CN106567192A - Method for preparing multifunctional health-care nanofiber membrane - Google Patents
Method for preparing multifunctional health-care nanofiber membrane Download PDFInfo
- Publication number
- CN106567192A CN106567192A CN201610941514.6A CN201610941514A CN106567192A CN 106567192 A CN106567192 A CN 106567192A CN 201610941514 A CN201610941514 A CN 201610941514A CN 106567192 A CN106567192 A CN 106567192A
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- CN
- China
- Prior art keywords
- health care
- fibrous membrane
- microgranule
- preparation
- spinning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002121 nanofiber Substances 0.000 title abstract description 21
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- 229920000642 polymer Polymers 0.000 claims abstract description 28
- 239000002105 nanoparticle Substances 0.000 claims abstract description 27
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- 238000002360 preparation method Methods 0.000 claims abstract description 17
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- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 11
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
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- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
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- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 claims 2
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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Abstract
The invention discloses a method for preparing a multifunctional health-care nanofiber membrane. The method comprises: natural ore nano particles and dispersing agents are added into a polymer spinning solution and uniform ultrasonic mixing is carried out, thereby obtaining a natural ore nano particle/ polymer spinning solution; standing and defoaming, electrostatic spinning, and vacuum drying are carried out successively and then the temperature is cooled to a room temperature, so that a health-care nanofiber membrane is obtained. The electrostatic spinning parameters are as follows: the electrostatic pressure is 10 to 25KV; the propulsion speed is 0.1-2mL/h, the receiving distance is 10-25cm; and a receiving device is in a rotation receiving mode and the receiving speed is 20 to 40r/min. According to the preparation method, the nano-level natural ore nano particles are dispersed into the spinning solution uniformly and are added into the fibers during the electrostatic spinning process, so that the nanofiber membrane including the natural ore nano particles can be obtained. The nanofiber membrane has healthcare functions as the natural ore, wherein the functions include negative ion releasing, far infrared ray releasing, anti-ultraviolet, and anti-bacterial functions.
Description
Technical field
The invention belongs to textile fiber technology field, more particularly to a kind of preparation side of multi-functional health care nanometer fibrous membrane
Method.
Background technology
With the economic fast-developing and improvement of people's living standards, in safety and health care more and more concerned the present
My god, people put forward higher requirement to textile, not only to meet textile comfortableization, the demand of fashion-orientation, and to accord with
Close the themes of the times of green health.Therefore, the textile with health care be textile garment field development emphasis direction it
One.In nature, the raw material resources with health-care effect are innumerable, from traditional natural ramie fiber product, bamboo fiber products,
To the chitin fiber as staple fibre product, acid fiber by polylactic, bamboo carbon fiber etc., scientific worker be devoted to always by
Natural health resource is applied to health textile field, develops new type of health textile, increases value-added content of product.At present, it is single
Pure natural fiber and synthetic fibers or single functional textiles can not meet the demand of people.Therefore it is new strong
The multi-function health-care textile of health ecological, environmental protective has become the focus of research, and work(is carried out to fiber with natural crystal nano material
Energy property is modified and prepares healthcare function fiber study hotspot even more in recent years.
Maifanitum：Maifanitum is the silicate of granite, is China's application natural crystal earlier.Containing silicon dioxide
65%～70%, potassium oxide, sodium oxide 9%, calcium oxide 2%, magnesium oxide 2%, also ferrum, zinc, strontium, manganese etc. more than 40 plants inorganic unit
The health care medicinal that element is nontoxic, tasteless wherein for 12 kinds of the necessary trace element of human body, and part rare element, had no side effect
Stone.(Zhang Baoguo. study of pharmacy progress [J] of Maifanitum. Chinese patent medicine, 2005,27 (10)：It is discussed in detail in 1205-1208)
The pharmacological action of Maifanitum, animal experiment is it has proven convenient that Maifanitum is in defying age, resisting fatigue, anoxia enduring, enhancing immunity, rush
Enter growth promoter, promote erythropoiesis, promote wound healing, promote union of fracture, suppress hyperlipidemia, calmness, anti-sclerotin to dredge
The aspects such as pine, mutation, anticancer have obvious pharmacological action, and without toxicity.Jilin Chemical Fiber Group Co., Ltd.
