724838 A CN 201910724838A CN 110438665 A CN110438665 A CN 110438665A
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/31—Hydrocarbons
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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
- A61K8/30—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
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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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
- A61K8/30—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
- A61K8/34—Alcohols
- A61K8/347—Phenols
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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
- A61K8/30—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
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
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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
- A61K8/30—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
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
- A61K8/602—Glycosides, e.g. rutin
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/673—Vitamin B group
- A61K8/675—Vitamin B3 or vitamin B3 active, e.g. nicotinamide, nicotinic acid, nicotinyl aldehyde
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
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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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/678—Tocopherol, i.e. vitamin E
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- 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
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/413—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties containing granules other than absorbent substances
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
Abstract
The present invention provides a kind of preparation method of self-supporting solid-state multicomponent facial mask.Oil-soluble skin-care effect substance is dissolved in polyvinylpyrrolidone as stratum nucleare spinning solution by the present invention, water-soluble skin-care effect substance is dissolved in polyvinyl alcohol as shell layer spinning solution, water-soluble both effectiveness substance is loaded into fiber shell by coaxial electrostatic spinning method, oil-soluble both effectiveness substance loads to fiber stratum nucleare, it to two or more skin-care effect substances for keeping dissolubility different while loading in tunica fibrosa, facial mask can be assigned more preferably or multiple efficacies.Preparation process of the present invention is simple, easy-regulating component and fibre structure；Gained facial mask mechanical property is good, can self-supporting, good permeability.
Description
Technical field
The present invention relates to a kind of preparation methods of self-supporting solid-state multicomponent facial mask, belong to material science and cosmetic art
Field.
Background technique
Facial mask is one kind of skin care item, and the function of facial mask is varied, such as cleans skin, anti-wrinkle antiplaque, antioxygen whitening, mends
Water moisturizing, balance water and oil balance, anti-inflammatory anti-acne etc..The type of facial mask mainly include tear-pull, smear type (paste and creams shape),
Application type.Application type facial mask becomes most widely used facial mask type because having opposite simplicity of operation.Application type facial mask is
The film cloth for using polymer to produce is in a liquid state deposit in film cloth as carrier, various skin-care nutrient liquid and essence, and user can
Directly the film cloth for being loaded with the both effectiveness substance of liquid is applied in face, both effectiveness substance enters skin and plays a role.Sticking type facial mask
Film cloth be broadly divided into non-aqueous non-woven fabrics and water soluble polymer film, preparation method mainly have upper slurry processes, spun lacing method,
Physically or chemically Method for bonding, but all there is more or less deficiency in some aspects in these methods: such as, the preparation side of upper slurry processes
Method is complicated for operation, is unsuitable for the production of factory's batch；Although spun lacing method can produce soft and ventilative non-woven fabrics, behaviour
It is cumbersome to make equipment, operating cost is high；Physically or chemically Method for bonding requires bonding to reinforce, the film cloth that furthermore prepared by this kind of method
Fiber is thick, can not be bonded completely with face.In addition, application type facial mask storage when, liquid skin care in its film cloth after by bruising
The distribution of nutrient solution and essence in facial mask can become uneven；Its chemical stability of the effect of liquid property substance keeps impermanent, and
The organic solvent of Multiple components therein has skin certain injury；More liquid the effect of property substance be unfavorable for using
Person spreads in face for application type facial mask is smooth；The both effectiveness substance of excessive liquid easily drips along face in use, this
The usage comfort and functionality of application type facial mask are leveraged a bit.
Solid-state facial mask is the nearest emerging facial mask kind to grow up, because its is easy to use, preservative free due to deep used
Person's favor.The film cloth of current solid-state facial mask is mainly non-woven fabrics, and preparation method is mainly: facial mask cloth being immersed in skin care first
In the both effectiveness substance solution of liquid, then baked film cloth, finally cut out it is obtained.A small amount of water is uniformly poured on film using preceding by user
On cloth, after standing a few minutes, the film cloth of wetting is applied in face.Solid-state facial mask can guarantee the chemical state of both effectiveness substance
Stablize, guarantee will not go bad because of high temperature, humidity or weather relationship.But its preparation process requires harsh, the both effectiveness object of liquid
The dissolubility of the Multiple components homogenieity and final solid-state that just can guarantee the both effectiveness substance solution of liquid as similar as possible in matter
The homogenieity of facial mask, which limits being used in conjunction with for the biggish both effectiveness substance of solubility properties difference；And for a long time
In high temperature drying course, some low-boiling both effectiveness substances are easy inactivation；The transdermal effect of both effectiveness substance also needs to be considered.
