CN103132194A - Orientation electro-spinning nanometer fiber spinning method and device thereof - Google Patents
Orientation electro-spinning nanometer fiber spinning method and device thereof Download PDFInfo
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Abstract
The invention discloses an orientation electro-spinning nanometer fiber spinning method and a device thereof. A metal shower nozzle which exerts positive and negative high pressure is adopted to spin two strands of nanometer fibers with opposite charges, an electric field line of a spinning electric field, relative to a common spinning electric field, is straight, stability of spinning is effectively restrained, and the spinning nanometer fibers are straight. Two strands of the fibers surround the yarn tail and form a cone-shaped twisting trigonum on the upper portion of a metal twisting machine, and enable the nanometer fibers to be further oriented and twisted to form yarn through electric field force, tractive force of the yarn and acting force of the metal twisting force. The spinning nanometer fiber yarn is conducted heat shaping through a heat processing device under certain tensile force, degree of orientation of the nanometer fibers along the axial direction of the yarn, breaking force and yarn levelness are further improved, and the yarn after shaped is collected by a winding bobbin. The device can achieve the aim that orientation nanometer fiber yarn can be continuously prepared, is simple in device, convenient to operate, and good in resultant yarn continuity, yarn breaking strength and yarn levelness, and not only can spin pure nanometer fiber yarn, but also can spin nanometer fibers/ filament core composite yarn. The orientation nanometer fiber spinning method and the device thereof have important application value in the fields, such as a biomedical field and a sensor field.
Description
Technical field
The invention belongs to field of textiles, relate to a kind of orientation electro spinning nano fiber spinning method and preparation facilities thereof.
Background technology
Electrostatic spinning is the popular spining technology for preparing in recent years nanofiber.The electro spinning nano fiber diameter than the thin 100-1000 of traditional spinning fibre doubly, has huge specific area, at aspects such as filtering material, wound clad material, nano composite material, sensor, bio-medical materials, has wide practical use.Because the size of electrospinning fibre diameter and n cell epimatrix biological macromolecule material is close, its high specific area also provides ideal platform for effective release of active factors.Therefore, electro spinning nano fiber is particularly noticeable as the research of tissue engineering bracket, Antiadhesive film, wound repair material, artificial blood vessel etc.Electrospinning collagen, fibroin albumen, chitin nanofiber have been used for building the research of blood vessel, bone tissue engineering scaffold and human body repair materials by scientist.
Owing to being subject to the crooked instable restriction of charged jet, electro spinning nano fiber is collected with the form of nonwoven fabric usually, and there is very large problem in the disordered structure of fiber in the application aspect the device fabrication that needs regular arrangement and height-oriented structure such as microelectronics, photonic propulsion etc.Realize that the orientations of electro spinning nano fiber also contributes to improve the mechanical property of electrospinning support, significant in the tissue engineering bracket preparation.Simultaneously, in the building process such as tissue engineering nerve, tendon, muscle, the support with orientations fibre structure can guide cell directional migration and growth, and finally controls the structure of regenerating tissues.Therefore, with the fiber of non-weaving cloth form, compare, separable orientation electro spinning nano fiber yarn Application Areas is more extensive each other.
For collecting orientations electro spinning nano fiber boundling resultant yarn, many researchers explore.Some researchers adopt the water-bath mode to collect, with static state or collect electro spinning nano fiber with the water of whirlpool, fiber is orientated under the active force of water, then it is wound up on the cylinder of rotation and obtains continuous yarn (Teo W, Gopal R, Ramaseshan R, et al.POLYMER.2007,48 (12): 3400-3405.).This method is resultant yarn continuously, and can more automatically to fiber, carry out stretch orientation, is a kind of good method, but device is more complicated, and is not suitable for water-soluble polymer.Also there are some researchers to adopt auxiliary electrode to collect.As adopting two metal rings that are arranged in parallel as receiving system, this method is easy to obtain the nanofiber of orientations, reproducible, and the impact that changed by electric-field intensity is less.One of them is received to ring is connected with the stainless steel tube that scribbles Teflon, stainless steel tube drives and receives the ring rotation under the driving of motor, can obtain diameter and be less than 5 microns, length is at multiple PCL fiber filament bundle (the Dalton P D of the distortion of 50mm, Klee D, Moller M.POLYMER.2005,46 (3): 611-614.).Yan etc. connect motor reversed turning by two metal rings that are arranged in parallel, and after the nanofiber twisting that is arranged in parallel of collection, by the bobbin between two annulus, are reeled and are collected.This method can realize continuous production oriented nanofibers yarn, but the nanofiber waste is more, and the larger twist has affected orientation (Yan H, the Liu L of fiber, Zhang Z.MATERIALS LETTERS.2011,65 (15-16): 2419-2421.).
