CN102534822A - 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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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 for preparing the polysulfonamides nanometer fiber net.
Background technology
Polysulfonamides fibre (being called for short the PSA fiber) has another name called polysulphonamide fiber, and formal name used at school is a 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 is to have good heat resistance and heat endurance, and anti-flammability is high, and chemical-resistant stability is good, except that several kinds of the polarity very strong solvent such as the concentrated sulfuric acid, at normal temperatures chemicals is all had good stable property.Polysulfonamides fibre is as a kind of novel textile material, has high-strength, lightweight, resistant to elevated temperatures characteristics and is applied to protection and other civil areas that fire-retardant requirement is arranged under aerospace field, the high-temperature work environment.The polysulfonamides viscosity is bigger, and electric conductivity is relatively poor, and the method for preparing polysulfonamides fibre at present mainly is a wet spinning process.
Electrostatic spinning technique has had the history in more than 70 year, and it is from 1934 the earliest, and Formhal has invented with electrostatic force and prepared the experimental provision of polymer fiber and applied for patent, has announced how polymer solution forms jet between electrode.。The preparation nanofiber has a lot of methods at present; As the method for reeling off raw silk from cocoons (Ondarcuhu T, Joachim C.Drawing a single nanofibre over hundreds of microns [J] .Europhys Left, 1998; 215), template synthetic method (Feng L 42 (2):; Li S.Super-hydrophobic surface of aligned poly-acrylonitrile nanofibers [J] .Angrew Chem Int, 2002,41 (7): 1221-1223; Martin C R.Membrane-based synthesis of nanomaterials [J] .Chem Mater; 1996; 8 (8): 1739-1746.), split-phase method (Ma PX, Zhang R Y.Synthetic nano-scale fibrous 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-A European; 1999, (5): 2740-2750.) and method of electrostatic spinning.The shortcoming of the method for reeling off raw silk from cocoons is that solution viscosity is required too harshness; The shortcoming of template synthetic method is the continuous fibers that can not prepare the division of root root; Split-phase method and self-assembly method productivity ratio are all lower.The fibre diameter that electrostatic spinning technique makes generally arrives hundreds of nanometers at tens nanometer, and its specific area is bigger, and has successional structure, and the film that makes has the big fine quality of porosity.This characteristics determined this kind nanofiber have remarkable advantages at aspects such as assembling, nanoprocessings.At present, the electrostatic spinning fiber material has good application in a lot of fields, as is used for aspects such as filtering material, wound clad material and tissue engineering bracket.Along with development in recent years, the kind and the choice of Solvent of raw material dropped into more research.
People are applied to prepare nearly 100 kinds of polymer nanofibers with electrostatic spinning technique, comprise Merlon (OGHITZKI M, CZAKO W; FRESE T, et al.Nanostructured fibers via electrospinning [J] .Advanced Materials, 2001; 13 (1): 70-72) polysulfones (GOPAL R, KAUR S, 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.) wait the solvable synthesising macromolecule copolymer of organic solvent, polyvinyl alcohol (JAEGER R; BERGSHOEF M M, BATLLE C M I, et al.Elecrospinning of ultra-thin polymer fibers [J] .Macromolecular Symposia; 1998,127:141-150.), PEO (DOSHI J; RENEKER D H.Electrospinning process and applications of elecrospun fibers [J] .Journal of Elecrostatics, 1995,35 (2-3): water-soluble synthesising macromolecule copolymer, PLA (TAN S H such as 151-160.); INAI R, KOTAKI M, et al.Systematic parameter study for ultra-fine fiber fabrication via electrospinning process [J] .Polymer; 2005,46 (16): 6128-6134) wait synthesized degradable high molecular polymer and cellulose (KIM C, FREY M; MARQUEZ M; Et al.Preparation of submicron-scale, elecrospun cellulose fibers via direct dissolution [J] .Journal of Polymer Science Part B:Polymer Physics, 2005; 43 (13): 1673-1683.), fibroin (BUCHKOA C J; CHENAL C, SHENA Y, et al.Processing and microstructural characterization of porous biocompatible protein polymer thin films [J] .Polymer; 1999,40:7397-7407.) wait natural polymers and derivative thereof.
