CN114891149B - Porous structure material for patch type mask base material, patch type mask containing porous structure material and preparation method of porous structure material - Google Patents
Porous structure material for patch type mask base material, patch type mask containing porous structure material and preparation method of porous structure material Download PDFInfo
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- CN114891149B CN114891149B CN202210377632.4A CN202210377632A CN114891149B CN 114891149 B CN114891149 B CN 114891149B CN 202210377632 A CN202210377632 A CN 202210377632A CN 114891149 B CN114891149 B CN 114891149B
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- porous structure
- structure material
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- water
- mask
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- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 229940072106 hydroxystearate Drugs 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- 235000021239 milk protein Nutrition 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- RZRNAYUHWVFMIP-UHFFFAOYSA-N monoelaidin Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-UHFFFAOYSA-N 0.000 description 1
- MDYPDLBFDATSCF-UHFFFAOYSA-N nonyl prop-2-enoate Chemical compound CCCCCCCCCOC(=O)C=C MDYPDLBFDATSCF-UHFFFAOYSA-N 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 231100000370 skin sensitisation Toxicity 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229950006451 sorbitan laurate Drugs 0.000 description 1
- 235000011067 sorbitan monolaureate Nutrition 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 description 1
- XZHNPVKXBNDGJD-UHFFFAOYSA-N tetradecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C=C XZHNPVKXBNDGJD-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical class C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- 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
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/32—Polymerisation in water-in-oil emulsions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1811—C10or C11-(Meth)acrylate, e.g. isodecyl (meth)acrylate, isobornyl (meth)acrylate or 2-naphthyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1818—C13or longer chain (meth)acrylate, e.g. stearyl (meth)acrylate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses a porous structure material for a patch type mask substrate, a patch type mask containing the porous structure material and a preparation method, wherein the porous structure material is formed by high internal phase emulsion polymerization, and compared with the traditional substrate such as non-woven fabric, natural fibers such as silk and pectin fibers, hydrogel and the like, the mask substrate has higher liquid carrying rate and liquid retention capacity, better air permeability and better skin fit, and can achieve a good antibacterial effect by adjusting and controlling the structure composition, and compared with the traditional mask substrate, the mask substrate has better comprehensive performance.
Description
Technical Field
The invention relates to the technical field of porous materials and skin care products, in particular to a porous structure material for a patch type facial mask base material, a patch type facial mask containing the porous structure material and a preparation method of the porous structure material.
Background
At present, the common facial masks on the market are mainly divided into paste type, tearing type, patch type and the like for painting, wherein more than 80% of the facial masks are patch type. The base materials (base cloth) of the patch type facial mask mainly comprise non-woven fabrics, hydrogel, biological fibers and the like, wherein the non-woven fabrics are the most common, the common non-woven fabric facial mask base materials comprise pure cotton fibers, viscose fibers, silk fibers, copper ammonia fibers, tencel fibers and the like, the conventional non-woven fabrics have poor degree of adhesion with skin, low absorption capacity, mask essence is easy to drop, low liquid retention capacity and general air permeability; the hydrogel mask has good skin fitness, mild properties, low liquid carrying rate, poor air permeability, uncomfortable feeling after long-time application, and certain limitation on the adaptable mask essence. In order to ensure the performance effect in the service life, most of the non-woven fabrics or hydrogel mask patches need to be added with a certain content of antiseptic antibacterial components such as sodium benzoate, parahydroxybenzoate, methylisothiazolinone and the like, which have a certain sensitization and stimulation effect on the skin.
In order to solve the problems, patent CN107349111B discloses different applications of metal-organic framework materials and covalent organic framework materials in cleaning masks, antiallergic masks and functional masks, and the porous framework material is used as a component to be applied to smearing masks, and the structure and the component of the porous framework material are regulated according to different application fields. Patent CN11534926B discloses a high-porosity mask base cloth prepared by milk protein cellulose composite spinning and a preparation method thereof, and compared with the traditional non-woven fabric mask base cloth, the high-porosity mask base cloth has the advantages of high porosity, good air permeability and good hygroscopicity, but has complex preparation, high preparation cost, large shrinkage and unstable size, and needs to be added with anti-corrosion antibacterial components.
Innovations of the presently disclosed patch type mask base material are focused on nonwoven materials, but still cannot thoroughly solve the problems existing in the prior art.
Disclosure of Invention
The invention aims to provide a porous structure material suitable for a patch type mask substrate, which is prepared by high internal phase emulsion polymerization, and has the advantages of high liquid carrying rate and liquid retention, good skin fit, good air permeability, wide adaptability to mask essence, self-carried antibacterial effect, strong industrialization realization and the like compared with the mask substrate disclosed by the prior art.
Another object of the present invention is the use of such porous structure materials as a patch mask.
Still another object of the present invention is to provide a method for preparing a patch type mask using the porous structure material as a base fabric.
In order to achieve the above object, the present invention adopts the following technical scheme:
a porous structure material for a patch type mask substrate is obtained by water-in-oil type high internal phase emulsion polymerization, the number average pore size of the porous structure material is 1-100 mu m, the porosity is not less than 60%, the thickness after wet saturation is not more than 1mm, and the transverse and longitudinal bending rigidity of the porous structure material is not more than 0.2gf cm 2 /cm。
In a specific embodiment, the porous structure material has a number average cell pore size of 1-50 μm, a porosity of 70-90%, a thickness after wet saturation of 0.05-1 mm, and a transverse and longitudinal flexural rigidity of 0.001-0.2 gf cm 2 /cm。
In a specific embodiment, when the porous structure material is used as a mask substrate, the liquid carrying rate of the mask liquid with different viscosities is not lower than 1000%, and is preferably 1000% -3000%.
In a specific embodiment, when the porous structure material is used as a mask substrate, the liquid retention rate of the mask liquid with different viscosities is not lower than 80%, and preferably 80% -95%.
In another aspect, a patch mask is made from a porous structural material comprising the foregoing substrate for a patch mask.
