CN101979726A - Solvent circulation electrostatic spinning device - Google Patents
Solvent circulation electrostatic spinning device Download PDFInfo
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- CN101979726A CN101979726A CN 201010534832 CN201010534832A CN101979726A CN 101979726 A CN101979726 A CN 101979726A CN 201010534832 CN201010534832 CN 201010534832 CN 201010534832 A CN201010534832 A CN 201010534832A CN 101979726 A CN101979726 A CN 101979726A
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Abstract
The invention relates to a solvent circulation electrostatic spinning device, which comprises a double-channel axial flow injection pump, a guide pipe, a metal spinning head, a high-pressure generator and a fiber collection plate. Polymer spinning solution is filled into one axial flow injector in the double-channel axial flow injection pump, and a circulation solvent is filled into the other axial flow injector in the double-channel axial flow injection pump, wherein the axial flow injector filled with the circulation solvent is connected with the guide pipe; the axial flow injector filled with the polymer spinning solution is connected with the metal spinning head; the metal spinning head passes through the side wall of the guide pipe; and a coaxial spinning head structure is formed by the metal spinning head and the guide pipe. The fiber collection plate is arranged below the coaxial spinning head structure. One end of the high-pressure generator is connected with the metal spinning head by a high-pressure joint, and the other end of the high-pressure generator is connected with the fiber collection plate and is earthed.
Description
Technical field
The present invention relates to the preparation field of polymer superfine fibre, particularly relate to a kind of solvent circulation electrostatic spinning apparatus.
Background technology
The high-voltage electrostatic spinning technology is a kind of nano-fabrication technique of (top-down) from top to bottom, the surface tension of liquid and the viscoelastic power of making every effort to overcome the most advanced and sophisticated drop of clothes shower nozzle by extra electric field form jet, under electrostatic repulsion, Coulomb force and surface tension acting in conjunction, liquid jet after being atomized by the high frequency bending, draw, divide, drafted thousands of times in a few tens of milliseconds obtains nano-scale fiber through solvent evaporates or melt cooling at receiving terminal.This technical matters process is simple, control conveniently, select that material ranges is extensive, controllability strong and can have the nanofiber of microstructure characteristic by the sprinkler design preparation, be considered to most possibly realize a kind of method of continuous nano-fibre suitability for industrialized production, use this technology and prepare functional nano-fiber and have good prospect.
But up to the present, the spinning technique of nearly all bibliographical information all is to carry out the nanofiber preparation under atmospheric environment.As when preparation 25% polyvinylpyrrolidone singly the spinning of (PVP), usually adopt syringe needle (No. 1 stainless steel syringe needle that scabbles, internal diameter 1.0mm) as the capillary that sprays thread, high pressure generator (ZGF2000 type, Shanghai Su Te Electrical Appliances Co., Ltd), in order to control the micro-injection pump (U.S. of spinning solution flow
Company) with in order to receive fiber aluminium foil flat board.Spinning solution is that 25.0g PVP K60 powder is scattered in 100 milliliters of absolute ethyl alcohols at normal temperatures, and jolting becomes faint yellow homogeneous transparent liquid in shaking table then, carries out high-voltage electrostatic spinning in atmosphere, the preparation nano fibrous membrane.Weave under following technological parameter: the flow velocity of micro-injection pump is 1.0mL/h; the aluminium foil flat board is 15cm from the spinneret distance; the voltage of high pressure generator is 12kV; environment temperature is (23 ± 1) ℃; ambient humidity is 62 ± 4%; because the quick volatilization of solvent in atmosphere of polymer dope usually can cause spinneret to stop up, interrupt the quality of spinning process, impact polymer nanofiber during preparation.For the solution of this problem, also do not find relevant report at present.
Summary of the invention
Technical problem to be solved by this invention provides a kind of solvent circulation electrostatic spinning apparatus, solves spinneret blockage problem in the electrospinning process, the preparation polymer superfine fibre, and improve the electrospinning process yield.
The technical solution adopted for the present invention to solve the technical problems is: a kind of solvent circulation electrostatic spinning apparatus is provided, comprise binary channels axial flow syringe pump, conduit, metal spinneret, high pressure generator and fiber collecting plate, be placed with polymer dope in the axial flow syringe in the described binary channels axial flow syringe pump, be placed with the circulation solvent in another axial flow syringe; The described axial flow syringe that is placed with the circulation solvent links to each other with conduit; The described axial flow syringe that is placed with polymer dope links to each other with the metal spinneret; Described metal spinneret passes described duct wall, and forms coaxial spinneret structure with conduit; Described coaxial spinneret structure below is provided with described fiber collecting plate; Described high pressure generator one end links to each other with described metal spinneret by high pressure connection, and the other end links to each other with described fiber collecting plate and ground connection.
