CN1687493A - Method for preparing nano fiber endless tow - Google Patents
Method for preparing nano fiber endless tow Download PDFInfo
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- CN1687493A CN1687493A CN 200510038571 CN200510038571A CN1687493A CN 1687493 A CN1687493 A CN 1687493A CN 200510038571 CN200510038571 CN 200510038571 CN 200510038571 A CN200510038571 A CN 200510038571A CN 1687493 A CN1687493 A CN 1687493A
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Abstract
The production method of filament of nanofibers is a simply and high efficiency way. It adopts spinning trunk (3). There are two lines of nozzles (1) whose spout are opposite at the height of the top of the trunk. There are several group of pare of thread guide roller (2) in the trunk.. The distance between thread guide roller and nozzles are equal. The material process is: 1) Transport high polymer solution to nozzles in the trunk of filament of nanofibers; 2) Bring high-voltage DC of opposite polarity to bear to the nozzles. 3) High polymer solution at the top of the nozzles is stretched and whipping responded to form nanofibers which contain electric charge. The opposite nozzle spray nanofibers contains contrary electric charge. They are allure and collide in the air and form nanofibers. The nanofibers are stretched and towed by nozzle and filament of nanofibers comes into being. The operation is simple, highly effective and has no losing of nanofibers.
Description
Technical field
The present invention relates to a kind of nano fiber endless tow preparation method, belong to the technical field of special fibre preparation.
Background technology
First chemical fibre---since cellulose nitrate was born, the research of synthetic fiber and exploration obtained development rapidly, and correspondingly, various spinning process also arise at the historic moment in the world from 1883.Use now the most general spinning process and mainly contain melt spinning, dry spinning and wet spinning, other all be the special process spinning process that new development is got up as methods such as phase separation spinning, flash-spinning, electrostatic spinning, fiber spinning from crystalline state, reaction spinning.
Method of electrostatic spinning has been acknowledged as a kind of advantages of simplicity and high efficiency tunica fibrosa technology of preparing.The diameter of electrospinning fibre than the little 100-1000 of fibre diameter that common spinning process obtained doubly and has huge specific area.It not only can be used as the high efficiency filter material, and has wide application prospects in fields such as biomedical material, chemical sensor, protective materials, nano composite materials.
Typical electrostatic spinning technique is that polymer solution or colloidal sol adding are had in the syringe of micron number magnitude nozzle, makes fluid be subjected to several ten thousand volt electric field force effects.Polymer fluid splits into the minimum fiber of many diameters rapidly from nozzle ejection back air, the receiving system that is grounded receives, and obtains the continuous fibers aggregate of netted or flocculus shape at last.(US6713011B2 US6743273B2) has all designed many nozzle continuous electrostatic spinnings device and has obtained continuous nano fibrous membrane United States Patent (USP) for US6616435B2, US6689374B2.
Yet, because the size of electrospinning fibre is at nanometer or submicron order, thus the situation that usually exists fiber to scatter and disappear, and in the electrospinning process since polymer have like charges and repel mutually, fiber to around scatter, be difficult for making long bundles of nanofibers or long filament.
Someone adopts a kind of metal recipient of ground connection when electrospinning, accept to come from the nanofiber that a shower nozzle produces, and is processed into the nanofiber long filament, and this method efficient is low.
Someone adopts many nozzle systems when electrospinning, the like charges nanofiber that many shower nozzles produce must be first and bright and clean the metal recipient of ground connection gather the formation long filament again after contacting the dissipation electric charge, but the like charges nanofiber that many shower nozzles produce repelled before arriving the metal recipient mutually, fiber disperses, and causes loss.
Therefore, be necessary to invent a kind of method that more effectively prepares the nanofiber long filament.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of nano fiber endless tow preparation method, this method can be produced nano fiber endless tow simply, efficiently.
Technical scheme:
A kind of preparation method of nano fiber endless tow adopts a spinning manifold, at the relative electrospinning shower nozzle of the parallel placement two row's spouts of the sustained height on spinning manifold top, it is right to be provided with some groups of godet rollers at the spinning manifold middle part, and the distance of the godet roller pair electrospinning shower nozzle relative with two row's spouts all equates.The step of the concrete preparation of a kind of nano fiber endless tow is as follows: (1) flows to electrospinning shower nozzle in the nano fiber endless tow spinning manifold with high polymeric solution; (2) arrange the dc high voltage 10KV-100KV that the relative electrospinning shower nozzle of spouts applies opposite polarity respectively to two; (3) nanofiber that the Polymer Solution on electrospinning shower nozzle top stretches under the effect of electric field force, the moving formation of whip has electric charge, the nanofiber of the electrospinning shower nozzle ejection that spout is relative has opposite charges, aloft attract each other, collide, the composite nano fiber that forms forms endless tow after godet roller is to traction, stretching.The spacing of shower nozzle is 5-30cm in every row's electrospinning shower nozzle; Two arrange the relative electrospinning shower nozzle of spouts at a distance of 10-50cm.