In still another aspect, a method for preparing the patch type facial mask includes the following steps:
1) Preparing water-in-oil emulsion containing the following oil phases, forming the oil phases into uniform oil phases under the shearing and dispersing effects, and maintaining the temperature of the oil phases at 20-90 ℃; wherein, based on the total weight of the oil phase, the oil phase comprises:
a) 80% to 99% by weight of a substantially water insoluble monomer component;
b) 1-20% by weight of an emulsifier component which is soluble in the oil phase and which forms a stable water-in-oil emulsion;
2) The water phase comprises 0.5-15 wt% of water-soluble inorganic salt based on the total weight of the water phase, and the temperature of the water phase is maintained at 20-90 ℃; preferably, the water-soluble or oil-soluble initiator accounts for 1-10% of the total weight of the monomers based on the total weight of the monomers in the oil phase;
3) Gradually adding the water phase into the oil phase under the shearing action to emulsify the water phase into stable HIPPE emulsion; preferably at a shear rate of 50rpm to 5000 rpm;
4) Solidifying the water-in-oil emulsion to form a porous structure material; preferably, the emulsified HIPPE emulsion is coated with a thickness of 0.05-1 mm, and then is cured in an oven or a water bath or a UV box, preferably at a curing temperature of 45-120 ℃ for 5 s-30 min;
5) Washing, squeezing and dehydrating the solidified porous material, directly immersing the porous material into a pre-prepared mask essence without drying, and soaking the porous material until saturated absorption is achieved, thus obtaining the mask.
In a specific embodiment, the ratio of the volume of the aqueous phase to the mass of the oil phase in the HIPPE emulsion in step 3) is not less than 20mL:1g, preferably 20 mL-40 mL:1g.
In a specific embodiment, the monomer component in step 1) is selected from alkyl acrylate monomers or alkylstyrene monomers containing one or more carbon-carbon double bonds; preferably, the oil phase a) further comprises 0-3% of hydrophobically modified nano zinc oxide, preferably 0.05% -3% of the total weight of the oil phase.
In a specific embodiment, the oil phase a) further comprises cellulose nano-particles, wherein the addition amount of the cellulose nano-particles accounts for 0% -2% of the total weight of the oil phase; preferably, the cellulose nanoparticle is selected from any one of cellulose nanocrystals, microcrystalline cellulose, cellulose nanofibers, nanocrystalline cellulose, nanocellulose.
In a specific embodiment, the porous structure material after curing in step 5) has a glass transition temperature after drying in the range of-30 ℃ to 25 ℃.
Compared with the prior art, the porous structure material mask substrate has the following beneficial effects:
compared with the traditional non-woven fabric base materials, hydrogel base materials and various cellulose base materials, the porous structure material suitable for the patch type mask base materials is creatively prepared by utilizing high internal phase emulsion polymerization, has good absorbability to low-viscosity and high-viscosity mask essence, prevents the mask essence from dripping in the taking process, and improves the utilization rate and application range of the mask essence; in addition, the mask has good air permeability and good skin fit degree as a mask base material, and can have good antibacterial effect when the mask base material preferably contains the hydrophobic modified nano zinc oxide, and the mask base material is safer to the skin without adding a preservative. The porous structure material has balanced performance and good comprehensive performance, has better application prospect in the patch type mask base material, and is prepared by using the high internal phase emulsion for the first time.
Drawings
Fig. 1 is an SEM spectrum (magnified 1000 times) of a porous structure material suitable for a patch type mask substrate prepared in example 1 of the present invention.
Detailed Description
The following examples will further illustrate the method provided by the present invention for a better understanding of the technical solution of the present invention, but the present invention is not limited to the examples listed but should also include any other known modifications within the scope of the claims of the present invention.
A method of making a porous structural material for a patch mask substrate using a High Internal Phase Emulsion (HIPE), comprising the steps of:
1) Preparing a water-in-oil emulsion comprising an oil phase, wherein the oil phase comprises, based on the total weight of the oil phase:
a) 80 to 99 weight percent of a substantially water insoluble monomer component, substantially water insoluble meaning that the monomer is slightly soluble, poorly soluble or insoluble in water at 20 ℃;
b) 1-20% by weight of an emulsifier component which is soluble in the oil phase and which forms a stable water-in-oil emulsion;
2) Ultrasonic-treating the oil phase in an ultrasonic oscillator to obtain a uniform oil phase, and maintaining the temperature of the oil phase at 20-90 ℃;
3) The water phase comprises 0.5-15 wt% of water-soluble inorganic salt based on the total weight of the water phase, and the temperature of the water phase is maintained at 20-90 ℃; gradually adding the water phase into the oil phase under the shearing action to emulsify the water phase into stable HIPPE emulsion;
4) Solidifying the water-in-oil emulsion to form a porous structure material; curing is preferably carried out by placing in a UV box or oven or water bath or steam;
5) The solidified porous material is directly immersed into the prepared mask essence to be saturated and absorbed after being washed, extruded and dehydrated without being dried.
Wherein the aqueous phase of the water-in-oil emulsion comprises:
a) 0.5-15% by weight, based on the weight of the aqueous phase, of a water-soluble electrolyte, the electrolyte being a water-soluble inorganic salt; preferably, the water-soluble inorganic salt is selected from monovalent, divalent inorganic salts of alkali metal and alkali metal halide or sulfate salts;
b) A water-soluble or oil-soluble initiator accounting for 1-10% of the total weight of the monomers based on the total weight of the monomers of the oil phase; preferably, the initiator is selected from at least any one of photoinitiators such as diphenyl ketones, alpha-hydroxyacetophenones, benzyl ketals, alpha-aminoalkylphenones or acylphosphine oxides; persulfates, azobisiso Ding Mi hydrochloride, or redox initiation systems, such as sodium persulfate, ammonium persulfate, potassium persulfate, azobisisobutylimbic hydrochloride, azobisiso Ding Mi hydrochloride, or at least any one of persulfate-sodium bisulfite, persulfate-ascorbic acid, persulfate-sodium thiosulfate, and the like, may also be selected.
Wherein the weight ratio of the volume of the water phase to the oil phase of the water-in-oil emulsion is not less than 20mL:1g, for example 25mL:1g, 30mL:1g, 35mL:1g, 40mL:1g, 50mL:1g, 60mL:1g, preferably 20 mL-40 mL:1g.
Wherein the monomer component in a) of the oil phase comprises:
i) 60 to 95% by weight, based on the total weight of the monomers contained in the oil phaseA percentage of at least one monofunctional comonomer that is substantially insoluble in water; preferably, the monofunctional comonomer is selected from the group consisting of styrene, alkyl acrylate, alkyl methacrylate, and mixtures thereof; more preferably, 70% to 90% by weight of a monomer component selected from the group consisting of: acrylic acid C 4 -C 18 Alkyl esters, methacrylic acid C 4 -C 18 Alkyl ester esters, styrene, alkylstyrenes, and mixtures thereof;
ii) from 5% to 40% by weight, based on the total weight of monomers contained in the oil phase, of at least one substantially water-insoluble polyfunctional crosslinking agent; preferably, the multifunctional crosslinker is selected from the group consisting of divinyl aromatics, alkyl acrylamides, diacrylates or dimethacrylates of polyols, and mixtures thereof; more preferably, 10 to 30 weight percent of a multifunctional crosslinking agent selected from any one or a mixture of any of divinylbenzene, trivinylbenzene, divinyltoluene, divinylxylene, ethylene glycol dimethacrylate, 1, 4-butanediol dimethacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, hexanediol dimethacrylate, 1, 12-dodecyl dimethacrylate, 1, 14-tetradecyl glycol dimethacrylate, and the like.