Electrostatic spinning technique can continuously prepare the adjustable micro nanometer fiber film of fibre diameter, and electrospun fibers film has group
Divide the features such as various, structure is easily adjusted, diameter is adjustable, specific surface area is high, porosity is high, hole interlinking is good.Using Static Spinning skill
Organic biological active molecule and inorganic particulate can be added in electrospun fibers film by art, and it is a variety of to assign electrostatic spinning fiber film
Function.The biggish specific surface area of static spinning membrane, can be improved the chance of active material molecules and skin contact, can be supplied to thin
Born of the same parents more contact site, and the active material molecules for loading it are easy to discharge and be absorbed, and electrospun fibers film is saturating
Gas is good, and fibre diameter is small, good with biology base bottom compactness, and the small pore-size distribution of tunica fibrosa can also effectively stop entering for bacterium
It invades, this both contributes to electrostatic spinning fiber film in the application in facial mask field.Chinese patent literature CN107898716A discloses one kind
The preparation method of nanofiber dry type facial mask: it is quiet that Multi needle is carried out after water-soluble polymer solution and water-soluble nutrient solution are mixed
Electrospun uses facial mask to use non-woven fabrics base material as receiving screen, and one layer of nanofiber is finally formed on mask nonwoven fabric substrate
Film is made composite cellulosic membrane, is used as facial mask after cutting, molding, sterilizing.Chinese patent literature CN109825949A discloses one kind
The preparation method of all solid state functional nanofiber membrane: by the water-soluble polymer solution containing functional component and water-insoluble height
As electrostatic spinning after spinning solution after molecular solution mixing, eyelet fabric is to receive substrate, by resulting Static Spinning after spinning
All solid state functional nanofiber membrane is obtained after the drying of silk fiber film-eyelet fabric composite material, is used as facial mask.Foregoing invention system
Standby fiber facial mask needs to use non-woven fabrics base material or eyelet fabric as supporting layer, and the stickiness of supporting layer and static spinning membrane compared with
It is difficult to control, if the efficiency of the bad meeting extreme influence facial mask of compactness.Chinese patent literature CN109576817A discloses one kind
The preparation method of solid nanofibers facial mask: by water soluble polymer polyvinyl alcohol (PVA) aqueous solution, sodium alginate aqueous solution,
Electrostatic spinning obtains facial mask after the solution mixing of water-soluble beauty treatment particle；Sodium alginate is used to increase the toughness of gained facial mask, has
Effect reduces fibrous physics underbraced；Facial mask obtained by the invention includes solid nanofibers layer and is adsorbed on layers of nanofibers
Beauty treatment particle.In the invention preparation process, need to prepare a variety of solution, and need by PVA aqueous solution, sodium alginate aqueous solution and
Spinning mixture carries out the pre-treatment of residue filter after standing, operating process is cumbersome；And this facial mask contain only water-soluble beauty treatment at
Point, the oil-soluble beauty treatment ingredient that is insoluble in water powerful to skin-protecting function is not directed to.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of self-supporting solid-state multicomponent facial mask.This hair
It is bright that oil-soluble skin-care effect substance is dissolved in polyvinylpyrrolidone as stratum nucleare spinning solution, by water-soluble skin-care effect
Property substance be dissolved in polyvinyl alcohol as shell layer spinning solution, will water-soluble both effectiveness substance load by coaxial electrostatic spinning method
To fiber shell, oil-soluble both effectiveness substance loads to fiber stratum nucleare, thus two or more skin cares for keeping dissolubility different
Both effectiveness substance loads in tunica fibrosa simultaneously, can assign that facial mask is more preferable or multiple efficacies.Preparation process of the present invention is simple, easily
Regulate and control component and fibre structure；Gained facial mask mechanical property is good, can self-supporting.
Term explanation:
Room temperature: there is meaning well known in the art, refer to 25 ± 5 DEG C.
Technical scheme is as follows:
A kind of preparation method of self-supporting solid-state multicomponent facial mask, comprising steps of
(1) polyvinylpyrrolidone (PVP) is dissolved in dehydrated alcohol and obtains PVP solution；Then oil-soluble skin care is added
Both effectiveness substance obtains stratum nucleare spinning solution after dissolution；
(2) polyvinyl alcohol (PVA) is dissolved in deionized water and obtains PVA solution；Then water-soluble skin-care effect is added
Substance obtains shell layer spinning solution after dissolution；
(3) at room temperature, stratum nucleare spinning solution and shell layer spinning solution are subjected to coaxial electrostatic spinning and obtain solid-state electrostatic spinning fibre
Tie up film；Then vacuum dried to obtain self-supporting solid-state multicomponent facial mask.
