CN103952778B - There is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function - Google Patents
There is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function Download PDFInfo
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- CN103952778B CN103952778B CN201410185560.9A CN201410185560A CN103952778B CN 103952778 B CN103952778 B CN 103952778B CN 201410185560 A CN201410185560 A CN 201410185560A CN 103952778 B CN103952778 B CN 103952778B
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Abstract
The present invention discloses the air-flow auxiliary electrostatic spinning instrument </b> that a kind of <b> has real-time sampling function, comprise electrospinning cabinet, sampler chamber, damp and hot conditioning chamber and master control room, the relatively independent and rational deployment of each several part is in a larger box cloche; Its feature is that described electrospinning cabinet adopts bottom feed, top receives the patten's design of Electrospun product; The syringe needle fixed bar of Electrospun indoor being equipped with auxiliary blower, for forming the secondary air of rising in the process of electrostatic spinning, electrostatic spinning can be carried out continually and steadily; Described sampler chamber can realize Electrospun sample collection at any time and without the need to interrupting Electrospun; The sample that sampler chamber obtains can at preliminary observation under high-power microscope, or observes further under the characterization device of such as ESEM; Described damp and hot conditioning chamber is provided with heating rod, and is connected with dehumidifier, for controlling the temperature and humidity of electrospinning cabinet.To overcome the long filament phenomenon occurred in electrostatic spinning process, electrostatic spinning is carried out sustainedly and stably.
Description
Technical field
The present invention relates to electrostatic spinning field, particularly one there is sampling apparatus and use the preliminary Electrospun sample of high-power microscope, be provided with the integral type electrostatic spinning machine of " secondary air ".
Background technology
As compared to preparation method's (as extension, template synthesis method and phase separation method etc.) of other nanofiber, electrostatic spinning technique has higher process controllability, the widely scope of application, simpler equipment, directly, continuously can prepare polymer nanofiber, and the fiber prepared by method of electrostatic spinning have the advantages such as less diameter, larger specific area and larger draw ratio.Therefore, method of electrostatic spinning has become the study hotspot preparing superfine fibre and nanofiber, has huge industrialization potential and application prospect.According to statistics, be engaged in current global range and exceeded 200 institutes with the colleges and universities of electrostatic spinning correlative study and scientific research institution, also a lot of company is had, as eSpinTechnologies, the companies such as NanoTechnics, KATOTech, Donaldson and Freudenberg are devoted to produce electrostatic spinning fiber, and are applied in real life.Further, Electrospun product is used for wound dressing by PTC patent WO98/0326, United States Patent (USP) 4043331 and 4878908 and Chinese patent ZL201010130864.7 etc., show many advantages.
Electrostatic spinning process is generally that droplet or melt droplet bring electric charge from the teeth outwards under the effect of high-voltage electrostatic field, when the charge repulsion on its surface is greater than or equal to its surface tension, drop surface will form little liquid stream (i.e. " jet ") these jets and be stretched under the effect of electric field force, is deposited on dash receiver after solvent evaporates with solidification, just defines electrospun fibers.
There are some problems in traditional electrostatic spinning, the efficiency of electrostatic spinning is restricted.First, what electrostatic spinning machine most at present adopted is its top feed, bottom accepts the mode of Electrospun product, but there is certain defect in this method, such as, because some factors of instability makes Electrospun stoste drip on dash receiver, damage Electrospun product quality, these destabilizing factors may be that the sudden change of voltage or feeding speed causes or syringe needle blocks the injection of the Electrospun stoste caused.Secondly, may be the difference of the character due to Electrospun stoste, as electrical conductivity etc., make Electrospun when starting or after having carried out the regular hour, occur " long filament phenomenon " (can with reference to accompanying drawing 1 and accompanying drawing 2), namely some thread materials are grown from take-up reel, the last phenomenon connected together with metal needle, makes spinning be difficult to carry out; Again, the factor affecting electrostatic spinning is many especially, as temperature, humidity and feeding speed etc., therefore provides the stable theoretical research of electrospinning conditions to Static Spinning to be necessary; Finally, the voltage that electrostatic spinning generally uses when carrying out is 10kv ~ 100kv, belongs to high voltage, there is certain danger in operating process.
In addition, in the process studying electrostatic spinning or production electricity spinning fibre, the observation obtained product being carried out to pattern is inevitably needed.At present, the conventional method for observing subtitle substance appearance form has: light microscope, ESEM and transmission electron microscope.As compared with light microscope, electron microscope has obvious advantage: resolution ratio is large, multiplication factor is high and continuously adjustabe, formed clear picture, the depth of field large, third dimension is stronger, therefore, scanning electron microscopic observation is often used in the form of Electrospun product or the observation of section, or even for the qualification of general fiber.But, scanning electron microscopic observation Electrospun product is utilized also to there are some limitation, as required, sample can tolerate vacuum, sample wants preliminary treatment to remove the composition such as moisture and volatile materials, spraying layer of conductive material (being often metal spraying process) etc. is needed for nonconducting sample, therefore the cycle of scanning electron microscopic observation Electrospun sample is longer, and operating process is more loaded down with trivial details, not only consumes the more energy and material, also occupy a large amount of time, reduce efficiency.Light microscope utilizes light source to be visible ray, although can not as ESEM careful appearance form of observing Electrospun product clearly, but be through suitable process, light microscope also can observe Electrospun product, compared with ESEM, more directly, rapidly can observe, preliminarily determine its appearance form, save time, and investment cost, raise the efficiency, in the heuristic process of the better condition of electrostatic spinning, there is larger effect, have certain meaning to the research of electrostatic spinning and suitability for industrialized production.
Summary of the invention
In view of above problem, the object of the present invention is to provide a kind of device of electrostatic spinning, especially provide
a kind of air-flow auxiliary electrostatic spinning instrument with real-time sampling function, to realize the real-time sampling of electrostatic spinning, and use Powerful Light Microscope to carry out preliminary observation to Electrospun product.
