CN103726110B - A kind of electrospinning device and the method for the preparation of electrostatic spinning thereof - Google Patents
A kind of electrospinning device and the method for the preparation of electrostatic spinning thereof Download PDFInfo
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- CN103726110B CN103726110B CN201310675931.7A CN201310675931A CN103726110B CN 103726110 B CN103726110 B CN 103726110B CN 201310675931 A CN201310675931 A CN 201310675931A CN 103726110 B CN103726110 B CN 103726110B
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Abstract
The invention provides a kind of electrospinning device of high yield.The formation of its equipment mainly comprises: metal jet device (1), solution feeding system (2), arc receiving system (3), wherein, comprising can at the solution feeding system (2) of metal jet device (1) optional position feed flow for metal jet device.Equipment of the present invention can be used for the spinning of gas chromatography or organic-inorganic composition etc., the ultrahigh in efficiency of spinning, and productivity ratio single spraying head spinning equipment exceeds more than three orders of magnitude, is in current same category of device, a equipment that spinning efficiency is the highest.
Description
Technical field
The invention belongs to material Preparation equipment field, particularly a kind of electrospinning device, and it adopts the method received without shower nozzle spining technology, the supply of multi-angle solution and arc for the preparation of electrostatic spinning.
Background technology
Method of electrostatic spinning have technique simple, prepare the remarkable advantages such as quick, with low cost, environmental friendliness, be considered to one of technology of the most promising current suitability for industrialized production nano material.The general principle of electrostatic spinning is: Polymer Solution or melt are placed in high-voltage electrostatic field, it is made to bring high-pressure electrostatic, charged solution forms Taybr cone under electric field force and capillary effect on drop summit, just injection thread is formed when electric field force is greater than the surface tension of solution, thread solidifies through solvent evaporation or melt cooling, thus obtains fiber.
The basic device of conventional electrostatic spinning mainly comprises four parts such as high voltage source, solution storage feeding mechanism, injection apparatus, gathering-device.(1), high voltage source: high-voltage electrostatic field needed for spinning is provided, allows the enough electrostatic charges of spun solution band epipodium, make drop taylor cone tip place produce jet.(2), solution storage feeding mechanism: device for storing liquid generally adopts syringe, draws a metal electrode and is connected with high voltage source.When adopting syringe to do solution storage device, power end can be clipped in single nozzle position of syringe.(3), injection apparatus: the capillary or the syringe single spraying head that are generally internal diameter 0.5-2mm.(4), gathering-device: generally can use metallic plate, graphite paper, conveyer belt, cylinder or grid etc.
Along with the development of electrostatic spinning technique, and improving constantly electrospinning fibre demand.Novel spinning process and device are constantly gushed out.Electrostatic spinning technique from initial single spraying head electrostatic spinning apparatus to multiple injector electrostatic spinning device, the most backward development without shower nozzle many jet flow static electricities spinning technique and transformation.Single spraying head unit is due to device complexity, and shower nozzle limited amount, shower nozzle easily blocks up, and is thus unfavorable for that industrial scale is produced.Though many shower nozzles electrostatic effectively can improve spinning efficiency, there is electric field influence between shower nozzle, the clean difficulty of device, between shower nozzle, necessary space causes the floor space of device large, still contradicts with industrialization Production requirement.Therefore, in order to electrostatic spinning technique is applied to suitability for industrialized production, R & D design the shifting without shower nozzle technique device gradually to high yield of electrospinning device.There is a lot of different electrospinning device without shower nozzle technical field at present, include column type, centrifugal, tens kinds of spinning process such as porous type, fence type.But all without in shower nozzle spinning equipment, comprise the nanometer spider of Ai Ermake company of Czech, and the Electrospun nano-fibers equipment that prior art CN103215660A provides, what adopt is all feed flow bottom common liquid bath, conveyor type is picked, injector head just sprays to single direction, and roller bearing is not fully utilized.
So, in order to enhance productivity further, ensure the quality of producing electrostatic spinning, need further research and develop.
Summary of the invention
In view of the technical problem that prior art exists, be experimental studies have found that by a large amount of, be achieved through the following technical solutions the technical problem that the present invention solves:
A kind of electrospinning device, comprise: metal jet device 1, solution feeding system 2, arc receiving system 3, metal jet device 1 one end is connected with positive source, the other end is connected with variable-speed motor 13, it is characterized in that, comprising can at the solution feeding system 2 of metal jet device 1 optional position feed flow.
