CN109208106A - A kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric - Google Patents

A kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric Download PDF

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CN109208106A
CN109208106A CN201810994534.9A CN201810994534A CN109208106A CN 109208106 A CN109208106 A CN 109208106A CN 201810994534 A CN201810994534 A CN 201810994534A CN 109208106 A CN109208106 A CN 109208106A
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collagen
facial mask
temperature
parts
superpro
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胡次兵
蒋东明
赵金晶
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Foshan Science And Technology Co Ltd
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Foshan Science And Technology Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0208Tissues; Wipes; Patches
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/65Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives

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  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
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  • Biotechnology (AREA)
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Abstract

The present invention relates to a kind of preparation methods rich in collagen SuperPro outlet capacity facial mask fabric, belong to skincare product preparation technical field.The present invention obtains filtrate by raw material of Garlic Seeds, again pigskin and fish tail are impregnated to obtain viscosity solution in n-butanol and acetic acid, obtained oxidation product is mixed with viscosity solution, electrostatic spinning, it is made and is rich in collagen SuperPro outlet capacity facial mask fabric, there are antibacterial substances in organic substance in Garlic Seeds, it can play the role of to face skin clean, certain antisepsis is played to fabric simultaneously, and to fiber each in fabric, molecule has strong cohesive property energy, the good hydrophily of graphene oxide, the collagen of extraction is adsorbed in surface of graphene oxide, effectively contact area of the enhancing collagen to external environment, to enhance collagen to the repairing effect of face skin, it has broad application prospects.

Description

A kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric
Technical field
The present invention relates to a kind of preparation methods rich in collagen SuperPro outlet capacity facial mask fabric, belong to skincare product Preparation technical field.
Background technique
Facial mask is one of the important composition of the daily skin nursing of women.Its principle is exactly to utilize to be covered on the of short duration of face Time is temporarily isolating extraneous air and pollution, improves skin temperature, expand the pore of skin, promote sweat gland secretion with newly Old metabolism rises the oxygen content of skin, is conducive to skin and excludes the product of epidermal cell metabolism and the grease type of accumulation Substance, the moisture in facial mask go deep into the cuticula of epidermis, and skin is made to become soft, and light is flexible naturally for skin.
Currently, by texture grading, facial mask is broadly divided into pureed facial mask, membranaceous facial mask there are many kinds of facial masks on the market With 3 class of skin care products facial mask.Pureed facial mask has the function of absorption grease, after use mostly using kaolin, green clay as main component It can feel that skin is salubriouser, accelerate metabolism aging cutin and acne etc..Membranaceous facial mask majority is using some stationeries, does not knit Cloth, biological fiber etc. are substrate, discharge various Essences to skin, utilize the characteristic that " film " is airtight, keeps the temperature, and skin is accelerated to inhale Receive the ability of skin care products.For this facial mask of skin care products facial mask like general skin care products, some is in gel, some presentation emulsion forms Or creams shape, it is desirable that directly very thin one layer of smearing on the face, is having moisturizing, nourishing, conditioning functions.
Currently, the mounted facial mask of makeups is just increasingly liked that mounted facial mask is mainly impregnated by mask substrate by consumer It is constituted in Essence.General Requirement to mask substrate be soft comfortable, it is conformable it is good, it is frivolous it is transparent, moisture retention is strong, because This, the mask substrate of mainstream is to be prepared by regenerated celulose fibre such as copper ammonia fiber, tencel etc. through spunlace non-woven cloth technique, facial mask Base fabric plays the role of Essence carrier, and essence used then usually by water, glycerine, hyaluronic acid, xanthan gum and other Effective component composition.