The present invention also aims to add " secondary air " at " jet " injection direction of electrostatic spinning, to overcome " long filament phenomenon ", electrostatic spinning can stably be carried out.
The present invention also aims to the mode adopting " bottom feed, top accepts Electrospun product ", promote the quality of electrostatic spinning product.
The present invention also aims to, by electrostatic spinning machine integration, strengthen the influence factor to electrostatic spinning process, and promote the security of electrostatic spinning operation.
Adopt technical scheme as follows for realizing object of the present invention: described
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, comprise electrospinning cabinet, sampler chamber, damp and hot conditioning chamber and master control room, the relatively independent and rational deployment of each several part is in a larger box cloche; It is characterized in that: described electrospinning cabinet adopts bottom feed, top receives the patten's design of Electrospun product; The syringe needle fixed bar of Electrospun indoor being equipped with auxiliary blower, for forming the secondary air of rising in the process of electrostatic spinning, electrostatic spinning can be carried out continually and steadily; Described sampler chamber can realize Electrospun sample collection at any time and without the need to interrupting Electrospun; The sample that sampler chamber obtains can at preliminary observation under high-power microscope, or observes further under the characterization device of such as ESEM; Described damp and hot conditioning chamber is provided with heating rod, and is connected with dehumidifier, for controlling the temperature and humidity of electrospinning cabinet.
Described electrospinning cabinet is used for electrostatic spinning; Injection needle tube is fixed in micro-injection pump draw-in groove, and the afterbody of injection needle tube leans against on the pusher of micro-injection pump; The head of injection needle tube is connected with stainless steel syringe needle by silicone tube, and under the pushers of micro-injection pump, Electrospun stoste is quantitatively delivered stainless steel syringe needle by silicone tube, and micro-injection pump controls the flowing velocity of Electrospun stoste in injection needle tube; The base plate of electrospinning cabinet is fixed with syringe needle fixed bar, and described syringe needle fixed bar height is adjustable, can regulate the distance of stainless steel syringe needle and take-up reel; Metal needle fixator is arranged at syringe needle fixed bar top, and metal needle fixator is built-in with magnet piece; Sheet metal is inhaled on magnet piece side, and sheet metal is connected with the anode of high voltage source; Stainless steel syringe needle is inhaled by the suction of magnet piece and is leaned against on sheet metal side, syringe needle fixed bar is provided with glass baffle plate, glass baffle plate has syringe needle perforation, the needle section of stainless steel syringe needle exposes on glass baffle plate through syringe needle set on glass baffle plate perforation; With glass baffle plate at a distance of required distance and the position be positioned on directly over stainless steel syringe needle is provided with take-up reel; Take-up reel is made up of metal material, and in disc, the center of discoidal take-up reel is connected by the negative electrode of wire with the high voltage source in master control room; Take-up reel is connected by the motor of hollow connecting rod with wet thermo-regulated chamber, can rotate, can be controlled the rotating speed of motor and take-up reel by master control room under the drive of motor; A temperature inductor is equipped with for detecting the temperature of electrospinning cabinet at the take-up reel back side.
Immediately below the middle and upper part of the syringe needle fixed bar in Electrospun indoor, stainless steel syringe needle, the auxiliary blower that can produce toward the secondary air risen is equipped with at place; The height of auxiliary blower can regulate; By regulating the rotating speed of auxiliary blower, and form the secondary air of different in flow rate; Glass baffle plate is provided with some uniform passages, secondary air can be allowed to pass through, electrostatic spinning can be carried out sustainedly and stably.
Be fixed with a drier receptacle in the side of electrospinning cabinet, dryer is placed with beaker, and beaker is equipped with drier, and drier receptacle is provided with side gate and early gate; By opening early gate, closing side gate, can change drier safely, after drier is changed, open side gate, closes early gate, makes the humidity that electrospinning cabinet remains lower.
Described sampler chamber is placed in the side of electrospinning cabinet, and sampler chamber has side gate and the early gate of two independent switches; Open early gate and close side gate simultaneously, can sampler be loaded onto; Open side gate in sampling process, closes early gate, can realize the sealing of sampling process and ensure the safety of operating personnel.
Described sampler chamber is provided with thief rod, the material of thief rod is insulator, thief rod is through a side of sampler chamber, its one end is placed in sampler chamber inside and sampler fixator is housed, sampler fixator is provided with sampler, and the thief rod other end is in the outside of sampler chamber and can fold, by promoting thief rod, sampler can be moved on to the surface of take-up reel, gather Electrospun sample; Pull thief rod again, can sample be sent back to sampler chamber, and take out observation.
Sampler in described sampler chamber adopts cover glass or slide, the sample that cover glass or slide gather directly, preliminarily can observe Electrospun sample under high-power microscope, also can observe further under characterization device (as surface sweeping Electronic Speculum etc.) after reprocessing; If when using high-power microscope to carry out preliminary observation to Electrospun product, the duration of sampling in sampling process should be selected according to feeding speed, sampling time, the position of sampling was selected, in the center near take-up reel, to make the sample of collection have more representativeness between 20s ~ 120s.
Described damp and hot conditioning chamber is positioned at the top of electrospinning cabinet, plays the control of the temperature and humidity to electrospinning cabinet; Be provided with an opening at damp and hot conditioning chamber, described opening can be connected with the dehumidifier at the back side being placed in electrostatic spinning machine, opens dehumidifier, can make the humidity that electrospinning cabinet remains lower; Wet thermo-regulated chamber is provided with radiator fan, and heating rod is fixed on above radiator fan, by heating and dispelling the heat, makes electrospinning cabinet maintain within stationary temperature scope; At damp and hot conditioning chamber built with exhaust fan, exhaust fan can get rid of the gas that electro-spinning process evaporates, and the interface of exhaust fan and damp and hot conditioning chamber is provided with exhaust gate, closes exhaust gate in electro-spinning process, prevent pouring in down a chimney of external air flow, maintain the stable of the interior condition of electrospinning cabinet; Between damp and hot conditioning chamber and electrospinning cabinet, there is glass plate to separate, the glass plate being positioned at the take-up reel back side has several holes, make good the communicating of energy between electrospinning cabinet with damp and hot conditioning chamber two Room, be convenient to regulate the temperature and humidity of electrospinning cabinet and the gas after getting rid of electrostatic spinning.