Described metal jet device 1 is metal roller bearing or metal roller, and with solution feeding system 2 for local surface contacts, it is arbitrarily angled that metal jet device 1 spray angle can be accomplished in 345 °.
The feed flow port of described solution feeding system 2 is arc, can contact feed flow at each surface location of injection apparatus 1 with roller bearing.
The reservoir part of described solution feeding system 2 can arrange volume size according to actual needs, and in reservoir, slip plate 2C slides up and down and controls the pressure of feed flow port and the size of liquid supply rate.
Described solution feeding system 2 contacts with metal jet device 1, the top edge 2A of solution feeding system is be curved surface with curvature with metal jet device 1, and the gap between metal jet device 1 is adjustable, lower limb 2B is be curved surface with curvature with metal jet device 1, and with metal roller bearing close contact.
Within gap between the top edge 2A of solution feeding system and metal jet device 1 is preferably 5mm.
The continuous receiving system 3 of wide-angle arc dynamically receives for arc, similar conveyer belt form is adopted to operate, receiving angle is arbitrarily angled in 345 °, and arc radius regulates according to receiving range metal roller bearing diameter, and arc Basolateral is equipped with same curvature curved metal soft board line shell 5 and connects power cathode.
More specifically, in the preferred embodiments of the invention, a kind of electrospinning device, comprising: metal jet device 1, and one end is that terminals 4 are connected with positive source, and the other end is connected with variable-speed motor 13 with insulating bar 12 by shaft coupling 11;
Solution feeding system 2, the port of feed flow is the curved surface identical with roller bearing curvature and metal roller bearing contacts;
Arc receiving system 3 bracing or strutting arrangement ensures that fiber accepts cloth 6 is along receiving system 3 transmission, and arc receiving angle is arbitrarily angled in 345 °; Line shell 5 is connected with power cathode; Driving shaft 7, is connected with variable-speed motor by shaft coupling, controls the transmission speed of whole arc fiber accepts cloth; Driven shaft 8, for fiber accepts cloth rollback and provide;
The support 9 of whole equipment, sprays roller bearing 1 for support metal, solution feeding system 2, arc receiving system 3.
In a preferred embodiment of the present invention, slide up and down containing slip plate 2C, slip plate 2C in the reservoir of feed system 2 and control the pressure of feed flow port and the size of liquid supply rate.
In a preferred embodiment of the present invention, upper contact plate edge 2A is arc, and adjustable with the gap of roller bearing, prevents contact plate to be suspended to solution in metal shaft; Lower contact plate edge 2B is arc, with metal roller bearing close contact, prevents solution feeding system leakage, improves the tightness degree of contact and the uniformity of feed flow.
Particularly go up contact plate edge 2A, and metal roller bearing 1 there is identical curved surface segmental arc and adjustable with the clearance of metal roller bearing 4.Lower contact plate edge 2B, and metal roller bearing 1 have identical curved surface segmental arc and with metal roller bearing 4 close contact, the gained electrostatic spinning uniformity is high.
Material of the present invention and electrode connection mode preferable alloy injection apparatus 1, can adopt cast iron process Hou Du Chrome, or stainless steel processing.Solution feeding system 2, adopts nonmetallic materials to make, curved support device 3, adopts nonmetallic materials to make, and positive terminal 4 and the positive source of metal jet device 1 adopt overlapping mode, and negative terminal shell 5 is connected with power cathode by binding post.
The present invention is by combining without the solution supplying device of nozzle electrospinning method and multi-angle and the fiber accepts device of wide-angle, and producing can be higher than nanometer spider efficiency, the electrospinning device of the making polymer nanofibre film that output is larger.
Electrospinning device provided by the invention comprises the steps: for the preparation of the method for polymer electrospun
(1), by positive and negative polar curve be connected on metal jet device and receiving system shell respectively, actuating motor drives metal jet device and arc receiving system (3) to run well; (2), by the spinning solution configured join in solution feeding system (2), the plate height in regulator solution feed system (2) reservoir controls liquid supply speed; (3) open high voltage source, gradually in high voltage to the solution of cylinder surface with abundant electric charge, the electric field force that drop is subject to is greater than surface tension, till drop is elongated and forms spinning a large amount of continuously after taylor cone.