By the Maifanitum Jing high-tech technique special handlings of high-quality, in being added to spinning liquid, Maifanitum functional fiber is made, its guarantor
Strong effect is embodied in：Improve internal microcirculation, promote normal metabolism, the trace element lacked in human body can be supplemented
Can also be emitting far-infrared etc..
Rare ice stone：Rare ice stone is a kind of crystal that there is permanent electrode, with thermoelectricity and piezoelectric effect.Rare ice stone nano powder
Exactly according to the property of rare ice stone crystal, with a kind of superfine powder made by high-tech means, it mainly by sodium, potassium, calcium, ferrum,
Aluminum, silicon, boron element and its oxide etc. are constituted.Rare ice stone nano powder has typical characteristic of semiconductor, its Intrinsic Gettering band master
Far-infrared band is located at, because thermoelectricity, piezoelectric effect cause dipole moment to change, thus with stronger far infrared transmission ability.
Further, since various adhesions coexist between its character defect and atom, thus can slowly discharge in water it is beneficial to human body from
Son.Patent of invention CN1360092A Oxyanionic polyester fibre and preparation method disclose one kind with rare ice stone powder as function ingredients
The method for preparing negative oxygen ion modified polyester fibre.The anion modified polyester fibre has negative ion-releasing function, can be used for
Make high-grade summer T-shirt, winter underwear fabric etc..But the fiber function is relatively simple, only there is a kind of health care, it is impossible to full
Demand of the sufficient people to multi-function health-care textile.
Jade：Jade is just from ancient times health preserving sage's product.It is beneficial to the mineral of human body and micro unit containing abundant in jade
Element, such as zinc, magnesium, ferrum, copper, selenium, chromium, manganese, cobalt.Prove according to mineral medical research, jade can produce the photoelectric effect of high intensity,
In process can focusing energy storage, formed magnetic field, the resonance for being beneficial to human body can be produced when wearing.Additionally, jade is special
Molecular structure can launch wavelength for 8-15 μm can be by the far-infrared electromagnetic wave of human body resonance absorption, this electromagnetic wave is to human body
Produce good biological agent.Novel nano health fiber-jade fiber in China's scientific worker's independent research in 2006.
Its preparation technology is the Subnano-class granule that jade and other beneficial mineral matters are added in spinning melt (with extracting and receive
Rice technology reaches Subnano-class), then Jing spinning is processed.For a long time jade fiber product is worn, contribute to improving blood
Liquid microcirculation, enhances metabolism, and bodily waste is discharged in time, and makes human cell tissue more vibrant, reaches removing heat from blood, drop
Press, calm the nerves, the health care such as fatigue alleviating, with good development prospect.
Tai Ji stone：Tai Ji stone is a kind of natural crystal, and its main component is silicon dioxide, additionally containing lot of trace
Metalliferous mineral element.Its high-frequency resonance frequency is fairly close with the resonant frequency of human body cell molecule, human body can be aided in receive,
The magnetic field energy that earth natural magnetic field is discharged is supplemented, promotes absorption of human body and aggregation positive energy.Tai Ji stone can discharge far infrared
Line, emissivity is up to 93.36%, can promote blood microcirculation, metabolism.Additionally, Tai Ji stone have anti-ultraviolet function,
The effects such as antibacterial, with various excellent health cares.At present, R and D of the Tai Ji stone in textile garment field are one
Bright spot.Patent of invention 201210017287.X discloses a kind of Tai Ji stone cup with high-frequency resonance effector function, is in cover
1-99 Tai Ji stone granule is provided with cup, these Tai Ji stone granules are a diameter of 20mm-50mm of irregular ellipsoid, can be produced
Natural magnetic field, by the natural positive energy of aggregation female breast is directly acted on, and promotes the blood microcirculation and metabolism of mammary gland,
With good health-care effect.
