CN203923470U - The electrostatic spinning machine with air-flow miscellaneous function - Google Patents
The electrostatic spinning machine with air-flow miscellaneous function Download PDFInfo
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- CN203923470U CN203923470U CN201420225760.8U CN201420225760U CN203923470U CN 203923470 U CN203923470 U CN 203923470U CN 201420225760 U CN201420225760 U CN 201420225760U CN 203923470 U CN203923470 U CN 203923470U
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Abstract
The utility model discloses a kind of electrostatic spinning machine with air-flow miscellaneous function, comprises electrospinning cabinet, sampler chamber, damp and hot conditioning chamber and master control room, and feature is that the afterbody of the indoor injection needle tube of Electrospun 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; On the base plate of electrospinning cabinet, be fixed with syringe needle fixed bar; 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 in magnet piece one side, and sheet metal is connected with the anode of high voltage source; Stainless steel syringe needle is inhaled and is leaned against in sheet metal one side by the suction of magnet piece, and its needle section exposes on glass baffle plate through the syringe needle perforation on glass baffle plate; Position on being positioned at directly over stainless pin head is provided with take-up reel; The center of take-up reel is connected with the negative electrode of high voltage source by wire; Take-up reel is connected with the motor in damp and hot conditioning chamber by hollow connecting rod.Can overcome long filament phenomenon.
Description
Technical field
The utility model relates to electrostatic spinning field, and particularly a kind of have 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
Compare with preparation method's (as extension, template synthetic method and phase separation method etc.) of other nanofiber, electrostatic spinning technique has higher process controllability, the scope of application, simpler equipment widely, can prepare directly, continuously polymer nanofiber, and the prepared fiber of method of electrostatic spinning have less diameter, larger specific area and the larger advantages such as draw ratio.Therefore, method of electrostatic spinning has become the study hotspot of preparing superfine fibre and nanofiber, has huge industrialization potential and application prospect.According to statistics, in global range, be engaged at present with the colleges and universities of electrostatic spinning correlative study and scientific research institution over 200, also there are a lot of companies, as eSpin Technologies, the companies such as NanoTechnics, KATO Tech, Donaldson and Freudenberg are devoted to produce electrostatic spinning fiber, and are applied in real life.Have again, PTC patent WO98/0326, United States Patent (USP) 4043331 and 4878908 and Chinese patent ZL201010130864.7 etc. by Electrospun product for wound dressing, show many advantages.
Electrostatic spinning process is generally that droplet or melt droplet are with from the teeth outwards electric charge under the effect of high-voltage electrostatic field, when its surperficial charge repulsion is greater than or equal to its surface tension, drop surface will form little liquid stream (i.e. " jet ") these jets and under the effect of electric field force, be stretched, through solvent evaporates and after solidifying, is deposited on dash receiver, has just formed electrospun fibers.
There are some problems in traditional electrostatic spinning, the efficiency of electrostatic spinning is restricted.First, what at present most electrostatic spinning machine adopted is its top feed, the mode of Electrospun product is accepted in bottom, 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 the syringe needle injection of stopping up the Electrospun stoste cause.Secondly, may be the difference due to the character of Electrospun stoste, as electrical conductivity etc., make Electrospun when starting or carried out having occurred after the regular hour " long filament phenomenon " (can with reference to accompanying drawing 1 and accompanying drawing 2), from take-up reel, grow some thread materials, the last phenomenon connecting together with metal needle, makes spinning be difficult to carry out; Again, the factor that affects electrostatic spinning is many especially, and as temperature, humidity and feeding speed etc., therefore providing a stable Electrospun condition is necessary to the theoretical research of Static Spinning; Finally, electrostatic spinning general voltage using when carrying out is 10 kv～100 kv, belongs to high voltage, has certain danger in operating process.