In U.S. Pat 2009324950-A1, Kim etc. utilizes the disk orientation to collect the electrospinning fibre of a plurality of shower nozzles ejections, then fibre bundle is stripped coiling and be gathered into the oriented nanofibers yarn, this yarn has certain brute force, but yarn texture is loose, and bar is dry poor.In U.S. Pat 6106913-A, Balonis etc. utilizes flow deposition to the guiding long filament the electrospinning fibre of a shower nozzle ejection, reels and makes high-tenacity nanofiber cladded yarn through traction, and utilize this yarn to be woven into the nanofiber device.The method affects fiber laydown efficiency because like charges between nanofiber repels mutually.In Chinese patent CN200710021149.8, the employing macromolecule long filament such as Li Xinsong or yarn are the core seal wire, one or more pairs of spinning head conjugate spinnings prepare nanofiber, the nanofiber of the spinning head ejection that spout is relative is with opposite charges, aloft attract each other, be deposited on the core seal wire, traction is reeled and is made the High tenacity yarn of surperficial clad nano fiber.The method makes yarn does not have the twist, loosely organized, and bar is dry poor.In published Chinese invention patent CN101974814A, the chitosan solution electrostatic spinning is prepared to nanometer chitosan fiber, cotton yarn or the dimity are passed through and receive nanometer chitosan fiber between the anode of electrostatic spinning apparatus and negative electrode, make the complex yarn product.In current disclosed nano-fibre yams preparation method, exist the nanofiber degree of orientation lower, poor continuity, fiber are wasted more and yarn mechanical performance and the dry poor shortcoming of bar.
Therefore, be necessary to invent a kind of nanofiber high to the degree of orientation in yarn axis, good mechanical property, the fiber waste is few, oriented nanofibers yarn preparation method and device that bar makes a good job of.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of orientation electro spinning nano fiber spinning method and device thereof, by applying respectively positive or negative high voltage on the spinning head of relative configuration and spraying charged jet, form respectively the nanofiber with positive and negative charge after erratic process, below configuration neutral metal twister in shower nozzle, the metal twister polarizes in high-voltage electrostatic field, under the electrostatic induction effect, make near on a side band of shower nozzle with the opposite polarity electric charge of this shower nozzle, and collect to metal twister one side near this shower nozzle with the nanofiber of shower nozzle band like charges.Two strands of nanofibers with positive and negative charge are drawn from the metal twister, by metal twister rotation twisting, and, by after annealing device, reeling and collect, make the orientation electro spinning nano fiber yarn with good strength and extension property.
Technical scheme: a kind of orientation electro spinning nano fiber spinning method of the present invention adopts configuration relatively and applies respectively the Metallic Nozzle At The Ingot 8 charged jets of injection of positive or negative high voltage and solidify to form nanofiber.This Metallic Nozzle At The Ingot 8 forms the spinning electric field with metal twister 9 to be seen shown in Fig. 2 a, and wherein the zone between Metallic Nozzle At The Ingot 8 and metal twister 9 is spinning boundling resultant yarn zone.Common needle plate spinning electric field is shown in shown in Fig. 2 b, and the zone in figure between Metallic Nozzle At The Ingot 8 and metal plate 14 is the spinning zone.As can be seen from Figure 2 spinning electric field lines of the present invention is relatively straight, suppressed the crooked unstability of spinning jet, thereby make more straight nanofiber, nanofiber further better is orientated under the effect of spinning electric field, twister and yarn tractive force, thereby makes the nano-fibre yams that the degree of orientation is high.
Spinning method of the present invention is applicable to solution and melting electrostatic spinning, spinning material both can adopt the fiber-forming polymer material as polyester (PET), polyvinyl alcohol (PVA), polyacrylonitrile (PAN), poly-(6-caprolactone) (PCL) etc., also can adopt the natural material extract as collagen (Collagen), fibroin albumen (Silk fibroin) etc., also can adopt two or more raw materials mixing and doping function nano material as CNT (MWNTs), titanium dioxide (TiO
2) and zinc sulphide (ZnS) etc.The method both can be spun pure nano-fibre yams, but also spinning nano fibre is shell, the nanofiber/filament core-spun yarn with good strength and extension property that long filament is sandwich layer.