Described conduit is a silicone tube.
Described metal spinneret links to each other with described high pressure connection by alligator forceps.
Described fiber collecting plate is the aluminium foil flat board.
Described polymer dope is that polyvinylpyrrolidonepowder powder is dispersed at normal temperatures in the absolute ethyl alcohol and forms with the shaking table jolting; Described circulation solvent is a N,N-dimethylacetamide.
Beneficial effect
Owing to adopted above-mentioned technical scheme, the present invention compared with prior art has following advantage and good effect: (1) adopts the present invention to prepare polymer fiber, and technology is simple, is suitable for suitability for industrialized production.(2) because the circulation solvent can lubricate spinneret, stop separating out and adhesion of polymer, the jet surface cure effect that can also effectively stop the too early volatilization of polymer dope solvent and cause, therefore the present invention solves that spinneret easily stops up and problem such as the electrospinning productive rate is low, can carry out spinning to the high concentration polymer spinning solution.(3) the obtained ultra-fine fiber construction uniform outer surface of the present invention is smooth.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is a coaxial spinneret structural representation of the present invention;
Fig. 3 is the sem photograph that adopts the fiber of the present invention's preparation;
Fig. 4 is the diameter distribution map that adopts the fiber of the present invention's preparation.
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.
As shown in Figure 1, a kind of solvent circulation electrostatic spinning apparatus comprises binary channels axial flow syringe pump 1, conduit 2, metal spinneret 3, high pressure generator 4 and fiber collecting plate 5.Be placed with polymer dope in the axial flow syringe in the described binary channels axial flow syringe pump 1, be placed with the circulation solvent in another axial flow syringe, can control the flow-rate ratio of circulation solvent and polymer dope by the axial flow syringe of two selection different volumes.Wherein, the axial flow syringe that is placed with the circulation solvent links to each other with conduit 2, and the described axial flow syringe that is placed with polymer dope links to each other with metal spinneret 3.As shown in Figure 2, described metal spinneret 3 passes described conduit 2 sidewalls, and forms coaxial spinneret structure with conduit 2.Described coaxial spinneret structure below is provided with described fiber collecting plate 5.Described high pressure generator 4 one ends link to each other with described metal spinneret 3 by high pressure connection, and the other end links to each other with described fiber collecting plate 5 and ground connection.In this device, conduit 2 adopts elastomeric silicone tube; The fiber collecting plate is the aluminium foil flat board; High pressure connection directly is connected with metal spinneret 3 by alligator forceps.Need to prove, can adopt two single channel axial flow syringe pumps to replace binary channels axial flow syringe pumps in the present invention, only need in use the flow of two single channel axial flow syringe pumps that circulation solvent and polymer dope are housed is regulated and control to get final product respectively.
Below the simple process that adopts the present invention from 30%PVP, to prepare fiber of introducing.At first, 30.0g PVP K60 powder is scattered in 100 milliliters of absolute ethyl alcohols at normal temperatures, jolting becomes 30% faint yellow homogeneous transparent spinning solution in shaking table afterwards.Then, this 30% faint yellow homogeneous transparent spinning solution is packed in the axial flow syringe in the binary channels axial flow syringe pump as polymer dope, again N,N-dimethylacetamide is packed in another axial flow syringe in the binary channels axial flow syringe pump as the circulation solvent.Then, the aluminium foil flat board is placed on 15cm place, spinning nozzle (i.e. the coaxial spinneret structure that is formed by metal spinneret and conduit) below, connects high pressure generator, and its voltage is made as 12kV.At last, opening power prepares ultra-fine PVP fiber, and the environment temperature of this moment is (23 ± 1) ℃, and ambient humidity is 62 ± 4%.In preparation process, it is 1cm/h that binary channels axial flow syringe pump advances speed, and can adopt the syringe of two different volumes to regulate and control the relative discharge of polymer dope and circulation solvent.As the syringe volume that polymer dope is housed is 10ml, and the syringe volume that the circulation solvent is housed is 1,2,5 and 10ml, that is to say that the flow-rate ratio of circulation solvent and polymer dope was respectively 0.1: 1 0.2: 1,0.5: 1 and 1: 1.