The oil-soluble emulsifier in b) of the oil phase is preferably soluble in the oil phase and is capable of forming a stable water-in-oil emulsion, the oil-soluble emulsifier being selected from branched or linear C16-C24 fatty acid glycerides, branched or linear C16-C24 fatty acid sorbitan fatty acid esters, sucrose fatty acid esters, alkylphenol ethoxylates or mixtures of these components.
When preparing the antibacterial porous structure mask substrate, in a preferred scheme, the oil phase a) can contain 0-3 weight percent of hydrophobic modified nano zinc oxide particles, preferably, the particle size of the hydrophobic modified nano zinc oxide is 1-100nm, and the hydrophobic modified nano zinc oxide particles can be selected from long-chain fatty acid modified nano zinc oxide, organosilicon modified nano zinc oxide, surfactant modified nano zinc oxide, polyethylene glycol modified nano zinc oxide, various inorganic particle hybridization nano zinc oxide or zinc oxide particles modified in any other way to achieve the aim of changing the surface hydrophilicity of the hydrophobic porous structure mask substrate; preferably, the hydrophobic modified nano zinc oxide is C9-C24 long chain saturated or unsaturated fatty acid modified nano zinc oxide, organosilicon modified nano zinc oxide, silane coupling agent modified nano zinc oxide, titanate coupling agent modified nano zinc oxide, surfactant modified nano zinc oxide, polyethylene glycol modified nano zinc oxide or other modified zinc oxide particles modified in any way so as to achieve the aim of changing the surface hydrophilicity and hydrophobicity; more preferably, any one or a mixture of more than one of lauric acid modified nano zinc oxide, stearic acid modified nano zinc oxide, silane coupling agent or titanate coupling agent modified nano zinc oxide, surfactant modified nano zinc oxide, chitosan modified nano zinc oxide, polyethylene glycol modified nano zinc oxide and titanate coupling agent modified nano zinc oxide is selected.
Specifically, the modification method of the hydrophobic modified nano zinc oxide comprises the steps of for example, adding zinc oxide nano particles with certain mass into ethanol solution, adding a certain amount of C12-C22 long-chain fatty acid such as lauric acid, wherein the fatty acid content can be more than 1%, carrying out centrifugal separation after continuously stirring for a proper time, and drying to obtain fatty acid modified nano zinc oxide particles with hydrophobic surfaces; for example, the preparation of the silane coupling agent modified nano zinc oxide can be carried out by adding a certain mass of silane coupling agent into absolute ethyl alcohol, adjusting pH value to about 5-6 by hydrochloric acid, adding nano zinc oxide at about 80 ℃, carrying out ultrasonic treatment, and finally centrifuging and drying to obtain the silane coupling agent modified nano zinc oxide particles; for example, preparing cationic surfactant modified zinc oxide particles, stirring a certain amount of nano zinc oxide particles in a cetyl trimethyl ammonium bromide solution with a certain concentration at a high speed for 2 hours, centrifuging, and freeze-drying to obtain cetyl trimethyl ammonium bromide modified nano zinc oxide particles; the preparation method is not limited to the examples in the invention, any preparation method capable of achieving the aim of hydrophobic modification can be used for obtaining the hydrophobic modified nano zinc oxide, and the hydrophobic modified nano zinc oxide can be directly purchased in the market.
In a preferred embodiment, the oil phase a) may further comprise the cellulose nanoparticles, preferably, cellulose nanoparticles selected from any one of cellulose nanocrystals, microcrystalline cellulose, cellulose nanofibers, nanocrystalline cellulose, nanocellulose, nanofibrillated cellulose or bacterial nanocellulose; the addition amount of the cellulose nano particles can be 0-2% of the total weight of the oil phase, preferably 0.5-2%, and the addition of the cellulose nano particles can improve the hydrophilicity and flexibility of the material.
Wherein, the oil phase and the water phase of the water-in-oil emulsion prepared in the step 3) are mixed and emulsified at the temperature of 20 ℃ to 90 ℃ and form stable water-in-oil emulsion under the mixing shearing speed of 50rpm to 5000 rpm.
The curing temperature of the water-in-oil emulsion in the step 4) is 45-120 ℃, the curing time is not more than 0.5 hour, and the residual monomer content of the cured material is lower than 100ppm of the weight of the polymer.
The porous structure material prepared in the step 4) has a number average cell diameter of 1-100 μm, preferably the porous structure material has a number average cell diameter of 1-50 μm; the porosity is not less than 60%, preferably 70% -90%; the thickness of the porous material after the porous material absorbs the mask essence is not higher than 1mm, preferably 0.05-1 mm; the liquid carrying rate of the porous material to the facial mask essence within the viscosity range of 50 cp-2000 cp is not lower than 1000%, preferably 1000% -3000%, and the liquid retention rate is not lower than 80%, preferably 80% -95%; the transverse and longitudinal bending rigidity of the porous material after absorbing the facial mask essence is not more than 0.2gf cm 2 Preferably 0.001 to 0.2gf cm 2 /cm。
When the porous structure material is used as a mask substrate, the safety is equivalent to or better than that of a traditional mask substrate, wherein the traditional mask substrate is a non-woven fabric, silk, tencel, cuprammonium yarn, bamboo fiber, natural cotton, biological fiber, chitosan, composite fiber, hydrogel substrate and the like.
The porous material can be compounded with wood pulp fiber, non-woven fiber, other viscose fiber and the like before or during emulsion curing, or coated on a thermoplastic fiber net, so that the prepared mask substrate has higher strength.
When the oil phase contains 0.05 to 3 percent of hydrophobically modified nano zinc oxide particles, the antibacterial rate of the prepared porous material on staphylococcus aureus can reach more than 70 percent after 1 hour in an antibacterial test.
A preferred scheme is a preparation method of a porous structure mask with good air permeability, high liquid carrying rate, good skin fitting degree, wide adaptation mask essence and antibacterial effect, which comprises the following specific preparation steps:
(1) At 20-50 ℃, forming a stable and uniform oil phase by the oil phase containing the hydrophobic modified nano zinc oxide, the polymeric monomer, the cross-linking agent and the emulsifying agent under the ultrasonic action;
(2) Mixing the oil phase as a continuous phase with the aqueous phase as a dispersed phase containing an electrolyte at a temperature of 40 ℃ to 90 ℃, preferably 40 ℃ to 80 ℃, to form a stable hipe water-in-oil emulsion;
(3) Placing the HIPPE emulsion in an oven or water bath or under UV illumination to cure for 30s-30 min;
(4) Washing, squeezing and dehydrating the solidified porous material, and putting the porous material into the prepared mask essence to be absorbed to saturation.
