CN109825949A - A kind of preparation and application of all solid state functional nanofiber membrane - Google Patents
A kind of preparation and application of all solid state functional nanofiber membrane Download PDFInfo
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- CN109825949A CN109825949A CN201910181273.3A CN201910181273A CN109825949A CN 109825949 A CN109825949 A CN 109825949A CN 201910181273 A CN201910181273 A CN 201910181273A CN 109825949 A CN109825949 A CN 109825949A
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Abstract
The invention belongs to material science and cosmetic field, disclose the preparation and application of a kind of all solid state functional nanofiber membrane.The preparation method is the following steps are included: mix to obtain spun component liquid 1 for water soluble polymer, functional component and water；Water-insoluble macromolecular polymer and dehydrated alcohol are mixed into obtain spun component liquid 2；Spun component liquid 1 and spun component liquid 2 mix, and adjust its pH and obtain spinning solution, carry out electrostatic spinning then up to target product；All solid state functional nanofiber membrane of the invention is combined by water-insoluble macromolecular polymer and water soluble polymer, in use process, water soluble polymer group meets instant water dissolution, and effect small molecule quickly absorbs, the easy to use and saving plenty of time；Water-insoluble macromolecule is attached on eyelet fabric, can use the principle that macromolecular chain is mutually wound prevent water soluble polymer dissolve after adhere to or penetrate into skin, safe ready.
Description
Technical field
The invention belongs to material science and cosmetic field, in particular to a kind of system of all solid state functional nanofiber membrane
Standby and application.
Background technique
With the continuous development of society, people increasingly pay attention to skin care and beauty, and facial mask industry has also welcome rapidly
Development.Currently, facial mask occupies lion's share in entire Cosmetic Market, wherein fiber-like film cloth accounts for the 70% of facial mask
More than.Facial mask can be divided into compression-type facial mask and non-depressed miniature facial mask, non-depressed miniature facial mask, that is, traditional facial mask, user according to finished product
Method is, after face cleaning, takes out moisturizing face paste, and throws off protective film, is covered in face according to face shape, 15~remove down after twenty minutes, to skin
After skin absorbs 2~3 minutes, cleaned with clear water；Compression-type facial mask is for the improvement easy to carry to non-depressed miniature facial mask, size
As five dime coins, in use, compression facial mask is placed in container, container, face paper are filled with toner (self-control water)
Moisture is absorbed, expands, quickly forms shape of face face paper of a size, lightly apply in face, wait for quietly 10~15 minutes
It after facial mask parches, removes from below to up, applies a little skin cream.
A good facial mask, the selection of facial mask cloth is particularly significant, and the selection of facial mask cloth is mainly from the aspect of three, i.e. film
Cloth density, docile sense and material.Thicker face paper is selected, thicker face paper can be by Essence or the opposite lock of nutritional ingredient
It lives calmly；The material and cut out knife number that the docile degree of facial mask and face depends on facial mask；The material of facial mask, which will affect facial mask, to be made
Comfort and effect are divided into silk, cotton, terylene, blended, tencel, biological fiber etc., natural pure cotton according to material
The facial mask of quality is that most popular material, synthetic fibers material are taken second place in recent years, and Biofibre facial mask paper is best, blended face paper
It is worst.Slightly thick, important face paper can absorb enough moisturizing essence, more preferable to the package effect of skin " pressurization ".
To sum up, the phenomenon that " wet to rattle away " can all be occurred in use by compressing facial mask and uncompressed facial mask, and be used
Process is complicated, and the application time is longer.The water lock and comfort of facial mask cloth are an important factor for influencing the selection of traditional facial mask cloth.Cause
It is necessary to develop a kind of solid-state facial mask without the concern for film cloth water lock function for this.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of all solid state function
The preparation method of energy property nano fibrous membrane.
Another object of the present invention is to provide all solid state functional nanofiber membrane of above method preparation.