Described master control room, for controlling the main process of electrostatic spinning, is made up of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system and control inerface, can realizes the control of electrostatic spinning process.
Specifically, of the present invention
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, comprise electrospinning cabinet, sampler chamber, damp and hot conditioning chamber and master control room, the relatively independent and rational deployment of each several part is in a larger box cloche.The mode that described electrospinning cabinet adopts bottom feed, top receives Electrospun product; The syringe needle fixed bar of Electrospun indoor being equipped with auxiliary blower (a kind of small-sized exhaust fan), for being formed in the process of electrostatic spinning " secondary air " that rise, electrostatic spinning can be carried out continually and steadily; Described sampler chamber can realize the collection at any time of Electrospun sample, and without the need to interrupting Electrospun; The sample that sampler chamber obtains at preliminary observation under high-power microscope, also can be observed further under other characterization device such as ESEM; Described damp and hot conditioning chamber is provided with heating rod, and is connected with dehumidifier, for controlling the temperature and humidity of electrospinning cabinet.
Preferably, the material used in above-mentioned electrostatic spinning machine selects insulator as far as possible, and to ensure the safety of experimental implementation, the gate etc. communicated with the external world does encapsulation process, assurance device has certain sealing, maintains electrostatic spinning and carries out under the condition of relative constancy.
Preferably, there is in above-mentioned electrostatic spinning machine the sampler chamber that can sample at any time, without the need to interrupting electrostatic spinning in sampling process.Sampler chamber is placed in the side of electrospinning cabinet, there is the gate of early gate and these two independent switches of side gate, close side gate, open early gate and can load onto sampler, close early gate, open side gate can carry out the collection of sample, therefore in sampling process without the need to interrupting electrostatic spinning, realize the sealing of instrument and ensure the safety of operating personnel.
Preferably, in above-mentioned electrostatic spinning machine, sampler chamber has thief rod, and the material of thief rod is insulator.Thief rod is through a side of sampler chamber, and one end is inner at sampler chamber, and sampler fixator is housed, and sampler fixed by sampler fixator.The other end, in the outside of sampler chamber, can fold.By promoting thief rod, sampler can be moved on to the surface of take-up reel, gathering Electrospun sample; Pull thief rod again, can sample be sent back to sampler chamber, and take out observation.
Preferably, the sampler in above-mentioned electrostatic spinning machine in sampler chamber can be the transparent carrier such as cover glass or slide.So, the sample gathered both directly, preliminarily can observe Electrospun sample under high-power microscope, observed further under also can being used in other characterization device such as ESEM after reprocessing.In addition, other thin slice also can be selected as sampler, the sample of acquisition is used for the instruments such as ESEM.
Preferably, in the high-power microscope multiplication factor described in above-mentioned electrostatic spinning machine more than 600 times, camera function is had, camera lens pixel more than 5,000,000.
Preferably, the duration of sampling in the sampling process of above-mentioned electrostatic spinning machine should be selected according to feeding speed, and the general sampling time, the position of sampling was typically chosen in the center near take-up reel between 20s ~ 120s.
Preferably, the electrospinning cabinet described in above-mentioned electrostatic spinning machine comprises syringe needle fixed bar, auxiliary blower, metal needle fixator, drier receptacle, the take-up reel of Electrospun product and temperature sensor.Needle head fixer under, take-up reel, upper, adopts bottom feed, and top receives the mode of Electrospun product.
Preferably, in above-mentioned electrostatic spinning machine, the height of metal needle fixator can be regulated by fixed bar, and the top of fixator is the unit of plastic of one piece of insulation, built-in magnet piece.Unit of plastic upper surface has the glass plate that a slice area is slightly large, is provided with an opening, syringe needle can be allowed to pass, and expose, and arranges several access openings equably simultaneously, " secondary air " can be allowed to pass through smoothly near opening.A side of unit of plastic is sheet metal, and stainless steel syringe needle is fixed on sheet metal side under the attraction of built-in magnet piece.Sheet metal is connected with the high voltage source anode in master control room, thus realizes the connection of metal needle and high voltage source anode.
Preferably, in above-mentioned electrostatic spinning machine, auxiliary blower (a kind of small-sized exhaust fan) is equipped with in metal needle fixed bar middle and upper part, with syringe needle homonymy, is positioned at immediately below syringe needle.By regulating the rotating speed of auxiliary blower, the secondary air of different in flow rate can be formed, can overcome " the long filament phenomenon " that occur in electro-spinning process, allow Electrospun carry out sustainedly and stably; The height of auxiliary blower can regulate.
Preferably, be provided with a drier receptacle in the electrospinning cabinet side of above-mentioned electrostatic spinning machine, receptacle is provided with two gates, and early gate and side gate, have and add sealing strip, ensures sealing.Open early gate to can be used for loading or taking out drier, side gate then for being communicated with or isolated electrospinning cabinet, like this, can realize the replacing at any time of drier, ensures that electrospinning cabinet is in the state of low humidity.
Preferably, in above-mentioned electrostatic spinning machine, Electrospun take-up reel is circular, and position immobilizes, and the center of disk is connected with the high voltage source negative electrode in master control room by wire (being placed in hollow connecting rod).Disk is connected by the motor of hollow connecting rod with wet thermo-regulated chamber, can rotate under the drive of motor, can be controlled the rotating speed of take-up reel by master control room.