Preferred according to the present invention, in step (1), the weight average molecular weight of the polyvinylpyrrolidone is 40 0000-
1390000；Preferably, the weight average molecular weight of the polyvinylpyrrolidone is 78 0000-120 0000.PVP material and human body
Toxic side effect will not be generated after contact, it is highly-safe, there is good biocompatibility.
It is preferred according to the present invention, in step (1), in PVP solution, the quality of polyvinylpyrrolidone and dehydrated alcohol
Volume ratio is 0.04-0.12g/mL；Preferably, in PVP solution, the quality of polyvinylpyrrolidone and the volume ratio of dehydrated alcohol
For 0.06-0.1g/mL.Polyvinylpyrrolidone and the suitable mass volume ratio of dehydrated alcohol can guarantee the conductivity of spinning solution
Properly, make stratum nucleare solution that there is good spinnability, and guarantee that tunica fibrosa has self-supporting after spinning.
In preparation method of the present invention, the concentration of PVP is important in PVP solution.The concentration of PVP it is too small (quality of PVP and
The volume ratio of dehydrated alcohol is less than 0.02g/mL), there is drop to drip in spinning process, tunica fibrosa is imperfect.The concentration of PVP is excessive
(quality of PVP and the volume ratio of dehydrated alcohol are greater than 0.15g/mL), it is unable to spinning.
Preferred according to the present invention, in step (1), the additional amount of the oil-soluble skin-care effect substance is polyethylene
The 1%-10% of pyrrolidones quality；Preferably, the additional amount of the oil-soluble skin-care effect substance is polyvinyl pyrrole
The 2%-8% of alkanone quality.Spinning high molecular polythene pyrrolidones has suppression to both effectiveness material molecule during the spinning process
The effect of crystallization is made, the additional amount of suitable both effectiveness substance can be such that both effectiveness substance exists in tunica fibrosa with non-crystalline,
Be conducive to absorption of the skin to both effectiveness substance.
According to the present invention, in step (1), the oil-soluble skin-care effect substance is can be dissolved in ethyl alcohol oil-soluble
Skin-care effect substance.Preferably, in step (1), the oil-soluble skin-care effect substance be resveratrol, arbutin,
The combination of one or more of vitamin E, isopropyl myristate, saualane or catechin.
Preferred according to the present invention, in step (2), the number-average molecular weight of the polyvinyl alcohol is 2 0000-10 0000；
Preferably, the number-average molecular weight of the polyvinyl alcohol is 6 0000-8 0000.Polyvinyl alcohol good film-forming property is a kind of extremely safe
Macromolecule organic, it is nontoxic to the human body, it is without side-effects, have good biocompatibility.
It is preferred according to the present invention, in step (2), in PVA solution, the quality of the polyvinyl alcohol and the body of deionized water
Product is than being 0.05-0.14g/mL；Preferably, in PVA solution, the quality of the polyvinyl alcohol and the volume ratio of deionized water are
0.06-0.1g/mL.Polyvinyl alcohol and the suitable mass volume ratio of deionized water can guarantee that the conductivity of spinning solution is suitable, make
Shell solution has good spinnability, is further ensured that the self-supporting of tunica fibrosa after spinning.
In preparation method of the present invention, the concentration of PVA is important in PVA solution.The concentration of PVA it is too small (quality of PVA and
The volume ratio of deionized water is less than 0.03g/mL) will affect the self-supporting of tunica fibrosa, the concentration of PVA it is excessive (quality of PVA and
The volume ratio of deionized water is greater than 0.16g/mL), it is unable to spinning.
Preferred according to the present invention, in step (2), the additional amount of the water-soluble skin-care effect substance is polyethylene
The 1%-10% of alcohol quality；Preferably, the additional amount of the water-soluble skin-care effect substance is polyvinyl alcohol quality
2%-8%.Spinning high-molecular polyivnyl alcohol has the function of inhibiting to crystallize to both effectiveness material molecule during the spinning process, properly
The additional amount of the effect of property substance can be such that both effectiveness substance exists in tunica fibrosa with non-crystalline, be conducive to skin to both effectiveness
The absorption of substance.
According to the present invention, in step (2), the water-soluble skin-care effect substance is the water-soluble shield that can be dissolved in water
The both effectiveness substance of skin.Preferably, the water-soluble skin-care effect substance be niacinamide, water-soluble beta glucan, malic acid,
The combination of one or more of Sodium Hyaluronate, L-vitamin C or sorbierite.
It is preferred according to the present invention, in step (3), in the polyvinyl alcohol and stratum nucleare spinning solution in the shell layer spinning solution
The mass ratio of polyvinylpyrrolidone is 1:0.6-1.2.