In addition, in the process of research electrostatic spinning or production electricity spinning fibre, unavoidable ground need to carry out to the product making the observation of pattern.At present, for observing the conventional method of subtitle substance appearance form, have: 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 adjustable, the clear picture that becomes, the depth of field is large, third dimension is stronger etc., therefore, scanning electron microscopic observation is often used in the form of Electrospun product or the observation of section, or even for the generally evaluation of fiber.But, utilize scanning electron microscopic observation Electrospun product also to exist some limitation, as require sample can tolerate vacuum, sample wants preliminary treatment to remove the compositions such as moisture and volatile materials, for nonconducting sample, need to spray layer of conductive material (being often that metal spraying is processed) etc., so the cycle of scanning electron microscopic observation Electrospun sample is longer, operating process is more loaded down with trivial details, has not only consumed the more energy and material, also take a large amount of time, reduced efficiency.It is visible ray that light microscope utilizes light source, although can not be as ESEM careful appearance form of observing clearly Electrospun product, but through suitable processing, light microscope also can be observed Electrospun product, compare with ESEM, can be more directly, observe rapidly, tentatively 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, the research of electrostatic spinning and suitability for industrialized production are had to certain meaning.
Summary of the invention
In view of above problem, the purpose of this utility model is to provide a kind of device of electrostatic spinning, especially provides
a kind of electrostatic spinning machine with air-flow miscellaneous function, to realize the real-time sampling of electrostatic spinning, and use Powerful Light Microscope to carry out preliminary observation to Electrospun product.
The purpose of this utility model is also to add " secondary air " at " jet " injection direction of electrostatic spinning, to overcome " long filament phenomenon ", electrostatic spinning can stably be carried out.
The purpose of this utility model is also to adopt the mode of " bottom feed, Electrospun product is accepted at top ", promotes the quality of electrostatic spinning product.
The purpose of this utility model is also electrostatic spinning machine integrated, strengthens the influence factor to electrostatic spinning process, and promotes the security of electrostatic spinning operation.
For realizing the purpose of this utility model, adopt technical scheme as follows: described
the electrostatic spinning machine with air-flow miscellaneous function, comprising electrospinning cabinet, sampler chamber, damp and hot conditioning chamber and master control room, its design feature is that described electrospinning cabinet comprises injection needle tube, and 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 Electrospun stoste can be quantitatively transported to stainless steel syringe needle by silicone tube; On the base plate of electrospinning cabinet, be fixed with syringe needle fixed bar, 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 in magnet piece one side, and sheet metal is connected with the anode of high voltage source; Stainless steel syringe needle is inhaled and is leaned against in sheet metal one side by the suction of magnet piece, on syringe needle fixed bar, be provided with glass baffle plate, on glass baffle plate, have syringe needle perforation, the needle section of stainless steel syringe needle exposes on glass baffle plate through syringe needle perforation set on glass baffle plate; Be provided with take-up reel with the position of glass baffle plate at a distance of desired distance and on being positioned at directly over stainless steel syringe needle; Take-up reel is made by metal material, is disc, and the center of discoidal take-up reel is connected with the negative electrode of high voltage source in master control room by wire; Take-up reel is connected with the motor in damp and hot conditioning chamber by hollow connecting rod; At the take-up reel back side, be equipped with a temperature inductor for surveying the temperature of electrospinning cabinet.
Under the middle and upper part of the indoor syringe needle fixed bar of Electrospun, stainless steel syringe needle, locate to be equipped with the auxiliary blower that can produce toward the secondary air rising; On glass baffle plate, be separately provided with some uniform passages.
A side at electrospinning cabinet is fixed with a drier receptacle, and dryer is placed with beaker, and beaker is equipped with drier, and drier receptacle is provided with side gate and early gate.
Described sampler chamber is placed in a 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 load onto sampler.
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, the thief rod other end is the outside of sampler chamber and can fold, sampler can be moved on to the surface of take-up reel, collection Electrospun sample by promotion thief rod; Pull again thief rod, can send sample back to sampler chamber, and take out observation.
Described damp and hot conditioning chamber is positioned at the top of electrospinning cabinet; At damp and hot conditioning chamber, be provided with an opening, described opening can be connected with the dehumidifier that is placed in the back side of electrostatic spinning machine; In damp and hot conditioning chamber, be provided with radiator fan, heating rod is fixed on above radiator fan; In damp and hot conditioning chamber, exhaust fan is housed, exhaust fan can be got rid of the gas that Electrospun process evaporates, and the interface of exhaust fan and damp and hot conditioning chamber is provided with exhaust gate; Between damp and hot conditioning chamber and electrospinning cabinet, have glass plate to separate, on the glass plate at the take-up reel back side, having out several holes to make can good communicating between electrospinning cabinet and damp and hot conditioning chamber two Room.