But since existing face mask substrate material is developed by clothings fabrics such as cotton fiber, viscose rayon, copper ammonia fiber base fabrics And come, it needs in production process using a large amount of chemical reagent, is remained on the basic material of facial mask more, and tencel fiber etc. is pure Biological fiber is also required to that a large amount of anticorrosive additive is added when in use, and the poor biocompatibility of these substances easily causes Skin sensitivity, shouting pain and redness, Long Term Contact skin may make skin be damaged.Face mask substrate material patch skin performance is general, facial mask After being attached on the face, the one side of facial mask and skin attachement, nutrient solution can be absorbed by the skin, but facial mask is backwards to the one of skin Face, nutrient solution distribute more serious, reduce the using effect of nutrient solution.In addition, this kind of facial mask there is also ductility bad, water holding Performance is poor, does not have the defect of radiation protection, and the abandon after also can cause environmental pollution, therefore upgrading facial mask face in time The quality of material is only and solves the problems, such as the basic of this.
Therefore it provides a kind of water absorbing and retaining properties are good, the facial mask fabric of pro-skin, no pollution to the environment, there is important theory Meaning and application value.
Summary of the invention
The technical problems to be solved by the invention, for current facial mask fabric fungistatic effect difference cause facial mask antiseptic property compared with Difference, while insufficient, nutritional ingredient provides one kind and is rich in the defect of facial skin repair effect difference for fabric water retention property The preparation method of collagen SuperPro outlet capacity facial mask fabric.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric, it is characterised in that specific preparation step are as follows:
(1) 500~700g Garlic Seeds are weighed to be put into beaker, with distillation water retting Garlic Seeds, are placed the beaker permanent in water-bath Warm water boils, and is cooled to room temperature after boiling, and salt acid for adjusting pH value is added dropwise to 5~6, stands 6~8h under room temperature, is obtained by filtration after standing Filtrate is spare;
(2) pigskin and fish tail are cut into pieces and is uniformly mixed obtained hybrid solid in the investment four-hole boiling flask of 3 ︰ 1 in mass ratio, with steaming Distilled water impregnates hybrid solid, and sodium hydroxide solution is added dropwise into four-hole boiling flask and adjusts pH value to 8~9, increases four mouthfuls with heating mantle Filter residue is obtained by filtration with blender to be mixed in temperature in flask after stirring;
(3) according to parts by weight, 3~5 parts of above-mentioned filter residues, 12~15 parts of n-butanols and 22~25 parts of acetic acid solution investments are weighed to burn In cup, sonic oscillation in sonic oscillation instrument is placed the beaker, sticky filtrate is obtained by filtration, sticky filtrate and spare filtrate are pressed 1 ︰ 3 of mass ratio, which puts into be mixed in high speed dispersion instrument, is made mixed serum, and mixed serum is put into Rotary Evaporators and is concentrated To constant weight, viscosity solution is obtained, it is spare;
(4) according to parts by weight, 3~5 parts of graphite powders, 15~17 potassium permanganate powders and 110~115 parts of sulfuric acid solutions are weighed to throw Enter in three-necked flask, three-necked flask is placed in ice-water bath, stirred with blender, bath temperature is increased, carries out constant-temperature condensation Suspension is made in reflux;
(5) hydrogen peroxide with quality such as suspensions is added into above-mentioned three-necked flask, constant temperature stands 30~40min, is obtained by filtration Filter residue is reacted, successively cleans reaction filter residue 3~5 times with hydrochloric acid and distilled water, temperature drying to constant weight is put into and obtains oxidized solid;
(6) above-mentioned oxidized solid and spare viscosity solution 1 ︰ 20 in mass ratio are put into beaker, places the beaker ultrasonic vibration It swings the obtained solidliquid mixture of sonic oscillation in instrument and weighs 7~9 parts of solidliquid mixtures, 1.2~1.6 portions of lemons according to parts by weight It is stirred in sour sodium and 15~17 parts of ethanol solution investment high speed dispersion instrument, mixed liquor is made, mixed liquor is injected into Electrospun Composite fibre is made in machine, composite fibre is put into vacuum oven, is made superpower rich in collagen under normal temperature conditions Water lock ability facial mask fabric.
