CN215828937U - Device for continuously preparing aerogel fibers with skin-core structures - Google Patents
Device for continuously preparing aerogel fibers with skin-core structures Download PDFInfo
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- CN215828937U CN215828937U CN202121293130.0U CN202121293130U CN215828937U CN 215828937 U CN215828937 U CN 215828937U CN 202121293130 U CN202121293130 U CN 202121293130U CN 215828937 U CN215828937 U CN 215828937U
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Abstract
The utility model relates to a device for continuously preparing aerogel fibers with a skin-core structure, which comprises a fiber extrusion unit, a fiber solidification unit, a fiber freezing unit, a fiber collection unit and a fiber drafting unit matched with the fiber solidification unit and the fiber freezing unit, wherein the fiber extrusion unit, the fiber solidification unit, the fiber freezing unit and the fiber collection unit are sequentially arranged along the fiber movement direction. Compared with the prior art, the method provided by the utility model combines controllable solvent replacement and an ice template to obtain the aerogel fiber with a skin-core structure, and can realize continuous and large-scale preparation of the aerogel fiber.
Description
Technical Field
The utility model belongs to the technical field of aerogel fiber preparation, and relates to a device for continuously preparing aerogel fibers with skin-core structures.
Background
The spinning apparatus is a machine that forms a fiber-forming polymer solution or melt into filaments. Conventional spinning is classified into solution spinning, melt spinning, and the like according to a fiber spinning method.
Solution spinning refers to a method in which a concentrated solution of a high polymer is quantitatively extruded from a spinneret orifice, and a thin stream of the solution is solidified into fibers by a coagulating bath, hot air or hot inert gas. After the high polymer solution is extruded, the high polymer solution enters a coagulating bath or hot air, molecular chains can be subjected to stretching orientation, and the high polymer solution enters the coagulating bath to be subjected to double diffusion to form a compact structure, so that the mechanical properties of the fiber can be improved. The solution spinning has the advantages of high efficiency and simple operation.
The melt spinning is a forming method which takes polymer melt as raw material and adopts a melt spinning machine to spin. In the spinning process, the polymer needs to be heated to its melting point, and for some polymers, the operating temperature is high and the energy consumption is large.
In addition, the porosity of the fiber prepared by traditional solution spinning or melt spinning is low, and the requirement of people on the high-heat-preservation heat-insulation fabric cannot be met.
Researches find that the aerogel fiber with high porosity, low density and low thermal conductivity can be prepared by freeze spinning, and the heat preservation and insulation capability of the fabric can be effectively improved. The freeze spinning is a method for preparing aerogel fibers by combining a solution spinning method and an ice template method, liquid nitrogen (-196 ℃) ultralow temperature is utilized to enable ice crystals to grow rapidly, and the aerogel fibers with three-dimensional porous network structures are obtained after freeze drying, so that the transformation from blocky aerogels to fibrous aerogels is realized, and the application field of the aerogel fibers is widened. However, the efficiency of the freeze spinning is low, and the porous structure on the fiber wall causes the low mechanical strength of the fiber, thereby limiting the application of the aerogel fiber.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a device for continuously preparing aerogel fibers with a skin-core structure, which can be used for preparing porous aerogel fibers with the skin-core structure by combining a controllable solvent replacement method and an ice template method, realizes continuous large-scale preparation of the aerogel fibers, and is simple to operate, low in cost and environment-friendly.
The purpose of the utility model can be realized by the following technical scheme:
the utility model provides a device for continuous preparation has aerogel fibre of skin-core structure, the device include along fibre extrusion unit, fibre solidification unit, fibre freezing unit and the fibre collection unit that fibre direction of motion set gradually, the device still include with fibre solidification unit and fibre freezing unit looks adaptation's fibre draft unit. The fiber extruded by the fiber extruding unit enters the solidifying unit, is drawn by the fiber drawing unit and then enters the fiber freezing unit, and then the fiber after freezing is collected by the fiber collecting unit.
Further, the fiber extrusion unit comprises an injector and an injector control mechanism matched with the injector, wherein the injector control mechanism is an injection pump or a pneumatic control capacity tank so as to power the injector. In the fiber extrusion unit, the extrusion of the fiber can adopt mechanical injection or pneumatic extrusion. The flow rate of the extruded spinning solution is controlled by the injection pump through the piston of the extrusion injector, and the flow rate of the extrusion piston of the injection pump can be selected from 50 mul min-1～100ml min-1. Further preferably 50. mu.l min-1. The syringe may be 10. mu.l to 1L in size.