In the step (1), the hydrophobically modified nano zinc oxide contained in the oil phase accounts for 0.05% -3% of the total oil phase, for example, including but not limited to, the hydrophobically modified nano zinc oxide contained in the oil phase accounts for 0.05%, 0.1%, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0% of the total oil phase, preferably the hydrophobically modified nano zinc oxide accounts for 0.2% -3% of the total oil phase, more preferably the hydrophobically modified nano zinc oxide accounts for 0.2% -1% of the total oil phase; the hydrophobic modified nano zinc oxide is selected from fatty acid modified nano zinc oxide, organosilicon modified nano zinc oxide, surfactant modified nano zinc oxide, chitosan modified nano zinc oxide, polyethylene glycol modified nano zinc oxide, titanate coupling agent modified nano zinc oxide, multi-particle composite hybrid nano zinc oxide and the like, and is preferably selected from fatty acid modified nano zinc oxide, organosilicon modified nano zinc oxide and surfactant modified nano zinc oxide.
In step (1), the substantially water-insoluble monomer component contained in the oil phase comprises 80% to 99% of the total weight of the oil phase, including, but not limited to, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, preferably 90% to 95% of the total weight of the oil phase.
Wherein the monomer component comprises: i) 60 to 95 weight percent, based on the total weight of monomers contained in the oil phase, of at least one substantially water-insoluble monofunctional comonomer; preferably, the monofunctional comonomer is selected from the group consisting of styrene, alkyl acrylate, alkyl methacrylate, aryl acrylate, and mixtures thereof; more preferably, 70% to 90% by weight of a monomer component selected from the group consisting of: acrylic acid C 4 -C 18 Alkyl esters, methacrylic acid C 4 -C 18 Alkyl esters, styrene, alkylstyrenes and mixtures thereof. Such as butyl acrylate, isooctyl acrylate, n-octyl acrylate, n-hexyl acrylate, nonyl acrylate, decyl acrylate, isodecyl acrylate, dodecyl acrylate, tetradecyl acrylate, hexyl methacrylate, isooctyl methacrylate, decyl methacrylate, isodecyl methacrylate, dodecyl methacrylate, tetradecyl methacrylate or octadecyl methacrylate; the monomer component may also contain water insoluble comonomers such as vinyl chloride, isoprene or chloroprene.
ii) from 5% to 40% by weight, based on the total weight of monomers contained in the oil phase, of at least one substantially water-insoluble polyfunctional crosslinking agent; for example, including but not limited to, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40% by weight of the total monomer weight of at least one substantially water insoluble polyfunctional crosslinker selected from the group consisting of divinyl aromatics, diacrylates or dimethacrylates of polyols, and mixtures thereof; more preferably, 10% to 30% by weight of a multifunctional crosslinker selected from any one of divinylbenzene, trivinylbenzene, divinyltoluene, divinylxylene, 1, 4-ethyleneglycol dimethacrylate, 1, 6-hexanediol dimethacrylate, ethyleneglycol dimethacrylate, hexanediol dimethacrylate, and the like, or a mixture of these components, the crosslinker component being capable of providing the desired elasticity and strength of the material.
In step (1), the oil phase comprises 1% -20% by weight of the total weight of the oil phase of an emulsifier component which is soluble in the oil phase and forms a stable water-in-oil emulsion, including but not limited to 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%, 16%, 17%, 18%, 19%, 20% by weight of the total oil phase of an emulsifier component which is soluble in the oil phase and forms a stable water-in-oil emulsion, in particular the oil soluble emulsifier is selected from branched or linear C 16 -C 24 Fatty acid glycerides, branched or straight chain C 16 -C 24 Fatty acid sorbitan fatty acid esters, sucrose fatty acid esters, alkylphenol ethoxylates, or mixtures of these components, such as sorbitan monooleate, sorbitan laurate, bis (poly) glyceryl stearate, bis (poly) glyceryl monooleate, polyglyceryl succinate, sucrose stearate, and the like.
In the step (1), the oil phase may further include various fibers, such as cellulose fibers, microcrystalline cellulose, cellulose nanofibers, cotton fibers, wood pulp fibers, various artificial fibers, viscose fibers, and the like, and experiments show that the fiber materials can improve the strength and flexibility of the porous structure material, have high strength while the thickness of the material is very thin, and enhance the use strength of the thinner mask substrate.
In the step (2), the mixing shear speed of the oil phase and the water phase is 50 rpm-5000 rpm, including, but not limited to, 50rpm, 100rpm, 300rpm, 500rpm, 700rpm, 900rpm, 1100rpm, 1300rpm, 1500rpm, 1700rpm, 1900rpm, 2000rpm,3000rpm, 4000rpm, 5000rpm, more preferably, the mixing shear speed is 200-1500 rpm; the mass ratio of the volume of the water phase to the oil phase is 20 mL-40 mL:1g, for example, includes but is not limited to 10mL:1g, 15mL:1g, 20mL:1g, 25mL:1g, 30mL:1g, 35mL:1g, 40mL:1g; more preferably, the mass ratio of the volume of the aqueous phase to the oil phase is 20mL:1 g-30 mL:1g.
In the step (2), the aqueous phase contains 0.5% -15% of water-soluble electrolyte by weight, for example, including but not limited to 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15% of water-soluble electrolyte by weight, and the electrolyte is inorganic water-soluble salt selected from calcium chloride, magnesium chloride, or magnesium sulfate and calcium sulfate. The water-soluble electrolyte can minimize the solubility of the monomer and the crosslinking agent in water, and the size and the number of the material foam holes can be controlled by adjusting the addition amount of the electrolyte.