The bath temperature of water-bath as described in step (1) is 95~100 DEG C, and the constant temperature boiling time is 3~4h, hydrochloric acid Mass fraction is 6~10%.
The mass fraction of sodium hydroxide solution described in step (2) is 10~15%, four-hole boiling flask temperature is increased to 50~ 55 DEG C, the revolving speed of blender is 300~330r/min, and mixing time is 2~3h.
The mass fraction of acetic acid solution described in step (3) is 30~40%, the frequency in sonic oscillation instrument is 40~ 45kHz, sonic oscillation time are 3~5h, and the revolving speed in high speed dispersion instrument is 1300~1400r/min, and mixing time is 30~40min, the temperature in Rotary Evaporators are 40~45 DEG C.
The mass fraction of sulfuric acid solution described in step (4) is 80~90%, and the revolving speed of blender is 200~220r/ Min, mixing time are 100~120min, and bath temperature is increased to 40~45 DEG C, and constant-temperature condensation return time is 12~13h.
The mass fraction of hydrogen peroxide described in step (5) is 10~15%, and the mass fraction of hydrochloric acid is 10~15%, baking oven In temperature be 105~110 DEG C.
Frequency in sonic oscillation instrument described in step (6) is 40~42kHz, and the sonic oscillation time is made for 5~6h Solidliquid mixture, the mass fraction of ethanol solution are 30~35%, and the revolving speed in high speed dispersion instrument is 1500~1600r/min, are stirred Mixing incorporation time is 60~80min, and the flow velocity in Electrospun machine is 2~4mL/h, and voltage is 60~70V, in vacuum oven Vacuum degree is 80~100Pa, and drying time is 12~14h.
The method have the benefit that:
(1) Garlic Seeds are carried out high temperature boiling, and normal temperature dipping in an acidic solution first by the present invention, and filtrate is obtained by filtration, then Pigskin and fish tail chopping are mixed in lye high temperature to impregnate, filter residue is obtained by filtration after immersion, and impregnated with n-butanol and acetic acid Filter residue, sonic oscillation are simultaneously concentrated obtained viscosity solution, then react graphite powder with potassium permanganate in concentrated sulfuric acid solution, react After filter, be dried to obtain oxidation product, then mix oxidation product with viscosity solution, inject electric spinning machine in electrostatic spinning, do It being made after dry and is rich in collagen SuperPro outlet capacity facial mask fabric, Garlic Seeds are raw material by the present invention, high temperature boiling is carried out, then Soak extraction goes out the organic substance in garlic in an acidic solution, and there are antibacterial substances in these organic substances, can be to face Skin plays the role of clean, while playing certain antisepsis to fabric, hinders corrosion function of the microorganism to fabric, and And itself has the organo-functional groups such as hydroxyl, epoxy group, phenolic hydroxyl group, has strong cohesive property energy to fiber each in fabric, molecule, makes Structure is even closer between each molecule, while these groups have hydrophily, and have certain water retention, and hydrone is inhaled It is attached in facial mask fabric between each molecule, reduces hydrone and air contact area, be more difficult to volatilize, to further add Strong water lock effect;
(2) present invention reacts graphite with potassium permanganate in concentrated sulfuric acid, generates oxidation nanometer grapheme material, graphene oxide Surface has sulfonic acid group, has good hydrophily, extracts collagen from pigskin, fish tail, can pass through collagen It is each intermolecular to enhance that Hydrogen Binding Adsorption, intermolecular force absorption and the absorption of other Chemical bondings are generated to other molecules Bond effect, while being adsorbed in surface of graphene oxide, enhance the mechanical strength of fabric, and formed with graphene oxide micro- Ball effectively enhances collagen to the contact area of external environment, thus enhance collagen to the repairing effect of face skin, It has broad application prospects.