As described above, exploitation of the natural crystal such as Maifanitum, rare ice stone, jade, Tai Ji stone in healthcare field in recent years
Have much with research.But do not occur applying it to field of textiles with electrostatic spinning technique at present and prepare health care nanometer fiber
The research of film.
The content of the invention
It is an object of the invention to provide a kind of preparation method of multi-functional health care nanometer fibrous membrane, what the present invention was provided
Nano fibrous membrane has the health cares such as anion releasing, releasing far infrared, uvioresistant or antibacterial.
The purpose of the present invention is achieved through the following technical solutions：
The present invention relates to a kind of preparation method of health care nanometer fibrous membrane, methods described comprises the steps：
S1, in polymer dope add natural crystal nanoparticle, dispersant, ultrasound wave mix homogeneously, be obtained day
Right Ore nanoparticle/polymer dope；
S2, standing and defoaming, electrostatic spinning is cooled to room temperature after vacuum drying, obtain final product the health care nanometer fibrous membrane；It is described
Electrospinning parameters are：Electrostatic pressure is 10～25KV, and fltting speed is 0.1～2mL/h, and it is 10～25cm to receive distance, is received
Device is Rotation of receiver, and reception speed is 20～40r/min.
Only in the range of electrospinning parameters, the natural crystal nanoparticle/polymer dope of the present invention can be obtained
Health care nanometer fibrous membrane is obtained with successful spinning.
Preferably, in the natural crystal nanoparticle/polymer dope natural crystal nanoparticle mass fraction
For 1%～10%.More preferably 3%～6%.
Preferably, the particle diameter of the natural crystal nanoparticle is 20～100 nanometers.
Preferably, the natural crystal nanoparticle is selected from tourmaline particles, rare ice stone microgranule, maifanite particle, jade
One or more in microgranule, Tai Ji stone microgranule.
Preferably, the natural crystal nanoparticle is the natural crystal nanoparticle after titanate coupling agent modified.Tool
Body is that natural crystal nanoparticle is immersed in into 10～30min in titanate coupling agent.Natural crystal nanoparticle is in polymer
Bad dispersibility in spinning liquid, easily reunites, and has a strong impact on end product quality.The present invention is by adding titanate coupling agent to natural ore
Stone microgranule plays the Surface Modification Effect：Titanate esters are coated on the surface of natural crystal microgranule by adhesion, hydrogen bond, have completely cut off pole
Directly contact between the natural crystal microgranule of property；When natural ore particles are immersed in titanate esters, due to hydrogen bond, electrostatic attraction
And Van der Waals force, titanate esters absorption forms orderly mixture in natural crystal microparticle surfaces, so as to fixed or film forming is coated on
The surface of natural crystal microgranule, or even multilayer coating structure is formed, hence in so that particle surface is presented the superficiality similar with polymer
Matter.In addition, when natural ore particles select tourmaline, the ehter bond of titanate esters can be with the tourmaline powder body surface in fine ore powder
The oh group reaction in face generates covalent bond, and further surface chemical modification effect is played to it, preferably promotes it in polymerization
Dispersion in thing spinning liquid.
Preferably, the mass fraction of dispersant is 1%～3% in the natural crystal nanoparticle/polymer dope.
Preferably, the dispersant is eight isobutyl group caged silsesquioxanes.The dispersant can be with titanate coupling agent
The titanate coupling agent of modified natural crystal nano-particle surface plays cooperative effect, and playing natural crystal microgranule is prevented
While reunion with settlement action, also further such that modified natural crystal nanoparticle obtains good in spinning liquid
Dispersion, and degree of scatter of the natural crystal nanoparticle in spinning liquid exactly determines final products-cellulose membrane quality
It is crucial.