Preferably, in above-mentioned electrostatic spinning machine, the damp and hot conditioning chamber of electrostatic spinning machine is made up of heating rod, radiator fan, dehumidifier connector, motor and exhaust fan, by controlling the heating of heating rod, thus the temperature realizing electrospinning cabinet controls, radiator fan is placed in below heating rod, makes the temperature in instrument reach uniform state fast for accelerating heat radiation; Dehumidifier connector is connected with the dehumidifier be placed in electrostatic spinning machine, the humidity making electrospinning cabinet remain lower by the dehumidifier effect of dehumidifier; Motor is for controlling the rotation of Electrospun indoor reception dish; Exhaust fan is used for the gas that Electrospun terminates rear discharge electrospinning cabinet, and the interface of exhaust fan and damp and hot conditioning chamber is provided with baffle plate, closing baffle plate in electro-spinning process, prevents pouring in down a chimney of external air flow, maintains the stable of the interior condition of electrospinning cabinet.
Preferably, at the master control room of above-mentioned electrostatic spinning machine for controlling the main process of electrostatic spinning, be made up of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system, control inerface, the control of electrostatic spinning process can be realized.Be placed with the injection needle tube loading Electrospun stoste above micro-injection pump, injection needle tube is connected with stainless steel syringe needle by silicone tube, under the promotion of micro-injection pump, quantitatively Electrospun stoste can be delivered to stainless steel syringe needle, be convenient to the control of flow rate of liquid.
As can be seen from above-mentioned technical scheme, tool of the present invention has the following advantages:
Various piece reasonably concentrates in a box cloche by this electrostatic spinning machine, takes insulation and seal approach, can not only maintain the condition relative constancy of Electrospun, the safety of the protection operating personnel that are good at.
This electrostatic spinning machine be provided with sampling apparatus, and sample mode is simple and safe, and can sample at any time when not interrupting electrostatic spinning, can obtain representative higher sample, facilitate the research of electrostatic spinning.
This electrostatic spinning machine can adopt thin slice that cover glass or slide etc. are transparent as samplers sample Electrospun product, and the sample of collection can use Powerful Light Microscope to carry out preliminary observation, saves time and raises the efficiency.
This electrostatic spinning machine is provided with auxiliary blower, can produce " secondary air ", to overcome " the long filament phenomenon " that occur in electrostatic spinning process, electrostatic spinning is carried out sustainedly and stably.
This electrostatic spinning machine adopts bottom feed, prevents electro-spinning process Raw from dropping onto on Electrospun product, can arrive the better Electrospun product of quality.
The metal needle fixator of this electrostatic spinning machine has built-in magnet, can easily fixing metal syringe needle, and the height of fixator can regulate.
The drier receptacle of this electrostatic spinning machine can change drier at any time, maintains the low humidity state of electrospinning cabinet with dehumidifier acting in conjunction.
The exhaust fan of this electrostatic spinning machine is provided with baffle plate, plays reverse flowing of air flows, ensures the closure of electrostatic spinning machine.
Accompanying drawing explanation
fig. 1for " long filament phenomenon " figure that certain polymer solution in conventional electrostatic spinning machine experimentation occurs.Can see, the masking foil in take-up reel has received certain thickness Electrospun product, but after having spent a period of time, position, intermediate portion grows thread material at leisure, in " column type ", and has the trend continuing upper length.
fig. 2for " long filament phenomenon " figure that polymer solution another kind of in conventional electrostatic spinning machine experimentation occurs.Can see, the masking foil in take-up reel has received certain thickness Electrospun product, but after having spent a period of time, its position, marginal portion grows thread material at leisure, in " bowl-shape type ", and can continue to rise.
fig. 3for the schematic diagram of electrostatic spinning machine proposed by the invention.
fig. 4the light microscope figure of the PAN fiber that embodiment 1 obtains.
fig. 5the scanning electron microscope (SEM) photograph of the PAN fiber that embodiment 1 obtains.
fig. 6the light microscope figure of the PAN fiber that embodiment 2 obtains.
fig. 7the light microscope figure of the PVP fiber that embodiment 3 obtains.
fig. 8the scanning electron microscope (SEM) photograph of the PVP fiber that embodiment 3 obtains.
fig. 9cu (the NO that embodiment 4 obtains
3)
2/ Ce (NO
3)
3the light microscope figure of/PAN composite fibre.
Detailed description of the invention
In order to more clearly explain the present invention, to be briefly described by some accompanying drawings below, apparently, accompanying drawing listed is below only some embodiments of the present invention, for this exercising ordinary skill, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Below in conjunction with accompanying drawing, 3 couples of the present invention are described in more detail, to make the reference of those skilled in the art's energy and to implement.
As shown in Figure 3, the present invention---a kind of air-flow auxiliary electrostatic spinning instrument with real-time sampling function, comprises four major parts, is respectively electrospinning cabinet A, sampler chamber B, damp and hot conditioning chamber C and master control room D.