Specific embodiment
It weighs 500~700g Garlic Seeds to be put into beaker, with distillation water retting Garlic Seeds, placing the beaker bath temperature is In 95~100 DEG C of water-bath, constant temperature 3~4h of boiling is cooled to room temperature after boiling, and the salt that mass fraction is 6~10% is added dropwise Acid adjusts pH value to 5~6, and 6~8h is stood under room temperature, filtrate is obtained by filtration after standing, spare;Pigskin is cut into fish tail broken Piece 3 ︰ 1 in mass ratio, which are put into four-hole boiling flask, is uniformly mixed obtained hybrid solid, with distillation water retting hybrid solid, burns to four mouthfuls The sodium hydroxide solution that mass fraction is 10~15% is added dropwise in bottle and adjusts pH value to 8~9, is increased in four-hole boiling flask with heating mantle 2~3h is mixed to 50~55 DEG C, with blender with the revolving speed of 300~330r/min in temperature, and filter residue is obtained by filtration after stirring; According to parts by weight, the second that 3~5 parts of above-mentioned filter residues, 12~15 parts of n-butanols and 22~25 parts of mass fractions are 30~40% is weighed Acid solution is put into beaker, is placed the beaker in sonic oscillation instrument and is vibrated 3~5h with the frequency ultrasound of 40~45kHz, filters To sticky filtrate, sticky filtrate and spare filtrate 1 ︰ 3 in mass ratio are put into high speed dispersion instrument with 1300~1400r/min Revolving speed be mixed 30~40min, be made mixed serum, mixed serum is put into Rotary Evaporators, temperature be 40~ It is concentrated into constant weight under conditions of 45 DEG C, obtains viscosity solution, it is spare;According to parts by weight, 3~5 parts of graphite powders, 15~17 are weighed The sulfuric acid solution that potassium permanganate powder and 110~115 parts of mass fractions are 80~90% is put into three-necked flask, by three-necked flask It is placed in ice-water bath, 100~120min is stirred with the revolving speed of 200~220r/min with blender, bath temperature is increased to 40 ~45 DEG C, suspension is made in constant-temperature condensation 12~13h of reflux;The matter with quality such as suspensions is added into above-mentioned three-necked flask The hydrogen peroxide that score is 10~15% is measured, constant temperature stands 30~40min, reaction filter residue is obtained by filtration, and is successively 10 with mass fraction ~15% hydrochloric acid and distilled water cleaning reaction filter residue 3~5 times is put into baking oven dry to constant weight with 105~110 DEG C of temperature Obtain oxidized solid;Above-mentioned oxidized solid and spare viscosity solution 1 ︰ 20 in mass ratio are put into beaker, placed the beaker In sonic oscillation instrument, the obtained solidliquid mixture of 5~6h is vibrated with the frequency ultrasound of 40~42kHz and weighs 7 according to parts by weight The ethanol solution that~9 parts of solidliquid mixtures, 1.2~1.6 parts of sodium citrates and 15~17 parts of mass fractions are 30~35% puts into high In fast separating apparatus, it is stirred 60~80min under conditions of revolving speed is 1500~1600r/min, mixed liquor is made, will mix Liquid injects in Electrospun machine, composite fibre is made under conditions of flow velocity is 2~4mL/h and voltage is 60~70V, by compound fibre Dimension is put into vacuum oven, and dry 12~14h, which is made, under conditions of room temperature and vacuum degree are 80~100Pa is rich in collagen egg White SuperPro outlet capacity facial mask fabric.