Described master control room is comprised of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system and control interface, can realize the control of electrostatic spinning process.
Sampler in described sampler chamber adopts cover glass or slide, the sample that cover glass or slide gather can directly, tentatively be observed Electrospun sample under high-power microscope, maybe can after process again, be used under other sign instruments such as ESEM and further observe.
Specifically, described in the utility model
the electrostatic spinning machine with air-flow miscellaneous function, comprising 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.Described electrospinning cabinet adopts bottom feed, top to receive the mode of Electrospun product; On the indoor syringe needle fixed bar of Electrospun, auxiliary blower (a kind of small-sized exhaust fan) is housed, for the process at electrostatic spinning, forms " secondary air " rising, electrostatic spinning can be carried out continually and steadily; Described sampler chamber can be realized the collection at any time of Electrospun sample, and without interrupting Electrospun; The sample that sampler chamber obtains can, at preliminary observation under high-power microscope, also can further be observed under other sign instruments 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 using in above-mentioned electrostatic spinning machine is selected insulator as far as possible, and to guarantee the safety of experimental implementation, the gate communicating with the external world etc. is done encapsulation process, assurance device has certain sealing, maintains electrostatic spinning and carries out under relatively constant condition.
Preferably, in above-mentioned electrostatic spinning machine, there is the sampler chamber that can sample at any time, in sampling process without interrupting electrostatic spinning.Sampler chamber is placed in a side of electrospinning cabinet, the gate with these two independent switches of early gate and 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 interrupting electrostatic spinning, realize the sealing of instrument and guarantee operating personnel's safety.
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 fixator is fixed sampler.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, gather Electrospun sample; Pull again thief rod, can send sample back to sampler chamber, and take out observation.
Preferably, in above-mentioned electrostatic spinning machine, the sampler in sampler chamber can be the transparent carriers such as cover glass or slide.So, the sample gathering both can directly, tentatively be observed Electrospun sample under high-power microscope, also can after process again, be used under other sign instruments such as ESEM and further observe.In addition, also can select other thin slice as sampler, the sample of acquisition is for instruments such as ESEMs.
Preferably, in the high-power microscope multiplication factor described in above-mentioned electrostatic spinning machine, more than 600 times, have camera function, camera lens pixel is 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 20 s～120 s.
Preferably, at the electrospinning cabinet described in above-mentioned electrostatic spinning machine, comprise 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 is upper, adopts bottom feed, top receives the mode of Electrospun product.
Preferably, in above-mentioned electrostatic spinning machine, the height of metal needle fixator can regulate by fixed bar, and the top of fixator is the unit of plastic of an 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, can allow syringe needle pass, and expose, and several access openings is set equably near opening simultaneously, can allow " secondary air " to pass through smoothly.A side of unit of plastic is sheet metal, and stainless steel syringe needle is fixed on sheet metal one side under the attraction of built-in magnet piece.Sheet metal is connected with the high voltage source anode in master control room, thereby realizes being connected 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 under syringe needle.By regulating the rotating speed of auxiliary blower, can form the secondary air of different in flow rate, can overcome " the long filament phenomenon " that in Electrospun process, occur, allow Electrospun carry out sustainedly and stably; The height of auxiliary blower can regulate.
