CN102534822B - Device and method for preparing polysulfonamide nanometer fiber nets by means of airflow-electrostatic combination - Google Patents
Device and method for preparing polysulfonamide nanometer fiber nets by means of airflow-electrostatic combination Download PDFInfo
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- CN102534822B CN102534822B CN201210037687.7A CN201210037687A CN102534822B CN 102534822 B CN102534822 B CN 102534822B CN 201210037687 A CN201210037687 A CN 201210037687A CN 102534822 B CN102534822 B CN 102534822B
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- 238000009987 spinning Methods 0.000 claims abstract description 35
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- 239000005030 aluminium foil Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 238000010041 electrostatic spinning Methods 0.000 abstract description 16
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- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 1
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- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 1
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- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 description 1
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- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a device and a method for preparing polysulfonamide nanometer fiber nets by means of airflow-electrostatic combination. The device comprises a liquid storage tank, an air chamber, an electrostatic generator and a receiving device, a plurality of spinnerets are arranged at the bottom of the liquid storage tank, the air chamber is arranged outside the liquid storage tank, air outlets in the number equal to that of the spinnerets at the bottom of the liquid storage tank are arranged at the bottom of the air chamber, the spinnerets are arranged inside the air outlets, an electrode with multiple pins are led from the positive electrode of the electrostatic generator to be connected with the spinnerets, and a lead is led from the negative electrode of the electrostatic generator to be connected with the receiving device. The method includes steps of combining the airflow method and the electrostatic spinning method effectively to prepare the polysulfonamide nanometer fiber nets. By the device and the method for preparing the polysulfonamide nanometer fiber nets, the specific surface area of the polysulfonamide nanometer fibers is enlarged greatly, the problem of blockage of existing electrostatic spinning needles due to inflow of the airflow is alleviated greatly, and spinning efficiency is improved. Besides, nanometer fibers can be prepared at the normal temperature directly, so that production procedures are simplified and production cost is saved.
Description
Technical field
The invention belongs to the preparation field of polysulfonamides, particularly a kind of device for spinning and method preparing polysulfonamides nanometer fiber net.
Background technology
Polysulfonamides fibre (being called for short PSA fiber) has another name called polysulphonamide fiber, and formal name used at school is PPSU terephthalamide fiber, belongs to p-aramid fiber series, is the high-performance synthetic fiber that China's independent research has independent intellectual property rights.Its main feature has excellent heat resistance and heat endurance, and anti-flammability is high, and chemical-resistant stability is good, except the very strong solvent of several polarity is as except the concentrated sulfuric acid, all has good stability at normal temperatures to chemicals.Polysulfonamides fibre as a kind of novel textile material, have high-strength, lightweight, resistant to elevated temperatures feature and protection under being applied to aerospace field, high-temperature work environment and other have the civil area of flame-retardancy requirements.Polysulfonamides viscosity is comparatively large, and electric conductivity is poor, prepares the method mainly wet spinning process of polysulfonamides fibre at present.
Electrostatic spinning technique there has been the history of more than 70 year, and it is from 1934 the earliest, and Formhal has invented and prepared the experimental provision of polymer fiber with electrostatic force and applied for patent, discloses polymer solution and how between electrode, to form jet.。Prepare nanofiber at present and have a lot of method, as the method for reeling off raw silk from cocoons (Ondarcuhu T, Joachim C.Drawing a single nanofibre over hundreds of microns [J] .EurophysLeft, 1998,42 (2): 215), template synthesis method (Feng L, Li S.Super-hydrophobic surface ofaligned poly-acrylonitrile nanofibers [J] .Angrew Chem Int, 2002,41 (7): 1221-1223, Martin C R.Membrane-based synthesis of nanomaterials [J] .ChemMater, 1996, 8 (8): 1739-1746.), split-phase method (Ma PX, Zhang R Y.Synthetic nano-scalefibrous extrace-llular matrix [J] .J Biomed Mater Res, 1999, 46 (1): 60-66.), self-assembly method (Liu G J, Ding JF.Polystyrene block-poly (2-cinnamoylet-hyl methacrylate) nanofibers-Preparation, characterization, and liquid crystalline properties [J] .Chem-AEuropean, 1999, : 2740-2750.) and method of electrostatic spinning (5).The shortcoming of method of reeling off raw silk from cocoons requires too harshness to solution viscosity; The shortcoming of template synthesis method to prepare the continuous fibers of root root division; Split-phase method is all lower with self-assembly method productivity ratio.The obtained fibre diameter of electrostatic spinning technique generally at tens nanometer to hundreds of nanometer, its specific area is comparatively large, and has successional structure, and the film obtained has the large fine quality of porosity.This characteristics determined this kind of nanofiber has obvious advantage in assembling, nanoprocessing etc.At present, electrostatic spinning fiber material has good application in a lot of field, as aspects such as filtering material, wound clad material and tissue engineering brackets.Along with development in recent years, more research is dropped into the kind of raw material and the selection of solvent.