It is preferred according to the present invention, in step (3), the condition of the coaxial electrostatic spinning are as follows: spinning voltage is in 17-
The speed ratio of injecting of 25kV, shell layer spinning solution and stratum nucleare spinning solution is (1-5): 1, the rate of injecting of stratum nucleare spinning solution is 0.02-
The spray distance of 0.1mm/min, syringe needle and receiver is 15-20cm；Preferably, shell layer spinning solution and stratum nucleare spinning solution are injected
Speed ratio is 3:1.Control shell layer spinning solution and stratum nucleare spinning solution inject speed ratio, it is ensured that the long-time of spinning process is steady
It is fixed to carry out；According to the property of shell layer spinning solution and stratum nucleare spinning solution, the condition of coaxial electrostatic spinning is adjusted, adjusting is filametntary can
The property spun.
It is preferred according to the present invention, in step (3), the vacuum drying condition are as follows: the dry 2-5h of room temperature in vacuo；It is preferred that
, the vacuum drying condition are as follows: the dry 3-4h of room temperature in vacuo.
Technical characterstic of the invention and the utility model has the advantages that
1, oil-soluble skin-care effect substance is dissolved in polyvinylpyrrolidone ethanol solution as stratum nucleare by the present invention
Water-soluble skin-care effect substance is dissolved in polyvinyl alcohol water solution as shell layer spinning solution, by coaxial quiet by spinning solution
Water-soluble both effectiveness substance is loaded to fiber shell by electrical spinning method, and oil-soluble both effectiveness substance loads to fiber stratum nucleare,
To make two or more biggish skin-care effect substances of dissolubility gap while load in tunica fibrosa, facial mask can be assigned
More preferable or multiple efficacies；Simultaneously by adjusting the condition (spinning solution property and process conditions) of coaxial electrostatic spinning, preparation can be certainly
The solid-state facial mask of support.The present invention makees core layer material, high molecular material polyethylene using high molecular material polyvinylpyrrolidone
Alcohol makees Shell Materials, nontoxic to the human body, without side-effects, highly-safe, has good biocompatibility.Preparation process of the present invention
Simply, cost is relatively low, less energy intensive, component and fibre structure easy-regulating；The method of the present invention can substantially reduce functional materials mistake
A possibility that living.
2, all both effectiveness substances of water-soluble skin care that can be dissolved in water and the oil-soluble skin care that ethyl alcohol can be dissolved in the present invention
Both effectiveness substance can load in self-supporting solid-state facial mask by means of the present invention, and load capacity is big, can be easily and effectively
It realizes the compound of a variety of skin-care effect material compositions that dissolubility differs greatly, while guaranteeing the chemical stabilization of both effectiveness substance
Property, have a wide range of application；And can assign facial mask a variety of or more preferable effects, overcome a kind of existing facial mask only to have a kind of or specific few
The defect of several effects of number.
3, skin-care effect substance is individually fixed in polyvinylpyrrolidone and polyvinyl alcohol by the present invention, can be reduced
A possibility that both effectiveness substance crystallization, is present in both effectiveness substance in tunica fibrosa with non-crystalline, non-crystalline there are shapes
State is conducive to absorption of the skin to it.
4, the present invention avoids its bring defect without using non-woven fabrics base material or eyelet fabric as supporting layer；Using
Main material of the polyvinylpyrrolidone as stratum nucleare, main material of the polyvinyl alcohol as shell, by controlling spinning condition
Be prepared can self-supporting solid-state facial mask.The self-supporting property of solid-state facial mask of the present invention depends primarily on stratum nucleare and shell high score
Higher macromolecular solid content in the good film forming of sub- solution and tunica fibrosa.Gained solid-state facial mask of the invention has preferable power
Learn performance, good permeability；Fibre diameter is smaller (200-500nm), and specific surface area is larger, so that wherein loading the effect of property substance
The chance of molecule and skin contact is more, is easy to be released and be absorbed by the skin, may be directly applied to skin, comfort level is good.
Solid-state facial mask skin attachement of the present invention is good, in use, user can directly spread on facial use after drenching face.Spread on face
Behind portion, because stratum nucleare and shell macromolecule play the role of both effectiveness substance to inhibit crystallization, both effectiveness substance is in tunica fibrosa
Exist with non-crystalline, it is transdermal into skin, absorption to be conducive to both effectiveness substance.The both effectiveness substance of shell and the both effectiveness object of stratum nucleare
Matter successively direct Transdermal absorption.