Still a further object of the present invention is to provide the application of above-mentioned all solid state functional nanofiber membrane.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of all solid state functional nanofiber membrane, comprising the following steps:
(1) water soluble polymer, functional component and water are mixed, is completely dissolved to obtain spun component liquid 1；
(2) water-insoluble macromolecular polymer and dehydrated alcohol are mixed, spun component liquid 2 is obtained after being completely dissolved；
(3) obtained spun component liquid 1 and spun component liquid 2 are mixed, its pH=5.9~6.5 are adjusted after being uniformly dispersed,
Up to spinning solution；
(4) spinning solution is subjected to electrostatic spinning, receives gained spinning film all solid state functionality obtained by drying after spinning
Rice tunica fibrosa；
Water soluble polymer described in step (1) is polyethylene glycol oxide, polyethylene glycol, polyvinyl alcohol and poly- second
At least one of alkene pyrrolidone can be the carrier of the functional component；
The ingredient of the effect of described in step (1) include dendrobium candidum skim the cream off milk, hydrolyzed coffee ambrette extract, dipeptides two
Aminobutyryl benzyl amide diacetin, acetyl group octapeptide -3, palmitoyl oligopeptide, palmityl tripeptides -8, -1 copper of tripeptides, molecular weight
At least one of Sodium Hyaluronate less than or equal to 400000；
Water soluble polymer described in step (1), functional component and water quality ratio be 0.5~6:0.002~
3:70~80；
Water-insoluble macromolecular polymer described in step (2) is polyvinyl butyral, alcohol-soluble polyurethane and alcohol
At least one of soluble polyacrylate；
The mass ratio of water-insoluble macromolecular polymer described in step (2) and dehydrated alcohol is 0.1~2:15~20；
The dosage of spun component liquid 1 described in step (3) and spun component liquid 2 meets spun component liquid 1 and spinning group
The mass ratio of liquid separation 2 is 18:1~1:18.
Reception substrate in electrostatic spinning described in step (4) is eyelet fabric, and the eyelet fabric shape of a mesh is unlimited, net
Eye size is 70 mesh~7 mesh, more preferably 50 mesh~20 mesh；
Preferably, the reception substrate material in electrostatic spinning described in step (4) includes polyamide fibre, cotton synthetic fibre, terylene, ammonia
One of synthetic fibre, silk are a variety of, and grammes per square metre is 10~100g；
Electrospinning device described in step (4) is pin type or wire type electrospinning device, and needle type static spinning is set
Standby spinning condition are as follows: receive 15~24cm of distance, 9~15KV of spinning voltage, humidity 30~55%；Wire type electrostatic spinning is set
Standby spinning condition are as follows: receive 15~24cm of distance, 25~55KV of spinning voltage, humidity 35~50%.
Drying temperature described in step (4) is set according to functional component therein, is usually set to 20~45 DEG C.
A kind of all solid state functional nanofiber membrane prepared by the above method.
Above-mentioned all solid state functional nanofiber membrane by be cut into different shape can be used as facial mask, eye mask, hand film,
Foot mould, nose film, medical dressing and other dressing etc., thus above-mentioned all solid state functional nanofiber membrane can be applicable to facial mask,
Eye mask, hand film, foot mould, nose film, medical dressing and other dressing fields, especially solvable or gradually in terms of molten facial mask and eye mask
Using.
When above-mentioned all solid state functional nanofiber membrane as facial mask in use, application method are as follows: first face is drenched,
All solid state functional nanofiber membrane prepared by the present invention directly is applied, water soluble polymer moment is molten in coating materials
Solution, releases immediately functional component, skin is allowed quickly to absorb；Either first apply all solid state functional nano prepared by the present invention
Tunica fibrosa, then spray water, water soluble polymer moment dissolves in coating materials, releases immediately functional component, makes skin fast
Speed absorbs.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) all solid state functional nanofiber membrane material sheet prepared by the present invention is as solid nanofibers, without any anti-
Rotten agent.
(2) all solid state functional nanofiber membrane material prepared by the present invention is by water-insoluble macromolecular polymer and water solubility
High molecular polymer compounding ingredients are made, and in use process, water-insoluble macromolecule is attached on eyelet fabric, can use high score
Skin, safe ready are adhered to or penetrated into the principle that subchain is mutually wound after preventing water soluble polymer from dissolving；
(3) all solid state functional nanofiber membrane material prepared by the present invention meets water soluble polymer component wink after water
Between dissolve, effect small molecule quickly absorbs, and easy to use, use can save the plenty of time.
(4) all solid state functional nanofiber membrane material prepared by the present invention can cleave functional component at nano molecular, more
Easily absorb.
(5) in use, instant process visualization has all solid state functional nanofiber membrane material prepared by the present invention
There is superpower visual effect.
(6) all solid state functional nanofiber membrane material prepared by the present invention does not have to consider facial mask cloth using eyelet fabric as substrate
Water lock.
Detailed description of the invention
Fig. 1 is that film prepared by embodiment 1 and embodiment 2 amplifies 100 times of shape appearance figures observed under an optical microscope,
In (a) represent the film 1 prepared in embodiment 1, (b) represent embodiment 2 preparation film 2.
