CN101215762A - Device and method for preparing highly effective continuous electrostatic spinning nano fibre felt - Google Patents
Device and method for preparing highly effective continuous electrostatic spinning nano fibre felt Download PDFInfo
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- CN101215762A CN101215762A CNA2008100322476A CN200810032247A CN101215762A CN 101215762 A CN101215762 A CN 101215762A CN A2008100322476 A CNA2008100322476 A CN A2008100322476A CN 200810032247 A CN200810032247 A CN 200810032247A CN 101215762 A CN101215762 A CN 101215762A
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Abstract
The invention relates to a preparing device of a high-effective continuous-type electro-spin nanometer fiber felt, the invention comprises a fluid supply system, a metal roller, a receiving device and a spinning fluid recycling groove. The process for preparing comprises firstly, preparing polymer spinning fluid with correct concentration in a dissolution kettle, temporarily storing in a liquid storage tank after passing through a filter, secondly, connecting the metal roller and the positive electrode of a high-pressure electrostatic generator, applying correct electrostatic pressure, leading an aluminium screen cloth to connect ground, thirdly, leading the metal roller to rotate in correct rotary speed, fourth, starting a measuring pump, feeding spinning liquid from the liquid storage tank to an even allotter, leading the spinning liquid to be evenly allocated to a spraying hole on the front end of the even allotter, sputtering from the spraying hole to the surface of a rotating metal roller to form Taylor awl, fifthly, leading a coiling drum to rotate to drive a fiber receiving net to move, and continuously receiving nanometer fiber felt. The process for preparation of the nanometer fiber felt of the invention has high production efficiency, which is suitable for scale production of electro-spinning.
Description
Technical field
The invention belongs to the electrostatic spinning nano fiber felt field, particularly relate to the preparation facilities and the preparation method of highly effective continuous electrostatic spinning nano fibre felt.
Background technology
Before 70 years, the someone begins one's study and prepares nanometer stage material with electrospinning process, can prepare hundreds of polymer nanofiber at present.This method technology is simple, easy to operate, and the diameter of its fiber is littler 100～1000 times than the fibre diameter that common spin processes obtained, and has huge specific area and complicated pore structure.These particular performances make the electrospun fibers material have broad application prospects, and not only can be used as filtering material efficiently, and can be used for fields such as biomedical material, chemical sensor, protective materials, nano composite material.
But traditional electrospinning process generally adopts single needle hair style electrostatic spinning apparatus, and this method production efficiency is very low, and approximately hourly output is 0.1～1.0 gram, can not satisfy the suitability for industrialized production requirement far away.In recent years, in order to improve electrostatic spinning production efficiency, people have done some researchs on device for spinning and production method.United States Patent (USP) (US6616435B2, US6689374B2, US6713011B2, US6743273B2) has designed many nozzle continuous electrostatic spinnings device.Chinese patent (application number 200310109222.9, publication number CN1546753A) has designed the multi-nozzle electrospinning device of coaxial compound continuous nano/micron fiber.But, in the multi-nozzle electrospinning system, the nanofiber that ejects of periphery shower nozzle is because of the Coulomb repulsion of the nanofiber that has like charges that is subjected to adjacent shower nozzle injection, cause the nanofiber of peripheral shower nozzle ejection to disperse, and influenced the volatilization of solvent, therefore multi-nozzle electrospinning device nozzle needle head arrangement at present is all more sparse, and general two adjacent shower nozzles have restricted the raising of output greatly at a distance of 10～20 centimetres.
European patent (WO2005024101) has designed a kind of no shower nozzle nanofiber spinning machine: in the partially submerged polymer solution thereunder of live metal rod, the surface of drawing solution and solution being taken out of metal bar by the rotation of metal bar is drawn into silk then to form the Taylor awl under electrostatic field.But experiment showed, that when metal bar rotates form the one layer of polymeric film on the metal bar surface especially easily, along with the carrying out of experiment, the thickness of polymer film is understood thickening, has a strong impact on the carrying out of spinning in polymer solution.Therefore, this kind electrospinning process, metal bar is immersed being provided with of technological parameters such as the rotating speed of the degree of depth, metal bar of spinning solution and solution concentration require harsh, in case condition does not reach, just can not form the Taylor awl on the metal bar surface, thereby make spinning be difficult to carry out.