The electrospinning device provided of the present invention may be used for comprising PVA, PVP, PVA-PVP, the preparation of the polymer electrospuns such as PEO, also comprise other gas chromatography preparing electrostatic spinning or organic-inorganic compositions, preparation process adopts the configuration of distilled water equal solvent to be applicable to the solution of concentration, solution quality volume ratio (w/v) concentration preferably 6%-15%, add a certain amount of NaCl solution if desired, prepare nano fibrous membrane.
Described mass volume ratio (w/v) is the ratio of quality g and volume mL.
Compared to existing technology, the invention has the advantages that:
1, electrospinning device provided by the invention adopts shower nozzle technology, easily blocking up without solving conventional belt shower nozzle equipment shower nozzle, being unfavorable for that industrialization is produced, between shower nozzle, there is electric field influence, the clean difficulty of device, between shower nozzle, necessary space causes the problem that the floor space of device is large.
2, prior art novel without in shower nozzle spinning equipment, what major part adopted is all feed flow bottom common liquid bath, conveyor type is picked, injector head just sprays to single direction, roller bearing is not fully utilized, electrospinning device provided by the invention makes roller bearing make full use of, and improves service efficiency.
3, electrospinning device provided by the invention substantially increases the efficiency of electrostatic spinning, and the uniformity of tunica fibrosa thickness, and under equal conditions, the output of electrostatic spinning is more than 2000 times of single spraying head.
4, carry out electrostatic spinning preparation by electrospinning device provided by the invention, simple to operate, reduce clean, maintenance cost, high efficiency, products obtained therefrom thickness is even, is easy to industrial scale application.
Accompanying drawing explanation
Fig. 1 is the right schematic diagram of electrospinning device structure of the present invention.
Fig. 2 is the rear schematic diagram of electrospinning device structure of the present invention.
Fig. 3 A is the solution feeding system figure of the non-insert state of slip plate; Fig. 3 B is the solution feeding system figure of slip plate insert state.
Fig. 4 A is the partial enlarged drawing of solution feeding system; Fig. 4 B is the partial enlarged drawing of roller bearing contact surface in solution feeding system.
Fig. 5 is that the PVA nano fibrous membrane that present device obtains is schemed at Scanning Electron microscope SEM.
Fig. 6 is that the PVP nano fibrous membrane that present device obtains is schemed at Scanning Electron microscope SEM.
Fig. 7 is that the PVA-PVP nano fibrous membrane that present device obtains is schemed at Scanning Electron microscope SEM.
Fig. 8 is that the PEO nano fibrous membrane that present device obtains is schemed at Scanning Electron microscope SEM.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Embodiment 1
Shown in Fig. 1 and Fig. 2, the electrospinning device of high yield of the present invention comprises:
Metal jet device 1 is roller bearing, and one end is that terminals 4 are connected with positive source, and the other end is connected with variable-speed motor 13 with insulating bar 12 by shaft coupling 11;
Solution feeding system 2, the port of feed flow is the curved surface identical with roller bearing curvature and metal roller bearing contacts;
Arc receiving system 3 bracing or strutting arrangement ensures that fiber accepts cloth 6 is along receiving system 3 transmission, and arc receiving angle is 345 °; Line shell 5 is connected with power cathode; Driving shaft 7, is connected with variable-speed motor by shaft coupling, controls the transmission speed of whole arc fiber accepts cloth; Driven shaft 8, for fiber accepts cloth rollback and provide;
The support 9 of whole equipment, sprays roller bearing 1 for support metal, solution feeding system 2, arc receiving system 3.
Embodiment 2
Shown in Fig. 1, Fig. 2, Fig. 3 A and Fig. 3 B, the electrospinning device of high yield of the present invention comprises:
Metal jet device 1 is roller bearing, and one end is that terminals 4 are connected with positive source, and the other end is connected with variable-speed motor 13 with insulating bar 12 by shaft coupling 11;
Solution feeding system 2, the port of feed flow is the curved surface identical with roller bearing curvature and metal roller bearing contacts, and solution feeding system 2 has slip plate 2C, and slip plate 2C slides up and down and controls the pressure of feed flow port and the size of liquid supply rate;
Arc receiving system 3 bracing or strutting arrangement ensures that fiber accepts cloth 6 is along receiving system 3 transmission, and arc receiving angle is 300 °; Line shell 5 is connected with power cathode; Driving shaft 7, is connected with variable-speed motor by shaft coupling, controls the transmission speed of whole arc fiber accepts cloth; Driven shaft 8, for fiber accepts cloth rollback and provide;
The support 9 of whole equipment, sprays roller bearing 1 for support metal, solution feeding system 2, arc receiving system 3.
