CN106400134A - Reciprocating liquid feeding type nozzle-free electrostatic spinning device and method for producing nano-fiber membranes by using same - Google Patents

Reciprocating liquid feeding type nozzle-free electrostatic spinning device and method for producing nano-fiber membranes by using same Download PDF

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Publication number
CN106400134A
CN106400134A CN201610989957.2A CN201610989957A CN106400134A CN 106400134 A CN106400134 A CN 106400134A CN 201610989957 A CN201610989957 A CN 201610989957A CN 106400134 A CN106400134 A CN 106400134A
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China
Prior art keywords
stainless steel
reservoir
seal wire
steel silk
spinning
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Application number
CN201610989957.2A
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CN106400134B (en
Inventor
刘呈坤
于群
贺海军
孙润军
陈美玉
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Xian Polytechnic University
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Xian Polytechnic University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

The invention discloses a reciprocating liquid feeding type nozzle-free electrostatic spinning device. The reciprocating liquid feeding type nozzle-free electrostatic spinning device comprises a hollow groove barrel and an airbag arranged in a cavity of the hollow groove barrel, wherein an opening of the airbag is connected with one end of the hollow groove barrel; an electronic air pump is arranged at the end of the hollow groove barrel; the other end of the hollow groove barrel is connected with a liquid storage groove; wire guide blocks are arranged on two opposite side walls of the liquid storage groove; a stainless steel wire is arranged between the wire guide blocks; one end of the stainless steel wire is connected with a positive electrode of a direct-current and high-voltage generator; and a collection curtain is arranged above the liquid storage groove. The invention further discloses a method for preparing nano-fiber membranes by adopting the device. The reciprocating liquid feeding type nozzle-free electrostatic spinning device takes the stainless steel wire as a carrier and keeps an immobilized state in a spinning process; requirements on control conditions are relatively low and the fineness uniformity of nano-fibers can be effectively improved; and the electronic air pump is adopted and a fully filled state of the air pump is controlled through periodically inflating and exhausting air at a certain speed, and a liquid level height is continuously adjusted so that the spinning can be continuously carried out.