5, the sequence of stratum nucleare and shell of the present invention is more important.If nuclear shell sequence is exchanged, spinning process after exchange
It is often caused blockages at middle syringe needle, needs frequently to wipe syringe needle and continue spinning；And obtained tunica fibrosa slag ball is more, shadow
Ring its application.
6, the selection of the high molecular material of nuclear shell of the present invention is important.Shell macromolecule need good biocompatibility,
Spinnability is good and spinning good film-forming property, and environmentally protective nontoxic in view of solvent, and shell macromolecule selects in ethanol
The preferable macromolecule of dissolubility；Stratum nucleare macromolecule needs to be screened according to the shell macromolecule having determined, two kinds of solution are same
Axis spinning must be independent of each other, spinning continuous-stable, and obtained tunica fibrosa must be smooth membranaceous and good separate from receiver
It just can be with.So spinning is often carried out repeated screening with high molecular material by the present invention has determined macromolecule used in nucleocapsid, Qi Tagao
The compounding of molecular material does not find good result.
Detailed description of the invention
Fig. 1 is the optical photograph of self-supporting solid-state multicomponent facial mask prepared by embodiment 1；
Fig. 2 is low power scanning electron microscope (SEM) photo of self-supporting solid-state multicomponent facial mask prepared by embodiment 2；
Fig. 3 is low power scanning electron microscope (SEM) photo of self-supporting solid-state multicomponent facial mask prepared by embodiment 3；
Fig. 4 is high power scanning electron microscope (SEM) photo of self-supporting solid-state multicomponent facial mask prepared by embodiment 4；
Fig. 5 is X-ray powder diffraction (XRD) figure of self-supporting solid-state multicomponent facial mask prepared by embodiment 5.
Specific embodiment
The present invention is described further combined with specific embodiments below, but not limited to this.
Experimental method described in following embodiments is unless otherwise specified conventional method simultaneously；The reagent and material
Material, unless otherwise specified, commercially obtains.
Embodiment 1:
A kind of preparation method of self-supporting solid-state multicomponent facial mask, steps are as follows:
(1) polyvinylpyrrolidone (PVP) (weight average molecular weight is 78 0000) is added to absolute ethanol, is stirred at room temperature,
The PVP that concentration is 0.09g/mL (quality/dehydrated alcohol volume of polyvinylpyrrolidone) is made in PVP after being completely dissolved molten
Liquid；Then resveratrol (additional amount of resveratrol is the 2% of PVP mass) is added in PVP solution, continues stirring to dissolution
Afterwards, as stratum nucleare spinning solution；
(2) polyvinyl alcohol (PVA) (number-average molecular weight 63800) is added in deionized water, then heats to 70 DEG C, stirs
Mix lower condensing reflux, after PVA is completely dissolved, be cooled to room temperature, be made concentration be 0.08g/mL (quality of polyvinyl alcohol/go from
The volume of sub- water) PVA solution；Then niacinamide (additional amount of niacinamide is the 2% of PVA mass) is added in PVA solution,
Stirring is to after dissolving, as shell layer spinning solution；
(3) stratum nucleare spinning solution and shell layer spinning solution (mass ratio of PVP and PVA are 1.1:1) are carried out at room temperature coaxial quiet
The rate of injecting of Electrospun, spinning voltage 18.0kV, shell layer spinning solution is 0.2mm/min, and stratum nucleare spinning solution injects rate
The ratio between rate of injecting for 0.04mm/min, i.e. shell layer spinning solution and stratum nucleare spinning solution is 5:1, is received and is spun using fixed reception device
The spray distance of silk fiber, syringe needle and receiver is 15cm, obtains electrospun fibers film.
(4) electrospun fibers film is dried in vacuo 4 hours at room temperature to get self-supporting solid-state multicomponent facial mask.
Fig. 1 is the optical photograph of self-supporting solid-state multicomponent facial mask obtained by the present embodiment, obtained solid as can be seen from Figure 1
State multicomponent facial mask mechanical property is preferable, can self-supporting, its surface does not have slight crack after being folded into starfish shape, and flexibility is good.