Because polysulfonamides viscosity is big; Poorly conductive; Add method of electrostatic spinning itself and have problems such as fiber production is low, pore obstruction, solution evaporation; The nanoscale polysulfonamides fibre that obtains certain output is difficulty very, and is considerably less for utilizing electrostatic spinning to prepare the research of polysulfonamides nanofiber at present, has only patent CN101724919A to mention and utilizes the magnetized electrostatic spinning legal system to be on the waiting list to arranging the polysulfonamides superfine fibre.
The present invention is a spinning solution with polysulfonamides solution, utilizes air-flow-method of electrostatic spinning (the multi-nozzle electrospinning device through having vibrating device and air flow system is realized) to prepare the polysulfonamides nanometer fiber net in enormous quantities.And best spinning technology parameter proposed.
Summary of the invention
The problem big to polysulfonamides viscosity, that poorly conductive and method of electrostatic spinning yield poorly, the present invention proposes the apparatus and method that a kind of air-flow-static combines preparation polysulfonamides nanometer fiber net.
For this reason, technical scheme of the present invention is following:
A kind of air-flow-static combines the device of preparation polysulfonamides nanometer fiber net, comprises liquid storage tank, gas compartment, electrostatic generator and receiving system;
Said liquid storage tank connects outside liquid feed device through 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, and the liquid storage tank bottom is provided with several spinning heads;
Said gas compartment is arranged on the liquid storage tank outside and is connected with feeder, the closed front of its top and said liquid storage tank, and the bottom is provided with and the identical gas outlet of spinning head quantity, liquid storage tank bottom, and said spinning head is arranged in the said gas outlet;
The positive pole of said electrostatic generator is drawn multistylus electrode and is linked to each other with spinning head, and negative pole is drawn lead and linked to each other 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 between spinning head and receiving system is controlled at 5～25cm.
Said feeder is a nitrogen cylinder, connects gas compartment and controls air velocity through flowmeter through wireway.
Said receiving system comprises swing roller, toggle and motor; The rotary axle box of said swing roller is on slide bar; One end of turning cylinder is connected through revolute pair with toggle makes swing roller be implemented in the transverse movement on the slide bar, and the other end connects motor makes swing roller realize that transhipment is moving.
On the said swing roller aluminium foil can be set, but said motor connection speed controller is to control its rotating speed.
A kind of air-flow-static combines to prepare the method for polysulfonamides nanometer fiber net, may further comprise the steps:
(1) the unlatching liquid feed device spins solution through woven hose injection liquid storage tank with DMAC (dimethylacetylamide) static of polysulfonamides, keeps solution not have 2/3 place of bar-shaped sensor;
(2) open supersonic generator solution is carried out ultrasonic vibration, supersonic frequency is 30～40KHz; Open receiving system swing roller is moved reciprocatingly with the speed of 5cm/min, rotate with the speed of 800～1000rpm; Open feeder to the 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.
It is 5%～16% that the DMAC static of polysulfonamides described in the step (1) spins the mass percent concentration of solution, preferred 12%.
The preferred 20KV of voltage in the step (2) between the 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 the rotating speed of motor.
The problem big to polysulfonamides viscosity, that poorly conductive and method of electrostatic spinning yield poorly, the present invention has taked technique scheme; Realized that air-flow power and electrostatic field force overcome the surface tension of polysulfonamides solution jointly on the one hand, correlation stream stretches, and makes the fiber that makes thinner; More even, aggravated the evaporation rate of solvent simultaneously, reduced the drop amount; The drop area is corresponding to be reduced, and finally makes polysulfonamides nanofiber specific area increase greatly; On the other hand, the introducing of air-flow makes original electrostatic spinning syringe needle blocking problem alleviate greatly, has improved spinning efficiency, increases polysulfonamides nanometer fiber net output; In addition, the present invention directly prepares nanofiber at normal temperatures, does not need heating, has simplified production stage, has practiced thrift production cost, and environmentally safe has been opened up a kind of new situations that polysulfonamides is used for electrostatic spinning technique, and good market prospects are arranged.