Electrospinning cabinet A is mainly used in carrying out electrostatic spinning, and injection needle tube 1 is fixed under the effect of micro-injection pump 2 draw-in groove, and the afterbody of injection needle tube 1 is close to the pusher of micro-injection pump 2; The head of injection needle tube 1 is connected with stainless steel syringe needle 4 by silicone tube 3, under the promotion of micro-injection pump 2, Electrospun stoste is quantitatively delivered stainless steel syringe needle 4 by silicone tube 3, and micro-injection pump 2 controls the flowing velocity of Electrospun stoste in injection needle tube 1.The base plate of electrospinning cabinet A is fixed with syringe needle fixed bar 9, and the height of described syringe needle fixed bar 9 can regulate; Metal needle fixator 6 is arranged on syringe needle fixed bar 9, and metal needle fixator 6 is built-in with magnet piece 5, and sheet metal 8 is inhaled on magnet piece 5 side.Sheet metal 8 is connected with the anode of high voltage source, opens high voltage source, can be syringe needle and applies a high voltage.Stainless steel syringe needle 4 is inhaled by magnet piece 5 suction and is leaned against on sheet metal 8 side, syringe needle fixed bar 9 is provided with glass baffle plate 7, glass baffle plate 7 has syringe needle perforation, inhale the needle section leaning against the stainless steel syringe needle 4 of sheet metal 8 side and expose on glass baffle plate 7 through the syringe needle perforation that glass baffle plate 7 has.On glass baffle plate 7 and with glass baffle plate 7 in a distance, be positioned at place directly over stainless steel syringe needle 4 and be provided with take-up reel 10, take-up reel 10 is made up of metal material, intermediate portion is connected with wire one end, and wire is placed in its other end in hollow connecting rod 12 and is connected with the negative electrode of high voltage source.A temperature inductor 14 is equipped with for detecting the temperature of electrospinning cabinet at take-up reel 10 back side.Immediately below the middle and upper part of syringe needle fixed bar 9, stainless steel syringe needle 4, the auxiliary blower 11 that can produce toward the secondary air risen is equipped with at place in addition, by the flow velocity regulating the rotating speed of fan can control secondary air, the secondary air formed is toward rising, the some uniform passage that can be arranged above by glass baffle plate 7, a power is upwards produced to Electrospun product, thus makes that Electrospun is stable to carry out constantly.Be fixed with a drier receptacle 15 in the side of electrospinning cabinet A, dryer 15 is placed with beaker, and beaker is equipped with drier, and drier receptacle 15 is provided with side gate 16 and early gate 17; By the unlatching early gate 17 of gate, close side gate 16, with time change drier safely, after drier is changed, open side gate 16, closes early gate 17, makes electrospinning cabinet A maintain lower humidity.
Sampler chamber B is fixed on the side at the top of electrospinning cabinet, just can level be advisable being attached in take-up reel 10 when its position enters into electrospinning cabinet to ensure sampler 18.The thief rod 19 of sampler chamber passes the outside of sampler chamber, can fold, one end outside, the other end is in sampler chamber and be connected with the sampler fixator 20 in sampler chamber, sampler 18 is arranged on the sampler fixator 20 in sampler chamber, and sampler 18 is detachable installation with the sampler fixator 20 in sampler chamber.In the process of Electrospun, close the side gate 21 of sampler chamber, open the early gate 22 of sampler, sampler 18 is installed to above sampler fixator 20, after fastening early gate 22, beat side throttle valve 21, after a period of stabilisation, thief rod 19 is stretched to horizontal level, then promotion slowly, sampler fixator 20 is sent into electrospinning cabinet together with sampler 18, until sampler 18 stops promoting after being placed on the correct position of take-up reel 10.Stablize enough for a long time, pull thief rod 19, sampler 18 is shifted out electrospinning cabinet to sampler chamber, first close side gate 21, making early gate 22, take off sampler 18, the sample of acquisition can be directly used in ultramicroscopic observation and carry out preliminary observation or use ESEM to carry out careful observation after treatment.
Damp and hot conditioning chamber C is positioned at the top of electrospinning cabinet, plays the control of the temperature and humidity to electrospinning cabinet.Be provided with an opening 23 at damp and hot conditioning chamber, described opening 23 can be connected with the dehumidifier at the back side being placed in sub-electrostatic spinning machine (dehumidifier is installed in airtight little lattice), opens dehumidifier, can make the humidity that electrospinning cabinet remains lower.Wet thermo-regulated chamber is provided with radiator fan 25, and heating rod 24 is fixed on above radiator fan 25, by heating and dispelling the heat, electrospinning cabinet is maintained within stationary temperature scope.Motor 13 is for driving the rotation of take-up reel 10, and Electrospun product is collected equably, and its rotating speed can be regulated by master control room.At damp and hot conditioning chamber built with exhaust fan 26, after Electrospun terminates, first open the discharge air lock door of exhaust fan, then open exhaust fan 26 and can get rid of the gas that electro-spinning process evaporates.Between damp and hot conditioning chamber and electrospinning cabinet, there is glass plate to separate, the glass plate at take-up reel 10 back side there are out several holes make good the communicating of energy between electrospinning cabinet with damp and hot conditioning chamber two Room, are convenient to regulate the temperature and humidity of electrospinning cabinet and the gas after getting rid of electrostatic spinning.
Master control room D is made up of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system and control inerface, can realize the control of electrostatic spinning process, be the prior art that persons skilled in the art can realize.Various piece is reasonably integrated on electrostatic spinning machine, realizes the integration of electrostatic spinning machine, i.e. Appropriate application space, has again certain sealing, reduces exposing of circuit, improves the security of operation.The gauge tap of control inerface primary step some parts and indicator lamp, facilitating the control of instrument.
When carrying out Electrospun experiment, key step is as follows:
(1) check and fasten the gate communicated with the external world, as the gate etc. of the side gate 21 of the side gate 16 of drier receptacle, early gate 17, sampler chamber, early gate 22 and exhaust fan 26, and check that the drier of drier receptacle 15 is the need of renewal, words in need first can upgrade drier.
(2) connect relevant power supply, open dehumidifier, open " master switch " of instrument, " power supply indicator " lights; Open again " temperature switch ", the real time temperature of now temperature registration " PV " value display electrospinning cabinet, by rotating " temperature adjustment " knob, the temperature that setting Electrospun needs, i.e. " SV " value; By the time instrument first reaches predetermined temperature and lower humidity is tested again.