A kind of orientation electro spinning nano fiber spinning apparatus, comprise conjugation electrospinning filament forming device, orientation twisting apparatus, yarn heat treating apparatus and coiling gathering-device, and the apparatus structure schematic diagram as shown in Figure 1.Conjugation electrospinning filament forming device, adopt polymer solution and melt as spinning material, and raw material is by former material conveying pump 7 from relative configuration Metallic Nozzle At The Ingot 8 outputs, and transporting velocity is 0.1～30.0ml/h.Metallic Nozzle At The Ingot 8 applies respectively positive or negative high voltage, and voltage value is 6kV～50kV.The shower nozzle quantity that applies identical high pressure can be single head, can be also bull, and shower nozzle quantity is 1～100.Metallic Nozzle At The Ingot 8 with positive or negative high voltage configures relatively, the long 20～55mm of Metallic Nozzle At The Ingot 8, and diameter 0.2～0.9mm, configure Metallic Nozzle At The Ingot 8 distance 120～300mm relatively.Charged jet is taken out after long drawing-down to relative dispenser nozzles 8 cores motions through stable and unstable stage under the effect of high-voltage electrostatic field, during follow spin solvent volatilization or melt cooling to solidify to form the nanofiber 6 that diameter is 50～1000nm diameter.
The orientation twisting apparatus is configuring Metallic Nozzle At The Ingot 8 central lower 20～70mm places configuration diameter 50～90mm metal twisters 9 relatively, and metal twister 9 can be discoid or arch.The metal twister is neutral, and in applying positive or negative high voltage shower nozzle 8 formation high-voltage electrostatic fields, after electrostatic induction, near shower nozzle one side band and shower nozzle opposite charges, shower nozzle ejection nanofiber 6 is to a lateral movement of metal twister 9 close shower nozzles 8.Metal twister 9 center drillings, draw a core silk 10 with the linear velocity of 5～200m/h, and metal twister 9 is with the speed revolution of 10～900rpm simultaneously.Nanofiber 6 will be at electric field force, under long filament tractive force and metal twister active force, around core silk 10, forms coniform twist triangle zone 5.Conjugation electrospinning filament forming device constantly sprays nanofiber 6 and, in coniform twist triangle zone 5 cohesion twisting, the yarn after twisting constantly is pulled roller 3 and pulls out formation nano fibre yarn 4, fineness of yarn 15～500dtex.If prepare pure nano-fibre yams, after the cladded yarn resultant yarn is stable, long filament 10 is drawn in metal twister 9 centers cuts off and gets final product before twist triangle zone 5, pure nano-fibre yams fineness 5～450dtex, yarn evenness 5～10CV%, yarn breaking force 3～120cN.
Winding bobbin 1 is 1.2～1: 1 with traction roller 3 linear velocity ratios, thereby makes nano fibre yarn pass through yarn heat treating apparatus 2 under some tension.Annealing device 2 can be the cylinder of a heating, and in cylinder, 60～320 ℃ of temperature are adjustable; Or hot water storgae, in groove, the hot water temperature is 60～98 ℃.The nano fibre yarn 4 drawn is processed 3～400s in annealing device 2, so that nanofiber 6 makes yarn strength be improved further along yarn 4 axial orientations, also makes yarn meet bio-medical or sensor application requirements.Winding bobbin 1 is wound into cop by the yarn after heat treatment with the linear velocity of 5～200m/h.
Beneficial effect: the present invention compared with prior art, has following advantage:
(1) a kind of orientation electro spinning nano fiber spinning method of the present invention, the relatively common spinning electric field of spinning electric field line is straight, effectively suppresses the spinning unstability, spins to such an extent that nanofiber is straight; And make nanofiber further be orientated by electric field force, yarn tractive force and metal twister active force.The present invention can continuous production nanofiber or nanofiber/filament core-spun yarn, and it is higher to the degree of orientation along yarn axis to make in yarn nanofiber.
(2) a kind of orientation electro spinning nano fiber spinning apparatus of the present invention, adopt the Metallic Nozzle At The Ingot that applies respectively positive or negative high voltage to spin to obtain the oppositely charged nanofiber, two strands of nanofibers form conical twist triangle zone twisting resultant yarn on metal twister top around the yarn tail.This device for spinning is simple, easy to operate, and the resultant yarn continuity is good, and yarn breaking force, bar are done better.
(3) a kind of orientation electro spinning nano fiber spinning apparatus of the present invention, adopting winding bobbin is 1.2～1: 1 with traction roller linear velocity ratio, make nano fibre yarn under some tension by the annealing device HEAT SETTING, further improve nanofiber along yarn axis to the degree of orientation and ultimate strength and the bar of yarn dry.