Preferably, the polymer dope is mixed in a solvent by polymer dissolving；The polymer choosing
One or more in autopolyester, polyacrylonitrile, polyamide, polyurethane, viscose, polyvinyl alcohol.
In the present invention, originating without special restriction to polymer, can adopt the commercial goods of the polymer,
Can voluntarily prepare according to the technical scheme for preparing the polymer well known to those skilled in the art.
Preferably, the solvent is selected from amides compound, water, methanol, ethanol, n-butyl alcohol, isopropanol, hexafluoro isopropyl
Alcohol, trifluoroethanol, phenol, formic acid, acetic acid, trifluoroacetic acid, dichloromethane, dichloroethanes, chloroform, acetone, tetrahydrofuran,
One or more in pyridine, toluene, N-Methyl pyrrolidone, decahydronaphthalenes, hexamethylene and Carbon bisulfide.
In the present invention, to ensure that the mass concentration of polymer in the mixture reaches above-mentioned for the consumption of the solvent
In the range of requirement.The present invention originating without special restriction to the solvent, using the commercial goods of the solvent
.
Preferably, the mass fraction of polymer is 10%～30% in the polymer dope.
Preferably, in the ultrasound wave mix homogeneously, the frequency of the ultrasound wave is 20～30KHz, power is 300～
500W, process time is 2～4h.
Preferably, the vacuum drying baking temperature is 80 DEG C～100 DEG C, and drying time is 1～4h.
Compared with prior art, the present invention has the advantages that：
1st, by the way that nano level natural crystal microgranule is evenly dispersed in spinning liquid, add during electrostatic spinning
To the inside of fiber, so as to obtain the nano fibrous membrane containing natural crystal microgranule.
2nd, the nano fibrous membrane for obtaining has the health care that natural crystal has, and such as anion releasing, release is remote red
Outside line, uvioresistant, antibacterial etc. so that the nano fibrous membrane that the present invention is provided has various excellent health-care effecies, will protect
Strong field is widely used, and has wide market prospect.
Description of the drawings
Fig. 1 is that the Tai Ji stone microgranule for the preparing/polyester nano multifunctional fibre film in embodiment 1 amplifies 500 times
SEM schemes；
Fig. 2 is that the Tai Ji stone microgranule for the preparing/polyester nano multifunctional fibre film in embodiment 1 amplifies 10000 times
SEM figure.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Equipment：KQ-50B type ultrasonic cleaners, magnetic stirring apparatuss, KH-2 type electrostatic spinning machines.
Embodiment 1
A. polyester slice is dissolved in into (the body of trifluoroacetic acid and dichloromethane in mixed solvent of the trifluoroacetic acid with dichloromethane
Product is than being 4: 1), magnetic agitation is carried out at room temperature 2 hours, prepares the Direct-spinning of PET Fiber liquid that mass percent concentration is 25%；
B. will add in the Direct-spinning of PET Fiber liquid obtained in step a and be dried to obtain too after titanate coupling agent dipping 10min
Pole stone microgranule and the appropriate isobutyl group caged silsesquioxane of dispersant eight so as to the mass percent concentration of middle Tai Ji stone microgranule
For 3%, the mass fraction of dispersant is 2%, then using ultrasonic Treatment 2 hours, obtains Tai Ji stone microgranule/Direct-spinning of PET Fiber
Liquid；
C. by the Tai Ji stone microgranule obtained in step b/Direct-spinning of PET Fiber liquid standing and defoaming, to mixed solution bubble-free；
D. by the Tai Ji stone microgranule/Direct-spinning of PET Fiber liquid obtained in step c by electrospinning process make Tai Ji stone microgranule/
Polyester nano fibrous membrane；Electrospinning parameters：Spinning temperature is 45 DEG C, and relative humidity is 30%, rate of flooding (fltting speed)
For 0.1mL/h, it is 15cm to receive distance, and spinning electrostatic pressure is 20KV；Reception device is Rotation of receiver, and reception speed is 20r/
min。
E. the Tai Ji stone microgranule/polyester nano fibrous membrane obtained in step d is put in vacuum drying oven, is done at 80 DEG C
Dry 2h, is cooled to after room temperature and obtains Tai Ji stone microgranule/polyester nano fibrous membrane.