Preferably, in electrospinning cabinet one side of above-mentioned electrostatic spinning machine, be provided with a drier receptacle, receptacle is provided with two gates, and early gate and side gate, have the sealing strip of adding, and guarantees sealing.Open early gate and can be used for packing into or taking out drier, side gate, for being communicated with or isolated electrospinning cabinet, like this, can be realized the replacing at any time of drier, guarantees the state of electrospinning cabinet in 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 with the motor in damp and hot conditioning chamber by hollow connecting rod, under the drive of motor, can rotate, and can control 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 comprised of heating rod, radiator fan, dehumidifier connector, motor and exhaust fan, by controlling the heating of heating rod, thereby the temperature that realizes electrospinning cabinet is controlled, radiator fan is placed in heating rod below, for accelerating heat radiation, makes the temperature in instrument reach fast uniform state; Dehumidifier connector is connected with the dehumidifier in being placed in electrostatic spinning machine, and the dehumidifier effect by dehumidifier makes electrospinning cabinet maintain lower humidity; Motor is for controlling the rotation of the indoor take-up reel of Electrospun; Exhaust fan finishes the gas of rear discharge electrospinning cabinet for Electrospun, and the interface of exhaust fan and damp and hot conditioning chamber is provided with baffle plate, and closing baffle plate in Electrospun process prevents pouring in down a chimney of extraneous air-flow, maintains the stablizing of interior condition of electrospinning cabinet.
Preferably, the main process that is used for controlling electrostatic spinning at the master control room of above-mentioned electrostatic spinning machine, by micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system, control interface, formed, can realize the control of electrostatic spinning process.Above micro-injection pump, be placed with the injection needle tube that packs Electrospun stoste into, injection needle tube is connected with stainless steel syringe needle by silicone tube, under the promotion of micro-injection pump, can quantitatively Electrospun stoste be delivered to stainless steel syringe needle, is convenient to the control of flow rate of liquid.
From above-mentioned technical scheme, can find out, the utlity model has following advantage:
This electrostatic spinning machine reasonably concentrates on various piece in a box cloche, takes insulation and seal approach, and the condition that can not only maintain Electrospun is relatively constant, is good at protecting operating personnel's safety.
This electrostatic spinning machine be provided with sampling apparatus, and sample mode is simple and safe, and can sampling at any time in the situation that not interrupting electrostatic spinning, can obtain representative higher sample, facilitates the research of electrostatic spinning.
This electrostatic spinning machine can adopt the thin slice that cover glass or slide etc. are transparent to gather Electrospun product as sampler, and the sample of collection can be used 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 " occurring in electrostatic spinning process, electrostatic spinning is carried out sustainedly and stably.
This electrostatic spinning machine adopts bottom feed, prevents that Electrospun 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 be changed 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, guarantees the closure of electrostatic spinning machine.
Accompanying drawing explanation
fig. 1for " long filament phenomenon " figure that in conventional electrostatic spinning machine experimentation, certain polymer solution occurs.Can see, the masking foil in take-up reel has received certain thickness Electrospun product, but has crossed after a period of time, and position, intermediate portion grows thread material at leisure, is " column type ", and has the trend that continues upper length.
fig. 2for " long filament phenomenon " figure that in conventional electrostatic spinning machine experimentation, another kind of polymer solution occurs.Can see, the masking foil in take-up reel has received certain thickness Electrospun product, but has crossed after a period of time, and its position, marginal portion grows thread material at leisure, is " bowl-shape type ", and can continue to rise.
fig. 3the schematic diagram of the electrostatic spinning machine proposing for the utility model.
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.
The specific embodiment
In order more clearly to explain the utility model, to be briefly described by some accompanying drawings below, apparently, below listed accompanying drawing be only embodiment more of the present utility model, for this field those of ordinary skill, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Below in conjunction with 3 pairs of the utility model of accompanying drawing, be described in more detail, so that those skilled in the art can be with reference to also implementing.