High polymeric solution is a high polymeric solution of the same race, or the xenogenesis high polymeric solution; High polymeric solution is that high polymer is dissolved in the solvent or high polymer and additive agent mixture solution; Wherein, high polymer is polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, Merlon, polyurethane, epoxy resin, polyacrylonitrile, polyacrylic acid family macromolecule, polyphenylene oxide, poly-acid anhydrides, poly--a-amino acid, polyphenylene sulfide, or two or more blend wherein; Or a kind of or their derivative in the chitin, shitosan, hyaluronic acid, chondroitin sulfate, collagen, gelatin, glucan, fibrin, silk-fibroin or two or more blend wherein; Or biology can absorb synthetic high polymer poly--L-lactic acid, poly--(D, L)-and the copolymer of a kind of or following at least two kinds of monomers in lactic acid, polyglycolic acid, polycaprolactone, poly-butyrolactone, poly-valerolactone, polyester dioxane, poly-acid anhydrides, poly--a-amino acid: L-lactic acid, D, L-lactic acid, glycolic acid, 3-hydroxybutyric acid, 3-hydroxypentanoic acid, caprolactone, butyrolactone, valerolactone, amino acid, or two or more blend wherein; Additive is antiseptic, pesticide, anti-inflammation drugs.
Beneficial effect: the present invention compared with prior art has following advantage:
(1) the present invention adopts a kind of nano fiber endless tow preparation method, on the relative electrospinning shower nozzle of spout, apply the opposite polarity dc high voltage respectively, the nanofiber of the oppositely charged that the electrospinning shower nozzle produces aloft attracts each other, collides, make fiber with electric-charge-dissipating, avoided effectively that nanofiber is skyborne to disperse and lose, improve production efficiency, and can not use the metal recipient of earth connection.
(2) the present invention has avoided various disturbances to cause the product defect that instability has caused when spraying electrospinning shower nozzle horizontal positioned, has improved the production efficiency of certified products.
(3) the present invention can prepare nano fiber endless tow simple to operate, efficiently.
(4) the present invention can prepare composite nano fiber endless tow simply, efficiently to the defeated different high polymeric solution of the relative electrospinning shower nozzle of spout.
Description of drawings
Fig. 1 is a general structure schematic diagram of the present invention.
Fig. 2 is a fundamental diagram of the present invention.
Have among the above figure: electrospinning shower nozzle 1, godet roller to 2, spinning manifold 3.
The specific embodiment
A kind of preparation method of nano fiber endless tow adopts a spinning manifold, at the relative electrospinning shower nozzle of the parallel placement two row's spouts of the sustained height on spinning manifold top, it is right to be provided with some groups of godet rollers at the spinning manifold middle part, and the distance of the godet roller pair electrospinning shower nozzle relative with two row's spouts all equates.The step of the concrete preparation of a kind of nano fiber endless tow is as follows: (1) flows to electrospinning shower nozzle in the nano fiber endless tow spinning manifold with high polymeric solution; (2) arrange the dc high voltage 10KV-100KV that the relative electrospinning shower nozzle of spouts applies opposite polarity respectively to two; (3) nanofiber that the Polymer Solution on electrospinning shower nozzle top stretches under the effect of electric field force, the moving formation of whip has electric charge, the nanofiber of the electrospinning shower nozzle ejection that spout is relative has opposite charges, aloft attract each other, collide, the composite nano fiber that forms forms endless tow after godet roller is to traction, stretching.The spacing of shower nozzle is 5-30cm in every row's electrospinning shower nozzle; Two arrange the relative electrospinning shower nozzle of spouts at a distance of 10-50cm.