Fig. 1 is that the Tai Ji stone microgranule for the preparing/polyester nano multifunctional fibre film in embodiment 1 amplifies 500 times
SEM schemes, and Fig. 2 is that the Tai Ji stone microgranule for the preparing/polyester nano multifunctional fibre film in embodiment 1 amplifies 10000 times
SEM scheme, from Fig. 1,2, obtained nano fibrous membrane has good fiber morphology.
Embodiment 2
A. polyacrylonitrile fibre is dissolved in dimethylacetamide solvent, mechanical agitation 1.5 is carried out in the case where being heated to 60 DEG C
Hour, prepare the polyacryl-nitrile spinning fluid that mass percent concentration is 15%；
B. will add in the polyacryl-nitrile spinning fluid obtained in step a and be dried to obtain after titanate coupling agent dipping 10min
Maifanite particle and the appropriate isobutyl group caged silsesquioxane of dispersant eight so as to the mass percent of middle maifanite particle
Concentration is 5%, and the mass fraction of dispersant is 1%, then using ultrasonic Treatment 2 hours, obtains maifanite particle/polypropylene
Nitrile spinning liquid；
C. by the maifanite particle obtained in step b/polyacryl-nitrile spinning fluid standing and defoaming, it is to mixed solution bubble-free
Only；
D. maifanite particle/the polyacryl-nitrile spinning fluid obtained in step c is made into Maifanitum by electrospinning process
Microgranule/polyacrylonitrile nanofiber film；Electrospinning parameters：Spinning temperature is 40 DEG C, and relative humidity is 30%, and rate of flooding is
0.1mL/h, it is 15cm to receive distance, and spinning voltage is 18KV；Reception device is Rotation of receiver, and reception speed is 30r/min.
E. the maifanite particle obtained in step d/polyacrylonitrile nanofiber film is put in vacuum drying oven, 100
2h is dried at DEG C, is cooled to after room temperature and is obtained maifanite particle/polyacrylonitrile nanofiber film.
Embodiment 3
A. polyester slice is dissolved in into (the body of trifluoroacetic acid and dichloromethane in mixed solvent of the trifluoroacetic acid with dichloromethane
Product is than being 4: 1), magnetic agitation is carried out at room temperature 2 hours, prepares the Direct-spinning of PET Fiber liquid that mass percent concentration is 25%；
B. will add in the Direct-spinning of PET Fiber liquid obtained in step a and be dried to obtain too after titanate coupling agent dipping 20min
Pole stone microgranule and jade microgranule, and the appropriate isobutyl group caged silsesquioxane of dispersant eight, Tai Ji stone microgranule is micro- with jade
The mass ratio of grain is 1: 1 so as to which the mass percent concentration of middle Tai Ji stone microgranule and jade microgranule is 5%, the quality of dispersant
Fraction is 3%, then using ultrasonic Treatment 3 hours, obtains Tai Ji stone microgranule/jade microgranule/Direct-spinning of PET Fiber liquid；
C. by the Tai Ji stone microgranule obtained in step b/jade microgranule/Direct-spinning of PET Fiber liquid standing and defoaming, to mixed solution without
Till bubble；
D. the Tai Ji stone microgranule obtained in step c/jade microgranule/Direct-spinning of PET Fiber liquid is made too by electrospinning process
Pole stone microgranule/jade microgranule/polyester nano fibrous membrane；Electrospinning parameters：Spinning temperature is 45 DEG C, and relative humidity is 30%,
Rate of flooding is 0.1mL/h, and it is 15cm to receive distance, and spinning voltage is 22KV；Reception device is Rotation of receiver, receives speed and is
40r/min。
E. the Tai Ji stone microgranule obtained in step d/jade microgranule/polyester nano fibrous membrane is put in vacuum drying oven,
2h is dried at 80 DEG C, is cooled to after room temperature and is obtained Tai Ji stone microgranule/jade microgranule/polyester nano fibrous membrane.