Description

The method back and forth giving liquid formula no nozzle electrostatic spinning apparatus and its nano fibrous membrane processed
Technical field
The invention belongs to electrostatic spinning technique field, it is related to one kind back and forth to liquid formula no nozzle electrostatic spinning apparatus, this The bright method further relating to prepare nano fibrous membrane using said apparatus.
Background technology
Nanofiber is big due to specific surface area, leads to its surface energy and surface activity to increase, thus creating small size effect Should, surface or interfacial effect, quantum size effect and macro quanta tunnel effect etc., in optics, electricity, magnetics and calorifics etc. Aspect shows excellent property, obtains extensive concern in fields such as physics, chemistry, electronics and materials.At present, in multiple preparations In the method for nanofiber, method of electrostatic spinning with simple to operate, applied widely the advantages of and be widely used.
The maximum shortcoming of conventional electrostatic spining technology is as spinning head using single syringe needle at present, and a general syringe needle is only Can produce a branch of jet, ejection efficiency very low it is impossible to meet multiple application requirements, therefore how to realize mass manufacture Nanowire Dimension is the key that electrostatic spinning technique obtains commercial Application.Up to the present, the technology improving nanofiber yield mainly includes Multiinjector electrostatic spinning technique, no nozzle electrostatic spinning technique, air-flow auxiliary multiinjector electrostatic spinning technique and centrifugation Static Spinning Silk technology etc..
Wherein, multiinjector electrostatic spinning technique and no nozzle electrostatic spinning technique realize nano fiber batch metaplasia product Main path, the therefore research with regard to this respect are more.But for multiinjector electrostatic spinning apparatus, each needle point tip electric field phase Mutually affect, fibre net homogeneity is difficult to ensure that, and shower nozzle easily blocks, and so that production cannot be carried out continuously.So we more close The note many jet flow static electricities of needleless spin, and it can significantly improve that in pin Static Spinning, syringe needle easily blocks, and being capable of the more day of one's doom Degree ground improves the yield of electrostatic spinning fiber.
Content of the invention
It is an object of the invention to provide a kind of back and forth give liquid formula no nozzle electrostatic spinning apparatus, solve existing multiinjector quiet The susceptible to plugging problem of spinning head in electro-spinning process.
It is a further object of the present invention to provide receiving back and forth to the no nozzle electrostatic spinning apparatus preparation of liquid formula using above-mentioned one kind The method of rice fibrous membrane.
The technical solution adopted in the present invention is that one kind back and forth gives liquid formula no nozzle electrostatic spinning apparatus, including groove Cylinder and the air bag that is arranged in hollow grooved drum cavity, air bag opening is connected with hollow grooved drum one end, hollow grooved drum and air bag opening The one end connecting is provided with EAP Electronic Air Pump, and the hollow grooved drum other end is connected with reservoir, and communicates with reservoir;Reservoir is relatively Two side walls on be provided with seal wire block, be provided with stainless steel silk between seal wire block, stainless steel silk one end and high direct voltage are sent out Raw device positive pole connects, and is provided with collection curtain above reservoir, collects curtain ground connection.
The feature of the present invention also resides in,
Seal wire block is higher than the junction of reservoir and groove drum, and one of side wall that seal wire block is located is with hollow grooved drum even Connect.
Seal wire block hollow, seal wire block arranges perforation, and stainless steel silk is arranged mutually parallel through eyelet.
Another technical scheme of the present invention is, a kind of method preparing nano fibrous membrane, and the one kind being adopted is past Again to liquid formula no nozzle electrostatic spinning apparatus, including hollow grooved drum and the air bag being arranged in hollow grooved drum cavity, air bag opening It is connected with hollow grooved drum one end, one end that hollow grooved drum is connected with air bag opening is provided with EAP Electronic Air Pump, the hollow grooved drum other end It is connected with reservoir, and communicate with reservoir;It is provided with seal wire block on two relative side walls of reservoir, set between seal wire block It is equipped with stainless steel silk, stainless steel silk one end is connected with high voltage direct current generator positive pole, above reservoir, is provided with collection curtain, collect Curtain is grounded;
Seal wire block is higher than the junction of reservoir and groove drum, and one of side wall that seal wire block is located is with hollow grooved drum even Connect;
Seal wire block hollow, seal wire block arranges perforation, and stainless steel silk is arranged mutually parallel through eyelet;
Specifically implement according to following steps:
Spinning liquid is injected in reservoir, controls environment temperature and humidity, adjust stainless steel silk and the distance collecting curtain, open Open EAP Electronic Air Pump, adjust total amount and the speed of conveying gas, open high voltage direct current generator, adjust applied voltage, in electric field force In the presence of, on stainless steel silk, the spinning liquid of coating produces jet, and jet solidify to form nanofibres deposit on collecting curtain, warp Nano fibrous membrane is obtained after crossing the spinning of certain time.
The feature of the present invention also resides in,
Ambient temperature is room temperature, and RH range is 40%~60%.
Stainless steel silk is 100mm~300mm with the vertical dimension collecting curtain.
Applied voltage is 10kV~30kV.
Before EAP Electronic Air Pump is opened, in reservoir spinning liquid and stainless steel silk be in a kind of definitely close to but do not contact with each other State.
EAP Electronic Air Pump conveys total amount and the speed of gas, so that air bag produces stable change in volume, and in pneumatophore When long-pending maximum, spinning liquid is fully contacted with stainless steel silk and is defined.
The invention has the beneficial effects as follows,
1. apparatus of the present invention structure is simple, operation facility, can effectively improve Nanowire using no nozzle electrostatic spinning apparatus The yield of dimension film;
2. the present invention is used stainless steel silk as carrier, and the state remaining stationary in spinning process, control strip Part requirement is relatively low, can effectively improve the fineness uniformity of nanofiber;
3. the present invention adopts EAP Electronic Air Pump to control the full state of air pump with given pace periodically inflation pumping, continues Regulating liquid surface height, makes that spinning is sustainable uninterruptedly to be carried out.