As shown in Figure 3, the utility model---a kind of electrostatic spinning machine with air-flow miscellaneous 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 grooves, 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 transported to stainless steel syringe needle 4 by silicone tube 3, and micro-injection pump 2 is being controlled the flowing velocity of the interior Electrospun stoste of injection needle tube 1.On the base plate of electrospinning cabinet A, be fixed with syringe needle fixed bar 9, 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 in magnet piece 5 one sides.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 and is leaned against in sheet metal 8 one sides by magnet piece 5 suction, on syringe needle fixed bar 9, be provided with glass baffle plate 7, on glass baffle plate 7, have syringe needle perforation, the needle section of inhaling the stainless steel syringe needle 4 that leans against sheet metal 8 one sides exposes on glass baffle plate 7 through the syringe needle perforation having on glass baffle plate 7.On glass baffle plate 7 and with glass baffle plate 7 in a distance, locate to be provided with take-up reel 10 directly over being positioned at stainless steel syringe needle 4, take-up reel 10 is made by 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.At take-up reel 10 back sides, be equipped with a temperature inductor 14 for surveying the temperature of electrospinning cabinet.Under the middle and upper part of syringe needle fixed bar 9, stainless steel syringe needle 4, locate to be equipped with in addition the auxiliary blower 11 that can produce toward the secondary air rising, by regulating the rotating speed of fan, can control the flow velocity of secondary air, the secondary air forming is toward rising, the some uniform passage that can arrange above by glass baffle plate 7, Electrospun product is produced to the power making progress, thereby Electrospun is stablized, carry out constantly.A side at electrospinning cabinet A is fixed with a drier receptacle 15, and 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 safely drier, 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 a side at the top of electrospinning cabinet, just can level when its position enters into electrospinning cabinet to guarantee sampler 18 be advisable being attached in take-up reel 10.The thief rod 19 of sampler chamber is through the outside of sampler chamber, can fold, one end outside, the other end is connected in sampler chamber and 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, the early gate 22 of opening sampler, installs to sampler 18 above sampler fixator 20, fastens after 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.Stable enough for a long time after, pull thief rod 19, sampler 18 is shifted out to 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 to ultramicroscopic observation and carry out preliminary observation or use after treatment ESEM to carry out careful observation.
Damp and hot conditioning chamber C is positioned at the top of electrospinning cabinet, plays the control to the temperature and humidity of electrospinning cabinet.At damp and hot conditioning chamber, be provided with an opening 23, described opening 23 can be connected with the dehumidifier that is placed in the back side of sub-electrostatic spinning machine (dehumidifier is installed in airtight little lattice), opens dehumidifier, can make electrospinning cabinet maintain lower humidity.In damp and hot conditioning chamber, be provided with radiator fan 25, heating rod 24 is fixed on above radiator fan 25, by heating and dispelling the heat, makes within electrospinning cabinet maintains stationary temperature scope.Motor 13, for driving the rotation of take-up reel 10, is collected Electrospun product equably, and its rotating speed can regulate by master control room.Exhaust fan 26 is housed in damp and hot conditioning chamber, after Electrospun finishes, first opens the discharge air lock door of exhaust fan, then open exhaust fan 26 and can get rid of the gas that Electrospun process evaporates.Between damp and hot conditioning chamber and electrospinning cabinet, there is glass plate to separate, on the glass plate at take-up reel 10 back sides, having out several holes to make between electrospinning cabinet and damp and hot conditioning chamber two Room can good communicating, and is convenient to regulate the temperature and humidity of electrospinning cabinet and gets rid of the gas after electrostatic spinning.
Master control room D is comprised of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system and control interface, can realize the control of electrostatic spinning process, the prior art that can realize for persons skilled in the art.Various piece is reasonably integrated on electrostatic spinning machine, realizes the integrated of electrostatic spinning machine, rationally utilizes space, has again certain sealing, reduces exposing of circuit, improves the security of operation.Control interface and mainly gathered gauge tap and the indicator lamp of some parts, to facilitate the control of instrument.
While carrying out Electrospun experiment, key step is as follows:
(1) check and fasten the gate communicating with the external world, as gate 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 etc., and whether the drier of checking drier storeroom 15 need to upgrade, have if required and can first upgrade drier.
(2) connect relevant power supply, open dehumidifier, open " master switch " of instrument, " power supply indicator " lights; Open " temperature switch ", now temperature registration " PV " value shows the real time temperature of electrospinning cabinet again, by rotation " temperature adjusting " knob, sets the temperature that Electrospun needs, i.e. " SV " value; By the time instrument first reaches predetermined temperature and lower humidity is tested again.