Example 1
It weighs 500g garlic clove to be put into beaker, with distillation water retting garlic clove, places the beaker the water-bath that bath temperature is 95 DEG C In, constant temperature boiling 3h is cooled to room temperature after boiling, the hydrochloric acid that mass fraction is 6% is added dropwise, and adjusts pH value to 5, stands under room temperature Filtrate is obtained by filtration after standing in 6h, spare;Pigskin and fish tail are cut into pieces and mixed in the investment four-hole boiling flask of 3 ︰ 1 in mass ratio The sodium hydroxide that mass fraction is 10% is added dropwise into four-hole boiling flask with distillation water retting hybrid solid for uniformly obtained hybrid solid Solution adjusts pH value to 8, increases temperature in four-hole boiling flask with heating mantle and is mixed to 50 DEG C with blender with the revolving speed of 300r/min 2h is stirred, filter residue is obtained by filtration after stirring;According to parts by weight, 3 parts of above-mentioned filter residues, 12 parts of n-butanols and 22 parts of quality point are weighed Number is put into beaker for 30% acetic acid solution, is placed the beaker in sonic oscillation instrument and is vibrated 3h, mistake with the frequency ultrasound of 40kHz Filter obtains sticky filtrate, and sticky filtrate and spare filtrate 1 ︰ 3 in mass ratio are put into high speed dispersion instrument with 1300r/min's 30min is mixed in revolving speed, and mixed serum is made, mixed serum is put into Rotary Evaporators, the condition for being 40 DEG C in temperature Under be concentrated into constant weight, obtain viscosity solution, it is spare;According to parts by weight, 3 parts of graphite powders, 15 potassium permanganate powders and 110 are weighed The sulfuric acid solution that part mass fraction is 80% is put into three-necked flask, and three-necked flask is placed in ice-water bath, with blender with The revolving speed of 200r/min stirs 100min, bath temperature is increased to 40 DEG C, suspension is made in constant-temperature condensation reflux 12h;Upwards It states and the hydrogen peroxide for being 10% with the mass fraction of the quality such as suspension is added in three-necked flask, constant temperature stands 30min, is obtained by filtration Filter residue is reacted, the hydrochloric acid and distilled water for being successively 10% with mass fraction clean reaction filter residue 3 times, are put into baking oven with 105 DEG C Temperature drying to constant weight obtains oxidized solid;Above-mentioned oxidized solid and spare viscosity solution in mass ratio 1 ︰: 20 is put into and is burnt It in cup, places the beaker in sonic oscillation instrument, solidliquid mixture is made with the frequency ultrasound oscillation 5h of 40kHz, in parts by weight Meter weighs the ethanol solution that 7 parts of solidliquid mixtures, 1.2 parts of sodium citrates and 15 parts of mass fractions are 30% and puts into high speed dispersion instrument In, it is stirred 60min under conditions of revolving speed is 1500r/min, mixed liquor is made, mixed liquor is injected in Electrospun machine, Composite fibre is made under conditions of flow velocity is 2mL/h and voltage is 60V, composite fibre is put into vacuum oven, normal Drying 12h, which is made, under conditions of mild vacuum degree is 80Pa is rich in collagen SuperPro outlet capacity facial mask fabric.
Example 2
It weighs 600g garlic clove to be put into beaker, with distillation water retting garlic clove, places the beaker the water-bath that bath temperature is 97 DEG C In, constant temperature boiling 3h is cooled to room temperature after boiling, the hydrochloric acid that mass fraction is 8% is added dropwise, and adjusts pH value to 5, stands under room temperature Filtrate is obtained by filtration after standing in 7h, spare;Pigskin and fish tail are cut into pieces and mixed in the investment four-hole boiling flask of 3 ︰ 1 in mass ratio The sodium hydroxide that mass fraction is 13% is added dropwise into four-hole boiling flask with distillation water retting hybrid solid for uniformly obtained hybrid solid Solution adjusts pH value to 8, increases temperature in four-hole boiling flask with heating mantle and is mixed to 53 DEG C with blender with the revolving speed of 310r/min 2h is stirred, filter residue is obtained by filtration after stirring;According to parts by weight, 4 parts of above-mentioned filter residues, 13 parts of n-butanols and 23 parts of quality point are weighed Number is put into beaker for 35% acetic acid solution, is placed the beaker in sonic oscillation instrument and is vibrated 4h, mistake with the frequency ultrasound of 43kHz Filter obtains sticky filtrate, and sticky filtrate and spare filtrate 1 ︰ 3 in mass ratio are put into high speed dispersion instrument with 1350r/min's 35min is mixed in revolving speed, and mixed serum is made, mixed serum is put into Rotary Evaporators, the condition for being 43 DEG C in temperature Under be concentrated into constant weight, obtain viscosity solution, it is spare;According to parts by weight, 4 parts of graphite powders, 