Fig. 2 is the shape appearance figure of nanofiber film layer and reception basal layer after film prepared by embodiment 1 amplifies 50 times.
Fig. 3 is the anti-wrinkle effect figure of film 1 prepared by embodiment 1.
Fig. 4 is the Shu Min reparative experiment result figure of facial mask 2 prepared by embodiment 2.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
73.6g aseptic deionized water is weighed in 250mL conical flask, is put into magnetic stir bar, conical flask is placed in magnetic force
On blender, turn on agitator is gradually added into 2.0g polyethylene glycol oxide (molecular weight 600000) powder, and 2.0g dendrobium candidum extracts
Essence (enzymatic hydrolysis-fermentation method preparation), is then added the Hyal powder that 0.1g molecular weight is 6000,0.1g molecular weight is 20
The Hyal powder of~40w, -3 powder of 0.1g acetyl group octapeptide, 0.1g dipeptides diaminobutyryl benzyl amide diacetin
Powder, 25 DEG C are continued stirring and are completely dissolved to powder, obtain spun component liquid 1；Weigh 2.0g alcohol-soluble polyurethane (PU3514,
Three liters of Foshan trade Co., Ltd) powder is dissolved in 20g dehydrated alcohol, and stirring is allowed to sufficiently dissolve, and obtains spun component liquid
2；Finally spinning solution group liquid separation 1 and 2 is mixed, after being sufficiently stirred, the use of lemon acid for adjusting pH value is 5.9~6.5, obtains
To spinning solution 1, spinning is carried out using single needle formula spinning equipment, reception substrate is 35 mesh polyamide fibre eyelet fabrics, the 2h (spinning of spinning time
Voltage 12KV receives distance 21cm, humidity 50%), 0 DEG C of film Isosorbide-5-Nitrae drying is obtained, cuts to obtain facial mask 1 using die-cutting device.
Embodiment 2:
71.69g aseptic deionized water is weighed in 250mL conical flask, is put into magnetic stir bar, conical flask is placed in magnetic force
On blender, turn on agitator is gradually added into 4.0g polyvinylpyrrolidone, and 2.0g dendrobium candidum skims the cream off milk (enzymatic hydrolysis-fermentation
Method preparation), then be added -7 powder of 4 peptide of 0.01g palmityl, 0.1g palmitoyl oligopeptide powder, -8 powder of 0.1g palmityl tripeptides,
- 1 copper powders of 0.1g tripeptides, 25 DEG C are continued stirring and are completely dissolved to powder, obtain spun component liquid 1；Weigh 2.0g polyvinyl alcohol
Butyral (molecular weight 170000~250000) powder is dissolved in 20g dehydrated alcohol, and stirring is allowed to sufficiently dissolve, and obtains spinning
Group liquid separation 2；Finally spinning solution group liquid separation 1 and 2 is mixed, after being sufficiently stirred, using lemon acid for adjusting pH value be 5.9~
6.5, spinning solution 2 is obtained, carries out spinning using single needle formula spinning equipment, reception substrate is 30 mesh polyamide fibre eyelet fabrics, spinning time
2h (spinning voltage 35KV receives distance 18cm, humidity 45%), 40 DEG C of drying obtain film 2, cut to obtain using die-cutting device
Facial mask 2.
Interpretation of result:
(1) optical microscopy pattern
It is made to Example 1 and Example 2 of the present invention using Zeiss Elyra 7with Lattice SIM optical microscopy
Standby obtained film is characterized, and as a result as depicted in figs. 1 and 2, Fig. 1 (a) is pattern observed by film 1 amplifies 100 times, fiber
Diameter about 250~300nm；Fig. 1 (b) is pattern observed by film 2 amplifies 100 times, fibre diameter about 300~350nm；From figure
1 it can be seen that the nanometer spinning distribution on film 1 and film 2 is all visibly homogeneous.Fig. 2 (a) is that coating materials 1 amplifies 50 times from eyelet fabric side
The nanofiber film layer observed and the pattern for receiving basal layer, it can be seen that film and eyelet fabric ten that nanometer spinning is formed
Divide fitting；Fig. 2 (b) be coating materials 1 amplify 50 times from nano fibrous membrane unilateral observation to nanofiber film layer pattern, Cong Zhongke
To find out that the film that nanometer spinning is formed not is one layer of sealing, tunica fibrosa has gas permeability in other words.