In the step (2), the aqueous phase contains 1% -10% of water-soluble or oil-soluble initiator, including but not limited to 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10% of water-soluble or oil-soluble initiator, wherein the initiator is selected from photoinitiator or thermal initiator or redox pair initiator, and the optional photoinitiator is selected from benzophenone, alpha-hydroxyalkyl acetone (trade name 1173), benzyl ketal, alpha-amino alkyl benzophenone, acyl phosphine oxide, etc.; or a thermal initiator such as persulfate or azobisiso Ding Mi hydrochloride, e.g., ammonium persulfate, sodium persulfate, potassium persulfate, azobisisobutylimidine hydrochloride, azobisiso Ding Mi hydrochloride, etc., and may also be selected from at least any one of redox initiation systems, e.g., sodium persulfate, ammonium persulfate, potassium persulfate, azobisisobutylimidine hydrochloride, azobisiso Ding Mi hydrochloride, or persulfate-sodium bisulfite, persulfate-ascorbic acid, persulfate-sodium thiosulfate, etc.; preferably selected from photoinitiators comprising: benzophenone, 1-hydroxycyclohexyl phenyl ketone (trade name 184), 2-methyl-2- (4-morpholino) -1- [4- (methylthio) phenyl ] -1-propanone, 2-isopropylthioxanthone, α -hydroxyalkyl acetones (trade name 1173), benzyl ketal, α -aminoalkylphenones, and acylphosphine oxides (e.g., TPO) and the like which are soluble in the oil phase; or may be 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone, 2-azobis [2- (2-imidazolin-2-yl) propane ] dihydrochloride or sulfate, thioxanthone derivatives (such as trade name TX) etc. dissolved in the aqueous phase; preferably in the present invention the initiator is a persulfate initiator.
Wherein in the step (3), the emulsified high internal phase emulsion prepared in the step (2) is coated in a container made of polymethyl methacrylate or polyethylene or polypropylene or polytetrafluoroethylene at a thickness of 0.05-1 mm, and then is cured in an oven or water bath or a UV box, preferably at a curing temperature of 45-120 ℃ for 5 s-30 min, preferably 30 s-10 min, and after curing, the monomer conversion rate (calculated according to the mass percent of unreacted residual monomers in total monomers) in an oil phase is not less than 85%.
In the step (3), the high internal phase emulsion prepared in the step (2) can be directly coated on non-woven fabrics fiber nets/cloths made of various materials, so that a porous structure material with improved strength and toughness can be obtained.
In the step (4), the solidified porous structure material is washed with deionized water, and then is extrusion dehydrated by a press roll, and the washing and extrusion dehydration processes can be repeated several times, for example, 1 time, 2 times, 3 times, 4 times, 5 times or more, and the water content of the porous structure material after extrusion dehydration is not higher than 20% of the weight of the porous structure material.
In the step (4), the porous structure material after one or more times of washing, extrusion and dehydration can be directly immersed into the facial mask essence with the viscosity range of 50 cp-10000 cp to be absorbed to saturation, and the thickness of the facial mask after the absorption and saturation is 0.05-1 mm.
The invention discloses a preparation method of a porous structure material prepared from high internal phase emulsion for a patch type mask substrate and application of the porous structure material as the mask substrate, wherein the porous structure material has good absorption performance and high porosity, can be used as the mask substrate, has outstanding liquid carrying rate, liquid retention capacity and good air permeability, has good absorption performance for mask essence in a wider viscosity range, and has better comprehensive performance compared with the traditional mask substrate such as non-woven fabrics, pure cotton fibers, hydrogel, silk, tencel and the like, and has balanced absorption performance, skin fit performance, air permeability and the like. When the hydrophobic modified nano zinc oxide is added to prepare High Internal Phase Pickering Emulsion (HIPPE), the porous structure material obtained after solidification has good antibacterial and bacteriostatic effects under the action of the modified zinc oxide, and the addition amount of the preservative can be avoided or greatly reduced, so that the skin irritation and sensitization are reduced, and the comprehensive advantages are more obvious compared with the traditional base material.
All the raw materials of the invention are not particularly specified and can be purchased from the market.
The properties of the porous materials and masks prepared therefrom prepared in the present invention were tested and characterized using the methods described below:
A) Determination of material thickness
And (3) measuring a material sample saturated by absorbing the No. 1 mask liquid by adopting a sponge material thickness measuring instrument, taking measurements at different positions for 3 times, and taking an average value.
B) Determination of number average cell diameter
The size of the cells of the porous material is measured by adopting a Scanning Electron Microscope (SEM), the porous material is subjected to electron microscope test after being thoroughly dried, at least more than 50 cell diameters are measured in a proper visual field range, and the average value of the cell diameters is the number average cell diameter of the sample.
C) Determination of porosity
The porosity of the porous material samples was tested using the following method:
the extruded and dehydrated samples (unabsorbed mask essence) were measured with calipers for 3 samples of 5cm long by 5cm wide, the thickness of each sample was obtained by the method in a), the weight of each sample was weighed, the samples were placed in a closed container containing 2-propanol at room temperature, immersed for 0.5 hour, taken out, and weighed when the samples were no longer dripped with liquid, the porosity = (mass of sample after absorption of 2-propanol-mass of sample before absorption)/(density of 2-propanol × sample volume) × 100%.
The porosity of nonwoven fabrics, tencel or other fiber nonwoven materials is tested by a mass density method, namely, the actual volume of the fiber is obtained by utilizing the ratio of the material surface density to the fiber density, and then the porosity is obtained:
Porosity=1-m/(ρδ)
m is the surface density of the material, g/m 2 ；
ρ is the fiber density, g/cm 3 ；
Delta is the material thickness, mm.
D) Measurement of liquid carrying Rate
The liquid carrying rate of the mask substrate is characterized in that the substrate has the liquid carrying capacity of absorbing the essence of the mask, if the liquid carrying capacity of the mask is low, the absorbed essence is less, a lot of essence can be remained in the packaging bag when the mask is used, the mask is easy to drip, and the utilization rate of the essence is low. Measurement of the liquid carrying Rate Each sample was cut to a size of 10cm by 10cm with reference to GB/T24218.6-2010 test, and the initial weight M of each sample was weighed 0 Immersing the mask in the mask essence for 60 s, taking out, hanging vertically for 120s, and weighing M 1 . Fluid carrying rate= (M 1 -M 0 )/M 0 *100% per sample, three times, and the results averaged.
E) Testing of liquid retention
The samples were cut into 6.5 x 6.5cm size samples and weighed M 0 Immersing a sample in the mask liquid for 2min, taking out, hanging vertically for 1min, and weighing M 1 Immediately placing in YG601H moisture permeable instrument of Ningbo Dahe Instrument Co., ltd at 37deg.C and 65% RH for 20min, taking out and weighing M 2 Each sample was tested in triplicate and averaged. Retention = (M 2 -M 0 )/(M 1 -M 0 )*100％。
F) Air permeability test
Air permeability determination method in reference standard GB/T24218.15-2018 by utilizing Laizhou electronics YG461 type full-automatic air permeability tester of instrument factory tests air permeability of sample at 20deg.C and 65% humidity, sets testing pressure difference parameter to 50Pa, and testing area to 20cm 2 . And 5 positions are randomly selected for each sample, the test part of the sample is kept as smooth as possible and is not pulled by force, and the test result is averaged.