The accompanying drawing explanation
Fig. 1 is orientation electro spinning nano fiber spinning apparatus structural representation of the present invention.In Fig. 1, have: the 1-winding bobbin; The 2-annealing device; The 3-traction roller; The 4-nano fibre yarn; The 5-twist triangle zone; The 6-nanofiber; The former material conveying pump of 7-; The 8-Metallic Nozzle At The Ingot; 9-metal twister; 10-core silk; The 11-twizzle; The 12-high-voltage DC power supply; 13-long filament bobbin.
Fig. 2 is electro spinning nano fiber spinning apparatus spinning electric field schematic diagram of the present invention, and a is that conjugation electrospinning pin pin electrode and metal twister form electric field, and b is that needle plate electrode forms electric field.
Fig. 3 is nanofiber cladded yarn photo of the present invention, and a is the cladded yarn optical microscope photograph; B is cladded yarn cortex nanofiber electron scanning micrograph, the 14-metal plate.
The specific embodiment
Describe technical scheme of the present invention in detail below in conjunction with accompanying drawing.The embodiment of the present invention is only for the explanation concrete grammar, and the method is not subject to the restriction of embodiment.
Embodiment 1
Adopting polyvinyl alcohol (PVA) aqueous solution that mass percent concentration is 10% is spinning solution, speed with 1ml/h is extruded from Metallic Nozzle At The Ingot 8 by former material conveying pump 7, apply 8kV positive or negative high voltage electricity by high pressure generator 12 respectively on two Metallic Nozzle At The Ingots 8 of configuration relatively, the long 30mm of Metallic Nozzle At The Ingot, diameter 0.5mm, spacing 150mm.Spinning solution is taken out long drawing-down through stable and unstable stage and is formed nanofiber 6 under the effect of high-voltage electrostatic field, to metal twister 9, near a side of shower nozzle 8, collects.Core silk 10 is 100dtex PLA (PLA) long filament, from 13 unwindings of long filament bobbin, through twizzle 11, passes metal twister 9 centers.Metal twister 9 rotating speed 20rpm, long filament 10 linear velocity 5m/h.Two strands of nanofibers 6 with positive and negative charge form conical twist triangle zone 5 around long filament 10 on metal twister 9 respectively, add after being twisted nanofiber/long filament cored composite yarn 4 and drawn by traction roller, after the annealing device 2 that is 100 ℃ through excess temperature, by winding bobbin, with the linear velocity of 5.55m/h, be wound into cheese.As shown in Figure 3, wherein a is the cladded yarn optical microscope photograph to gained cladded yarn photo, and in figure, polyvinyl alcohol nano coats good to PLA core silk; B is the cladded yarn electron scanning micrograph, and in figure, polyvinyl alcohol nano is good along the yarn axial orientation.Cladded yarn fineness 123dtex, ultimate strength 89cN, bar evenness is 7.2CV%.
Embodiment 2
Adopt polyester (PET) section for spinning material, melting at 340 ℃ of temperature, melt is extruded from Metallic Nozzle At The Ingot 8 by former material conveying pump 7 with the speed of 5ml/h, apply 18kV positive or negative high voltage electricity by high pressure generator 12 respectively on eight Metallic Nozzle At The Ingots 8 of configuration relatively, the long 35mm of Metallic Nozzle At The Ingot, diameter 0.7mm, spacing 180mm.Polymer melt is taken out long drawing-down through stable and unstable stage and is formed nanofiber 6 under the effect of high-voltage electrostatic field, to metal twister 9, near a side of shower nozzle 8, collects.Core silk 10 is 92dtex terylene (PET) long filament, from 13 unwindings of long filament bobbin, through twizzle 11, passes metal twister 9 centers.Metal twister 9 rotating speed 80rpm, core silk 10 linear velocity 20m/h.Two strands of nanofibers 6 with positive and negative charge form conical twist triangle zone 5 around long filament 10 on metal twister 9 respectively, after spinning is stable, from metal twister 9 bottoms, cut off polyester filament.Add after being twisted pure nano-fibre yams 4 and drawn by traction roller 3, then be wound into cheese by winding bobbin with the linear velocity of 23m/h after the water-bath annealing device 2 that is 95 ℃ through excess temperature.Gained nano-fibre yams fineness 34dtex, ultimate strength 26cN, bar evenness is 6.2CV%.
