CN1537981A - Coaxial composite continuous nano/micron fiber and its preparation method - Google Patents
Coaxial composite continuous nano/micron fiber and its preparation method Download PDFInfo
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- CN1537981A CN1537981A CNA2003101081309A CN200310108130A CN1537981A CN 1537981 A CN1537981 A CN 1537981A CN A2003101081309 A CNA2003101081309 A CN A2003101081309A CN 200310108130 A CN200310108130 A CN 200310108130A CN 1537981 A CN1537981 A CN 1537981A
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Abstract
A coaxially composite continuous nano/micron fibre material is composed of core and surface layer, which are coaxial. Its preparing process includes such steps as respectively dissolving core material and surface layer material, loading them respectively in coaxial two containers with fine spray tube at lower end, respectively applying high-voltage DC electric field to them for driving them to be sprayed out via respective spray tubes to become coaxial composite fibre, and collected by a grounded collector.
Description
Technical field
The present invention relates to a kind of nano/micron material, specifically is a kind of coaxial compound continuous nano/micron fiber and preparation method thereof.
Background technology
Two kinds of materials is coaxial compound rather than mix and be combined into a kind of bar or filamentary material, can satisfy numerous demands of industrial cut stock or daily life aspect.Most typical is pencil, top layer and core matter be two kinds of different materials coaxial compound be a bar.When the diameter of this coaxial coupled pole line reached several microns or the following magnitude of micron, its Application Areas was then very extensive.
Although existing many maturation process aspect the preparation of the coaxial coupled pole line (such as pencil) of large scale, yet this class technology also is not suitable for the preparation of ultra-fine (the following magnitude of several microns to micron) coaxial composite fibre.By the spining technology in the conventional textile industry such as dry method or the resulting fibre diameter of wet spinning generally also all more than 7 microns, and fiber generally all is that the mixing of single or multiple material is compound.In the application of considering such as the coated cloth of burned body, the fiber of more tiny diameter will help the rapid degraded and absorbed of organism and the controlled release of antibiotic medicine.This is because the surface fibre that contact with wound face, and it is degraded fully and finish within the time of relatively lacking.This just requires the filametntary diameter must be very tiny, reaches the following or nanometer scale of micron.
Method of electrostatic spinning (Electrospinning) be the preparation super-fine continuous fibre a kind of efficient ways (Huang is contended, Y.-Z.Zhang, M.Kotaki, and S.Ramakrishna, A Review on Polymer Nanofibers byElectrospinning and Their Applications in Nanocomposites, Comp.Sci.﹠amp; Tech., 2003, Vol.63, pp.2223-2253).It is by high voltage electric field being added in the polymer solution, driving the latter and sentence the collecting device of vaporific directive ground connection from capillary outlet.In course of injection, vaporific polymer solution jet attenuates rapidly also and then solidifies and changes superfine fibre into.(contend etc., Comp.Sci.﹠amp by Huang between 3 to 3000 nanometers for spun filametntary diameter; Tech., 2003, Vol.63, pp.2223-2253).Yet, spun fiber all be that mixing material by single polymers or multiple polymers obtains basically.Recently, people such as Ripoll proposes a kind of inside and is food additives, outsidely can reaches nano level subparticle (Ripoll et al., Interational Publication Number:WO 02/060275A1 for coated capsule, diameter; International Application Number:PCT/US02/02787).But this only is particle, is not continuous fibers.Up at present, also find the continuous coaxial composite superfine of preparation (diameter be that micron is following arrive several micron orders) fiber
The report of embodiment.
Summary of the invention
The objective of the invention is to propose a kind of raw material wide material sources, cheap for manufacturing cost, continuous coaxial compound nano/micron fibrous material and preparation method thereof.
The coaxial compound continuous nano/micron fibrous material that the present invention proposes, by two kinds of coaxial being composited of different materials of top layer and core matter, its core matter is solid or fluent material, the top layer is polymer or is the composite of carrier with the polymer, the diameter of fiber is between several nanometers are to several microns, for example be between 3 nanometers to 10 micron, between 5 nanometers to 5 that more then is micron.
1), the single polymer (polymer that comprises biodegradable and non-degraded the top layer of above-mentioned fiber and core material itself can be separately:, and antibiotic, drug material such as antiviral), 2), the mixture of multiple polymers, 3), the mixture of polymer and metal, 4), the mixture of polymer and pottery.