(3) get a certain amount of electrostatic spinning raw material solution with injection needle tube, injection needle tube 1 is fixed on the draw-in groove of micro-injection pump 2, and make the afterbody of injection needle tube 1 only by the pusher of micro-injection pump 2; Silicone tube 3 on the head cover of injection needle tube 1, then load onto stainless steel syringe needle 4 at the other end of silicone tube 3, allow syringe pump proceed to Electrospun stoste soon and be full of silicone tube, regulate default flow velocity; Stainless steel syringe needle 4 is fixed on needle head fixer 6, regulates and the distance of fixed needle top and take-up reel, after shut the door of electrospinning cabinet.
(4) treat instrument reach pre-conditioned after, open " take-up reel switch ", rotate " rotational speed regulation " knob, select the rotating speed that is suitable, allow take-up reel rotate; Open " air flow switch " simultaneously, rotate " wind speed adjustments " knob, allow the rotating speed that auxiliary blower 11 reaches certain, formation secondary air.
(5) open " voltage switch ", rotate " voltage-regulation " knob, be adjusted to the value that " voltage readings " is predeterminated voltage, restart micro-injection pump time rear, then electrostatic spinning just starts to have carried out.
(6) in the process of Electrospun, close the side gate 21 of sampler chamber, open the early gate 22 of sampler, sampler 18 is installed to above sampler fixator 20, after fastening early gate 22, beat side throttle valve 21, after a period of stabilisation, thief rod 19 is stretched to horizontal level, then promotion slowly, sampler 18 is sent into electrospinning cabinet, until sampler 18 stops promoting after being placed on the correct position of take-up reel 10.Stablize enough for a long time, pull thief rod 19, sampler 18 is shifted out electrospinning cabinet to sampler chamber, first close side gate 21, making early gate 22, take off sampler 18, the sample of acquisition can be directly used in ultramicroscopic observation and carry out preliminary observation or use ESEM to carry out careful observation after treatment.
(7) after Electrospun terminates by the time, first close syringe pump, then turn off voltage, then stop the rotation of take-up reel 13 and auxiliary blower 19; Close dehumidifier and " temperature switch ", open after opening the gate of exhaust fan and open " air discharge cook ", make exhaust fan 26 start exhaust, after waiting a period of time, then open the door of electrospinning cabinet, Electrospun product is taken off from take-up reel 10, and lay down syringe needle 4, silicone tube 3 and syringe 1, finally close other switch, deenergization, cleaning instrument, makes instrument return to original state.
(8) if drier major part inefficacy in experimentation, should change as early as possible; If there is dangerous situation, " emergent stopping " button can be pressed, clear.
Embodiment 1
1. accurately take 1.000g polyacrylonitrile (PAN, Sigma-Aldrich, M
w=150,000) add DMF (DMF) solution of 17mL, at water-bath 35 DEG C, temperature constant magnetic stirring 3h is to dissolving completely, obtains Electrospun stoste;
2. get above-mentioned Electrospun stoste 8mL with Dispoable medical injection needle, electrostatic spinning is carried out by the general use step of instrument, the condition of electrostatic spinning is voltage 18.5kv, feeding speed 0.5mL/h, temperature 45 C, receiving range (namely syringe needle is to the distance of take-up reel) is 15cm, and auxiliary blower is not opened;
3. wait until electrostatic spinning carried out 15min after (Electrospun reaches stable state), start sampling, sampler is slide (specification: 25.4mm × 76.2mm, thickness is 1mm ~ 1.2mm), and the sampling time is 45s;
4. by the sample collected directly at the optical microphotograph Microscopic observation of high power and take pictures (multiplication factor is 600 times, camera lens pixel 9,000,000), observable Local map is as shown in Figure 4;
5. another sample thief (sampling time is long), uses scanning electron microscopic observation, the scanning electron microscope (SEM) photograph of the same amplification obtained 600 times, as shown in Figure 5 after treatment.
Observation Fig. 4 is known, under amplifying the condition of 600 times under an optical microscope, sparse, elongated filiform can be seen, filiform is the PAN fiber that Electrospun obtains, and conscientiously observe and can find, PAN fibre diameter is more close, some fiber surface is more even, and some fiber has more " spindle " (show as in the diagram: similar globule, two ends are comparatively thin, middle thicker point).
To the observation of Fig. 5, can know that Electrospun product can be clearly seen when amplifying 600 times under ESEM, it is also more elongated for observing PAN fiber, but very intensive (reason that the sampling time is long), conscientiously observe and also can see having more " spindle " to exist.Therefore light microscope preliminary observation obtains checking to effect in the observation of ESEM.
At this, it should be noted that the PAN fiber seen under an optical microscope be why sparse is that also only in this way, light through sampler, could observe Electrospun product because the time of sampling is shorter.
Embodiment 2
1. accurately take the DMF solution that 1.000gPAN adds 17mL, at water-bath 35 DEG C, temperature constant magnetic stirring 3h is to dissolving completely, obtains Electrospun stoste;
2. get above-mentioned Electrospun stoste 8mL with Dispoable medical injection needle, carry out electrostatic spinning by the general use step of instrument, the condition of electrostatic spinning is voltage 15.0kv, feeding speed 0.5mL/h, temperature 45 C, receiving range (be 15cm, do not open by auxiliary blower;
3., after waiting until that electrostatic spinning has carried out 15min, start sampling, sampler is slide, and the sampling time is 45s;
4. by the sample collected directly at the optical microphotograph Microscopic observation of high power and take pictures (multiplication factor is 600 times, camera lens pixel 9,000,000), observable Local map is as shown in Figure 6.
Can know from Fig. 6, amplify 600 times under an optical microscope, Electrospun product can be observed, and Electrospun product irregularly drops on sampler surface, the fibre diameter obtained is less, and continuity is better, also more even for observing significantly " spindle ".