G) Determination of the bacteriostatic Rate
Referring to the antibacterial experiments of the shake test samples provided in GBT 20944.3-2008, after 18h of shake contact, the antibacterial rate was calculated by comparing the live bacteria concentrations in the control and antibacterial fabric sample flasks. The sample was cut into 5.0mm х and 5.0mm specifications for testing, and staphylococcus aureus was selected as the test bacteria. The test was repeated 3 times, and the bacteriostasis rate was calculated and the average value was taken.
Antibacterial ratio= (number of viable bacteria recovered in blank control-number of viable bacteria recovered in sample)/number of viable bacteria recovered in blank control ×100%.
H) Determination of flexural rigidity
Referring to GB/T18318.1-2009, the flexural rigidity in the transverse and longitudinal directions of the material absorbing No. 1 mask liquid (refer to table 1) was tested by a bevel method using a bending tester model KES-FB2-a of Kato Tech co, the absorption mask sample was cut into 200mm samples, and the test was performed with an accuracy of 0.01gf cm 2 Each sample was tested three times in the transverse and longitudinal directions and the results averaged.
I) Determination of glass transition temperature Tg
The glass transition temperature characterizes the mechanical properties of the polymer, and in the invention, the TG of the HIPE foam is tested by Thermal Mechanical Analysis (TMA), and a METTLER TMA/SDTA instrument (compression mode) is used for cutting the foam sample into cuboid sample pieces with the thickness of 10mm multiplied by 5mm multiplied by 3mm, so that the upper surface and the lower surface are smooth. And placing the sample on an inner bracket of the instrument, placing a quartz gasket on the upper surface of the sample, lowering the probe, and starting the test.
The technical scheme of the present invention is further described below with reference to specific examples, but is not limited in any way.
The mask essence adopted in the experiment of the invention comprises the following components:
table 1 mask essence base formulation
Example 1
A) Preparation of HIPPE emulsions
An oil phase of stearic acid modified nano zinc oxide (available from darcy nanotechnology limited, 50nm,0.1 g) with isooctyl acrylate (15.5 g), styrene (0.5 g), ethylene glycol dimethacrylate (4.0 g), benzophenone (0.7 g) with citrol DPHS (PEG-30 dimer hydroxystearate available from CRODA,1.5 g) was obtained as a homogeneous oil phase. The aqueous phase was prepared by dissolving calcium chloride (7.6 g) in 560 ml deionized water.
Placing the obtained oil phase into a polypropylene container with a volume of 1 liter, stirring the oil phase by using an IKA stirrer, wherein the stirring paddle is an anchor stirring paddle made of polytetrafluoroethylene, the total length of the paddle is about 5 cm, stirring the oil phase at a rotating speed of 100 revolutions per minute is started, simultaneously adding all water phases within 5 minutes, preheating the water phases to 60 ℃ in advance, adding circulating water outside a dispersing container for heat preservation, and setting the temperature of the circulating water to 60 ℃; the stirring speed is gradually increased along with the addition of the water phase, and the rotating speed is about 400 rpm after the addition of the whole water phase, so that the stable high internal phase emulsion without layering is formed.
B) Curing of high internal phase emulsions
The prepared high internal phase emulsion was coated to a thickness of 0.3 mm. And (5) after coating, putting the film into a UV box for illumination, and taking out after 30 s.
C) Washing and dewatering treatment
Washing the solidified material with deionized water to remove residual emulsifying agent and inorganic salt, and squeezing to dewater, wherein the washing and squeezing dewatering process can be repeated for several times according to actual conditions.
D) Mask preparation
Cutting the dehydrated materials into the same size, respectively soaking in the mask liquid 1#, mask liquid 2# and mask liquid 3# to be absorbed until saturation.
Example 2
A) Preparation of high internal phase emulsions
Isooctyl acrylate (13.0 g), isooctyl methacrylate (4.0 g), 1, 4-butanediol dimethacrylate (3.0 g) and sucrose fatty acid ester S-370 (available from Mitsubishi chemical, 2.9 g) were mixed to give a homogeneous oil phase. Sodium chloride (12.2 g) was dissolved in 500 ml deionized water to prepare an aqueous phase. 0.9 g of sodium persulfate was dissolved in 15 ml of deionized water to obtain an initiator phase.
Placing the obtained oil phase into a polypropylene container with a volume of 1 liter, stirring the oil phase by using an IKA stirrer, wherein the stirring paddle is an anchor stirring paddle made of polytetrafluoroethylene, the total length of the paddle is about 5 cm, stirring the oil phase at a rotating speed of 200 revolutions per minute is started, simultaneously adding all water phases within 5 minutes, preheating the water phases to 65 ℃ in advance, adding circulating water outside a dispersing container for heat preservation, and setting the circulating water to 55 ℃; the stirring speed is gradually increased along with the addition of the water phase, and the rotating speed is about 500 rpm after the addition of the whole water phase, so that stable and delamination-free high internal phase emulsion is formed.
B) Curing of high internal phase emulsions
The prepared high internal phase emulsion was coated to a film thickness of 0.36 mm, and then put into an oven at 100℃for 20 minutes and taken out.
The subsequent treatment conditions and the mask preparation method are completely the same as those in example 1.
Example 3
A) Preparation of high internal phase Pickering emulsion
Lauric acid modified nano zinc oxide (available from darcy concentrated nanotechnology limited, 30nm,0.08 g) was combined with an oil phase of isodecyl acrylate (13.0 g), isooctyl methacrylate (1.0 g), divinylbenzene (6.0 g), glycerol succinate (available from national medicine, 1.7 g) and 1173 (0.86 g) to give a homogeneous oil phase. The aqueous phase was prepared by dissolving calcium chloride (18.1 g) in 680 ml deionized water.
Placing the obtained oil phase into a polypropylene container with a volume of 1 liter, stirring the oil phase by using an IKA stirrer, wherein the stirring paddle is an anchor stirring paddle made of polytetrafluoroethylene, the total length of the paddle is about 5 cm, stirring the oil phase at a rotating speed of 180 revolutions per minute is started, simultaneously adding all water phases within 5 minutes, preheating the water phases to 70 ℃ in advance, adding circulating water outside a dispersing container for heat preservation, and setting the circulating water to 70 ℃; the stirring speed is gradually increased along with the addition of the water phase, the rotating speed is about 600 rpm after the addition of the whole water phase, and the initiator solution is added and stirred for 1-3 minutes after the formation of stable and delamination-free high internal phase emulsion.
B) Curing of high internal phase emulsions
The prepared high internal phase emulsion was coated to a film thickness of 0.5 mm, and then placed in a UV box for 60 seconds and taken out.