Brief description
Fig. 1 is a kind of back and forth structural representation to liquid formula no nozzle electrostatic spinning apparatus of the present invention.
In figure, 1. air bag, 2. hollow grooved drum, 3. EAP Electronic Air Pump, 4. reservoir, 5. stainless steel silk, 6. seal wire block, 7. direct current High tension generator, 8. collects curtain.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The present invention is a kind of back and forth to give liquid formula no its structure of nozzle electrostatic spinning apparatus as shown in figure 1, including hollow grooved drum 2 He It is arranged at the air bag 1 in hollow grooved drum 2 cavity, air bag 1 opening is connected with hollow grooved drum 2 one end, and hollow grooved drum 2 is opened with air bag 1 One end that mouth connects is provided with EAP Electronic Air Pump 3, and hollow grooved drum 2 other end is connected with reservoir 4, and communicates with reservoir 4;Liquid storage Be provided with seal wire block 6 on two relative side walls of groove 4, between seal wire block 6, be provided with stainless steel silk 5, stainless steel silk 5 one end with High voltage direct current generator 7 positive pole connects, and is provided with collection curtain 8 above reservoir 4, collects curtain 8 and is grounded.
One of side wall that wherein seal wire block 6 is located is connected with hollow grooved drum 2, and seal wire block 6 is higher than reservoir 4 and groove drum 2 junction.
Seal wire block 6 hollow, seal wire block 6 arranges perforation, and stainless steel silk 5 is arranged mutually parallel through eyelet.
Back and forth prepare nano fibrous membrane using above-mentioned to liquid formula no nozzle electrostatic spinning apparatus, specifically real according to following steps Apply:
Spinning liquid is injected in reservoir 4, control ambient temperature is room temperature, RH range is 40%~60%, adjusts Section stainless steel silk 5 is 100mm~300mm with the distance collecting curtain 8, opens EAP Electronic Air Pump 3, adjusts total amount and the speed of conveying gas Degree is so that air bag 1 produces stable change in volume, and ensures that spinning liquid is abundant with stainless steel silk 5 when air bag 1 volume is maximum Contact;It is then turned on high voltage direct current generator 7, regulation applied voltage is 10kV~30kV, in the presence of electric field force, rustless steel Silk 5 on coating spinning liquid produce jet, jet solidification after formed nanofibres deposit collect curtain 8 on, through one timing Between spinning after obtain nano fibrous membrane.
In spinning process, stainless steel silk 5 is parallel with spinning liquid liquid level.Before EAP Electronic Air Pump 3 is opened, spinning liquid in reservoir 4 It is in state that is a kind of definitely close but not contacting with each other with stainless steel silk 5;Due to reservoir 4, hollow grooved drum 2 and EAP Electronic Air Pump Closely connect between 3, the internal space being constituted a closing with EAP Electronic Air Pump 3 of air bag 1, after EAP Electronic Air Pump 3 starts, is opened simultaneously Begin air bag 1 is inflated, so that gas in air bag 1 is increased, volume becomes big, so that spinning liquid in groove drum 2 is gradually moved in reservoir 4, Thus leading to spinning liquid level in reservoir 4 to raise, so that spinning liquid level is contacted with stainless steel silk 5, after contact, adjusting EAP Electronic Air Pump 3 Extract a certain amount of gas out, air bag 1 volume diminishes, part spinning liquid again returns to, in groove drum 2, make spinning liquid level and rustless steel simultaneously Silk 5 separates.After stainless steel silk 5 is separated with liquid level, stainless steel silk 5 surface can coat the solution of layer, Jin Er Make solution layer form projection in the presence of electric field force, finally produce nanofiber.To control thus by adjusting EAP Electronic Air Pump 3 The full state of air bag 1, is made spinning liquid be lifted with given pace, thus constantly being contacted with stainless steel silk 5, separating, realizes nanometer The preparation of fibrous membrane.
The present invention is used stainless steel silk as carrier, and the state remaining stationary in spinning process, control condition Require relatively low, the fineness uniformity of nanofiber can be effectively improved;The present invention adopts EAP Electronic Air Pump to fill with given pace periodicity Gas is evacuated controlling the full state of air pump, continues regulating liquid surface height, makes that spinning is sustainable uninterruptedly to be carried out.Due to using no Nozzle electrospinning device carries out spinning, effectively increases the yield of nano fibrous membrane.
Embodiment 1
Polyacrylonitrile (PAN) is dissolved in solvent DMF (DMF), being configured to concentration is 12wt%'s Spinning solution.In the environment of room temperature and relative humidity are 40%, spinning liquid is injected in reservoir 4, stainless steel silk 5 with receive The vertical dimension integrating curtain 8, as 100mm, is opened high voltage direct current generator 7, is gradually increased voltage, until Static Spinning jet just shape Become, now voltage is 10kV, on collecting curtain 8, the spinning time is 1 hour to nanofibres deposit, has obtained in uniform thickness receiving Rice fibrous membrane.Test result indicate that, using this equipment spinning, the yield in unit time of nanofiber is compared to single needle Static Spinning Silk improves 70 times, effectively improves the fineness uniformity of fiber simultaneously.
Embodiment 2
Polyvinyl alcohol (PVA) 1788 type powder is dissolved in 70 DEG C of distilled water, is made into the spinning liquid that concentration is 12wt%; In the environment of room temperature and relative humidity are 60%, spinning liquid is injected in reservoir 4, stainless steel silk 5 is hung down with collection curtain 8 Straight distance is 300mm, opens high voltage direct current generator 7, is gradually increased voltage, until Static Spinning jet is just formed, now electricity Press as 30kV, on collecting curtain 8, the spinning time is 1 hour to nanofibres deposit, has obtained nano fibrous membrane in uniform thickness. Test result indicate that, using this equipment spinning, the yield in unit time of nanofiber improves compared to single needle electrostatic spinning 100 times, effectively improve the fineness uniformity of fiber simultaneously.
Embodiment 3
Polyethylene glycol oxide (PEO) is dissolved in 60 DEG C of distilled water, is configured to the spinning liquid that concentration is 15wt%.In room temperature In the environment of being 50% with relative humidity, spinning liquid is injected in reservoir 4, the vertical dimension of stainless steel silk 5 and collection curtain 8 For 200mm, open high voltage direct current generator 7, be gradually increased voltage, until Static Spinning jet is just formed, now voltage is 20kV, on collecting curtain 8, the spinning time is 1 hour to nanofibres deposit, has obtained nano fibrous membrane in uniform thickness.Experiment Result shows, using this equipment spinning, the yield in unit time of nanofiber improves 80 times compared to single needle electrostatic spinning, Effectively improve the fineness uniformity of fiber simultaneously.