(2) patch test results
The Potential feasibility for causing human skin adverse reaction for detection coating materials, carries out patch examination using film 1 and film 2 respectively
It tests, sample and blank district are distributed in volunteer's forearm song side region, the spot tester of selection by test zone random distribution table
Face accumulates 64mm2, depth 1mm, amount of samples is about 0.0256g~0.0320g.After removing tested material spot tester 30min (to
Impression disappear after), for 24 hours, 48h by " cosmetics health specification " (version in 2007) skin closure type patch test dermoreaction classification
Standard sight dermoreaction, and record observation result.
Patch test results are as shown in table 1, the adverse reaction 1 of 1:1 grades of film, and 2 grades adverse reaction 0,3 grades of adverse reactions 0
Example, 4 grades adverse reaction 0.The adverse reaction 0 of 2:1 grades of film, 2 grades adverse reaction 0,3 grades adverse reaction 0,4 grades bad anti-
Answer 0.According to " cosmetics health specification (2007) ": skin closure type patch test results are explained: occurring 1 in 30 subjects
The number of grade skin adverse reaction is more than 2 (deodorising product patch tests 2 more than the number of 5 or 2 grades skin adverse reactions
The number of order reaction is more than 5), or when any 13 grades or 3 grades of appearance or more skin adverse reaction, determine tested material to human body
There is skin adverse reaction.Therefore, patch test results show that film 1 and film 2 have no adverse reaction to human skin.
1 human skin patch test result of table
(3) timely anti-wrinkle effect
Eye tail tester wrinkly is chosen to take one's test.Facial mask 1 is pasted at a tail by experimenter.Application method:
Corresponding site is sprayed with pure water and is moistened, film sample is affixed on corresponding site and removes face mask substrate material to being completely dissolved, then is sprayed
First use area moist is spilt, then soft massage.Photo opporunity: before use, 30 minutes after use.
Using Canfield Scientific, the VISIA-CR of Inc. production takes pictures to test 1 anti-wrinkle effect of facial mask
Comparison.As a result as shown in figure 3, by Fig. 3 it can clearly be seen that before using facial mask 1, eye wrinkle-removing is respectively 551.01,
367.54 and 468.47pix, after film 130 minutes, corresponding position wrinkle is respectively 400.72,313.18 and
It is crease-resistant in time well to show that facial mask 1 has effects that by 322.08pix.
(4) Shu Min reparative experiment result
By the crowd of questionnaire and the suitable skin sensitivity of lactic acid shouting pain experiment screening, 2 sample of facial mask is used continuously in subject
Product 28 days, application method are as follows: primary using target sample daily.It paid a return visit within period every 14 days primary.Before using sample, use sample
14 days after product, carry out keratoderma moisture content, the percutaneous water loss of skin, skin ferroheme and acid-base scale of skin within 28 days
Measurement, and acquire facial image analysis.Lactic acid shouting pain experiment is respectively carried out before using sample, using 28 days after sample, it is more newborn
Sour shouting pain threshold values.The experiment recruits volunteer 12 altogether, wherein 2 people drop by the wayside, effective volunteer is 10 and data are effective.
Test has carried out 4 weeks altogether, and skin moisture content, skin water loss amount, skin ferroheme, skin are detected before and after using sample
Skin color-redness a* value and lactic acid shouting pain value, compare its difference, test data is averaged.
Film is tested using the skin elasticity tester MPA580 that German CK is produced, wherein using Germany CK
Corneometer CM825 moisture of skin test probe test moisture of skin, uses German CK Tewameter TM300 skin
Water loss test probe test skin water loss, tests probe using German CK Mexameter MX18 skin pigment and surveys
Try skin ferroheme value.Test results are shown in figure 4, and after 2 sample of facial mask 4 weeks, skin moisture content has apparent increase,
Skin water loss is decreased obviously, and skin ferroheme value has apparent reduction, and skin redness a* has apparent reduction, volunteer couple
It improves the threshold of pain of lactic acid shouting pain.It therefore deduces that, 2 sample of facial mask has effects that preferable Shu Min is repaired.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of all solid state functional nanofiber membrane, it is characterised in that the following steps are included:
(1) water soluble polymer, functional component and water are mixed, is completely dissolved to obtain spun component liquid 1；
(2) water-insoluble macromolecular polymer and dehydrated alcohol are mixed, spun component liquid 2 is obtained after being completely dissolved；
(3) obtained spun component liquid 1 and spun component liquid 2 are mixed, adjusted after being uniformly dispersed its pH=5.9~6.5 to get
Spinning solution；
(4) spinning solution is subjected to electrostatic spinning, it is after spinning that gained spinning film all solid state functional nano obtained by drying is fine
Tie up film.