Embodiment 2
A kind of preparation method of self-supporting solid-state multicomponent facial mask, steps are as follows:
(1) polyvinylpyrrolidone (PVP) (weight average molecular weight is 90 0000) is added to absolute ethanol, is stirred at room temperature,
The PVP that concentration is 0.07g/mL (quality/dehydrated alcohol volume of polyvinylpyrrolidone) is made in PVP after being completely dissolved molten
Liquid；Then vitamin E (additional amount of vitamin E is the 3% of PVP mass) is added in PVP solution, continues stirring to dissolution
Afterwards, as stratum nucleare spinning solution；
(2) polyvinyl alcohol (PVA) (number-average molecular weight 75000) is added in deionized water, then heats to 70 DEG C, stirs
Lower condensing reflux is mixed, after PVA is completely dissolved, is cooled to room temperature, it is 0.1g/mL (quality/deionization of polyvinyl alcohol that concentration, which is made,
The volume of water) PVA solution；Then water-soluble beta glucan is added in PVA solution, and (additional amount of water-soluble beta glucan is
The 2% of PVA mass), stirring is to after dissolving, as shell layer spinning solution；
(3) stratum nucleare spinning solution and shell layer spinning solution (mass ratio of PVP and PVA are 0.7:1) are carried out at room temperature coaxial quiet
The rate of injecting of Electrospun, spinning voltage 18.0kV, shell layer spinning solution is 0.18mm/min, and stratum nucleare spinning solution injects rate
The ratio between speed of injecting for 0.06mm/min, i.e. shell layer spinning solution and stratum nucleare spinning solution is 3:1, is received and is spun using fixed reception device
The spray distance of silk fiber, syringe needle and receiver is 16cm, obtains electrospun fibers film.
(4) electrospun fibers film is dried in vacuo 3 hours at room temperature to get self-supporting solid-state multicomponent facial mask.
Fig. 2 is the low power SEM photograph of self-supporting solid-state multicomponent facial mask obtained by the present embodiment, is prepared as seen from Figure 2
Self-supporting solid-state multicomponent facial mask fiber it is continuous, diameter is evenly distributed and diameter is relatively thin (diameter dimension is about 500nm).
Embodiment 3
A kind of preparation method of self-supporting solid-state multicomponent facial mask, steps are as follows:
(1) polyvinylpyrrolidone (PVP) (weight average molecular weight is 100 0000) is added to absolute ethanol, room temperature is stirred
It mixes, the PVP that concentration is 0.1g/mL (quality/dehydrated alcohol volume of polyvinylpyrrolidone) is made in PVP after being completely dissolved molten
Liquid；Then arbutin (additional amount of arbutin is the 6% of PVP mass) is added in PVP solution, continues stirring to after dissolving,
As stratum nucleare spinning solution；
(3) polyvinyl alcohol (PVA) (number-average molecular weight 77000) is added in deionized water, then heats to 70 DEG C, stirs
Lower condensing reflux is mixed, after PVA is completely dissolved, is cooled to room temperature, it is 0.1g/mL (quality/deionization of polyvinyl alcohol that concentration, which is made,
The volume of water) PVA solution；Then malic acid (additional amount of malic acid is the 2% of PVA mass) is added in PVA solution, stirs
It mixes to dissolution, as shell layer spinning solution；
(3) stratum nucleare spinning solution and shell layer spinning solution (mass ratio of PVP and PVA are 1:1) are subjected to coaxial electrostatic at room temperature
The rate of injecting of spinning, spinning voltage 20.0kV, shell layer spinning solution is 0.4mm/min, and the rate of injecting of stratum nucleare spinning solution is
The ratio between rate of injecting of 0.08mm/min, i.e. shell layer spinning solution and stratum nucleare spinning solution are 5:1, receive spinning using fixed reception device
The spray distance of fiber, syringe needle and receiver is 16cm, obtains electrospun fibers film.
(4) electrospun fibers film is dried in vacuo 4 hours at room temperature to get self-supporting solid-state multicomponent facial mask.
Fig. 3 is the low power SEM photograph of self-supporting solid-state multicomponent facial mask obtained by the present embodiment, is prepared as seen from Figure 3
Self-supporting solid-state multicomponent facial mask fiber it is continuous, diameter is evenly distributed and diameter is relatively thin (diameter dimension is about 500nm).
Embodiment 4:
A kind of preparation method of self-supporting solid-state multicomponent facial mask, steps are as follows:
(1) polyvinylpyrrolidone (PVP) (weight average molecular weight is 90 0000) is added to absolute ethanol, is stirred at room temperature,
The PVP solution that concentration is 0.1g/mL (quality/dehydrated alcohol volume of polyvinylpyrrolidone) is made in PVP after being completely dissolved；
Then in PVP solution be added isopropyl myristate, saualane (additional amount of isopropyl myristate be PVP mass 3%,
The additional amount of saualane is the 1% of PVP mass), continue stirring to after dissolving, as stratum nucleare spinning solution；
(4) polyvinyl alcohol (PVA) (number-average molecular weight 63800) is added in deionized water, then heats to 70 DEG C, stirs
Mix lower condensing reflux, after PVA is completely dissolved, be cooled to room temperature, be made concentration be 0.09g/mL (quality of polyvinyl alcohol/go from
The volume of sub- water) PVA solution；Then Sodium Hyaluronate is added in PVA solution, and (additional amount of Sodium Hyaluronate is PVA matter
The 4% of amount), stirring is to after dissolving, as shell layer spinning solution；
(3) stratum nucleare spinning solution and shell layer spinning solution (mass ratio of PVP and PVA are 1.1:1) are carried out at room temperature coaxial quiet
The rate of injecting of Electrospun, spinning voltage 21.0kV, shell layer spinning solution is 0.28mm/min, and stratum nucleare spinning solution injects rate
The ratio between rate of injecting for 0.07mm/min, i.e. shell layer spinning solution and stratum nucleare spinning solution is 4:1, is received and is spun using fixed reception device
The spray distance of silk fiber, syringe needle and receiver is 17cm, obtains electrospun fibers film.