Claims (9)

1. one kind back and forth gives liquid formula no nozzle electrostatic spinning apparatus it is characterised in that including hollow grooved drum (2) and being arranged at hollow Air bag (1) in groove drum (2) cavity, air bag (1) opening is connected with hollow grooved drum (2) one end, hollow grooved drum (2) and air bag (1) One end that opening connects is provided with EAP Electronic Air Pump (3), and hollow grooved drum (2) other end is connected with reservoir (4), and and reservoir (4) communicate;It is provided with seal wire block (6), seal wire block is provided with rustless steel between (6) on two relative side walls of reservoir (4) Silk (5), stainless steel silk (5) one end is connected with high voltage direct current generator (7) positive pole, and reservoir is provided with collection curtain above (4) (8), collect curtain (8) ground connection.
2. according to claim 1 a kind of back and forth give liquid formula no nozzle electrostatic spinning apparatus it is characterised in that described seal wire One of side wall that block (6) is located is connected with hollow grooved drum (2), and seal wire block (6) is higher than the company of reservoir (4) and groove drum (2) Meet place.
3. according to claim 1 a kind of back and forth give liquid formula no nozzle electrostatic spinning apparatus it is characterised in that described seal wire Block (6) hollow, seal wire block (6) is upper to arrange perforation, and stainless steel silk (5) is arranged mutually parallel through eyelet.
4. a kind of method preparing nano fibrous membrane is it is characterised in that the one kind being adopted is back and forth to liquid formula no nozzle Static Spinning Silk device, including hollow grooved drum (2) with the air bag (1), air bag (1) opening and the groove that are arranged in hollow grooved drum (2) cavity Cylinder (2) one end connects, and one end that hollow grooved drum (2) is connected with air bag (1) opening is provided with EAP Electronic Air Pump (3), hollow grooved drum (2) The other end is connected with reservoir (4), and communicates with reservoir (4);It is provided with seal wire on two relative side walls of reservoir (4) Block (6), is provided with stainless steel silk (5) between seal wire block (6), stainless steel silk (5) one end is with high voltage direct current generator (7) positive pole even Connect, above reservoir (4), be provided with collection curtain (8), collect curtain (8) ground connection;
One of side wall that described seal wire block (6) is located is connected with hollow grooved drum (2), and seal wire block (6) is on reservoir (4) Edge;
Described seal wire block (6) is upper to arrange perforation, and stainless steel silk (5) is through eyelet parallel arrangement;
Specifically implement according to following steps:
Spinning liquid is injected in reservoir (4), control environment temperature and humidity, adjust stainless steel silk (5) with collect curtain (8) away from From, unlatching EAP Electronic Air Pump (3), adjust total amount and the speed of conveying gas, be then turned on high voltage direct current generator (7), adjust outer Making alive, in the presence of electric field force, the spinning liquid of the upper coating of stainless steel silk (5) produces jet, and jet solidify to form Nanowire Dimension is deposited in collection curtain (8), obtains nano fibrous membrane after the spinning of certain time.
5. the method preparing nano fibrous membrane according to claim 4 it is characterised in that described ambient temperature be room temperature, RH range is 40%~60%.
6. the method preparing nano fibrous membrane according to claim 4 it is characterised in that described stainless steel silk (5) with receive The vertical dimension integrating curtain (8) is as 100mm~300mm.
7. the method preparing nano fibrous membrane according to claim 4 it is characterised in that described applied voltage be 10kV~ 30kV.
8. the method preparing nano fibrous membrane according to claim 4 is it is characterised in that described EAP Electronic Air Pump (3) is opened Before, in reservoir (4), spinning liquid and stainless steel silk (5) are in state that is a kind of definitely close but not contacting with each other.
9. the method preparing nano fibrous membrane according to claim 4 is it is characterised in that described EAP Electronic Air Pump (3) conveys The total amount of gas and speed, so that air bag (1) produces stable change in volume, and the spinning liquid when air bag (1) volume is maximum It is fully contacted with stainless steel silk (5) and be defined.
CN201610989957.2A 2016-11-10 2016-11-10 The back and forth method without nozzle electrostatic spinning apparatus and its nano fibrous membrane processed to liquid formula Expired - Fee Related CN106400134B (en)