Under these conditions, the fiber that solvent-applied circulation high-voltage electrostatic spinning prepared obtains carries out adopting scanning electron microscopic observation behind the surperficial metal spraying, the result as shown in Figure 4, A represents that the flow-rate ratio of circulation solvent and polymer dope is that 0.1: 1, B represent that the flow-rate ratio of circulation solvent and polymer dope is that 0.2: 1, C represent that the flow-rate ratio of circulation solvent and polymer dope is that 0.5: 1, D represent that the flow-rate ratio of circulation solvent and polymer dope is 1: 1 among Fig. 4.Adopt Image J software that distribution of fiber diameters is carried out statistical analysis, the result as shown in Figure 5, same A represents that the flow-rate ratio of circulation solvent and polymer dope is that 0.1: 1, B represent that the flow-rate ratio of circulation solvent and polymer dope is that 0.2: 1, C represent that the flow-rate ratio of circulation solvent and polymer dope is that 0.5: 1, D represent that the flow-rate ratio of circulation solvent and polymer dope is 1: 1.As we know from the figure, in suitable solvent flux scope (flow-rate ratio of circulation solvent and polymer dope is 0.1: 1,0.2: 1,0.5: 1), smooth, the even structure of not only prepared fiber surface, and along with the increase of circulation solvent flow rate, fibre diameter dwindles gradually.
Claims (5)
1. solvent circulation electrostatic spinning apparatus, comprise binary channels axial flow syringe pump (1), conduit (2), metal spinneret (3), high pressure generator (4) and fiber collecting plate (5), it is characterized in that, be placed with polymer dope in the axial flow syringe in the described binary channels axial flow syringe pump (1), be placed with the circulation solvent in another axial flow syringe; The described axial flow syringe that is placed with the circulation solvent links to each other with described conduit (2); The described axial flow syringe that is placed with polymer dope links to each other with described metal spinneret (3); Described metal spinneret (3) passes described conduit (2) sidewall, and forms coaxial spinneret structure with conduit (2); Described coaxial spinneret structure below is provided with described fiber collecting plate (5); Described high pressure generator (4) one ends link to each other with described metal spinneret (3) by high pressure connection, and the other end links to each other with described fiber collecting plate (5) and ground connection.
2. solvent circulation electrostatic spinning apparatus according to claim 1 is characterized in that described conduit (2) is a silicone tube.
3. solvent circulation electrostatic spinning apparatus according to claim 1 is characterized in that described metal spinneret (3) links to each other with described high pressure connection by alligator forceps.
4. solvent circulation electrostatic spinning apparatus according to claim 1 is characterized in that described fiber collecting plate (5) is the aluminium foil flat board.
5. solvent circulation electrostatic spinning apparatus according to claim 1 is characterized in that, described polymer dope is that polyvinylpyrrolidonepowder powder is dispersed at normal temperatures in the absolute ethyl alcohol and forms with the shaking table jolting; Described circulation solvent is a N,N-dimethylacetamide.
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| CN 201010534832 CN101979726A (en) | 2010-11-08 | 2010-11-08 | Solvent circulation electrostatic spinning device |
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| CN 201010534832 CN101979726A (en) | 2010-11-08 | 2010-11-08 | Solvent circulation electrostatic spinning device |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220649A (en) * | 2011-04-24 | 2011-10-19 | 兰州大学 | Preparation method of nanofiber |
| CN102230231A (en) * | 2011-06-17 | 2011-11-02 | 上海理工大学 | Infrared-radiation-assisted high-voltage static spray device with coaxial spinning nozzle and application thereof |
| CN102240251A (en) * | 2011-06-17 | 2011-11-16 | 上海理工大学 | Constant-temperature high-voltage electrostatic spray device and method preparing polymer medicine-carrying nanoparticles by using same |
| CN102266825A (en) * | 2011-06-17 | 2011-12-07 | 上海理工大学 | Infrared radiation assisted high-voltage electrostatic spraying device with single nozzle and application thereof |