In general, the core material can adopt various external applications or innerlich anwenden thing and various antibiotic, antiviral material, and the polymeric material that can be absorbed by biodegradation is adopted on the top layer.This fiber can be used for aspects such as disease treatment, health, protection.
The continuous coaxial compound nano/micron fiber preparation method that the present invention proposes is, adopt method of electrostatic spinning, in core matter and skin-material solution, apply identical or different high-voltage dcs respectively, electric-field intensity is that some kilovolts are to tens kilovolts (as 2 kilovolts to 60 kilovolts), make that the jet that ejects the jet pipe of core matter liquid and top layer liquid but different-diameter coaxial from two is concentric stratified flow, the internal diameter of jet pipe is below 2 millimeters; Again under the electric field force effect, through high frequency draw, crooked whipping distortion and be cured as ultra-fine coaxial composite fibre, by the collecting device collection of ground connection (perhaps forming potential difference) with the high-voltage dc that is applied in the liquid.
The device that uses is made of a supporting coaxial composite tanks and a multiple tube of bilayer, and its structure as shown in Figure 1.It has in one, and flow container 2 is coaxial to place outer flow container 4, inside and outside flow container funnel, and the lower end of outer flow container 4 is outer liquid jet pipe 6, the lower end of interior flow container 2 is interior liquid jet pipe 5, between the interior outer nozzle certain interval is arranged.Generally, the internal diameter of inner nozzle 5 is 0.1～1.0 millimeter, outward through being 0.2～1.4 millimeter, and the internal diameter of outer nozzle 6 then is 0.3～1.8 millimeter.
According to shown in Figure 1, the detailed process for preparing continuous coaxial composite ultrafine fiber further specifies as follows.
In the flow container 2, skin-material liquid 3 placed in the outer flow container 4 in core material liquid 1 placed.(thousands of lie prostrate tens thousand of volts) DC electric field 8 and 9 adds high pressure in core matter liquid 1 and top layer liquid 3 respectively.When electric-field intensity was enough to overcome the surface tension of core matter liquid and top layer liquid, they just were driven respectively ejaculation from jet pipe (capillary) 5 that is connected with interior flow container 2 and outer flow container 4 and nozzle needle 6.Because inner nozzle is coaxial to be placed in the outer nozzle, the jet that sprays from two jet pipes is concentric stratified flow.Under the effect of electric field force, this jet produces distortion such as the drawing of high frequency, crooked whipping, makes that (0.3～1.8mm) attenuates rapidly and solidifies is transformed into ultra-fine coaxial composite fibre 7, is collected by the collecting device 10 of ground connection for the diameter of initial jet.Certainly, collecting device 10 also may not ground connection, and only the electrode that need be connected with this device is just passable with electrode 8 that is applied to liquid and 9 formation potential differences.
(core matter is Compressed Gas or volatilizable liquid, perhaps blocks the outlet of inner nozzle) under special circumstances, resultant fiber is exactly hollow continuous Nano/micro tube.
Concrete preparation method is as follows: inject Compressed Gas or volatile liquid in core matter jar, in skin-material solution, apply high-voltage dc (placing respectively in core matter and the skin-material liquid) such as the contact rod that will connect dc source, electric-field intensity is that some kilovolts are to tens kilovolts (as 2 kilovolts to 60 kilovolts), make the skin-material jet that ejects from outer nozzle envelope Compressed Gas or volatile liquid core matter, the internal diameter of jet pipe is below 2 millimeters; Again under the electric field force effect, through high frequency draw, crooked whipping distortion and be cured as ultra-fine hollow fibre, by the collecting device collection of ground connection (perhaps forming potential difference) with the high-voltage dc that is applied in the liquid.
Perhaps adopt following method: the inner nozzle outlet is blocked, only puts skin-material solution and apply high-voltage dc in the flow container outside, electric-field intensity is that some kilovolts are to tens kilovolts (as 2 kilovolts to 60 kilovolts), make that the skin-material jet that ejects from outer nozzle is a hollow annular stream, the internal diameter of jet pipe is below 2 millimeters; Again under the electric field force effect, through high frequency draw, crooked whipping distortion and be cured as ultra-fine hollow fibre, by the collecting device collection of ground connection (perhaps forming potential difference) with the high-voltage dc that is applied in the liquid.