(4) electrospun fibers film is dried in vacuo 4 hours at room temperature to get self-supporting solid-state multicomponent facial mask.
Fig. 4 is the high power SEM photograph of self-supporting solid-state multicomponent facial mask obtained by the present embodiment, is prepared as seen from Figure 4
Self-supporting solid-state multicomponent facial mask fiber surface it is smooth, do not occur crystalline particulate, illustrate skin-care effect substance with non-knot
Crystalline molecular state load is in the fibre；Fiber diameter size is uniform, and diameter is about 400nm.
Embodiment 5
A kind of preparation method of self-supporting solid-state multicomponent facial mask, steps are as follows:
(1) polyvinylpyrrolidone (PVP) (weight average molecular weight is 120 0000) is added to absolute ethanol, room temperature is stirred
It mixes, the PVP that concentration is 0.1g/mL (quality/dehydrated alcohol volume of polyvinylpyrrolidone) is made in PVP after being completely dissolved molten
Liquid；Then catechin (additional amount of catechin is the 6% of PVP mass) is added in PVP solution, continues stirring to after dissolving,
As stratum nucleare spinning solution；
(5) polyvinyl alcohol (PVA) (number-average molecular weight 79000) is added in deionized water, then heats to 70 DEG C, stirs
Lower condensing reflux is mixed, after PVA is completely dissolved, is cooled to room temperature, it is 0.1g/mL (quality/deionization of polyvinyl alcohol that concentration, which is made,
The volume of water) PVA solution；Then L-vitamin C, the sorbierite (additional amount of L-vitamin C are added in PVA solution
It is the 3% of PVA mass, the additional amount of sorbierite is the 3% of PVA mass), stirring is to after dissolving, as shell layer spinning solution；
(3) stratum nucleare spinning solution and shell layer spinning solution (mass ratio of PVP and PVA are 1:1) are subjected to coaxial electrostatic at room temperature
The rate of injecting of spinning, spinning voltage 22.0kV, shell layer spinning solution is 0.16mm/min, and the rate of injecting of stratum nucleare spinning solution is
The ratio between rate of injecting of 0.08mm/min, i.e. shell layer spinning solution and stratum nucleare spinning solution are 2:1, receive spinning using fixed reception device
The spray distance of fiber, syringe needle and receiver is 18cm, obtains electrospun fibers film.
(4) electrospun fibers film is dried in vacuo 4 hours at room temperature to get self-supporting solid-state multicomponent facial mask.
Fig. 5 is X-ray powder diffraction (XRD) figure of self-supporting solid-state multicomponent facial mask obtained by the present embodiment, can be with from Fig. 5
The self-supporting solid-state multicomponent facial mask fiber for seeing preparation is amorphous state, illustrates skin-care effect substance with non-crystalline molecule
State load is in the fibre.
Comparative example 1
A kind of preparation method of self-supporting solid-state multicomponent facial mask, as described in Example 1, except that: polyvinyl alcohol
Replace with polyethylene glycol (weight average molecular weight 20000)；Other steps and condition and embodiment 1 are consistent.Syringe needle in spinning process
Place frequently has drop to drip, and spinning process is discontinuous, and fiber film forming is poor, cannot completely separate from receiver.
Comparative example 2
A kind of preparation method of self-supporting solid-state multicomponent facial mask, as described in Example 2, except that: stratum nucleare and shell
Layer spinning solution exchanges, and often causes blockages at syringe needle in spinning process, needs frequently to wipe syringe needle and continues spinning；And
Obtained tunica fibrosa slag ball is more, influences its application.