(3) with injection needle tube, get a certain amount of electrostatic spinning raw material solution, injection needle tube 1 is fixed on to the draw-in groove of micro-injection pump 2, and make the afterbody of injection needle tube 1 only depend on the pusher of micro-injection pump 2; Head at injection needle tube 1 puts silicone tube 3, then loads onto stainless steel syringe needle 4 at the other end of silicone tube 3, allows syringe pump proceed to soon Electrospun stoste and is full of silicone tube, regulates 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 ", rotation " rotational speed regulation " knob, select a suitable rotating speed, allow take-up reel rotate; Open " air flow switch ", rotation " wind speed adjusting " knob, allows auxiliary blower 11 reach certain rotating speed, forms secondary air simultaneously.
(5) open " voltage switch ", rotation " voltage-regulation " knob, is adjusted to " voltage registration " for the value of predeterminated voltage, restarts micro-injection pump when rear, and electrostatic spinning just starts to have carried out.
(6) in the process of Electrospun, close the side gate 21 of sampler chamber, the early gate 22 of opening sampler, installs to sampler 18 above sampler fixator 20, fastens after 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.Stable enough for a long time after, pull thief rod 19, sampler 18 is shifted out to 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 to ultramicroscopic observation and carry out preliminary observation or use after treatment ESEM to carry out careful observation.
(7) after Electrospun finishes 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 the gate of exhaust fan and open and open " air discharge cook ", make exhaust fan 26 start exhaust, wait after a period of time, then open the door of electrospinning cabinet, from take-up reel 10, take off Electrospun product, 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 most of inefficacy in experimentation should change as early as possible; If there is dangerous situation, can press " emergent stopping " button, clear.
Embodiment 1
1. accurately take 1.000 g polyacrylonitrile (PAN, Sigma-Aldrich, M
w=150,000) add DMF (DMF) solution of 17 mL, at 35 ℃ of water-baths, temperature constant magnetic stirring 3 h, to dissolving completely, obtain Electrospun stoste;
2. with Dispoable medical injection needle, get above-mentioned Electrospun stoste 8 mL, general use step by instrument is carried out electrostatic spinning, the condition of electrostatic spinning is voltage 18.5 kv, feeding speed 0.5 mL/h, temperature 45 C, receiving range (being that syringe needle is to the distance of take-up reel) is 15 cm, and auxiliary blower is not opened;
3. by the time electrostatic spinning has carried out (Electrospun reaches stable state) after 15 min, starts sampling, and sampler is slide (specification: 25.4 mm * 76.2 mm, thickness is 1 mm～1.2 mm), and the sampling time is 45 s;
By the sample collecting directly the optical microphotograph Microscopic observation of high power 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 after treatment, the scanning electron microscope (SEM) photograph that the same amplification that obtains is 600 times, as shown in Figure 5.
Observation Fig. 4 is known, under light microscope, amplify under the condition of 600 times, can see sparse, elongated filiform, filiform is the PAN fiber that Electrospun obtains, and conscientiously observes and can find, PAN fibre diameter is more close, some fiber surface is more even, and some fiber has more " spindle " (show as in Fig. 4: similar globule, two ends are thinner, middle thicker point).
Observation to Fig. 5, can know that Electrospun product can be clearly seen while amplifying 600 times under ESEM, it is also more elongated observing PAN fiber, but very intensive (reason that the sampling time is long) conscientiously observed and also can be seen having more " spindle " to exist.Therefore light microscope preliminary observation has obtained checking to effect in the observation of ESEM.
At this, it should be noted that the PAN fiber seen under light microscope be why sparse be that also only in this way, light could see through sampler, observes Electrospun product because the time of sampling is shorter.
Embodiment 2
1. accurately take the DMF solution that 1.000 g PAN add 17 mL, at 35 ℃ of water-baths, temperature constant magnetic stirring 3 h, to dissolving completely, obtain Electrospun stoste;
2. with Dispoable medical injection needle, get above-mentioned Electrospun stoste 8 mL, by the general use step of instrument, carry out electrostatic spinning, the condition of electrostatic spinning is voltage 15.0 kv, feeding speed 0.5 mL/h, temperature 45 C, receiving range (be 15 cm, do not open by auxiliary blower;
3. electrostatic spinning has carried out after 15 min by the time, starts sampling, and sampler is slide, and the sampling time is 45 s;
By the sample collecting directly the optical microphotograph Microscopic observation of high power take pictures (multiplication factor is 600 times, camera lens pixel 9,000,000), observable Local map is as shown in Figure 6.