The subsequent treatment conditions and the mask preparation method are completely the same as those in example 1.
Example 4
A) Preparation of HIPPE emulsions
Silane coupling agent KH-570 modified nano zinc oxide (30 nm,0.28 g, available from Yumu New Material Co., ltd.) and ultrasonic dispersion were mixed in an oil phase mixed with octadecyl methacrylate (13.0 g), trimethylolpropane triacrylate (7.0 g), span 80 (1.93 g), benzophenone (0.89 g) to obtain a uniform oil phase. Calcium chloride (5.0 g) was dissolved in 650 ml deionized water to prepare an aqueous phase.
Placing the obtained oil phase into a polypropylene container with a volume of 1 liter, stirring the oil phase by using an IKA stirrer, wherein the stirring paddle is an anchor stirring paddle made of polytetrafluoroethylene, the total length of the paddle is about 5 cm, stirring the oil phase at a rotating speed of 140 revolutions per minute is started, simultaneously adding all water phases within 5 minutes, preheating the water phases to 60 ℃ in advance, adding circulating water outside a dispersing container for heat preservation, and setting the temperature of the circulating water to 60 ℃; the stirring speed is gradually increased along with the addition of the water phase, the rotating speed is about 500 r/min after the addition of the whole water phase, and the initiator solution is added and stirred for 1-3 min after the stable and delamination-free high internal phase emulsion is formed.
B) Curing of high internal phase emulsions
The high internal phase emulsion prepared was coated to a thickness of 0.56 mm. And (5) placing the curing mold into a UV box for illumination for 60 seconds, and taking out.
The subsequent treatment conditions and the mask preparation method are completely the same as those in example 1.
Example 5
A) Preparation of high internal phase Pickering emulsion
Microcrystalline cellulose (from Kain, shanghai, 0.11 g) was dispersed in a mixture of isooctyl acrylate (12.5 g), isooctyl methacrylate (1.0 g), 1, 6-hexanediol dimethacrylate (6.5 g) and triglyceryl stearate (2.3 g, from Guo Yao Chemicals), benzophenone (0.9 g) to give a homogeneous oil phase. An aqueous phase was prepared by dissolving calcium chloride (10.0 g) in 550 ml deionized water.
Placing the obtained oil phase into a polypropylene container with a volume of 1 liter, stirring the oil phase by using an IKA stirrer, wherein the stirring paddle is an anchor stirring paddle made of polytetrafluoroethylene, the total length of the paddle is about 5 cm, stirring the oil phase at a rotating speed of 100 revolutions per minute is started, simultaneously adding all water phase within 5 minutes, preheating the water phase to 76 ℃ in advance, adding circulating water outside a dispersing container for heat preservation, and setting the temperature of the circulating water to 76 ℃; the stirring speed is gradually increased along with the addition of the water phase, and the rotating speed is about 600 rpm after the addition of the whole water phase, so that the stable high internal phase emulsion without layering is formed.
B) Curing of high internal phase emulsions
The prepared high internal phase emulsion was coated at a thickness of 0.65mm at 30g/m 2 And (3) the polypropylene nonwoven fabric web is placed in a UV box to be irradiated for 60 seconds and then taken out.
The subsequent treatment conditions and the mask preparation method are completely the same as those in example 1.
Example 6
A) Preparation of high internal phase Pickering emulsion
Microcrystalline cellulose (0.1 g), stearic acid modified nano zinc oxide (0.2 g) were dispersed in a mixture of isooctyl acrylate (13.0 g), isooctyl methacrylate (4.0 g), 1, 4-butanediol dimethacrylate (3.0 g) and SPAN 80 (2.9 g) to give a homogeneous oil phase. The aqueous phase was prepared by dissolving calcium chloride (11.5 g) in 680 ml deionized water. 0.9 g of sodium persulfate was dissolved in 10 ml of water to obtain an initiation phase.
Placing the obtained oil phase into a polypropylene container with a volume of 1 liter, stirring the oil phase by using an IKA stirrer, wherein the stirring paddle is an anchor stirring paddle made of polytetrafluoroethylene, the total length of the paddle is about 5 cm, stirring the oil phase at a rotating speed of 100 revolutions per minute is started, simultaneously adding all water phase within 5 minutes, preheating the water phase to 62 ℃ in advance, adding circulating water outside a dispersing container for heat preservation, and setting the circulating water to 62 ℃; the stirring speed is gradually increased along with the addition of the water phase, the rotating speed is about 600 rpm after the addition of the whole water phase, and the stirring is carried out for 1-3 minutes after the addition of the initiator solution, so that the stable high internal phase emulsion without layering is formed.
B) Curing of high internal phase emulsions
The high internal phase emulsion prepared was coated at a thickness of 0.5mm at 30g/m 2 The polypropylene nonwoven fabric web of (2) was placed in an oven at 90℃for 30 minutes and then taken out.
The subsequent treatment conditions and the mask preparation method are completely the same as those in example 1.
Comparative examples 1 to 6
The mask base cloth such as the commercially available spun-bonded non-woven fabrics, pure cotton fibers, silk fibers, hydrogel, tencel and cuprammonium fibers is used as a comparative example 1 to 6, and is respectively cut into the same size specification and then immersed into the mask liquid of No. 1, no. 2 and No. 3 to be soaked and absorbed until saturation.
Table 2 absorbency against different facial mask essences
The porous structure material prepared from the high internal phase emulsion has very high absorption capacity and liquid retention capacity for different viscosities, especially for the high viscosity mask liquid, so that the full utilization of the mask liquid and a wider blending range are ensured; as can be seen from comparative examples 1 to 6, the conventional mask base material increases in viscosity, the liquid carrying rate and the liquid retaining amount when the viscosity of the mask liquid is low, and decreases in both the liquid carrying rate and the liquid retaining amount when the viscosity of the mask liquid is high (from 2# to 3 #), because the base material adheres and absorbs more mask liquid when the viscosity of the mask liquid is low, but the diffusion of liquid into the inside of the base material is affected when the viscosity of the mask liquid is high, and the porous structure material has a microstructure in which the pores communicate with each other due to the unique bubble connection thereof, and referring to the SEM diagram of the structure of FIG. 1, the unique structure enables the material to have a good liquid carrying rate and liquid retaining amount when the viscosity of the mask liquid is high.