Summary of the invention
The preparation facilities and the method that the purpose of this invention is to provide a kind of highly effective continuous electrostatic spinning nano fibre felt, preparation method's production efficiency height of this continuous nano-fibre felt is applicable to the large-scale production of electrostatic spinning.
The preparation facilities of highly effective continuous electrostatic spinning nano fibre felt of the present invention, this device receives net 12, coiling roller 8, unwinding roller 9 and solution receiving slit 10 by dissolution kettle 1, filter 2, liquid storing barrel 3, measuring pump 4, uniform distributor 5, metal roller 7, aluminum screen cloth 11, fiber to be formed, as shown in Figure 1.
Described uniform distributor is T-shape uniform distributor (Fig. 2), clothes hanger type uniform distributor (Fig. 3), preferred clothes hanger type uniform distributor;
Described metal roller is plough groove type metal roller (Fig. 5), brad formula metal roller (Fig. 6), preferred brad formula metal roller.
Among the present invention, dissolution kettle 1, filter 2, liquid storing barrel 3, measuring pump 4, uniform distributor 5 are formed liquid-supplying system; Aluminum screen cloth 11, fiber receive net 12, coiling roller 8, unwinding roller 9 composition receiving systems.
The polymer spinning solution that makes in dissolution kettle 1 filters through filter 2, enters liquid storing barrel 3, is delivered to uniform distributor 5 by measuring pump 4 then.Spinning solution is splashed on metal roller 7 surfaces of rotation through the spray orifice 6 of uniform distributor 5 front ends.Metal roller 7 connects the HV generator positive pole, aluminum screen cloth 11 ground connection, and under this high voltage electrostatic field, the drop on the metal roller 7 is stretched, and becomes silk by solvent evaporates, is deposited on the fiber reception net 12 and forms nanofiber mats.Fiber receives net 12 under the effect of unwinding cylinder 9 and winding drum 8, can realize the continuous reception of nanofiber mats.Receive reuse from the not filament-forming polymeric solution of metal roller 7 drippages by solution receiving slit 10.
The preparation method of highly effective continuous electrostatic spinning nano fibre felt of the present invention is to realize that by the preparation facilities of highly effective continuous electrostatic spinning nano fibre felt its concrete steps comprise:
(a) in dissolution kettle 1, prepare the polymer dope of suitable concn, be temporary in the liquid storing barrel 3 through behind the filter 2;
(b) metal roller 7 is connected with the positive pole of HV generator and applies suitable electrostatic pressure, aluminum screen cloth 11 ground connection;
(c) make the rotating speed revolution of metal roller 7 to be fit to;
(d) start measuring pump 4, spinning solution makes the spinning solution uniform distribution give the spray orifice 6 of uniform distributor 5 front ends from liquid storing barrel 3 weight feed uniform distributors 5, and is splashed to rotating metallic cylinder 7 surfaces thus upward to form the Taylor awl;
(e) make winding drum 8 revolutions, drive fiber and receive net 12 motions, receive nanofiber mats continuously.
Described polymer dope is that polymer is dissolved in solvent or solvent and additive agent mixture and the solution that forms, can be the multiple polymers spinning solution, wherein polymer can be a kind of in polyvinyl alcohol, poly(ethylene oxide), polyester, Merlon, polyurethane, polyamide, polyacrylonitrile, polyacrylic acid family macromolecule, the poly-acid anhydrides or two or more blend.
Described solvent is water, chloroform, dimethylacetylamide, dimethyl formamide, phenol;
Described additive is sodium chloride, lithium chloride, citric acid.
The fibre diameter of described nanofiber mats is 200-600nm.