From Fig. 6, can know, under light microscope, amplify 600 times, can observe Electrospun product, and Electrospun product irregularly drops on sampler surface, resulting fibre diameter is less, and continuity is better, also more even for observing obvious " spindle ".
Embodiment 3
1. accurately take 1.792 g polyvinylpyrrolidones (PVP) and add the absolute ethyl alcohol of 10 mL and the distilled water of 20 mL, at room temperature magnetic agitation 2 h, to dissolving completely, obtain Electrospun stoste;
2. with Dispoable medical injection needle, get above-mentioned Electrospun stoste 8 mL, by the general use step of instrument, carry out electrostatic spinning, the condition of electrostatic spinning is voltage 15.0 kv, feeding speed 1.0 mL/h, 30 ℃ of temperature, receiving range is 15 cm, auxiliary blower is not opened;
3. electrostatic spinning has carried out after 15 min by the time, starts sampling, and sampler is slide, and the sampling time is 25 s;
By the sample collecting directly the optical microphotograph Microscopic observation of high power 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 after treatment, the scanning electron microscope (SEM) photograph that the same amplification that obtains is 600 times, as shown in Figure 8.
By Fig. 7, can be clear that elongated PVP fiber, all in all PVP fiber thickness is more even, but careful observation can be found the relatively out-of-flatness of its edge.And can know that ESEM amplifies 600 times from Fig. 8, the silk edge of observing is also fuzzyyer.This may be that the water imbibition of PVP is more intense, easily absorbs airborne moisture and becomes and stuck with paste, and be likely also that the temperature of electrostatic spinning is lower, dissolve the infull reason of volatilization.
Embodiment 4
1. accurately take the PAN of 0.300 g copper nitrate, 1.200 g cerous nitrates and 2.000 g, then add the DMF solution of 34 mL, at 35 ℃ of lower magnetic forces of water-bath, stir 3 h to dissolving completely, obtain Electrospun stoste;
2. with Dispoable medical injection needle, get above-mentioned Electrospun stoste 8 mL, by the general use step of instrument, carry out electrostatic spinning, the condition of electrostatic spinning is voltage 22.0 kv, feeding speed 0.5 mL/h, temperature 45 C, (be 15 cm, secondary air flow velocity is middling speed to receiving range
3. electrostatic spinning has carried out after 15 min by the time, starts sampling, and sampler is slide, and the sampling time is 45 s.
By the sample collecting directly the optical microphotograph Microscopic observation of high power 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 that as seen from Figure 9 prepared by method of electrostatic spinning
3)
2/ Ce (NO
3)
3/ PAN composite fibre irregularly drops on above sampler, and the diameter of fiber is less, more even, and continuity is good.
Although embodiment of the present utility model is open as above, but it is not restricted to listed utilization in description and embodiment, it can be applied to the various fields of the present utility model that are applicable to completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the utility model is not limited to specific details and illustrates here and the legend of describing.
Claims (8)
1. one kind
the electrostatic spinning machine with air-flow miscellaneous functioncomprise electrospinning cabinet (A), sampler chamber (B), damp and hot conditioning chamber and master control room (D), it is characterized in that: described electrospinning cabinet (A) comprises injection needle tube (1), 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), and Electrospun stoste can be quantitatively transported to stainless steel syringe needle (4) by silicone tube; On the base plate of electrospinning cabinet (A), be fixed with syringe needle fixed bar (9), 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 is inhaled in magnet piece (5) one sides, and sheet metal (8) is connected with the anode of high voltage source; Stainless steel syringe needle (4) is inhaled and is leaned against in sheet metal (8) one sides by the suction of magnet piece (5), on syringe needle fixed bar (9), be provided with glass baffle plate (7), on glass baffle plate (7), have 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); Be provided with take-up reel (10) with the position of glass baffle plate (7) at a distance of desired distance and on being positioned at directly over stainless steel syringe needle; Take-up reel (10) is made by metal material, is disc, and middle the heart channel of Hang-Shaoyin wire of discoidal take-up reel (10) is connected with the negative electrode of the high voltage source in master control room; Take-up reel (10) is connected with the motor (13) in damp and hot conditioning chamber (C) by hollow connecting rod (12); At take-up reel (10) back side, be equipped with a temperature inductor (14) for surveying the temperature of electrospinning cabinet.