Electrostatic spinning technique has been applied to the nearly 100 kinds of polymer nanofibers of preparation by people, comprise Merlon (OGHITZKI M, CZAKO W, FRESE T, et al.Nanostructured fibers viaelectrospinning [J] .Advanced Materials, 2001, 13 (1): 70-72) polysulfones (GOPAL R, KAURS, FENG C Y, et al.Electrospun nanofibrous polysulfone membranes as pre-filters:particulate removal [J] .Journal of the Korean Mathematical Society, 2004, 41 (1): 30-36.) the solvable synthesising macromolecule copolymer of organic solvent such as, polyvinyl alcohol (JAEGER R, BERGSHOEF MM, BATLLE C M I, et al.Elecrospinning of ultra-thin polymerfibers [J] .Macromolecular Symposia, 1998, 127:141-150.), poly(ethylene oxide) (DOSHI J, RENEKER D H.Electrospinning process and applications of elecrospunfibers [J] .Journal of Elecrostatics, 1995, 35 (2-3): 151-160.) etc. water-soluble synthesising macromolecule copolymer, PLA (TAN S H, INAI R, KOTAKI M, et al.Systematic parameter study forultra-fine fiber fabrication via electrospinningprocess [J] .Polymer, 2005, 46 (16): 6128-6134) synthesized degradable high molecular polymer and cellulose (the KIM C such as, FREY M, MARQUEZ M, et al.Preparation of submicron-scale, elecrospuncellulose fibers via direct dissolution [J] .Journal of Polymer Science Part B:PolymerPhysics, 2005, 43 (13): 1673-1683.), fibroin (BUCHKOA C J, CHENAL C, SHENA Y, et al.Processing and microstructural characterization of porous biocompatible proteinpolymer thin films [J] .Polymer, 1999, 40:7397-7407.) etc. natural polymers and derivative thereof.
Because polysulfonamides viscosity is large, poorly conductive, add method of electrostatic spinning itself and there is the problems such as fiber production is low, clogging of pores, solution evaporation, the nanoscale polysulfonamides fibre obtaining certain output is very difficult, at present considerably less for utilizing electrostatic spinning to prepare the research of polysulfonamides nanofiber, only have patent CN101724919A to mention and utilize magnetized electrostatic spinning legal system for orientations polysulfonamides superfine fibre.
The present invention for spinning solution, utilizes air-flow-method of electrostatic spinning (being realized by the multiple injector electrostatic spinning device with vibrating device and air flow system) to prepare polysulfonamides nanometer fiber net in enormous quantities with polysulfonamides solution.And propose best spinning technology parameter.
Summary of the invention
Large for polysulfonamides viscosity, the problem that poorly conductive and method of electrostatic spinning yield poorly, the present invention proposes the apparatus and method that a kind of air-flow-electrostatical binding prepares polysulfonamides nanometer fiber net.
For this reason, technical scheme of the present invention is as follows:
Air-flow-electrostatical binding prepares a device for polysulfonamides nanometer fiber net, comprises liquid storage tank, gas compartment, electrostatic generator and receiving system;
Described liquid storage tank connects outside liquid feed device by woven hose, and liquid storage tank inside is provided with bar-shaped sensor, and bar-shaped sensor is positioned at 1/2 ~ 2/3 place of liquid storage tank height, and bar-shaped sensor is connected with supersonic generator, is provided with several spinning head bottom liquid storage tank;
Described gas compartment is arranged on liquid storage tank outside and is connected with feeder, the closed front of its top and described liquid storage tank, and bottom is provided with the gas outlet identical with spinning head quantity bottom liquid storage tank, and described spinning head is arranged in described gas outlet;
The positive pole of described electrostatic generator is drawn multistylus electrode and is connected with spinning head, and negative pole is drawn wire and is connected with receiving system.