TABLE 3 other Properties
As can be seen from Table 3, the porous structure material has a plurality of window holes on each cell in the structure, and the high-porosity structure enables the material to have good air permeability when the number average cell diameter is not required to be large, so that the porous structure material has higher porosity and better air permeability compared with the surface film base fabrics such as spunbonded non-woven fabrics, pure cotton fibers, hydrogels and the like. The softness of the base cloth is reflected by the bending stiffness, the softness is worse as the bending stiffness is larger, the poor skin fit degree is shown in experience sense, the foaming is realized, and compared with the traditional spun-bonded non-woven fabrics and pure cotton fibers, the porous structure material has better softness and similar softness to the hydrogel mask base material. When the porous material is obtained by curing HIPPE emulsion prepared by nano zinc oxide, the material has good antibacterial effect, and it can be seen that the antibacterial effect of the mask in examples 1, 3 and 4 is 0 when the mask liquid does not contain antibacterial agent, and the antibacterial effect of the mask in other examples and comparative examples which do not contain nano zinc oxide is still good. In addition, in example 5, the porous structure material was compounded on the nonwoven fabric web, so that the obtained mask base fabric had higher bending rigidity, lower softness and higher strength.
By analyzing the performances of the mask with different base materials according to the comprehensive table 2 and table 3, the porous structure material can be found to have very high liquid carrying rate and liquid retention capacity for mask liquid with different viscosity ranges, and meanwhile, the porous structure material has good skin adhesion degree and good air permeability, and can achieve the purpose of self-carrying antibacterial effect by adding modified nano zinc oxide, so that the porous structure material has better comprehensive performance compared with the conventional mask base cloth on the market.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Those skilled in the art will appreciate that certain modifications and adaptations of the invention are possible and can be made under the teaching of the present specification. Such modifications and adaptations are intended to be within the scope of the present invention as defined in the appended claims.
Claims (16)
1. A porous structure material for a patch type mask substrate is characterized in that the porous structure material is obtained by water-in-oil type high internal phase emulsion polymerization, the number average pore size of the porous structure material is 1-100 mu m, the porosity is not less than 60%, the thickness after wet saturation is not more than 1mm, and the transverse and longitudinal bending rigidity of the porous structure material is not more than 0.2gf cm 2 /cm；
When the porous structure material is used as a mask base material, the liquid carrying rate of the mask liquid with different viscosities is not lower than 1000%, and the liquid retention rate of the mask liquid with different viscosities is not lower than 80%;
the preparation method of the patch type mask comprises the following steps:
1) Preparing water-in-oil emulsion containing the following oil phases, forming the oil phases into uniform oil phases under the shearing and dispersing effects, and maintaining the temperature of the oil phases at 20-90 ℃; wherein, based on the total weight of the oil phase, the oil phase comprises:
a) 80% to 99% by weight of a substantially water insoluble monomer component;
b) 1-20% by weight of an emulsifier component which is soluble in the oil phase and which forms a stable water-in-oil emulsion;
2) The water phase contains 0.5-15 wt% of water-soluble inorganic salt based on the total weight of the water phase, and the temperature of the water phase is maintained at 20-90 ℃;
3) Gradually adding the water phase into the oil phase under the shearing action to emulsify the water phase into stable HIPPE emulsion;
4) Solidifying the water-in-oil emulsion to form a porous structure material;
5) Washing, squeezing and dehydrating the solidified porous material, directly immersing the porous material into a pre-prepared mask essence without drying, and soaking the porous material until saturated absorption is achieved, thus obtaining the mask.
2. The porous structure material for a patch-type mask substrate according to claim 1, wherein the porous structure material has a number average cell pore size of 1 to 50 μm, a porosity of 70% to 90%, a thickness after wet saturation of 0.05 to 1mm, and a transverse and longitudinal flexural rigidity of 0.001 to 0.2gf x cm 2 /cm。
3. The porous structure material for a patch-type mask base material according to claim 1 or 2, wherein the liquid carrying rate of the mask liquid with different viscosities is 1000% -3000% when the porous structure material is used as a mask base material.
4. The porous structure material for a patch-type mask base material according to claim 1 or 2, wherein the liquid retention rate of the mask liquid with different viscosities is 80% -95% when the porous structure material is used as a mask base material.
5. The porous structure material for a patch-type mask substrate according to claim 1, wherein the step 2) further comprises a water-soluble or oil-soluble initiator accounting for 1% -10% of the total weight of the monomers of the oil phase, based on the total weight of the monomers.
6. The porous structure material for a patch mask substrate according to claim 1, wherein the shearing in the step 3) is performed at a shearing speed of 50rpm to 5000 rpm.
7. The porous structure material for a patch type mask substrate according to claim 1, wherein the step 4) is to coat the emulsified hipe emulsion with a thickness of 0.05-1 mm and then cure it in an oven or water bath or UV box.
8. The porous structure material for a patch mask substrate according to claim 7, wherein the curing temperature is 45 ℃ to 120 ℃ and the curing time is 5s to 30min.
9. The porous structure material for a patch mask substrate according to claim 1, wherein the mass ratio of the volume of the water phase to the oil phase in the hipe emulsion in the step 3) is not less than 20mL:1g.
10. The porous structure material for the patch mask substrate according to claim 9, wherein the mass ratio of the volume of the water phase to the oil phase in the hipe emulsion in the step 3) is 20ml to 40ml:1g.
11. The porous structure material for a patch-type mask substrate according to claim 1, wherein the monomer component in the step 1) is selected from alkyl acrylate monomers or alkylstyrene monomers containing one or more carbon-carbon double bonds.
12. The porous structure material for a patch-type mask substrate according to claim 11, wherein the oil phase a) further comprises 0 to 3% of hydrophobically modified nano zinc oxide based on the total weight of the oil phase.
13. The porous structure material for a patch type mask substrate according to claim 1, wherein the oil phase a) further comprises cellulose nanoparticles, and the addition amount of the cellulose nanoparticles is 0% -2% of the total weight of the oil phase.
14. The porous structure material for a patch-type mask substrate according to claim 13, wherein the cellulose nanoparticle is selected from any one of cellulose nanocrystals, microcrystalline cellulose, cellulose nanofibers, nanocrystalline cellulose, nanocellulose.
15. The porous structure material for a patch-type mask substrate according to claim 1, wherein the glass transition temperature of the porous structure material after the curing in the step 5) is in the range of-30 ℃ to 25 ℃.
16. A patch-type mask, characterized by being made of a porous structure material for a patch-type mask base material according to any one of claims 1 to 15.
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| EP3433306B1 (en) * | 2016-03-21 | 2022-06-08 | The Procter & Gamble Company | High internal phase emulsion foam having cellulose nanoparticles |
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| US5147345A (en) * | 1991-08-12 | 1992-09-15 | The Procter & Gamble Company | High efficiency absorbent articles for incontinence management |
| CN1433444A (en) * | 2000-06-05 | 2003-07-30 | 陶氏环球技术公司 | Continuous process for polymerizing, curing and drying high internal phase emulsions |
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