Further, the fiber coagulation unit comprises a coagulation tank and a coagulation bath arranged in the coagulation tank. The coagulation bath is composed of a solvent which does not dissolve the solute in the dope but can be substituted with the dope solvent, and the specific composition varies depending on the dope. The temperature, concentration, time and distance of the coagulating bath are controlled, and controllable solvent replacement is carried out, so that the thickness of the aerogel fiber skin layer can be accurately controlled, and the fiber performance is optimized.
Preferably, the coagulation bath may be a glass bath, a polytetrafluoroethylene bath, or the like, and the temperature of the coagulation bath is-100 ℃ to 100 ℃.
Further, the fiber drafting unit comprises a plurality of drafting wheels.
Further, the fiber drafting unit comprises at least two first drafting wheels, a second drafting wheel and a third drafting wheel, the first drafting wheel is positioned in the coagulating bath, the third drafting wheel is positioned above the fiber freezing unit, and the second drafting wheel is positioned between the first drafting wheel and the third drafting wheel and positioned outside the coagulating tank.
Further, the fiber freezing unit comprises a freezing tank, and liquid nitrogen is contained in the freezing tank.
Or the fiber freezing unit also comprises a freezing ring arranged on the freezing groove, and a heat conducting rod is arranged between the freezing ring and the bottom of the freezing groove. The freezing ring and the heat conducting rod are high heat conducting materials, such as brass and red copper. The freezing ring is annular and is positioned above the liquid nitrogen, and the heat conducting rod is contacted with the cold source. The fiber solidified by the fiber solidification unit passes through a freezing ring of the fiber freezing unit, and the solvent which is not replaced inside forms an ice template at low temperature. The freeze ring is primarily intended to provide a temperature gradient in its vertical direction, while the heat conducting bars are primarily intended to transfer the temperature of the bottom of the freeze tank to the freeze ring, controlling the temperature of the freeze ring. The material of the freezing tank can be polystyrene foam and polytetrafluoroethylene.
Preferably, the temperature of the freeze ring is-120 ℃.
In this case, the fiber freezing unit includes a freezing tank, a low-temperature freezing cycle machine connected to the freezing tank, and a freezing ring connected to a wall surface of the freezing tank, and the low-temperature freezing cycle machine controls the temperature of the freezing tank.
Furthermore, the fiber collecting unit comprises a collecting roller and a motor in transmission connection with the collecting roller, and one end of the collecting roller extends into the freezing tank. The rotating speed of the motor can be controlled by adopting the existing control system, and the motor drives the collecting roller to rotate to collect the frozen fibers, so that the continuous collection of the fibers is realized.
Further, the fiber collecting unit further comprises a sliding table, and the motor is arranged on the sliding table. The position of motor can be controlled to the slip table for the motor moves from side to side around making the fibre evenly distributed on collecting the cylinder, realizes the automation of spinning.
Further, the device also comprises a multi-hole spinneret matched with the fiber extrusion unit. The number of holes of the multi-hole spinneret may be 2 to 30, and is preferably connected to a syringe.
Wet-freeze spinning is a process for preparing aerogel fibers by combining controlled solvent displacement with an ice template process. The fiber is subjected to controllable solvent exchange through a coagulating bath to form a micro-nano cortex, so that the mechanical property of the fiber can be improved. The utility model combines the controllable solvent replacement and the ice template technology to prepare the aerogel fiber with the skin-core structure. Specifically, the spinning solution is extruded by a fiber extrusion unit, enters a fiber solidification unit for controllable solvent replacement, is pulled by a fiber drawing unit, enters a fiber freezing unit, and is nucleated and grown to form a porous structure. Meanwhile, as the system undergoes micro-phase separation, the solute is displaced by the ice crystals and compressed in the voids between the ice crystals. The frozen fibers are collected by a fiber collection unit. After the ice crystals are completely frozen, removing the ice crystals by a subsequent freeze-drying method to obtain the aerogel fibers with the skin-core structure by taking the ice crystals as templates.
Compared with the prior art, the utility model has the following characteristics:
1) the device has simple structure, is simple to operate compared with the freeze spinning, can continuously prepare the aerogel fiber with the skin-core structure on a large scale, is suitable for industrial production, and can design different materials according to actual requirements.
2) Controllable solvent replacement can be carried out to the coagulating bath among this invention device for the fibre has micro-nano cortex, can improve fibrous mechanical properties, forms inclosed pore structure, improves aerogel fibrous heat-proof quality, and the fibre of preparation is hopeful to realize weaving.
3) In the freezing process of the fiber freezing unit in the device, liquid nitrogen is selected as a cold source, the obtained fiber pore structure is uniform, the pore diameter is small, and the heat insulation capability of the fiber can be improved.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus for preparing aerogel fibers according to example 1;
FIG. 2 is a schematic view of the structure of an apparatus for preparing aerogel fibers according to example 2;
FIG. 3 is a schematic view of the structure of an apparatus for preparing aerogel fibers according to example 3;
FIG. 4 is a schematic view of the structure of an apparatus for preparing aerogel fibers according to example 4;
fig. 5 is an SEM image of aerogel fibers prepared in the application example.