Beneficial effect of the present invention:
(1) this device adopts new liquid-supplying system, can be quantitatively, equably spinning solution is assigned on the live metal cylinder surface, and guaranteed the without interruption of spinning solution;
(2) charged rotating metallic cylinder has adopted sputter mode in top to get liquid (Fig. 4), be the spray orifice outflow of spinning solution by the uniform distributor front end, rely on the pressure of solution and gravity to drop onto on the rotating metallic cylinder as raindrop, because centrifugal action, drop forms the Taylor awl easily on metal roller, under high voltage electrostatic field, overcome the surface tension of solution easily, be stretched and thin down to silk, the carrying out that helps spinning, and spinning solution did not have electric charge before dropping onto on the metal roller, thereby more helped the control to spinning solution;
(3) adopt brad formula metal roller, when spinning solution is dropped in the metal roller surface, because the existence of brad shape projection forms the Taylor awl easily, thereby makes electrostatic spinning more smooth;
(4) length that can pass through the increase metal roller further improves output to increase the spinning area;
(5) adopt two-sided reception, can further improve output;
(6) adopt clothes hanger type uniform distributor, can make the flow path of polymer solution in clothes hanger type uniform distributor identical by optimal design, thereby make the polymer flow rate of each spray orifice identical, can improve the uniformity of spinning solution cross direction profiles on metal roller, finally improve the horizontal homogeneity of nanofiber mats;
(7) liquid supply part (uniform distributor) separates with spinning components (metal roller), makes spinning solution neutral before dropping onto the metal roller surface, therefore can pass through to increase the spray orifice density of uniform distributor front end to increase output.
Description of drawings
Fig. 1 is a sputter formula electrostatic spinning apparatus schematic diagram, wherein, and 1-dissolution kettle, 2-filter, 3-liquid storing barrel, the 4-measuring pump, 5-uniform distributor, 6-spray orifice, 7-metal roller, 8-coiling roller, 9-unwinding roller, 10-solution receiving slit, 11-aluminum screen cloth, the 12-fiber receives net;
Fig. 2 is the T-shape uniform distributor;
Fig. 3 is a clothes hanger type uniform distributor;
Fig. 4 is a sputter formula feed liquid way schematic diagram;
Fig. 5 is the plough groove type metal roller;
Fig. 6 is a brad formula metal roller.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Use electrostatic spinning apparatus to prepare nanofiber mats in the present embodiment, concrete enforcement may further comprise the steps: (a) prepare the polymer dope of suitable concn in dissolution kettle 1, be temporary in the liquid storing barrel 3 after filtering through filter 2; (b) metal roller 7 is connected with the positive pole of HV generator and applies suitable electrostatic pressure, aluminum screen cloth 11 ground connection; (c) make the rotating speed revolution of metal roller 7 to be fit to; (d) start measuring pump 4, spinning solution makes the spinning solution uniform distribution give the spray orifice 6 of uniform distributor 5 front ends from liquid storing barrel 3 weight feed uniform distributors 5, and is splashed to rotating metallic cylinder 7 surfaces thus upward to form the Taylor awl; (e) make winding drum 8 revolutions, drive fiber and receive net 12 motions, receive nanofiber mats continuously.
87g is dissolved in the 1000ml deionized water with polyvinyl alcohol 1750 (molecular weight 1700, alcoholysis degree 50%), adds an amount of sodium chloride and citric acid, makes the transparent nothing precipitation PVA spinning solution of concentration 8%.Adopt the T-shape uniform distributor, injection diameter is 2mm, and density is 2 spray orifices/cm.Adopt the plough groove type metal roller, length is 50cm, and diameter is 5cm, and rotating speed is 4r/min, applies electrostatic pressure to be+50kV.The receiving range that metal roller surface and fiber receive between the net is 35cm.According to above-mentioned implementation step, make nanofiber mats, distribution of fiber diameters is between 300-600nm, and average product is 20g/h.