Embodiment 4
A. granule of polyvinyl alcohol is added in deionized water, heated and stirred is prepared to being completely dissolved under the conditions of 90 DEG C
Mass percent concentration is 10% polyvinyl alcohol spinning liquid；
B. the polyvinyl alcohol spinning liquid obtained in step a is added into what is be dried to obtain after titanate coupling agent dipping 20min
Maifanite particle, rare ice stone microgranule and jade microgranule, and the appropriate isobutyl group caged silsesquioxane of dispersant eight, Tai Ji stone
The mass ratio of microgranule, rare ice stone microgranule and jade microgranule is 1: 1: 1 so as to which middle maifanite particle, rare ice stone microgranule and jade are micro-
The mass percent concentration of grain is 6%, and the mass fraction of dispersant is 3%, then using ultrasonic Treatment 4 hours, obtains wheat
Meal stone microgranule/rare ice stone microgranule/jade microgranule/polyvinyl alcohol spinning liquid；
C. the maifanite particle obtained in step b/rare ice stone microgranule/jade microgranule/polyvinyl alcohol spinning liquid is stood de-
Bubble, to mixed solution bubble-free；
D. by the maifanite particle obtained in step c/rare ice stone microgranule/jade microgranule/polyvinyl alcohol spinning liquid by quiet
Electrical spinning method makes maifanite particle/rare ice stone microgranule/jade microgranule/polyvinyl alcohol nanofiber membrane；Electrospinning parameters：
Spinning temperature is 35 DEG C, and relative humidity is 30%, and rate of flooding is 0.3mL/h, and it is 15cm to receive distance, and spinning voltage is
18KV；Reception device is Rotation of receiver, and reception speed is 25r/min.
E. the maifanite particle obtained in step d/rare ice stone microgranule/jade microgranule/polyvinyl alcohol nanofiber membrane is put
Enter in vacuum drying oven, at 100 DEG C 2h is dried, be cooled to after room temperature that to obtain maifanite particle/rare ice stone microgranule/jade micro-
Grain/polyvinyl alcohol nanofiber membrane.
Comparative example 1
A. polyacrylonitrile fibre is dissolved in dimethylacetamide solvent, mechanical agitation 1.5 is carried out in the case where being heated to 60 DEG C
Hour, prepare the polyacryl-nitrile spinning fluid that mass percent concentration is 15%；
B. will add in the polyacryl-nitrile spinning fluid obtained in step a and be dried to obtain after titanate coupling agent dipping 10min
Maifanite particle and appropriate dispersant cetyl trimethylammonium bromide so as to the mass percent of middle maifanite particle is dense
Spend for 5%, the mass fraction of dispersant is 1%, then using ultrasonic Treatment 2 hours, obtain maifanite particle/polyacrylonitrile
Spinning liquid；
C. by the maifanite particle obtained in step b/polyacryl-nitrile spinning fluid standing and defoaming, it is to mixed solution bubble-free
Only；
D. maifanite particle/the polyacryl-nitrile spinning fluid obtained in step c is made into Maifanitum by electrospinning process
Microgranule/polyacrylonitrile nanofiber film；Electrospinning parameters：Spinning temperature is 40 DEG C, and relative humidity is 30%, and rate of flooding is
0.1mL/h, it is 15cm to receive distance, and spinning voltage is 18KV；Reception device is Rotation of receiver, and reception speed is 30r/min.
E. the maifanite particle obtained in step d/polyacrylonitrile nanofiber film is put in vacuum drying oven, 100
2h is dried at DEG C, is cooled to after room temperature and is obtained maifanite particle/polyacrylonitrile nanofiber film.