The ultra-fine coaxial composite fibre that goes out produced according to the present invention because its diameter is tiny, specific area is high, functionalization is easy, is very suitable for the application at aspects such as medicine, fine filtering, biochemistry protection.Such as with the medicinal polymer of making the core material, can being degraded by bio-absorbable of antibiotic as skin-material, be prepared into the nonwoven gauze, paste at burn and wait the extensive wound position, just can remove from and change dressings, take off the huge misery that gauze brings to this class patient; For another example with this fibre bundle that includes the antibiotic medicine as operation suture thread, just can realize the controlled release of medicine, thereby mechanical stitch and biochemical treatment are combined together, will bring optimum efficiency to patient's wound healing; Again such as antiviral material being used as the core material, nontoxic to human body, harmless, scentless general polymer being used as skin-material, be prepared into nonwoven fabric, make mouth mask, protective clothing etc., just not only can isolate harmful virus to the infringement of human body, but also can not bring any discomfort to human body because of the defective of isolated material itself.Other application comprises being that the inorganic ceramic of carrier or metal are got and made skin-material with the polymer, handles through high temperature cabonization again, prepares the pottery or the ultra-fine pipe of metal of big L/D ratio.Find out that by schematic diagram 1 technology of the coaxial composite ultrafine fiber of preparation that the present invention proposes has that preparation technology is simple, equipment cost is cheap, wide advantage is used in market, has very considerable economic and social benefit.
Description of drawings
Fig. 1 is coaxial compound nano/micron fiber schematic diagram for method of electrostatic spinning prepares.
Number in the figure; 1 is core material liquid, and 2 is interior flow container, and 3 is skin-material liquid, and 4 is outer flow container, and 5 is interior liquid jet pipe, and 6 is outer liquid jet pipe, and 7 is coaxial composite fibre, and 8 are the voltage on the liquid in being added to, and 9 for being added to the voltage on the outer liquid, and 10 is collecting device.
The specific embodiment
The embodiment that the invention is further illustrated by the following examples.
Embodiment 1
A certain amount of Cefoxitin (Mefoxin, a kind of antibiotic and anti-infective medication) is dissolved in the dichloromethane solution of the amorphous PLA that concentration is 5%w/v (PDLA, molecular weight 100,000), and making its percentage by weight is 1%.The PLA solution that contains Cefoxitin will be as interior spinning solution.Weight concentration is 13%, molecular weight is that polycaprolactone carrene-dimethyl formamide (by 75: 25 weight ratio) solution of 80,000 is as outer spinning solution.The internal diameter of interior liquid nozzle needle is 0.3mm, and external diameter is 0.6mm; The internal diameter of outer liquid nozzle needle is 0.8mm, and external diameter is 1.2mm.Institute's making alive is 18 kilovolts.The two coaxial cospinning on the aluminium-foil paper of ground connection, is obtained having micron compress of receiving of controlled, sustained antibiotic effect.
Accurately take by weighing derivative one gelatin (Gelatin, type A) of a certain amount of natural macromolecular collagen, make its stirring and dissolving in trifluoroethanol (2,2,2-Trifluoroethanol TFE) obtains the Gelatin/TFE solution that concentration is 5%w/v in the organic solvent, be used as skin-material; Again with the polycaprolactone of 10%w/v (Polycaprolacton, PCL)/TFE solution is as the core material.The two coaxial cospinning (spinning condition: electric-field intensity 0.7KV/cm, spinning nozzle is 15cm with receiving the filament plate spacing, environmental condition: 20 ℃ of temperature, relative humidity: 75%, the nozzle needle diameter is the same), can obtain the modification of monofilament horizontal surface ultra-fine nano/micron fiber.Cell culture experiments shows, with the surface not the non-hydrophily polycaprolactone of the electrospinning nano/micron fiber of functionalization compare, the polycaprolactone nano/micron tunica fibrosa that monofilament horizontal surface functionalization is crossed has good cell compatibility and compatibility.This surface-functionalized fiber can be played effectiveness in application such as bleeding-stopping dressing and tissue engineering bracket material.