The internal orifice dimension of described spinning head is 0.4 ~ 1mm, and length is 8 ~ 12mm, and spacing is 10mm, and the distance controlling between spinning head and receiving system is at 5 ~ 25cm.
Described feeder is a nitrogen cylinder, connects gas compartment and control air velocity by flowmeter by wireway.
Described receiving system comprises swing roller, toggle and motor, the rotary axle box of described swing roller is on slide bar, one end of turning cylinder and toggle are connected by revolute pair makes swing roller realize the transverse movement on slide bar, and the other end connects motor, and to make swing roller realize transhipment dynamic.
Described swing roller can arrange aluminium foil, described motor can connection speed controller to control its rotating speed.
Air-flow-electrostatical binding prepares a method for polysulfonamides nanometer fiber net, comprises the following steps:
(1) open liquid feed device and DMAC (dimethylacetylamide) the Static Spinning solution of polysulfonamides is injected liquid storage tank by woven hose, keep solution not have 2/3 place of bar-shaped sensor;
(2) open supersonic generator and carry out ultrasonic vibration to solution, supersonic frequency is 30 ~ 40KHz; Opening receiving system makes swing roller move reciprocatingly with the speed of 5cm/min, rotates with the speed of 800 ~ 1000rpm; Open feeder to gas compartment air feed, air-flow velocity remains on 2 ~ 10L/min; Opening electrostatic generator makes voltage between its both positive and negative polarity at 12 ~ 28KV.
The mass percent concentration of the DMAC Static Spinning solution of polysulfonamides described in step (1) is 5% ~ 16%, preferably 12%.
The preferred 20KV of voltage in step (2) between electrostatic generator both positive and negative polarity, the preferred 15cm of receiving range, the preferred 8L/min of air-flow velocity, the preferred 850rpm of rotating speed of motor.
Large for polysulfonamides viscosity, the problem that poorly conductive and method of electrostatic spinning yield poorly, this invention takes technique scheme, achieve on the one hand the surface tension that air-flow power and electrostatic field force overcome polysulfonamides solution jointly, correlation stream stretches, make the fiber that obtains thinner, evenly, exacerbate the evaporation rate of solvent simultaneously, decrease drop amount, the corresponding reduction of drop area, finally makes polysulfonamides nanofiber specific area greatly increase; On the other hand, the problem that the introducing of air-flow makes original electrostatic spinning syringe needle block is alleviated greatly, improves spinning efficiency, increases polysulfonamides nanometer fiber net output; In addition, the present invention directly prepares nanofiber at normal temperatures, does not need heating, simplifies production stage, saved production cost, environmentally safe, open a kind of new situations of polysulfonamides for electrostatic spinning technique, have good market prospects.
Accompanying drawing explanation
Fig. 1 is the structural representation that air-flow-electrostatical binding of the present invention prepares the device of polysulfonamides nanometer fiber net.
Fig. 2 (a) is the SEM photo of polysulfonamides nanofiber prepared by the embodiment of the present invention 1.
Fig. 2 (b) is the SEM photo of polysulfonamides nanofiber prepared by the embodiment of the present invention 2.
Fig. 3 is the SEM photo of polysulfonamides nanofiber prepared by the embodiment of the present invention 3.
Fig. 4 is the form photo of the embodiment of the present invention 4 spinning process taylor cone.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.
Embodiment 1
As shown in Figure 1, air-flow-electrostatical binding of the present invention prepares the device of polysulfonamides nanometer fiber net, comprises liquid storage tank 100, gas compartment 200, electrostatic generator 300 and receiving system 400;
Liquid storage tank connects outside liquid feed device 120 by woven hose 110, liquid storage tank inside is provided with bar-shaped sensor 130, bar-shaped sensor is connected with supersonic generator 140, several spinning head 150 is provided with bottom liquid storage tank, the internal orifice dimension of spinning head is 0.4 ~ 1mm, length is 8 ~ 12mm, and spacing is 10mm; Distance controlling between spinning head and receiving system is at 5 ~ 25cm.