16 potassium permanganate powders and 113 are weighed The sulfuric acid solution that part mass fraction is 85% is put into three-necked flask, and three-necked flask is placed in ice-water bath, with blender with The revolving speed of 210r/min stirs 110min, bath temperature is increased to 43 DEG C, suspension is made in constant-temperature condensation reflux 12h;Upwards It states and the hydrogen peroxide for being 13% with the mass fraction of the quality such as suspension is added in three-necked flask, constant temperature stands 35min, is obtained by filtration Filter residue is reacted, the hydrochloric acid and distilled water for being successively 13% with mass fraction clean reaction filter residue 4 times, are put into baking oven with 107 DEG C Temperature drying to constant weight obtains oxidized solid;Above-mentioned oxidized solid and spare viscosity solution 1 ︰ 20 in mass ratio are put into beaker In, it places the beaker in sonic oscillation instrument, solidliquid mixture is made with the frequency ultrasound oscillation 5h of 41kHz, according to parts by weight, The ethanol solution that 8 parts of solidliquid mixtures, 1.4 parts of sodium citrates and 16 parts of mass fractions are 33% is weighed to put into high speed dispersion instrument, It is stirred 70min under conditions of revolving speed is 1550r/min, mixed liquor is made, mixed liquor is injected in Electrospun machine, is being flowed Speed be 3mL/h and voltage be 65V under conditions of composite fibre is made, composite fibre is put into vacuum oven, in room temperature and Drying 13h, which is made, under conditions of vacuum degree is 90Pa is rich in collagen SuperPro outlet capacity facial mask fabric.
Example 3
It weighs 700g garlic clove to be put into beaker, with distillation water retting garlic clove, places the beaker the water-bath that bath temperature is 100 DEG C In, constant temperature boiling 4h is cooled to room temperature after boiling, the hydrochloric acid that mass fraction is 10% is added dropwise, and adjusts pH value to 6, stands under room temperature Filtrate is obtained by filtration after standing in 8h, spare;Pigskin and fish tail are cut into pieces and mixed in the investment four-hole boiling flask of 3 ︰ 1 in mass ratio The sodium hydroxide that mass fraction is 15% is added dropwise into four-hole boiling flask with distillation water retting hybrid solid for uniformly obtained hybrid solid Solution adjusts pH value to 9, increases temperature in four-hole boiling flask with heating mantle and is mixed to 55 DEG C with blender with the revolving speed of 330r/min 3h is stirred, filter residue is obtained by filtration after stirring;According to parts by weight, 5 parts of above-mentioned filter residues, 15 parts of n-butanols and 25 parts of quality point are weighed Number is put into beaker for 40% acetic acid solution, is placed the beaker in sonic oscillation instrument and is vibrated 5h, mistake with the frequency ultrasound of 45kHz Filter obtains sticky filtrate, and sticky filtrate and spare filtrate 1 ︰ 3 in mass ratio are put into high speed dispersion instrument with 1400r/min's 40min is mixed in revolving speed, and mixed serum is made, mixed serum is put into Rotary Evaporators, the condition for being 45 DEG C in temperature Under be concentrated into constant weight, obtain viscosity solution, it is spare;According to parts by weight, 5 parts of graphite powders, 17 potassium permanganate powders and 115 are weighed The sulfuric acid solution that part mass fraction is 90% is put into three-necked flask, and three-necked flask is placed in ice-water bath, with blender with The revolving speed of 220r/min stirs 120min, bath temperature is increased to 45 DEG C, suspension is made in constant-temperature condensation reflux 13h;Upwards It states and the hydrogen peroxide for being 15% with the mass fraction of the quality such as suspension is added in three-necked flask, constant temperature stands 40min, is obtained by filtration Filter residue is reacted, the hydrochloric acid and distilled water for being successively 15% with mass fraction clean reaction filter residue 5 times, are put into baking oven with 110 DEG C Temperature drying to constant weight obtains oxidized solid;Above-mentioned oxidized solid and spare viscosity solution 1 ︰ 20 in mass ratio are put into beaker In, it places the beaker in sonic oscillation instrument, solidliquid mixture is made with the frequency ultrasound oscillation 6h of 42kHz, according to parts by weight, The ethanol solution that 9 parts of solidliquid mixtures, 1.6 parts of sodium citrates and 17 parts of mass fractions are 35% is weighed to put into high speed dispersion instrument, It is stirred 80min under conditions of revolving speed is 1600r/min, mixed liquor is made, mixed liquor is injected in Electrospun machine, is being flowed Speed be 4mL/h and voltage be 70V under conditions of composite fibre is made, composite fibre is put into vacuum oven, in room temperature and Drying 14h, which is made, under conditions of vacuum degree is 100Pa is rich in collagen SuperPro outlet capacity facial mask fabric.