Comparative example 2
A. polyacrylonitrile fibre is dissolved in dimethylacetamide solvent, mechanical agitation 1.5 is carried out in the case where being heated to 60 DEG C
Hour, prepare the polyacryl-nitrile spinning fluid that mass percent concentration is 15%；
B. will add what is be dried to obtain after silane coupler dipping 10min in the polyacryl-nitrile spinning fluid obtained in step a
Maifanite particle and appropriate dispersant cetyl trimethylammonium bromide so as to the mass percent concentration of middle maifanite particle
For 5%, the mass fraction of dispersant is 1%, then using ultrasonic Treatment 2 hours, obtains maifanite particle/polyacrylonitrile and spins
Silk liquid；
C. by the maifanite particle obtained in step b/polyacryl-nitrile spinning fluid standing and defoaming, it is to mixed solution bubble-free
Only；
D. maifanite particle/the polyacryl-nitrile spinning fluid obtained in step c is made into Maifanitum by electrospinning process
Microgranule/polyacrylonitrile nanofiber film；Electrospinning parameters：Spinning temperature is 40 DEG C, and relative humidity is 30%, and rate of flooding is
0.1mL/h, it is 15cm to receive distance, and spinning voltage is 18KV；Reception device is Rotation of receiver, and reception speed is 30r/min.
E. the maifanite particle obtained in step d/polyacrylonitrile nanofiber film is put in vacuum drying oven, 100
2h is dried at DEG C, is cooled to after room temperature and is obtained maifanite particle/polyacrylonitrile nanofiber film.
Comparative example 3
A. polyacrylonitrile fibre is dissolved in dimethylacetamide solvent, mechanical agitation 1.5 is carried out in the case where being heated to 60 DEG C
Hour, prepare the polyacryl-nitrile spinning fluid that mass percent concentration is 15%；
B. maifanite particle and the appropriate isobutyl group of dispersant eight will be added in the polyacryl-nitrile spinning fluid obtained in step a
Caged silsesquioxane so as to which the mass percent concentration of middle maifanite particle is 5%, the mass fraction of dispersant is 1%, so
Adopt ultrasonic Treatment 2 hours afterwards, obtain maifanite particle/polyacryl-nitrile spinning fluid；
C. by the maifanite particle obtained in step b/polyacryl-nitrile spinning fluid standing and defoaming, it is to mixed solution bubble-free
Only；
D. maifanite particle/the polyacryl-nitrile spinning fluid obtained in step c is made into Maifanitum by electrospinning process
Microgranule/polyacrylonitrile nanofiber film；Electrospinning parameters：Spinning temperature is 40 DEG C, and relative humidity is 30%, and rate of flooding is
0.1mL/h, it is 15cm to receive distance, and spinning voltage is 18KV；Reception device is Rotation of receiver, and reception speed is 30r/min.
E. the maifanite particle obtained in step d/polyacrylonitrile nanofiber film is put in vacuum drying oven, 100
2h is dried at DEG C, is cooled to after room temperature and is obtained maifanite particle/polyacrylonitrile nanofiber film.
Embodiment 5, fibrous mechanical property is tested
To above example 1～4 and fiber obtained in comparative example 1～3 is carried out now as Mechanics Performance Testing, as a result such as table
Shown in 1：
Table 1
In the present invention, the performance of Static Spinning natural crystal nanoparticle/polymer nanofibre film not only with nanoparticle
Son structure particle diameter it is relevant, the interfacial structure performance of clustered pattern and synergisticing performance, particle and matrix also with nanoparticle and
Processing combination process etc. is relevant.How nano level natural crystal microgranule is evenly dispersed in into spinning liquid, in electrostatic spinning mistake
It is added to the inside of fiber in journey, is the key point of present invention research.As shown in Table 1, in the electrostatic spinning liquid of the present invention
In system, using eight isobutyl group caged silsesquioxanes as dispersant, it receives with the natural crystal after titanate coupling agent modified
The titanate coupling agent of rice microparticle surfaces plays cooperative effect, and playing natural crystal particle agglomeration and depositional same is prevented
When, also further such that modified natural crystal nanoparticle obtains good dispersion in spinning liquid so that obtained fibre
Dimension film has excellent fibrous mechanical property.