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CN108034996A (en) * 2018-01-16 2018-05-15 河北耐诺科技有限公司 A kind of electrostatic spinning nozzle device
CN112680800A (en) * 2020-12-22 2021-04-20 江苏臻中滤料科技有限公司 Nanofiber non-woven fabric production device and application method
CN112680801A (en) * 2020-12-22 2021-04-20 江苏臻中滤料科技有限公司 Non-woven fabric production device for air filtration and use method
CN113718348A (en) * 2021-09-13 2021-11-30 西北工业大学 Carry prosthetic factor stylolite apparatus for producing

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CN104947211A (en) * 2015-05-27 2015-09-30 西安工程大学 Film-slitting method electrostatic spinning continuous nanofiber yarn device and nanofiber yarn preparing method
CN105113029A (en) * 2015-09-23 2015-12-02 厦门大学 Linear nozzle for electrostatic spinning
CN105734694A (en) * 2016-03-08 2016-07-06 西安工程大学 Pneumatic liquid-feeding type electrostatic spinning device and method thereof for preparing nanofiber mesh

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CN201415582Y (en) * 2009-05-18 2010-03-03 蔡瑞安 Closed liquid ornament with internal telescopic air sac
US20130241115A1 (en) * 2011-01-31 2013-09-19 Upma Sharma Electrospinning Process for Manufacture of Multi-Layered Structures
CN102828259A (en) * 2012-09-18 2012-12-19 天津工业大学 Saw tooth type needle-free electrostatic spinning device
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CN108034996A (en) * 2018-01-16 2018-05-15 河北耐诺科技有限公司 A kind of electrostatic spinning nozzle device
CN112680800A (en) * 2020-12-22 2021-04-20 江苏臻中滤料科技有限公司 Nanofiber non-woven fabric production device and application method
CN112680801A (en) * 2020-12-22 2021-04-20 江苏臻中滤料科技有限公司 Non-woven fabric production device for air filtration and use method
CN112680801B (en) * 2020-12-22 2021-11-23 江苏臻中滤料科技有限公司 Non-woven fabric production device for air filtration and use method
CN112680800B (en) * 2020-12-22 2022-01-07 咸宁优维科技有限公司 Nanofiber non-woven fabric production device and application method
CN113718348A (en) * 2021-09-13 2021-11-30 西北工业大学 Carry prosthetic factor stylolite apparatus for producing
CN113718348B (en) * 2021-09-13 2022-07-05 西北工业大学 Carry prosthetic factor stylolite apparatus for producing

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