2. as claimed in claim 1
the electrostatic spinning machine with air-flow miscellaneous function, it is characterized in that: under the middle and upper part of the syringe needle fixed bar (9) in electrospinning cabinet (A), stainless steel syringe needle (4), locate to be equipped with the auxiliary blower (11) that can produce toward the secondary air rising; On glass baffle plate (7), be separately provided with some uniform passages.
3. as claimed in claim 1 or 2
the electrostatic spinning machine with air-flow miscellaneous function, it is characterized in that: the side at electrospinning cabinet is fixed with a drier receptacle (15), and dryer (15) is placed with beaker, and beaker is equipped with drier, drier receptacle (15) is provided with side gate (16) and early gate (17).
4. as claimed in claim 1 or 2
the electrostatic spinning machine with air-flow miscellaneous function, it is characterized in that: described sampler chamber is placed in a side of electrospinning cabinet (A), sampler chamber (B) has side gate (21) and the early gate of two independent switches; Open early gate (22) and close side gate (21) simultaneously, can load onto sampler (18).
5. as claimed in claim 1 or 2
the electrostatic spinning machine with air-flow miscellaneous function, it is characterized in that: damp and hot conditioning chamber is positioned at the top of electrospinning cabinet (A); At damp and hot conditioning chamber (C), be provided with an opening (23), described opening (23) can be connected with the dehumidifier that is placed in the back side of electrostatic spinning machine; In damp and hot conditioning chamber, be provided with radiator fan (25), heating rod is fixed on radiator fan (25) above; Exhaust fan (26) is housed in damp and hot conditioning chamber, and exhaust fan (26) can be got rid of the gas that Electrospun process evaporates, and the interface of exhaust fan and damp and hot conditioning chamber is provided with exhaust gate; Between damp and hot conditioning chamber and electrospinning cabinet, have glass plate to separate, on the glass plate that is positioned at take-up reel (10) back side, having out several holes to make can good communicating between electrospinning cabinet and damp and hot conditioning chamber two Room.
6. as claimed in claim 1 or 2
the electrostatic spinning machine with air-flow miscellaneous function, it is characterized in that: described master control room is comprised of micro-injection pump, high voltage source, dehumidifier, temperature control system, fan control system, take-up reel control system and control interface, can realize the control of electrostatic spinning process.
7. electrostatic spinning machine as claimed in claim 5, 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 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 again thief rod, can send sample back to sampler chamber, and take out observation.
8. as claimed in claim 5
the electrostatic spinning machine with air-flow miscellaneous functionit is characterized in that: the sampler in described sampler chamber (18) adopts cover glass or slide, the sample that cover glass or slide gather can directly, tentatively be observed Electrospun sample under high-power microscope, maybe can after process again, be used under other sign instruments such as ESEM and further observe.
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| CN201420225760.8U CN203923470U (en) | 2014-05-05 | 2014-05-05 | The electrostatic spinning machine with air-flow miscellaneous function |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862788A (en) * | 2015-05-27 | 2015-08-26 | 西安工程大学 | Air jet assisting multi-needle electrostatic spinning device and method for preparing nanofiber net through air jet assisting multi-needle electrostatic spinning device |
| CN109186486A (en) * | 2018-08-10 | 2019-01-11 | 江南大学 | A kind of the three-dimensional geometry vision measurement machine and measurement method of electrostatic adherence standard ball |
-
2014
- 2014-05-05 CN CN201420225760.8U patent/CN203923470U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862788A (en) * | 2015-05-27 | 2015-08-26 | 西安工程大学 | Air jet assisting multi-needle electrostatic spinning device and method for preparing nanofiber net through air jet assisting multi-needle electrostatic spinning device |
| CN109186486A (en) * | 2018-08-10 | 2019-01-11 | 江南大学 | A kind of the three-dimensional geometry vision measurement machine and measurement method of electrostatic adherence standard ball |
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