Above-described embodiment is interpreted as being merely to illustrate the present invention rather than limits the scope of the invention.Reading
After the content of record of the present invention, those skilled in the art can make various changes or modifications to the present invention, these equivalent changes
Change and modification equally falls into the scope of the claims in the present invention.
Claims (10)
1. a kind of preparation method of health care nanometer fibrous membrane, it is characterised in that methods described comprises the steps：
S1, natural crystal nanoparticle, dispersant in polymer dope after addition titanate coupling agent modified, ultrasound wave
Mix homogeneously, is obtained natural crystal nanoparticle/polymer dope；The dispersant is eight isobutyl group caged silsesquioxanes
Alkane；
S2, standing and defoaming, electrostatic spinning is cooled to room temperature after vacuum drying, obtain final product the health care nanometer fibrous membrane；The electrostatic
Spinning parameter is：Electrostatic pressure is 10～25KV, and fltting speed is 0.1～2mL/h, receives distance for 10～25cm, reception device
For Rotation of receiver, reception speed is 20～40r/min.
2. the preparation method of health care nanometer fibrous membrane as claimed in claim 1, it is characterised in that the natural crystal nanometer is micro-
The mass fraction of natural crystal nanoparticle is 1%～10% in grain/polymer dope.
3. the preparation method of health care nanometer fibrous membrane as claimed in claim 1, it is characterised in that the natural crystal nanometer is micro-
The particle diameter of grain is 20～100 nanometers.
4. the preparation method of the health care nanometer fibrous membrane as described in claim 1,2 or 3, it is characterised in that the natural crystal
The one kind or several of nanoparticle in tourmaline particles, rare ice stone microgranule, maifanite particle, jade microgranule, Tai Ji stone microgranule
Kind.
5. the preparation method of health care nanometer fibrous membrane as claimed in claim 1, it is characterised in that the natural crystal nanometer is micro-
The mass fraction of dispersant is 1%～3% in grain/polymer dope.
6. the preparation method of health care nanometer fibrous membrane as claimed in claim 1, it is characterised in that the polymer dope is
Mixed in a solvent by polymer dissolving；The polymer is selected from polyester, polyacrylonitrile, polyamide, polyurethane, glutinous
One or more in glue, polyvinyl alcohol.
7. the preparation method of health care nanometer fibrous membrane as claimed in claim 6, it is characterised in that the solvent is selected from amide-type
Compound, water, methanol, ethanol, n-butyl alcohol, isopropanol, hexafluoroisopropanol, trifluoroethanol, phenol, formic acid, acetic acid, trifluoro second
It is acid, dichloromethane, dichloroethanes, chloroform, acetone, tetrahydrofuran, pyridine, toluene, N-Methyl pyrrolidone, decahydronaphthalene
One or more in naphthalene, hexamethylene and Carbon bisulfide.
8. the preparation method of health care nanometer fibrous membrane as claimed in claims 6 or 7, it is characterised in that the polymer spinning
The mass fraction of polymer is 10%～30% in liquid.
9. the preparation method of health care nanometer fibrous membrane as claimed in claim 1, it is characterised in that the ultrasound wave mix homogeneously
In, the frequency of the ultrasound wave is 20～30KHz, and power is 300～500W, and process time is 2～4h.
10. the preparation method of health care nanometer fibrous membrane as claimed in claim 1, it is characterised in that described vacuum drying dry
Dry temperature is 80 DEG C～100 DEG C, and drying time is 1～4h.
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| CN109293341A (en) * | 2018-12-05 | 2019-02-01 | 北京福元保科技有限公司 | A kind of synthetic material and preparation method thereof based on Tai Ji stone |
| CN111534879A (en) * | 2020-05-21 | 2020-08-14 | 常州纺织服装职业技术学院 | Preparation method of badminton net fiber |
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Application publication date: 20170419 |