Comparative example
The superpower water lock of collagen is rich in produced by the present invention as a comparison case with the facial mask fabric of Guangzhou company production Facial mask fabric in ability facial mask fabric and comparative example is detected, and testing result is as shown in table 1:
Moisture retention test
Respectively by the facial mask fabric system produced by the present invention rich in collagen SuperPro outlet capacity facial mask fabric and comparative example It is spare at facial mask.At room temperature (humidity be 60%~75%), the on probation of skin quality and facial skin water content no significant difference is selected Person 20 (every five are tried out a kind of sample, and test result is averaged), after warm water cleaning cheek 15 minutes, difference using face Film applies face 30 minutes, measures user face moisture content (wt%) with skinanalysis apparatus.
Skin repair measure of merit
60 female volunteers are selected to be tested, the age is 18 to 45 years old, average age 27 years old.Above-mentioned volunteer is divided into 4 A test group, is used respectively by produced by the present invention rich in collagen SuperPro outlet capacity facial mask fabric and right by every group 15 Facial mask is made in facial mask fabric in ratio.Behind volunteer's continuous use facial mask 4 weeks of test (3 times a week), it is evaluated.Evaluation It is divided into invalid (test rear face skin quality is without significant change or has obvious allergic phenomena), effectively (facial skin quality has part improvement, relaxes Suitable, greasy feeling is reduced, no allergic phenomena), it is effective (facial skin quality be improved significantly, water profit rich in gloss, and can be controlled effectively Oil, no allergic phenomena) it totally three keeps off.
Biocidal property measurement
The evaluation second part of GB/T20944.2-2007 antibacterial textile performance according to national standards: absorption process and succusion into Row test.
1 performance measurement result of table
According to data in table 1 it is found that facial mask is made rich in collagen SuperPro outlet capacity facial mask fabric by produced by the present invention, By still can keeping wet for a long time, there is excellent water retention property, antioxygenic property, bacteriostasis property and repairing effect, And to no skin irritation and toxicity, there is wide prospect of the application.