2. the preparation method of all solid state functional nanofiber membrane according to claim 1, it is characterised in that:
Water soluble polymer described in step (1) is polyethylene glycol oxide, polyethylene glycol, polyvinyl alcohol and polyethylene pyrrole
At least one of pyrrolidone；
The ingredient of the effect of described in step (1) include dendrobium candidum skim the cream off milk, hydrolyzed coffee ambrette extract, dipeptides diamino
Butyryl benzyl amide diacetin, acetyl group octapeptide -3, palmitoyl oligopeptide, palmityl tripeptides -8, -1 copper of tripeptides, molecular weight are less than
At least one of Sodium Hyaluronate equal to 400000；
Water soluble polymer described in step (1), functional component and water quality ratio are 0.5~6:0.002~3:70
~80.
3. the preparation method of all solid state functional nanofiber membrane according to claim 1, it is characterised in that:
Water-insoluble macromolecular polymer described in step (2) is polyvinyl butyral, alcohol-soluble polyurethane and alcohol-soluble
At least one of polyacrylate；
The mass ratio of water-insoluble macromolecular polymer described in step (2) and dehydrated alcohol is 0.1~2:15~20.
4. the preparation method of all solid state functional nanofiber membrane according to claim 1, it is characterised in that:
The dosage of spun component liquid 1 described in step (3) and spun component liquid 2 meets spun component liquid 1 and spun component liquid 2
Mass ratio be 18:1~1:18.
5. the preparation method of all solid state functional nanofiber membrane according to claim 1, it is characterised in that:
Reception substrate in electrostatic spinning described in step (4) is eyelet fabric, and the eyelet fabric shape of a mesh is unlimited, and mesh is big
Small is 70 mesh~7 mesh；
Reception substrate material in electrostatic spinning described in step (4) includes one in polyamide fibre, cotton synthetic fibre, terylene, spandex, silk
Kind is a variety of, and grammes per square metre is 10~100g.
6. the preparation method of all solid state functional nanofiber membrane according to claim 1, it is characterised in that:
Electrospinning device described in step (4) be pin type or wire type electrospinning device, needle type static spinning equipment
Spinning condition are as follows: receive 15~24cm of distance, 9~15KV of spinning voltage, humidity 30~55%；Wire type electrospinning device
Spinning condition are as follows: receive 15~24cm of distance, 25~55KV of spinning voltage, humidity 35~50%.
7. the preparation method of all solid state functional nanofiber membrane according to claim 1, it is characterised in that:
Drying temperature described in step (4) is 20~45 DEG C.
8. a kind of all solid state functional nanofiber membrane that methods described in any item according to claim 1~7 are prepared.
9. all solid state functional nanofiber membrane according to claim 8 is in facial mask, eye mask, hand film, foot mould, nose film, doctor
With the application in dressing field.
10. all solid state functional nanofiber membrane according to claim 9 is in facial mask, eye mask, hand film, foot mould, nose film, doctor
With the application in dressing field, it is characterised in that when as facial mask in use, application method are as follows: first face is drenched, directly apply
All solid state functional nanofiber membrane after upper cutting；All solid state functional nanofiber membrane after either first applying cutting,
It sprays water again.
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| CN110438665A (en) * | 2019-08-07 | 2019-11-12 | 山东省医学科学院药物研究所（山东省抗衰老研究中心、山东省新技术制药研究所） | A kind of preparation method of self-supporting solid-state multicomponent facial mask |
| CN111135119A (en) * | 2020-01-16 | 2020-05-12 | 华南协同创新研究院 | PVA nanofiber mask with slow release effect and preparation method and application thereof |
| CN112481738A (en) * | 2020-10-26 | 2021-03-12 | 杭州乐铭科技有限公司 | Hyaluronic acid fiber and production process thereof |
| CN112891282A (en) * | 2021-01-28 | 2021-06-04 | 东莞华工创为生物科技有限公司 | Nano-fiber mask with anti-aging effect and preparation method and application thereof |
| CN113134110A (en) * | 2020-01-16 | 2021-07-20 | 广州增城潮徽生物技术有限公司 | PVP/PVB slow-release nano-fiber medical dressing and preparation method and application thereof |
| CN115607458A (en) * | 2022-10-13 | 2023-01-17 | 厦门净境新材料科技有限公司 | Preparation method of efficient moisturizing invisible mask |
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Application publication date: 20190531 |
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