Embodiment 3
Shown in Fig. 1, Fig. 2, Fig. 3 A, Fig. 3 B, Fig. 4 A and Fig. 4 B, the electrospinning device of high yield of the present invention comprises:
Metal jet device 1 is roller bearing, and one end is that terminals 4 are connected with positive source, and the other end is connected with variable-speed motor 13 with insulating bar 12 by shaft coupling 11;
Solution feeding system 2, the port of feed flow is the curved surface identical with roller bearing curvature and metal roller bearing contacts, solution feeding system 2 has slip plate 2C, slip plate 2C slides up and down and controls the pressure of feed flow port and the size of liquid supply rate, upper contact plate edge 2A, have identical curved surface segmental arc with metal jet device 1 and adjustable with the gap of metal roller bearing 4, lower contact plate edge 2B, and metal jet device 1 have identical curved surface segmental arc and with metal roller bearing 4 close contact;
Arc receiving system 3 bracing or strutting arrangement ensures that fiber accepts cloth 6 is along receiving system 3 transmission, and arc receiving angle is 345 °; Line shell 5 is connected with power cathode; Driving shaft 7, is connected with variable-speed motor by shaft coupling, controls the transmission speed of whole arc fiber accepts cloth; Driven shaft 8, for fiber accepts cloth rollback and provide;
The support 9 of whole equipment, sprays roller bearing 1 for support metal, solution feeding system 2, arc receiving system 3.
Embodiment 4
Preparation mass volume ratio concentration is the distilled water solution of 10%PVA, adopts the electrospinning device of the embodiment of the present invention 3 to prepare electrostatic spinning, obtains nano fibrous membrane, the shape appearance figure 5 of tunica fibrosa under SEM characterizes.
Concrete grammar: (1), positive and negative polar curve is connected on respectively and sprays on roller bearing 1 and line shell 5, actuating motor drives metal roller bearing injector head and arc transmission gathering-device to run well, and rotating speed regulates according to the situation of solution concentration; (2), by the spinning solution configured join in solution feeding system 2, regulate the plate height in reservoir to control the size of liquid supply speed and liquid supply rate; (3) open high voltage source, gradually in high voltage to the solution of cylinder surface with abundant electric charge, the electric field force that drop is subject to is greater than surface tension, till drop is elongated and forms spinning a large amount of continuously after taylor cone.
Embodiment 5
Preparation mass volume ratio concentration is the distilled water solution of 15%PVP, adopts the electrospinning device of the embodiment of the present invention 3 to prepare electrostatic spinning, obtains nano fibrous membrane, Fig. 6 of the pattern of tunica fibrosa under SEM characterizes.
Concrete grammar: (1), positive and negative polar curve is connected on respectively and sprays on roller bearing 1 and line shell 5, actuating motor drives metal roller bearing injector head and arc transmission gathering-device to run well, and rotating speed regulates according to the situation of solution concentration; (2), by the spinning solution configured join in solution feeding system 2, regulate the plate height in reservoir to control the size of liquid supply speed and liquid supply rate; (3) open high voltage source, gradually in high voltage to the solution of cylinder surface with abundant electric charge, the electric field force that drop is subject to is greater than surface tension, till drop is elongated and forms spinning a large amount of continuously after taylor cone.
Embodiment 6
Join the distilled water solution that middle mass volume ratio concentration is the PVA-PVP (6:4) of 10%, adopt the electrospinning device of the embodiment of the present invention 3 to prepare electrostatic spinning, obtain nano fibrous membrane, Fig. 7 of the pattern of tunica fibrosa under SEM characterizes.
Concrete grammar: (1), positive and negative polar curve is connected on respectively and sprays on roller bearing 1 and line shell 5, actuating motor drives metal roller bearing injector head and arc transmission gathering-device to run well, and rotating speed regulates according to the situation of solution concentration; (2), by the spinning solution configured join in solution feeding system 2, regulate the plate height in reservoir to control the size of liquid supply speed and liquid supply rate; (3) open high voltage source, gradually in high voltage to the solution of cylinder surface with abundant electric charge, the electric field force that drop is subject to is greater than surface tension, till drop is elongated and forms spinning a large amount of continuously after taylor cone.