Claims (7)

1. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric, it is characterised in that specific preparation step Are as follows:
(1) 500~700g Garlic Seeds are weighed to be put into beaker, with distillation water retting Garlic Seeds, are placed the beaker permanent in water-bath Warm water boils, and is cooled to room temperature after boiling, and salt acid for adjusting pH value is added dropwise to 5~6, stands 6~8h under room temperature, is obtained by filtration after standing Filtrate is spare;
(2) pigskin and fish tail are cut into pieces and is uniformly mixed obtained hybrid solid in the investment four-hole boiling flask of 3 ︰ 1 in mass ratio, with steaming Distilled water impregnates hybrid solid, and sodium hydroxide solution is added dropwise into four-hole boiling flask and adjusts pH value to 8~9, increases four mouthfuls with heating mantle Filter residue is obtained by filtration with blender to be mixed in temperature in flask after stirring;
(3) according to parts by weight, 3~5 parts of above-mentioned filter residues, 12~15 parts of n-butanols and 22~25 parts of acetic acid solution investments are weighed to burn In cup, sonic oscillation in sonic oscillation instrument is placed the beaker, sticky filtrate is obtained by filtration, sticky filtrate and spare filtrate are pressed 1 ︰ 3 of mass ratio, which puts into be mixed in high speed dispersion instrument, is made mixed serum, and mixed serum is put into Rotary Evaporators and is concentrated To constant weight, viscosity solution is obtained, it is spare;
(4) according to parts by weight, 3~5 parts of graphite powders, 15~17 potassium permanganate powders and 110~115 parts of sulfuric acid solutions are weighed to throw Enter in three-necked flask, three-necked flask is placed in ice-water bath, stirred with blender, bath temperature is increased, carries out constant-temperature condensation Suspension is made in reflux;
(5) hydrogen peroxide with quality such as suspensions is added into above-mentioned three-necked flask, constant temperature stands 30~40min, is obtained by filtration Filter residue is reacted, successively cleans reaction filter residue 3~5 times with hydrochloric acid and distilled water, temperature drying to constant weight is put into and obtains oxidized solid;
(6) above-mentioned oxidized solid and spare viscosity solution 1 ︰ 20 in mass ratio are put into beaker, places the beaker ultrasonic vibration It swings the obtained solidliquid mixture of sonic oscillation in instrument and weighs 7~9 parts of solidliquid mixtures, 1.2~1.6 portions of lemons according to parts by weight It is stirred in sour sodium and 15~17 parts of ethanol solution investment high speed dispersion instrument, mixed liquor is made, mixed liquor is injected into Electrospun Composite fibre is made in machine, composite fibre is put into vacuum oven, is made superpower rich in collagen under normal temperature conditions Water lock ability facial mask fabric.
2. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric according to claim 1, special Sign is: the bath temperature of water-bath as described in step (1) is 95~100 DEG C, and the constant temperature boiling time is 3~4h, hydrochloric acid Mass fraction is 6~10%.
3. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric according to claim 1, special Sign is: the mass fraction of sodium hydroxide solution described in step (2) is 10~15%, four-hole boiling flask temperature is increased to 50~ 55 DEG C, the revolving speed of blender is 300~330r/min, and mixing time is 2~3h.
4. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric according to claim 1, special Sign is: the mass fraction of acetic acid solution described in step (3) is 30~40%, the frequency in sonic oscillation instrument is 40~ 45kHz, sonic oscillation time are 3~5h, and the revolving speed in high speed dispersion instrument is 1300~1400r/min, and mixing time is 30~40min, the temperature in Rotary Evaporators are 40~45 DEG C.
5. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric according to claim 1, special Sign is: the mass fraction of sulfuric acid solution described in step (4) is 80~90%, and the revolving speed of blender is 200~220r/ Min, mixing time are 100~120min, and bath temperature is increased to 40~45 DEG C, and constant-temperature condensation return time is 12~13h.
6. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric according to claim 1, special Sign is: the mass fraction of hydrogen peroxide described in step (5) is 10~15%, and the mass fraction of hydrochloric acid is 10~15%, baking oven In temperature be 105~110 DEG C.
7. a kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric according to claim 1, special Sign is: the frequency in sonic oscillation instrument described in step (6) is 40~42kHz, and the sonic oscillation time is that 5~6h is made solid Liquid mixture, the mass fraction of ethanol solution are 30~35%, and the revolving speed in high speed dispersion instrument is 1500~1600r/min, stirring Incorporation time is 60~80min, and the flow velocity in Electrospun machine is 2~4mL/h, and voltage is 60~70V, true in vacuum oven Reciprocal of duty cycle is 80~100Pa, and drying time is 12~14h.
CN201810994534.9A 2018-08-29 2018-08-29 A kind of preparation method rich in collagen SuperPro outlet capacity facial mask fabric Pending CN109208106A (en)

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Application publication date: 20190115