Embodiment 3
1. accurately take 1.792g polyvinylpyrrolidone (PVP) and add the absolute ethyl alcohol of 10mL and the distilled water of 20mL, at room temperature magnetic agitation 2h is to dissolving completely, obtains Electrospun stoste;
2. get above-mentioned Electrospun stoste 8mL with Dispoable medical injection needle, carry out electrostatic spinning by the general use step of instrument, the condition of electrostatic spinning is voltage 15.0kv, feeding speed 1.0mL/h, temperature 30 DEG C, and receiving range is 15cm, and auxiliary blower is not opened;
3., after waiting until that electrostatic spinning has carried out 15min, start sampling, sampler is slide, and the sampling time is 25s;
4. by the sample collected directly at the optical microphotograph Microscopic observation of high power and take pictures (multiplication factor is 600 times, camera lens pixel 9,000,000), observable Local map is as shown in Figure 7;
5. another collected specimens, uses scanning electron microscopic observation, the scanning electron microscope (SEM) photograph of the same amplification obtained 600 times, as shown in Figure 8 after treatment.
By Fig. 7, can be clear that elongated PVP fiber, all in all PVP fiber thickness is relatively more even, but careful observation can find that its edge compares out-of-flatness.And can know when ESEM amplifies 600 times from Fig. 8, the silk edge observed is also fuzzyyer.This may be that the water imbibition of PVP is stronger, easily absorbs the moisture in air and becomes paste and fallen, being also likely that the temperature of electrostatic spinning is lower, dissolving the reason that volatilization is incomplete.
Embodiment 4
1. accurately take the PAN of 0.300g copper nitrate, 1.200g cerous nitrate and 2.000g, then add the DMF solution of 34mL, stirring 3h to dissolving completely at water-bath 35 DEG C of lower magnetic forces, obtaining Electrospun stoste;
2. get above-mentioned Electrospun stoste 8mL with Dispoable medical injection needle, carry out electrostatic spinning by the general use step of instrument, the condition of electrostatic spinning is voltage 22.0kv, feeding speed 0.5mL/h, temperature 45 C, (be 15cm, secondary air flow velocity is middling speed to receiving range
3., after waiting until that electrostatic spinning has carried out 15min, start sampling, sampler is slide, and the sampling time is 45s.
4. by the sample collected directly at the optical microphotograph Microscopic observation of high power and take pictures (multiplication factor is 600 times, camera lens pixel 5,000,000), observable Local map is as shown in Figure 9.
Cu (the NO for preparing of method of electrostatic spinning as seen from Figure 9
3)
2/ Ce (NO
3)
3/ PAN composite fibre irregularly drops on above sampler, and the diameter of fiber is less, and more evenly, continuity is good.
Although embodiment of the present invention are open as above, but it is not restricted to listed in description and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. one kind
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, comprise electrospinning cabinet (A), sampler chamber (B), damp and hot conditioning chamber (C) and master control room (D), the relatively independent and rational deployment of each several part is in a larger box cloche; It is characterized in that: described electrospinning cabinet adopts bottom feed, top receives the patten's design of Electrospun product; The syringe needle fixed bar of Electrospun indoor being equipped with auxiliary blower, for forming the secondary air of rising in the process of electrostatic spinning, electrostatic spinning can be carried out continually and steadily; Described sampler chamber can realize Electrospun sample collection at any time and without the need to interrupting Electrospun; The sample that sampler chamber obtains at preliminary observation under high-power microscope, also can be observed further under characterization device; Described damp and hot conditioning chamber is provided with heating rod, and is connected with dehumidifier, for controlling the temperature and humidity of electrospinning cabinet; Described electrospinning cabinet (A) is for electrostatic spinning; Injection needle tube (1) is fixed in micro-injection pump (2) draw-in groove, and the afterbody of injection needle tube (1) leans against on the pusher of micro-injection pump (2); The head of injection needle tube (1) is connected with stainless steel syringe needle (4) by silicone tube (3), under the promotion of micro-injection pump (2), Electrospun stoste is quantitatively delivered stainless steel syringe needle by silicone tube (3), and micro-injection pump (2) controls the flowing velocity of the interior Electrospun stoste of injection needle tube (1); The base plate of electrospinning cabinet (A) is fixed with syringe needle fixed bar (9), and described syringe needle fixed bar (9) is highly adjustable, can regulate the distance of stainless steel syringe needle (4) and take-up reel (10); Metal needle fixator (6) is arranged at syringe needle fixed bar (9) top, and metal needle fixator (6) is built-in with magnet piece (5); Sheet metal (8) is inhaled on magnet piece (5) side, and sheet metal (8) is connected with the anode of high voltage source; Stainless steel syringe needle (4) is inhaled by the suction of magnet piece (5) and is leaned against on sheet metal (8) side, syringe needle fixed bar (9) is provided with glass baffle plate (7), glass baffle plate (7) has syringe needle perforation, the needle section of stainless steel syringe needle (4) exposes on glass baffle plate (7) through the upper set syringe needle perforation of glass baffle plate (7); With glass baffle plate at a distance of required distance and the position be positioned on directly over stainless steel syringe needle (4) is provided with take-up reel (10); Take-up reel is made up of metal material, and in disc, the center of discoidal take-up reel (10) is connected by the negative electrode of wire with the high voltage source in master control room; Take-up reel (10) is connected with the motor in damp and hot conditioning chamber (C) by hollow connecting rod (12), can rotate, can be controlled the rotating speed of motor (13) and take-up reel (10) by master control room under the drive of motor (13); A temperature inductor (14) is equipped with for detecting the temperature of electrospinning cabinet at take-up reel (10) back side.
2. as claimed in claim 1
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, it is characterized in that: immediately below the middle and upper part of the syringe needle fixed bar (9) in electrospinning cabinet (A), stainless steel syringe needle (4), the auxiliary blower (11) that can produce toward the secondary air risen is equipped with at place; The height of auxiliary blower can regulate; By regulating the rotating speed of auxiliary blower, and form the secondary air of different in flow rate; Glass baffle plate (7) is provided with some uniform passages, secondary air can be allowed to pass through, electrostatic spinning can be carried out sustainedly and stably.