Description of drawings
Fig. 1 is the structural representation that air-flow of the present invention-static combines the device of preparation polysulfonamides nanometer fiber net.
Fig. 2 (a) is the SEM photo of the polysulfonamides nanofiber of the embodiment of the invention 1 preparation.
Fig. 2 (b) is the SEM photo of the polysulfonamides nanofiber of the embodiment of the invention 2 preparations.
Fig. 3 is the SEM photo of the polysulfonamides nanofiber of the embodiment of the invention 3 preparations.
Fig. 4 is the form photo of the embodiment of the invention 4 spinning process taylor cones.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
As shown in Figure 1, air-flow of the present invention-static combines the device of preparation 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 through woven hose 110; Liquid storage tank inside is provided with bar-shaped sensor 130; Bar-shaped sensor is connected with supersonic generator 140, and the liquid storage tank bottom is provided with several spinning heads 150, and the internal orifice dimension of spinning head is 0.4～1mm; Length is 8～12mm, and spacing is 10mm; Distance between spinning head and receiving system is controlled at 5～25cm.
The positive pole of electrostatic generator is drawn multistylus electrode 310 and is linked to each other with spinning head, and negative pole 320 is drawn lead and linked to each other 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 is connected through revolute pair with toggle makes swing roller be implemented in the transverse movement on the slide bar, and the other end connects motor makes swing roller realize that transhipment is moving.
The step that the use said apparatus prepares concrete polysulfonamides nanometer fiber net is following:
(1) the preparation quality percent concentration is that the DMAC static of 5%～16% polysulfonamides PSA spins solution, and the preparation process is big with reference to gold, and envelope is inferior, Yan Xiong etc. the cryogenic fluid polycondensation prepares the research [J] of aromatic polysulfonamides. and synthetic fiber, 2007, (10): 27-36;
(2) the unlatching liquid feed device spins solution through woven hose injection liquid storage tank with the DMAC static of polysulfonamides, keeps solution not have 2/3 place of bar-shaped sensor;
(3) open supersonic generator solution is carried out ultrasonic vibration, supersonic frequency is 30～40KHz; Open receiving system swing roller is moved reciprocatingly with the speed of 5cm/min, rotate with the speed of 800～1000rpm; Open feeder to the 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 that the DMAC static of polysulfonamides spins solution is 12%, and the voltage between the 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.
By the above-mentioned spinning 1h that is provided with, make nanometer polysulfonamides nanometer fiber net, through electronic microscope photos, the formalness and the structure that obtain fiber are shown in Fig. 2 (a).
Through test, the average diameter of the polysulfonamides nanofiber that makes is 56nm, and the distribution of fiber diameters dispersion is little, mainly concentrates on 50～100nm, and fiber specific surface area is 51m
2/ g, the output of polysulfonamides nanofiber is 15mg/h.
Embodiment 2:
Present embodiment and embodiment 1 are basic identical, and different is that present embodiment does not feed air-flow.Observe spinning process, find that amount of droplets is more, the syringe needle clogging is more serious.Make fiber external structure form such as Fig. 2 (b) of polysulfonamides nanometer fiber net.Average diameter through testing the polysulfonamides nanofiber that makes is 85nm, and the distribution of fiber diameters dispersion is little, mainly concentrates on 75～150nm, and fiber specific surface area is 35.6m
2/ g, the output of polysulfonamides nanofiber is 6.1mg/h.
Embodiment 3:
Present embodiment and embodiment 1 are basic identical, and different is that present embodiment is not opened supersonic generator.The fiber external structure form that makes the polysulfonamides nanometer fiber net is as shown in Figure 3, can find the bead fiber, and the output of polysulfonamides nanofiber is 2.5mg/h.