High polymeric solution is a high polymeric solution of the same race, or the xenogenesis high polymeric solution; High polymeric solution is that high polymer is dissolved in the solvent or high polymer and additive agent mixture solution; Wherein, high polymer is polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, Merlon, polyurethane, epoxy resin, polyacrylonitrile, polyacrylic acid family macromolecule, polyphenylene oxide, poly-acid anhydrides, poly--a-amino acid, polyphenylene sulfide, or two or more blend wherein; Or a kind of or their derivative in the chitin, shitosan, hyaluronic acid, chondroitin sulfate, collagen, gelatin, glucan, fibrin, silk-fibroin or two or more blend wherein; Or biology can absorb synthetic high polymer poly--L-lactic acid, poly--(D, L)-and the copolymer of a kind of or following at least two kinds of monomers in lactic acid, polyglycolic acid, polycaprolactone, poly-butyrolactone, poly-valerolactone, polyester dioxane, poly-acid anhydrides, poly--a-amino acid: L-lactic acid, D, L-lactic acid, glycolic acid, 3-hydroxybutyric acid, 3-hydroxypentanoic acid, caprolactone, butyrolactone, valerolactone, amino acid, or two or more blend wherein; Additive is antiseptic, pesticide, anti-inflammation drugs.
Embodiment 1
Polyacrylonitrile (PAN) 100g is dissolved in 1000mlN, in the dinethylformamide, this high polymeric solution is flowed to each 100 electrospinning shower nozzle of the row of two in the nano fiber endless tow spinning manifold.The spacing of respectively arranging the electrospinning shower nozzle in the spinning manifold is 5cm, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 10cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 20kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 0.5mm.The speed of godet roller traction endless tow is 3cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Poly--L-lactic acid PLLA (viscosity average molecular weigh 100,000) 100g is dissolved in 500ml acetone and 500mlN, in the mixed solvent of dinethylformamide, this high polymeric solution is flowed to each 100 electrospinning shower nozzle of the row of two in the nano fiber endless tow spinning manifold.The spacing of shower nozzle is 30cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 50cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 10kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 0.2mm.The speed of godet roller traction endless tow is 6cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
(wherein quality is formed lactide 50% to the random copolymer PLGA of lactide and glycolide, glycolide 50%, viscosity average molecular weigh 100,000) 150g is dissolved in 500ml acetone and 500mlN, in the mixed solvent of dinethylformamide, this high polymeric solution is flowed to 1000 electrospinning shower nozzles of the row of one in the nano fiber endless tow spinning manifold.Poly--L-lactic acid PLLA (viscosity average molecular weigh 100,000) 100g is dissolved in 500ml acetone and 500mlN, in the mixed solvent of dinethylformamide, this high polymeric solution is flowed to 1000 electrospinning shower nozzles of another row in the nano fiber endless tow spinning manifold.The spacing of shower nozzle is 20cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 30cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 25kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 0.8mm.The speed of godet roller traction endless tow is 2cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Embodiment 4
(wherein quality is formed lactide 50% to the random copolymer PLGA of lactide and glycolide, glycolide 50%, viscosity average molecular weigh 100,000) 150g is dissolved in 500ml acetone and 500ml N, in the mixed solvent of dinethylformamide, add the 3g brufen again, fully after the dissolving this high polymeric solution is flowed to two in the nano fiber endless tow spinning manifold and arrange each 100 electrospinning shower nozzle.The spacing of shower nozzle is 10cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 30cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 10kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 0.3mm.The speed of godet roller traction endless tow is 3cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Embodiment 5
Polyacrylonitrile (PAN) 100g is dissolved in 1000ml N, in the dinethylformamide, adds the 10g nanometer Ag again
2O, sonic oscillation make it after the fully dissolving this high polymeric solution to be flowed to each 200 electrospinning shower nozzle of the row of two in the nano fiber endless tow spinning manifold.The spacing of shower nozzle is 15cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 35cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 20kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 1.0mm.The speed of godet roller traction endless tow is 1cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Embodiment 6
(wherein quality is formed lactide 50% to the random copolymer PLGA of lactide and glycolide, glycolide 50%, viscosity average molecular weigh 100,000) 150g is dissolved in 500ml acetone and 500ml N, in the mixed solvent of dinethylformamide, add the 3g brufen again, fully after the dissolving this high polymeric solution is flowed to two in the nano fiber endless tow spinning manifold and arrange each 1000 electrospinning shower nozzle.Poly--L-lactic acid PLLA (viscosity average molecular weigh 100,000) 100g is dissolved in 500ml acetone and 500ml N, in the mixed solvent of dinethylformamide, this high polymeric solution is flowed to 1000 electrospinning shower nozzles of another row in the nano fiber endless tow spinning manifold.The spacing of shower nozzle is 15cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 30cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 15kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 0.5mm.The speed of godet roller traction endless tow is 5cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Embodiment 7