Claims (10)
1. one kind is orientated the electro spinning nano fiber spinning method, apply respectively positive or negative high voltage and spray charged jet on the spinning head that it is characterized in that relatively configuring, form respectively two strands of nanofibers with positive and negative charge after erratic process, below configuration neutral metal twister in shower nozzle, the metal twister polarizes in high-voltage electrostatic field, under the electrostatic induction effect, make near on a side band of shower nozzle with the opposite polarity electric charge of this shower nozzle, and collect to metal twister one side near this shower nozzle with the nanofiber of shower nozzle band like charges.Two strands of nanofibers with positive and negative charge are drawn from the metal twister, by metal twister rotation twisting, and, by after annealing device, reeling and collect, make the orientation electro spinning nano fiber yarn with good strength and extension property.
2. a kind of orientation electro spinning nano fiber spinning method according to claim 1, it is characterized in that the relative Metallic Nozzle At The Ingot that configures and apply respectively positive or negative high voltage forms the relatively common needle plate spinning of electric field lines electric field straight, obtain more straight fiber thereby suppressed the crooked unstability of spinning jet, fiber further is orientated under the effect of spinning electric field, twister and yarn tractive force.
3. a kind of orientation electro spinning nano fiber spinning method according to claim 1, it is characterized in that being applicable to solution solvent and melting electrostatic spinning, spinning material both can adopt the fiber-forming polymer material as polyvinyl alcohol (PVA), polyacrylonitrile (PAN), poly-(6-caprolactone) (PCL), polyester (PET) etc., also can adopt the natural material extract as collagen (Collagen), fibroin albumen (Silk fibroin) etc., also can adopt two or more raw materials mixing and doping function nano material as CNT (MWNTs), titanium dioxide (TiO
2) and zinc sulphide (ZnS) etc.
4. a kind of orientation electro spinning nano fiber spinning method according to claim 1, it is characterized in that both can spinning pure nano-fibre yams, but also spinning nano fibre is shell the cladded yarn with good strength and extension property that long filament is sandwich layer.
5. an orientation electro spinning nano fiber spinning apparatus, comprise conjugation electrospinning filament forming device, orientation twisting apparatus, yarn heat treating apparatus and coiling gathering-device.
6. conjugation electrospinning filament forming device according to claim 5, is characterized in that adopting polymer solution and melt as spinning material, and raw material is exported from relative configuration Metallic Nozzle At The Ingot by delivery pump, and transporting velocity is 0.1～30.0ml/h; Metallic Nozzle At The Ingot applies respectively positive or negative high voltage, and voltage value is 6kV～50kV, and the shower nozzle quantity that applies identical high pressure can be single head, can be also bull, and shower nozzle quantity is 1～100.Metallic Nozzle At The Ingot with positive or negative high voltage configures relatively, the long 20～55mm of Metallic Nozzle At The Ingot, and diameter 0.2～0.9mm, configure Metallic Nozzle At The Ingot distance 120～300mm relatively.Charged jet under the effect of high-voltage electrostatic field through stable and unstable drawing-down and to the motion of shower nozzle core, during follow spin solvent volatilization or melt cooling to solidify to form the fiber that diameter is 50～1000nm diameter.
7. twisting apparatus according to claim 5, is characterized in that relatively configuring Metallic Nozzle At The Ingot central lower 20～70mm place configuration diameter 50～90mm metal twister, and the metal twister can be discoid or arch.The metal twister is neutral, and in applying positive or negative high voltage shower nozzle formation high-voltage electrostatic field, after electrostatic induction, near shower nozzle one side band and shower nozzle opposite charges, shower nozzle ejection nanofiber is to a lateral movement of the close shower nozzle of metal twister.Metal twister center drilling, draw a threads with the linear velocity of 5～200m/h, and the metal twister is with the speed revolution of 10～900rpm simultaneously.Nanofiber will form coniform twist triangle zone around long filament under electric field force, long filament tractive force and metal twister active force.
8. twisting apparatus according to claim 5, it is characterized in that conjugation electrospinning one-tenth silk part constantly sprays nanofiber and twists at coniform twisting partial agglomeration, yarn after twisting constantly is pulled out formation nanofiber/long filament cored composite yarn, fineness of yarn 15～500dtex.If prepare pure nano-fibre yams, after the cladded yarn resultant yarn is stable, long filament is drawn in metal twister center and cut off and get final product before twist triangle zone, pure nano-fibre yams fineness 5～450dtex.
9. yarn heat treating apparatus according to claim 5 is characterized in that by yarn 60～320 ℃ of lower heat treatments, or processes 3～400s in 60～98 ℃ of hot water that, so that nanofiber further is orientated, the yarn strength bar is dry to be improved.
10. coiling gathering-device according to claim 5, is characterized in that the yarn after heat treatment is wound into to cop with the linear velocity of 5～200m/h.
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