Embodiment 7
Preparation mass volume ratio concentration is the distilled water solution of 6%PEO, adds the NaCl of mass volume ratio concentration 0.2%, adopts the electrospinning device of the embodiment of the present invention 3 to prepare electrostatic spinning and obtains nano fibrous membrane, the shape appearance figure 8 of tunica fibrosa under SEM characterizes.
Concrete grammar: (1), positive and negative polar curve is connected on respectively and sprays on roller bearing 1 and line shell 5, actuating motor drives metal roller bearing injector head and arc transmission gathering-device to run well, and rotating speed regulates according to the situation of solution concentration; (2), by the spinning solution configured join in solution feeding system 2, regulate the plate height in reservoir to control the size of liquid supply speed and liquid supply rate; (3) open high voltage source, gradually in high voltage to the solution of cylinder surface with abundant electric charge, the electric field force that drop is subject to is greater than surface tension, till drop is elongated and forms spinning a large amount of continuously after taylor cone.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (8)
1. an electrospinning device, comprise: metal jet device (1), solution feeding system (2), arc receiving system (3), metal jet device (1) one end is connected with positive source, the other end is connected with variable-speed motor (13), it is characterized in that, comprising can at the solution feeding system (2) of metal jet device (1) optional position feed flow, described metal jet device (1) is metal roller bearing or metal roller, described solution feeding system (2) contacts with metal jet device (1), top edge (2A) and the metal jet device (1) of solution feeding system are the curved surface of same curvature, and the gap between metal jet device (1) is adjustable, lower limb (2B) is be curved surface with curvature with metal jet device (1), and with metal jet device close contact, gap between the top edge (2A) of solution feeding system and metal jet device (1) is within 5mm.
2. a kind of electrospinning device according to claim 1, it is characterized in that, described metal jet device (1) is metal roller bearing or metal roller, with solution feeding system (2) for local surface contacts, it is arbitrarily angled that metal jet device (1) spray angle can be accomplished in 345 °.
3. a kind of electrospinning device according to claim 1, is characterized in that, the feed flow port of described solution feeding system is arc, can contact feed flow at each surface location of metal jet device (1) with metal jet device.
4. a kind of electrospinning device according to claim 1, it is characterized in that, containing slip plate (2C) in the reservoir of described solution feeding system (2), slip plate (2C) slides up and down the size controlling liquid supply rate.
5. a kind of electrospinning device according to claim 1, it is characterized in that, comprise: metal jet device (1), one end is that terminals (4) are connected with positive source, and the other end is connected with variable-speed motor 13 with insulating bar (12) by shaft coupling (11);
Solution feeding system (2), the port of feed flow is the curved surface identical with metal jet device curvature and contacts with metal jet device;
Arc receiving system (3) bracing or strutting arrangement ensures that fiber accepts cloth (6) is along arc receiving system (3) transmission, and arc receiving angle is arbitrarily angled in 345 °, adjustable in receiving range certain limit; Line shell 5 is connected with power cathode; Driving shaft (7), is connected with variable-speed motor by shaft coupling, controls the transmission speed of whole arc fiber accepts cloth; Driven shaft (8), for fiber accepts cloth rollback and provide;
The support (9) of whole equipment, for support metal injection apparatus (1), solution feeding system (2), arc receiving system (3).
6. a preparation method for electrostatic spinning, is characterized in that, uses a kind of electrospinning device described in the arbitrary claim of claim 1-5 to adopt following preparation process:
(1), by positive and negative polar curve be connected on metal jet device and receiving system line shell respectively, start variable-speed motor and drive metal jet device and arc receiving system (3) to run well; (2), by the spinning solution configured join in solution feeding system (2), the plate height in regulator solution feed system (2) reservoir controls liquid supply speed; (3) open high voltage source, gradually in high voltage to the solution of metal jet apparatus surface with abundant electric charge, the electric field force that drop is subject to is greater than surface tension, till drop is elongated and forms spinning a large amount of continuously after taylor cone.
7. the preparation method of a kind of electrostatic spinning according to claim 6, is characterized in that, described spinning solution is the aqueous solution of polymer P VA, PVP, PVA-PVP or PEO.
8. the preparation method of a kind of electrostatic spinning according to claim 7, is characterized in that, described spinning solution is the mass volume ratio concentration of the aqueous solution of polymer P VA, PVP, PVA-PVP or PEO is 6%-15%, and water is distilled water.
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