Polyurethane PU 150g is dissolved in 1000ml N, in the dinethylformamide, this high polymeric solution is flowed to each 200 electrospinning shower nozzle of the row of two in the nano fiber endless tow spinning manifold.The spacing of shower nozzle is 10cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 20cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 25kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 1.0mm.The speed of godet roller traction endless tow is 2cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Embodiment 8
Poly-s 179 PPES100g is dissolved in the 1000ml methyl-sulfoxide, and this high polymeric solution is flowed to each 200 electrospinning shower nozzle of the row of two in the nano fiber endless tow spinning manifold.The spacing of shower nozzle is 30cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 50cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 20kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 1.0mm.The speed of godet roller traction endless tow is 3cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Embodiment 9
Polyacrylonitrile (PAN) 100g is dissolved in 1000ml N, in the dinethylformamide, adds the 10g nanometer Ag again
2O, sonic oscillation make it after the fully dissolving this high polymeric solution to be flowed to 1000 electrospinning shower nozzles of the row of one in the nano fiber endless tow spinning manifold.Polyurethane 150g is dissolved in 1000ml N, in the dinethylformamide, with this high polymeric solution flow in the nano fiber endless tow spinning manifold another row 1000 electrospinning shower nozzles.The spacing of shower nozzle is 20cm in every row's electrospinning shower nozzle, and two arrange the relative electrospinning shower nozzle of spouts at a distance of 20cm.Two row's spouts relative electrospinning shower nozzles are applied the dc high voltage ± 30kv of opposite polarity respectively, and electrospinning shower nozzle internal diameter is 1.0mm.The speed of godet roller traction endless tow is 5cm/s.The nanofiber that eject on electrospinning shower nozzle top forms endless tow and derives and collect after the godet roller traction.
Claims (3)
1, a kind of preparation method of nano fiber endless tow, it is characterized in that adopting a spinning manifold (3), at the relative electrospinning shower nozzle (1) of the parallel placement two row's spouts of the sustained height on spinning manifold (3) top, be provided with some groups of godet rollers to (2) at spinning manifold (3) middle part, godet roller equates all that to the distance of (2) the electrospinning shower nozzle (1) relative with two row's spouts the step of concrete preparation is as follows:
1) high polymeric solution is flowed to electrospinning shower nozzle (1) in the nano fiber endless tow spinning manifold (3);
2) arrange the dc high voltage 10KV-100KV that the relative electrospinning shower nozzle (1) of spouts applies opposite polarity respectively to two;
3) nanofiber that the Polymer Solution on electrospinning shower nozzle (1) top stretches under the effect of electric field force, the moving formation of whip has electric charge, the nanofiber of electrospinning shower nozzle (1) ejection that spout is relative has opposite charges, aloft attract each other, collide, the composite nano fiber that forms forms endless tow after godet roller is to (2) traction, stretching.
2, the preparation method of nano fiber endless tow according to claim 1 is characterized in that the spacing of the middle shower nozzle of every row's electrospinning shower nozzle (1) in the spinning manifold (3) is 5-30cm; Two arrange the relative electrospinning shower nozzle (1) of spouts at a distance of 10-50cm.
3, nano fiber endless tow preparation method according to claim 1 is characterized in that high polymeric solution is a high polymeric solution of the same race, or the xenogenesis high polymeric solution; High polymeric solution is that high polymer is dissolved in the solvent or high polymer and additive agent mixture solution; Wherein, high polymer is polyolefin, polyalkenyl halides, polysiloxanes, polyethers, polyamide, polyester, Merlon, polyurethane, epoxy resin, polyacrylonitrile, polyacrylic acid family macromolecule, polyphenylene oxide, poly-acid anhydrides, poly--a-amino acid, polyphenylene sulfide, or two or more blend wherein; Or a kind of or their derivative in the chitin, shitosan, hyaluronic acid, chondroitin sulfate, collagen, gelatin, glucan, fibrin, silk-fibroin or two or more blend wherein; Or biology can absorb synthetic high polymer poly--L-lactic acid, poly--(D, L)-and the copolymer of a kind of or following at least two kinds of monomers in lactic acid, polyglycolic acid, polycaprolactone, poly-butyrolactone, poly-valerolactone, polyester dioxane, poly-acid anhydrides, poly--a-amino acid: L-lactic acid, D, L-lactic acid, glycolic acid, 3-hydroxybutyric acid, 3-hydroxypentanoic acid, caprolactone, butyrolactone, valerolactone, amino acid, or two or more blend wherein; Additive is antiseptic, pesticide, anti-inflammation drugs.
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| WO2007054029A1 (en) * | 2005-11-11 | 2007-05-18 | Southeast University | Device and method for preparing filament tow of composite nanofibers |
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