52.6g is dissolved in the 1000ml deionized water with poly(ethylene oxide) (molecular weight 1000000), adds an amount of sodium chloride, makes the transparent nothing precipitation PEO spinning solution of concentration 5%.Adopt the T-shape uniform distributor, injection diameter is 1.5mm, and density is 2 spray orifices/cm.Adopt the plough groove type metal roller, length is 50cm, and diameter is 5cm, and rotating speed is 4r/min, applies electrostatic pressure to be+50kV.The receiving range that metal roller surface and fiber receive between the net is 35cm.According to above-mentioned implementation step, make nanofiber mats, distribution of fiber diameters is between 200-500nm, and average product is 18g/h.
Embodiment 3
87g is dissolved in the 1000ml deionized water with polyvinyl alcohol 1 750 (molecular weight 1700, alcoholysis degree 50%), adds an amount of sodium chloride and citric acid, makes the transparent nothing precipitation PVA spinning solution of concentration 8%.Adopt clothes hanger type uniform distributor, injection diameter is 2mm, and density is 2 spray orifices/cm.Adopt brad formula metal roller, length is 50cm, and diameter is 5cm, and rotating speed is 4r/min, applies electrostatic pressure to be+50kV.The receiving range that metal roller surface and fiber receive between the net is 35cm.According to above-mentioned implementation step, make nanofiber mats, distribution of fiber diameters is between 300-500nm, and average product is 23g/h.
Embodiment 4
52.6g is dissolved in the 1000ml deionized water with poly(ethylene oxide) (molecular weight 1000000), adds an amount of sodium chloride, makes the transparent nothing precipitation PEO spinning solution of concentration 5%.Adopt clothes hanger type uniform distributor, injection diameter is 1.5mm, and density is 2 spray orifices/cm.Adopt brad formula metal roller, length is 50cm, and diameter is 5cm, and rotating speed is 4r/min, applies electrostatic pressure to be+50kV.The receiving range that metal roller surface and fiber receive between the net is 35cm.According to above-mentioned implementation step, make nanofiber mats, distribution of fiber diameters is between 200-400nm, and average product is 25g/h.
Claims (9)
1. the preparation facilities of a highly effective continuous electrostatic spinning nano fibre felt is characterized in that: this device receives net (12), coiling roller (8), unwinding roller (9) and spinning solution accumulator tank (10) by dissolution kettle (1), filter (2), liquid storing barrel (3), measuring pump (4), uniform distributor (5), metal roller (7), aluminum screen cloth (11), fiber and forms.
2. the preparation facilities of highly effective continuous electrostatic spinning nano fibre felt according to claim 1, it is characterized in that: described uniform distributor (5) is a clothes hanger type uniform distributor.
3. the preparation facilities of highly effective continuous electrostatic spinning nano fibre felt according to claim 1, it is characterized in that: described metal roller (7) is a brad formula metal roller.
4. the preparation method of a highly effective continuous electrostatic spinning nano fibre felt, step comprises:
(a) in dissolution kettle (1), prepare the polymer dope of suitable concn, through being temporary in the liquid storing barrel (3) behind the filter (2);
(b) metal roller (7) is connected with the positive pole of HV generator and applies suitable electrostatic pressure, aluminum screen cloth (11) ground connection;
(c) make the rotating speed revolution of metal roller (7) to be fit to;
(d) start measuring pump (4), spinning solution makes the spinning solution uniform distribution give the spray orifice (6) of uniform distributor (5) front end from liquid storing barrel (3) weight feed uniform distributor (5), and is splashed to thus on rotating metallic cylinder (7) surface to form the Taylor awl;
(e) make winding drum (8) revolution, drive fiber and receive net (12) motion, receive nanofiber mats continuously.
5. the preparation method of highly effective continuous electrostatic spinning nano fibre felt according to claim 4 is characterized in that: described polymer dope is that polymer is dissolved in solvent or solvent and additive agent mixture and the solution that forms.
6. the preparation method of highly effective continuous electrostatic spinning nano fibre felt according to claim 5 is characterized in that: described polymer is a kind of or its blend in polyvinyl alcohol, poly(ethylene oxide), polyester, Merlon, polyurethane, polyamide, polyacrylonitrile, polyacrylic acid family macromolecule, the poly-acid anhydrides.