With Single Walled Carbon Nanotube (SWNT) lauryl sodium sulfate (Sodium dodecyl sulfate, SDS) making dispersant disperses in water under ultrasound condition, through constituent optimization, the 0.35wt% Single Walled Carbon Nanotube is dispersed in the aqueous solution of 1wt% lauryl sodium sulfate (as liquid in the spinning).With molecular weight be 120,000 degree of hydrolysis reach 99% polyvinyl alcohol (Polyvinyl alcohol, PVA) in 80 ℃ of deionized waters dissolving join the poly-vinyl alcohol solution (as outer spinning solution) of 10wt%.With the two coaxial cospinning (25 kilovolts of high pressure, the nozzle needle diameter is the same, 10 centimetres of spacings), obtain including the nano composite material fiber that CNT (carbon nano-tube) strengthens then, improved the mechanics and the electrology characteristic of fiber.
With a certain amount of molecular weight is that 500,000 polyvinyl acetate (PVac) is dissolved in N, and dinethylformamide (DMF) is joined to such an extent that concentration is spinning solution in the PVac/DMF of 10wt%.The process for preparation of outer spinning solution is: measure 10 gram 10wt%PVac/DMF solution, with 2.5 gram isopropyl titanates (TiP) and 1 gram acetic acid (HAc) respectively under strong agitation this solution of adding obtain clear solution (solution A).By hydrochloric acid (HCl) is added drop-wise in the tetraethoxysilane (TEOS), and continue to stir 2 hours, can make silica gel solution (solution B).Then, measure 2.5 gram silica gel solution (solution B) agitation and dropping to clear solution (solution A), obtain the outer spinning solution of yellow transparent at last.Inside and outside spinning solution adds 20 kilovolts, and spacing reaches coaxial cospinning under 15 centimetres of conditions (the nozzle needle diameter is the same), obtains the compound nano/micron fiber of core-shell structure.Through high temperature (1200 ℃) calcining, carbonization, can obtain hollow nano/micron ceramic fibre again.
Claims (7)
1, a kind of coaxial compound continuous nano/micron fiber, it is characterized in that by top layer and two kinds of coaxial being composited of different materials of core matter, its core matter is solid or fluent material, and the top layer is polymer or is the composite of carrier with the polymer, and the diameter of fiber is between 3 nanometers to 10 micron.
2, fiber according to claim 1,1), single polymer it is characterized in that top layer and core matter a kind of of following material that respectively do for oneself:, 2), the mixture of multiple polymers, 3), the mixture of polymer and metal, 4), the mixture of polymer and pottery.
3, fiber according to claim 1 is characterized in that the core material is various external applications or innerlich anwenden thing and various antibiotic, antiviral material.
4, fiber according to claim 1 is characterized in that boring.
5, a kind of as fiber preparation method as described in one of in the claim 1 to 3, it is characterized in that adopting method of electrostatic spinning, in core matter and skin-material solution, apply identical or different high-voltage dcs respectively, electric-field intensity is 2 kilovolts to 60 kilovolts, make that the jet that ejects the jet pipe of core matter liquid and top layer liquid but different-diameter coaxial from two is concentric stratified flow, the internal diameter of jet pipe is below 2 millimeters; Again under the electric field force effect, through high frequency draw, crooked whipping distortion and be cured as ultra-fine coaxial composite fibre, collect by collecting device.
6, a kind of as fiber preparation method as described in the claim 5, it is characterized in that adopting method of electrostatic spinning, in core matter jar, inject Compressed Gas or volatile liquid, in skin-material solution, apply high-voltage dc, electric-field intensity is 2 kilovolts to 60 kilovolts, make the skin-material jet that ejects from outer nozzle envelope Compressed Gas or volatile liquid core matter, the internal diameter of jet pipe is below 2 millimeters; Again under the electric field force effect, through high frequency draw, crooked whipping distortion and be cured as ultra-fine hollow fibre, collect by collecting device.
7, a kind of fiber production method as claimed in claim 5, it is characterized in that adopting method of electrostatic spinning, the inner nozzle outlet is blocked, only put skin-material solution and apply high-voltage dc in the flow container outside, electric-field intensity is 2 kilovolts to 60 kilovolts, make that the skin-material jet that ejects from outer nozzle is a hollow annular stream, the internal diameter of jet pipe is below 2 millimeters; Again under the electric field force effect, through high frequency draw, crooked whipping distortion and be cured as ultra-fine hollow fibre, collect by collecting device.
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| US8286413B2 (en) | 2007-02-05 | 2012-10-16 | Commonwealth Scientific And Industrial Research Organisation | Nanofibre yarns |
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