3. as claimed in claim 1 or 2
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, it is characterized in that: be fixed with a drier receptacle (15) in the side of electrospinning cabinet (A), drier receptacle (15) is placed with beaker, and beaker is equipped with drier, drier receptacle (15) is provided with side gate (16) and early gate (17); By opening early gate, closing side gate (16), can change drier safely, after drier is changed, open side gate (16), closes early gate, makes the humidity that electrospinning cabinet (A) remains lower.
4. as claimed in claim 1 or 2
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, it is characterized in that: described sampler chamber (B) is placed in the side of electrospinning cabinet (A), and sampler chamber (B) has the gate of two independent switches, is respectively side gate (21) and early gate (22); Open early gate (22) and close side gate (21) simultaneously, can sampler be loaded onto; Open side gate (21) in sampling process, closes early gate (22), can realize the sealing of sampling process and ensure the safety of operating personnel.
5. electrostatic spinning machine as claimed in claim 1 or 2, it is characterized in that: described sampler chamber is provided with thief rod (19), the material of thief rod (19) is insulator, thief rod (19) is through a side of sampler chamber, its one end is placed in sampler chamber inside and sampler fixator (20) is housed, sampler fixator (20) is provided with sampler (18), thief rod (19) other end is in the outside of sampler chamber and can fold, by promoting thief rod (19), sampler (18) can be moved on to the surface of take-up reel, gather Electrospun sample; Pull thief rod again, can sample be sent back to sampler chamber, and take out observation.
6. as claimed in claim 1 or 2
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling functionit is characterized in that: the sampler (18) in described sampler chamber (B) adopts cover glass or slide, the sample that cover glass or slide gather directly, preliminarily can observe Electrospun sample under high-power microscope, also can observe further under characterization device after reprocessing; If when using high-power microscope to carry out preliminary observation to Electrospun product, the duration of sampling in sampling process should be selected according to feeding speed, sampling time, the position of sampling was selected, in the center near take-up reel, to make the sample of collection have more representativeness between 20s ~ 120s.
7. as claimed in claim 1 or 2
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling function, it is characterized in that: damp and hot conditioning chamber (C) is positioned at the top of electrospinning cabinet (A), play the control of the temperature and humidity to electrospinning cabinet (A); Be provided with an opening (23) at damp and hot conditioning chamber (C), described opening (23) can be connected with the dehumidifier at the back side being placed in electrostatic spinning machine, opens dehumidifier, can make the humidity that electrospinning cabinet remains lower; Wet thermo-regulated chamber is provided with radiator fan, and heating rod (24) is fixed on above radiator fan (25), by heating and dispelling the heat, makes electrospinning cabinet maintain within stationary temperature scope; At damp and hot conditioning chamber built with exhaust fan (26), exhaust fan (26) can get rid of the gas that electro-spinning process evaporates, the interface of exhaust fan and damp and hot conditioning chamber is provided with exhaust gate, exhaust gate is closed in electro-spinning process, prevent pouring in down a chimney of external air flow, maintain the stable of the interior condition of electrospinning cabinet; Between damp and hot conditioning chamber and electrospinning cabinet, there is glass plate to separate, the glass plate being positioned at take-up reel (10) back side has several holes, to make good the communicating of energy between electrospinning cabinet with damp and hot conditioning chamber, be convenient to regulate the temperature and humidity of electrospinning cabinet and the gas after getting rid of electrostatic spinning.
8. as claimed in claim 1 or 2
there is the air-flow auxiliary electrostatic spinning instrument of real-time sampling functionit is characterized in that: described master control room (D) is for controlling the main process of electrostatic spinning, be made up of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system and control inerface, the control of electrostatic spinning process can be realized.
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| CN104865993B (en) * | 2015-03-25 | 2017-12-12 | 广东工业大学 | Climatic chamber and constant temperature and humidity method suitable for electrostatic spinning |
| CN105525366B (en) * | 2016-01-27 | 2018-02-09 | 上海同芮投资管理有限公司 | A kind of electrospinning device for preparing nanofiber |
| CN107366030B (en) * | 2017-08-10 | 2020-04-07 | 东华大学 | Micron fiber/nano fiber composite filter material and preparation method thereof |
| CN112553700B (en) * | 2020-12-07 | 2021-08-24 | 山东旭源塑业有限公司 | Emulsion electrospinning process for producing new high-performance fiber material |
| CN113388901B (en) * | 2021-07-15 | 2022-04-01 | 河北耐诺科技有限公司 | Electrostatic spinning equipment |
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| CN202744668U (en) * | 2012-02-23 | 2013-02-20 | 福建师范大学 | Tray type static spinning instrument with real-time image display function |
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| CN103409818A (en) * | 2013-07-16 | 2013-11-27 | 东华大学 | Multi-spraying-nozzle electrostatic spinning device with controllable spinning environment |
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| JP5698509B2 (en) * | 2010-12-06 | 2015-04-08 | トップテック・カンパニー・リミテッドＴＯＰＴＥＣ Ｃｏ．， Ｌｔｄ． | Nanofiber manufacturing equipment |
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| CN202744668U (en) * | 2012-02-23 | 2013-02-20 | 福建师范大学 | Tray type static spinning instrument with real-time image display function |
| CN202830247U (en) * | 2012-10-29 | 2013-03-27 | 黑龙江东方学院 | Laboratory electrostatic spinning whole set device |
| CN103334165A (en) * | 2013-06-13 | 2013-10-02 | 厦门大学 | Electrostatic spinning device |
| CN103409818A (en) * | 2013-07-16 | 2013-11-27 | 东华大学 | Multi-spraying-nozzle electrostatic spinning device with controllable spinning environment |
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