7. the preparation method of highly effective continuous electrostatic spinning nano fibre felt according to claim 5, it is characterized in that: described solvent is water, chloroform, dimethylacetylamide, dimethyl formamide or phenol.
8. the preparation method of highly effective continuous electrostatic spinning nano fibre felt according to claim 5, it is characterized in that: described additive is sodium chloride, lithium chloride or citric acid.
9. the preparation method of highly effective continuous electrostatic spinning nano fibre felt according to claim 4, it is characterized in that: the fibre diameter of described nanofiber mats is 200～600nm.
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| CN102551186A (en) * | 2011-12-14 | 2012-07-11 | 广东省金叶烟草薄片技术开发有限公司 | Technique and device for dry formation of low basis weight fluff pulp and capable of eliminating electrostatic flocculation |
| CN102931370A (en) * | 2012-10-24 | 2013-02-13 | 江苏大学 | Organic/inorganic composite nanofiber membrane of lithium ion power battery and preparation method of organic/inorganic composite nanofiber membrane |
| CN103451749A (en) * | 2012-05-30 | 2013-12-18 | 湖南博弈飞装备新材料研究所 | Continuous electrostatic spinning system and method for preparing fine fibers |
| CN103498285A (en) * | 2013-10-18 | 2014-01-08 | 苏州大学 | Method using electrospinning technique to prepare ordered nanometer magnetic composite material |
| CN103726110A (en) * | 2013-12-11 | 2014-04-16 | 哈尔滨工业大学深圳研究生院 | Electrostatic spinning device and method for manufacturing electrostatic spun yarns through electrostatic spinning device |
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| CN105401229A (en) * | 2015-08-24 | 2016-03-16 | 武汉医佳宝生物材料有限公司 | Electrostatic spinning multi-nuzzle arc jet apparatus |
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| CN102551186B (en) * | 2011-12-14 | 2014-05-21 | 广东省金叶烟草薄片技术开发有限公司 | Technique and device for dry formation of low basis weight fluff pulp and capable of eliminating electrostatic flocculation |
| CN102551186A (en) * | 2011-12-14 | 2012-07-11 | 广东省金叶烟草薄片技术开发有限公司 | Technique and device for dry formation of low basis weight fluff pulp and capable of eliminating electrostatic flocculation |
| CN103451749A (en) * | 2012-05-30 | 2013-12-18 | 湖南博弈飞装备新材料研究所 | Continuous electrostatic spinning system and method for preparing fine fibers |
| CN102931370A (en) * | 2012-10-24 | 2013-02-13 | 江苏大学 | Organic/inorganic composite nanofiber membrane of lithium ion power battery and preparation method of organic/inorganic composite nanofiber membrane |
| CN103498285A (en) * | 2013-10-18 | 2014-01-08 | 苏州大学 | Method using electrospinning technique to prepare ordered nanometer magnetic composite material |
| CN103498285B (en) * | 2013-10-18 | 2016-08-17 | 苏州大学 | Utilize the method that electrostatic spinning technique prepares ordered nano magnetic composite |
| CN103726110A (en) * | 2013-12-11 | 2014-04-16 | 哈尔滨工业大学深圳研究生院 | Electrostatic spinning device and method for manufacturing electrostatic spun yarns through electrostatic spinning device |
| CN103726110B (en) * | 2013-12-11 | 2015-12-09 | 哈尔滨工业大学深圳研究生院 | A kind of electrospinning device and the method for the preparation of electrostatic spinning thereof |
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| CN107109703A (en) * | 2014-08-05 | 2017-08-29 | 捷恩智株式会社 | Electrostatic spinning spinning head |
| US10662553B2 (en) | 2014-08-05 | 2020-05-26 | Jnc Corporation | Spinneret for electrostatic spinning |
| CN105401229A (en) * | 2015-08-24 | 2016-03-16 | 武汉医佳宝生物材料有限公司 | Electrostatic spinning multi-nuzzle arc jet apparatus |
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Open date: 20080709 |