| CN102517670A (en) * | 2011-11-08 | 2012-06-27 | 上海理工大学 | Method for preparing polyacrylonitrile nano-fibers by circulation and coaxial electrospinning of surface active agent solution |
| CN102560713A (en) * | 2011-11-08 | 2012-07-11 | 上海理工大学 | Method for preparing polyacrylonitrile nano-fiber by electrolyte solution circulation high-pressure electrostatic spinning |
| CN104480546A (en) * | 2015-01-19 | 2015-04-01 | 上海理工大学 | Electrospinning paralleling shaft spinning head with angle correlation and application |
| CN105369369A (en) * | 2015-12-24 | 2016-03-02 | 北京化工大学 | Centrifugal coaxial electrostatic spinning machine |
| CN106048891A (en) * | 2016-07-13 | 2016-10-26 | 上海理工大学 | Preparation method of poly (2-aminothiazole) nanofiber composite membrane |
| CN106591966A (en) * | 2016-11-21 | 2017-04-26 | 上海理工大学 | Electro-hydro dynamics preparation method for filament and particle parallel micro-nano structure |
| CN106757414A (en) * | 2016-11-30 | 2017-05-31 | 上海理工大学 | A kind of solvent circulation coaxial high pressure electrostatic spraying method and device |
| CN109295511A (en) * | 2018-09-26 | 2019-02-01 | 上海理工大学 | Detachable Coaxial nozzle, the preparation method of electric spinning equipment and core sheath nanofiber |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220649B (en) * | 2011-04-24 | 2012-07-11 | 兰州大学 | Preparation method of nanofiber |
| CN102220649A (en) * | 2011-04-24 | 2011-10-19 | 兰州大学 | Preparation method of nanofiber |
| CN102230231A (en) * | 2011-06-17 | 2011-11-02 | 上海理工大学 | Infrared-radiation-assisted high-voltage static spray device with coaxial spinning nozzle and application thereof |
| CN102240251A (en) * | 2011-06-17 | 2011-11-16 | 上海理工大学 | Constant-temperature high-voltage electrostatic spray device and method preparing polymer medicine-carrying nanoparticles by using same |
| CN102266825A (en) * | 2011-06-17 | 2011-12-07 | 上海理工大学 | Infrared radiation assisted high-voltage electrostatic spraying device with single nozzle and application thereof |
| CN102240251B (en) * | 2011-06-17 | 2014-04-16 | 上海理工大学 | Constant-temperature high-voltage electrostatic spray device and method preparing polymer medicine-carrying nanoparticles by using same |
| CN102517670A (en) * | 2011-11-08 | 2012-06-27 | 上海理工大学 | Method for preparing polyacrylonitrile nano-fibers by circulation and coaxial electrospinning of surface active agent solution |
| CN102517670B (en) * | 2011-11-08 | 2013-11-06 | 上海理工大学 | Method for preparing polyacrylonitrile nano-fibers by circulation and coaxial electrospinning of surface active agent solution |
| CN102560713A (en) * | 2011-11-08 | 2012-07-11 | 上海理工大学 | Method for preparing polyacrylonitrile nano-fiber by electrolyte solution circulation high-pressure electrostatic spinning |
| CN102560713B (en) * | 2011-11-08 | 2014-08-20 | 上海理工大学 | Method for preparing polyacrylonitrile nano-fiber by electrolyte solution circulation high-pressure electrostatic spinning |
| CN104480546A (en) * | 2015-01-19 | 2015-04-01 | 上海理工大学 | Electrospinning paralleling shaft spinning head with angle correlation and application |
| CN105369369A (en) * | 2015-12-24 | 2016-03-02 | 北京化工大学 | Centrifugal coaxial electrostatic spinning machine |
| CN106048891A (en) * | 2016-07-13 | 2016-10-26 | 上海理工大学 | Preparation method of poly (2-aminothiazole) nanofiber composite membrane |
| CN106048891B (en) * | 2016-07-13 | 2018-05-22 | 上海理工大学 | A kind of preparation method of poly- (thiazolamine) nano-fiber composite film |
| CN106591966A (en) * | 2016-11-21 | 2017-04-26 | 上海理工大学 | Electro-hydro dynamics preparation method for filament and particle parallel micro-nano structure |
| CN106591966B (en) * | 2016-11-21 | 2020-11-24 | 上海理工大学 | Electrohydrodynamic preparation method of silk particle parallel micro-nano structure |
| CN106757414A (en) * | 2016-11-30 | 2017-05-31 | 上海理工大学 | A kind of solvent circulation coaxial high pressure electrostatic spraying method and device |
| CN109295511A (en) * | 2018-09-26 | 2019-02-01 | 上海理工大学 | Detachable Coaxial nozzle, the preparation method of electric spinning equipment and core sheath nanofiber |
| CN109295511B (en) * | 2018-09-26 | 2022-05-31 | 上海理工大学 | Detachable coaxial nozzle, electrospinning device and preparation method of core-sheath nanofiber |
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Application publication date: 20110223 |