Gas compartment 200 is arranged on liquid storage tank outside and is connected with feeder, feeder is a nitrogen cylinder 210, connect gas compartment by wireway 220 and control air velocity by flowmeter 230, the closed front of gas compartment top and liquid storage tank, bottom is provided with the gas outlet 240 identical with spinning head quantity bottom liquid storage tank, and spinning head is arranged in gas outlet;
The positive pole of electrostatic generator is drawn multistylus electrode 310 and is connected with spinning head, and negative pole 320 is drawn wire and is connected with receiving system.
Receiving system comprises swing roller 410, toggle 420 and motor 430, the rotary axle box of swing roller is on slide bar 440, one end of turning cylinder and toggle are connected by revolute pair makes swing roller realize the transverse movement on slide bar, and the other end connects motor, and to make swing roller realize transhipment dynamic.
Swing roller is arranged aluminium foil 411, motor connection speed controller 431 is to control its rotating speed.
The step that use said apparatus is prepared concrete polysulfonamides nanometer fiber net is as follows:
(1) preparation quality percent concentration is the DMAC Static Spinning solution of the polysulfonamides PSA of 5% ~ 16%, preparation process is big with reference to gold, Feng Ya, Yan Xiong etc. the research [J] of Preparation of Polysulfonamide by Low-temperature Solution Polycondensation. and synthetic fiber, 2007, (10): 27-36;
(2) open liquid feed device and the DMAC Static Spinning solution of polysulfonamides is injected liquid storage tank by woven hose, keep solution not have 2/3 place of bar-shaped sensor;
(3) open supersonic generator and carry out ultrasonic vibration to solution, supersonic frequency is 30 ~ 40KHz; Opening receiving system makes swing roller move reciprocatingly with the speed of 5cm/min, rotates with the speed of 800 ~ 1000rpm; Open feeder to gas compartment air feed, air-flow velocity remains on 2 ~ 10L/min; Opening electrostatic generator makes voltage between its both positive and negative polarity at 12 ~ 28KV.
Choose optimum combination: the mass percent concentration of the DMAC Static Spinning solution of polysulfonamides is 12%, and the voltage between electrostatic generator both positive and negative polarity is 20KV, and receiving range is 15cm, and air-flow velocity is 8L/min, and the rotating speed of motor is 850rpm.
Spinning 1h is set by above-mentioned, obtained nanometer polysulfonamides nanometer fiber net, by electronic microscope photos, obtains the formalness of fiber and structure as shown in Fig. 2 (a).
After tested, the average diameter of obtained polysulfonamides nanofiber is 56nm, and distribution of fiber diameters dispersion is little, mainly concentrates on 50 ~ 100nm, and the specific area of fiber is 51m
2/ g, the output of polysulfonamides nanofiber is 15mg/h.
Embodiment 2:
The present embodiment is substantially the same manner as Example 1, unlike, the present embodiment does not pass into air-flow.Observe spinning process, find that amount of droplets is more, syringe needle clogging is more serious.The fibrous external structural form of obtained polysulfonamides nanometer fiber net is as Fig. 2 (b).The average diameter of polysulfonamides nanofiber obtained is after tested 85nm, and distribution of fiber diameters dispersion is little, mainly concentrates on 75 ~ 150nm, and the specific area of fiber is 35.6m
2/ g, the output of polysulfonamides nanofiber is 6.1mg/h.
Embodiment 3:
The present embodiment is substantially the same manner as Example 1, unlike, the present embodiment does not open supersonic generator.As shown in Figure 3, can find that there is bead fiber, the output of polysulfonamides nanofiber is 2.5mg/h to the fibrous external structural form of obtained polysulfonamides nanometer fiber net.
Embodiment 4:
The present embodiment is substantially the same manner as Example 1, unlike, the present embodiment does not pass into air-flow and does not open supersonic generator.Observe spinning process, find that spinning is more difficult and carry out, can only obtain less fiber, the taylor cone of shower nozzle end has shrinkage phenomenon, back to shower nozzle inside (see Fig. 4).