Embodiment 4:
Present embodiment and embodiment 1 are basic identical, and different is that present embodiment does not feed air-flow and do not open supersonic generator.Observe spinning process, discovery spinning difficulty is carried out, and can only obtain less fiber, and the terminal taylor cone of shower nozzle has shrinkage phenomenon, retreats into the inner (see figure 4) of shower nozzle.
Relatively four embodiment can know; Adopt embodiment 1 that shaking device and air flow system are opened simultaneously, more help realizing spinning acquisition polysulfonamides nanometer fiber net through static, the syringe needle blockage problem is alleviated greatly; Spinning process is more smooth; And the fiber that makes is thinner, and is more even, and specific area is bigger.
The foregoing description is interpreted as only being used to the present invention is described and is not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can do various changes or modification to the present invention, and these equivalences change and modify and fall into claim of the present invention institute restricted portion equally.
Claims (9)
1. the device of air-flow-static combination preparation polysulfonamides nanometer fiber net is characterized in that, comprises liquid storage tank, gas compartment, electrostatic generator and receiving system;
Said liquid storage tank connects outside liquid feed device through 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, and the liquid storage tank bottom is provided with several spinning heads;
Said gas compartment is arranged on the liquid storage tank outside and is connected with feeder, the closed front of its top and said liquid storage tank, and the bottom is provided with and the identical gas outlet of spinning head quantity, liquid storage tank bottom, and said spinning head is arranged in the said gas outlet;
The positive pole of said electrostatic generator is drawn multistylus electrode and is linked to each other with spinning head, and negative pole is drawn lead and linked to each other with receiving system.
2. air-flow according to claim 1-static combines the device of preparation polysulfonamides nanometer fiber net; It is characterized in that the internal orifice dimension of described spinning head is 0.4～1mm, length is 8～12mm; Spacing is 10mm, and the distance between spinning head and receiving system is controlled at 5～25cm.
3. air-flow according to claim 1-static combines the device of preparation polysulfonamides nanometer fiber net, it is characterized in that said feeder is a nitrogen cylinder, connects gas compartment and passes through flowmeter control air velocity through wireway.
4. air-flow according to claim 1-static combines the device of preparation polysulfonamides nanometer fiber net; It is characterized in that; Said receiving system comprises swing roller, toggle and motor; The rotary axle box of said swing roller is on slide bar, and an end of turning cylinder is connected through revolute pair with toggle makes swing roller be implemented in the transverse movement on the slide bar, and the other end connects motor makes swing roller realize that transhipment is moving.
5. air-flow according to claim 1-static combines the device of preparation polysulfonamides nanometer fiber net, it is characterized in that on the said swing roller aluminium foil is set, said motor connection speed controller is to control its rotating speed.
6. air-flow-static combination prepares the method for polysulfonamides nanometer fiber net, it is characterized in that, may further comprise the steps:
(1) the unlatching liquid feed device spins solution through woven hose injection liquid storage tank with the DMAC static of polysulfonamides, keeps solution not have 2/3 place of bar-shaped sensor;
(2) open supersonic generator solution is carried out ultrasonic vibration, supersonic frequency is 30～40KHz; Open receiving system swing roller is moved reciprocatingly with the speed of 5cm/min, rotate with the speed of 800～1000rpm; Open feeder to the 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.
7. air-flow according to claim 6-static combines to prepare the method for polysulfonamides nanometer fiber net, it is characterized in that it is 5%～16% that the DMAC static of polysulfonamides described in the step (1) spins the mass percent concentration of solution.
8. air-flow according to claim 6-static combines to prepare the method for polysulfonamides nanometer fiber net, it is characterized in that it is 12% that the DMAC static of polysulfonamides described in the step (1) spins the mass percent concentration of solution.
9. air-flow according to claim 6-static combines to prepare the method for polysulfonamides nanometer fiber net; It is characterized in that the voltage in the step (2) between the electrostatic generator both positive and negative polarity is 20KV, receiving range is 15cm; Air-flow velocity is 8L/min, and the rotating speed of motor is 850rpm.
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