Test example 1
Mechanical property test: measuring the tensile strength of solid-state multicomponent facial mask using fiber tester for elongation, according to
ASTMD882-02 standard (standard method of testing film and thin material tensile property) by solid-state multicomponent facial mask be cut into 6mm ×
The strip of 40mm (width x length), rate of extension 10mm/min, each sample are measured 5 times and are averaged.Test result is as follows table
It is shown:
1 tensile strength test data of table
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Tensile strength/MPa | 130.56 | 145.30 | 152.67 | 140.15 | 158.11 |
It, can self-supporting by above-mentioned 1 data of table it is found that facial mask mechanical property of the present invention is excellent；Its mechanical property is higher than current
The natural cotton fiber being commonly used on facial mask (tensile strength is about 110MPa).
Test example 2
The gas permeability of facial mask is tested according to GB/T5453-2007, test result is as follows shown in table:
1 permeability test data of table
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Gas permeability/% | 4134 | 4002 | 3927 | 4069 | 3872 |
By above-mentioned data it is found that facial mask good permeability of the present invention, skin will not feel sultry in use process, comfort compared with
It is good.
Claims (10)
1. a kind of preparation method of self-supporting solid-state multicomponent facial mask, comprising steps of
(1) polyvinylpyrrolidone is dissolved in dehydrated alcohol and obtains PVP solution；Then oil-soluble skin-care effect object is added
Matter obtains stratum nucleare spinning solution after dissolution；
(2) polyvinyl alcohol is dissolved in deionized water and obtains PVA solution；Then water-soluble skin-care effect substance is added, dissolves
Shell layer spinning solution is obtained afterwards；
(3) at room temperature, stratum nucleare spinning solution and shell layer spinning solution are subjected to coaxial electrostatic spinning and obtain solid-state electrospun fibers film；
Then vacuum dried to obtain self-supporting solid-state multicomponent facial mask.
2. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (1), institute
The weight average molecular weight for stating polyvinylpyrrolidone is 40 0000-139 0000；Preferably, the weight of the polyvinylpyrrolidone
Average molecular weight is 78 0000-120 0000.
3. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (1),
In PVP solution, the quality of polyvinylpyrrolidone and the volume ratio of dehydrated alcohol are 0.04-0.12g/mL；Preferably, PVP is molten
In liquid, the quality of polyvinylpyrrolidone and the volume ratio of dehydrated alcohol are 0.06-0.1g/mL.
4. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (1), institute
The additional amount for stating oil-soluble skin-care effect substance is the 1%-10% of polyvinylpyrrolidone quality；Preferably, the oil
The additional amount of the skin-care effect substance of dissolubility is the 2%-8% of polyvinylpyrrolidone quality.
5. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (2), institute
The number-average molecular weight for stating polyvinyl alcohol is 2 0000-10 0000；Preferably, the number-average molecular weight of the polyvinyl alcohol is 6
0000-8 0000。
6. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (2),
In PVA solution, the quality of the polyvinyl alcohol and the volume ratio of deionized water are 0.05-0.14g/mL；Preferably, PVA solution
In, the quality of the polyvinyl alcohol and the volume ratio of deionized water are 0.06-0.1g/mL.
7. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (2), institute
The additional amount for stating water-soluble skin-care effect substance is the 1%-10% of polyvinyl alcohol quality；Preferably, described water-soluble
The additional amount of skin-care effect substance is the 2%-8% of polyvinyl alcohol quality.
8. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that including the following conditions
In it is one or more:
A, in step (1), the oil-soluble skin-care effect substance is resveratrol, arbutin, vitamin E, myristic acid
The combination of one or more of isopropyl ester, saualane or catechin；
B, in step (2), the water-soluble skin-care effect substance is niacinamide, water-soluble beta glucan, malic acid, transparent
The combination of one or more of matter acid sodium, L-vitamin C or sorbierite.
9. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (3), institute
The mass ratio for stating the polyvinyl alcohol in shell layer spinning solution and the polyvinylpyrrolidone in stratum nucleare spinning solution is 1:0.6-1.2.
10. the preparation method of self-supporting solid-state multicomponent facial mask according to claim 1, which is characterized in that in step (3),
The condition of the coaxial electrostatic spinning are as follows: for spinning voltage in 17-25kV, shell layer spinning solution and stratum nucleare spinning solution inject speed ratio
For (1-5): 1, the rate of injecting of stratum nucleare spinning solution is 0.02-0.1mm/min, and the spray distance of syringe needle and receiver is 15-
20cm；Preferably, the speed ratio of injecting of shell layer spinning solution and stratum nucleare spinning solution is 3:1；
Preferably, in step (3), the vacuum drying condition are as follows: the dry 2-5h of room temperature in vacuo；It is further preferred that described
Vacuum drying condition are as follows: the dry 3-4h of room temperature in vacuo.
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