Relatively four embodiments are known, adopt embodiment 1 shaking device and air flow system to be opened simultaneously, more be conducive to realizing being spun by Static Spinning obtaining polysulfonamides nanometer fiber net, syringe needle blockage problem is alleviated greatly, spinning process is more smooth, and obtained fiber is thinner, evenly specific area is larger.
Above-described embodiment is interpreted as only being not used in for illustration of the present invention limiting the scope of the invention.After the content of having read the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalence changes and modification fall into the scope of the claims in the present invention equally.
Claims (3)
1. air-flow-electrostatical binding prepares a device for polysulfonamides nanometer fiber net, it is characterized in that, comprises liquid storage tank, gas compartment, electrostatic generator and receiving system;
Described liquid storage tank connects outside liquid feed device by woven hose, and liquid storage tank inside is provided with bar-shaped sensor, and bar-shaped sensor is positioned at 1/2 ~ 2/3 place of liquid storage tank height, and bar-shaped sensor is connected with supersonic generator, is provided with several spinning head bottom liquid storage tank;
Described gas compartment is arranged on liquid storage tank outside and is connected with feeder, the closed front of its top and described liquid storage tank, and bottom is provided with the gas outlet identical with spinning head quantity bottom liquid storage tank, and described spinning head is arranged in described gas outlet; The positive pole of described electrostatic generator is drawn multistylus electrode and is connected with spinning head, and negative pole is drawn wire and is connected with receiving system;
Described receiving system comprises swing roller, toggle and motor, the rotary axle box of described swing roller is on slide bar, one end of turning cylinder and toggle are connected by revolute pair makes swing roller realize the transverse movement on slide bar, the other end connects motor makes swing roller realization transhipment dynamic, described swing roller arranges aluminium foil, and described motor connection speed controller is to control its rotating speed.
2. air-flow-electrostatical binding according to claim 1 prepares the device of polysulfonamides nanometer fiber net, it is characterized in that, the internal orifice dimension of described spinning head is 0.4 ~ 1mm, and length is 8 ~ 12mm, spacing is 10mm, and the distance controlling between spinning head and receiving system is at 5 ~ 25cm.
3. air-flow-electrostatical binding according to claim 1 prepares the device of polysulfonamides nanometer fiber net, it is characterized in that, described feeder is a nitrogen cylinder, connects gas compartment and control air velocity by flowmeter by wireway.
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| CN111005078A (en) * | 2020-01-14 | 2020-04-14 | 中原工学院 | Airflow-assisted electrostatic spinning nozzle and using method thereof |
| CN111424370A (en) * | 2020-04-06 | 2020-07-17 | 南开大学 | Preparation method of super-hydrophobic melt electro-spun fabric |
| CN113913954B (en) * | 2021-10-12 | 2022-11-01 | 中原工学院 | Superfine nanofiber preparation device and method based on solution atomization and electrostatic-airflow take-over drafting |
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| JP4047744B2 (en) * | 2003-02-27 | 2008-02-13 | 日本バイリーン株式会社 | Electrostatic spinning method and electrostatic spinning apparatus |
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| CN101387018A (en) * | 2008-10-17 | 2009-03-18 | 东南大学 | Visualization preparation method of electro spinning hollow TiO2 fiber |
| CN101709534A (en) * | 2009-11-17 | 2010-05-19 | 天津工业大学 | Device and method for manufacturing airflow melting electrostatic spinning nano-fiber non-woven fabric |
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| JP4047744B2 (en) * | 2003-02-27 | 2008-02-13 | 日本バイリーン株式会社 | Electrostatic spinning method and electrostatic spinning apparatus |
| CN101142345A (en) * | 2004-12-27 | 2008-03-12 | 纳幕尔杜邦公司 | Electroblowing web formation process |
| CN101003916A (en) * | 2007-01-12 | 2007-07-25 | 东华大学 | Jet type electrostatic spinning equipment capable of producing Nano fiber in bulk |
| CN101387018A (en) * | 2008-10-17 | 2009-03-18 | 东南大学 | Visualization preparation method of electro spinning hollow TiO2 fiber |
| CN101709534A (en) * | 2009-11-17 | 2010-05-19 | 天津工业大学 | Device and method for manufacturing airflow melting electrostatic spinning nano-fiber non-woven fabric |
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