The notation in the figure is:
1-injection pump, 2-injector, 3-coagulating tank, 4-coagulating bath, 5-first drawing wheel, 6-second drawing wheel, 7-third drawing wheel, 8-freezing tank, 9-freezing ring, 10-heat-conducting rod, 11-collecting roller, 12-motor, 13-sliding table and 14-multi-hole spinning head.
Detailed Description
The utility model is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
the device for continuously preparing aerogel fibers with a skin-core structure as shown in fig. 1 comprises a fiber extruding unit, a fiber solidifying unit, a fiber freezing unit and a fiber collecting unit which are sequentially arranged along the fiber moving direction, and further comprises a fiber drafting unit matched with the fiber solidifying unit and the fiber freezing unit.
Wherein, the fiber extrusion unit comprises a syringe 2 and a syringe pump 1 matched with the syringe 2. The injector 2 is installed on the injection pump 1, and the injection pump 1 is used for controlling the extrusion of the spinning solution. The injection pump 1 has a built-in control system for regulating the extrusion speed. The injection pump 1 extrudes the spinning solution by controlling the piston of the extrusion injector 2, the injector 2 with the measuring range of 20ml is selected as the injector 2, and the flow rate of the extrusion piston of the injection pump 1 is selected as 0.05ml min-1。
The fiber coagulation unit includes a coagulation tank 3 and a coagulation bath 4 provided in the coagulation tank 3. The fiber drafting unit comprises at least two first drafting wheels 5, a second drafting wheel 6 and a third drafting wheel 7, wherein the first drafting wheel 5 is positioned in the coagulating bath 4, the third drafting wheel 7 is positioned above the fiber freezing unit, and the second drafting wheel 6 is positioned between the first drafting wheel 5 and the third drafting wheel 7 and is positioned outside the coagulating tank 3. The solidification tank 3 may be a glass tank. Different coagulation baths 4 are prepared depending on the spinning dope.
The fiber freezing unit comprises a freezing tank 8, and liquid nitrogen is contained in the freezing tank 8. The fiber freezing unit also comprises a freezing ring 9 arranged on the freezing groove 8, and a heat conducting rod 10 is arranged between the freezing ring 9 and the bottom of the freezing groove 8. The freezing tank 8 is heat-insulating polystyrene foam, has excellent heat-insulating property, and is filled with a certain amount of liquid nitrogen; the freezing ring 9 is made of brass material and is connected with the bottom of the freezing groove 8 through a heat conducting rod 10, so that the temperature transmission is convenient, and the temperature of the fibers entering the freezing ring 9 is controlled.
The fiber collecting unit comprises a collecting roller 11 and a motor 12 in transmission connection with the collecting roller 11, and one end of the collecting roller 11 extends into the freezing tank 8. The fibre collection unit further comprises a slide table 13, on which slide table 13 a motor 12 is arranged. The sliding table 13 controls the motor 12 to move back and forth and left and right, and the motor 12 controls the collecting roller 11 to rotate, so that the continuous and automatic collection of fibers is realized.
The working process of the device is as follows:
the spinning solution is extruded out by an injector 2 controlled by an injection pump 1, passes through a coagulating bath 4, is drawn and enters a fiber freezing unit, passes through a freezing ring 9, and ice crystals nucleate and grow, and meanwhile, as the system generates micro-phase separation, a solute is extruded by the ice crystals and is compressed in gaps among the ice crystals. The frozen fibres are collected by a collecting drum 11. After the ice crystals are completely frozen, removing the ice crystals by a freeze-drying method to obtain the porous fiber which takes the ice crystals as a template and has a skin-core structure.
Example 2:
as shown in fig. 2, the difference from embodiment 1 is that the freezing tank 8 in the fiber freezing unit is a copper box and is connected to a low-temperature freezing cycle machine, a freezing ring 9 is connected to the wall surface of the freezing tank 8, and the freezing cycle machine controls the temperature of the freezing tank 8.
Example 3:
as shown in fig. 3, the difference from example 1 is that the freezing ring 9 and the heat conducting rod 10 are not provided in the freezing tank 8, and the extruded fiber is directly introduced into the liquid nitrogen atmosphere.
Example 4:
as shown in FIG. 4, the difference from example 1 is that the head of the injector 2 is connected to a multi-hole spinneret 14, and the number of holes of the multi-hole spinneret 14 may be 2 to 30.
Application example:
aerogel fibers having a sheath-core structure were prepared using the apparatus of example 1.
(1) 0.5g chitosan powder was dissolved in 10ml 1% acetic acid solution at 800rpm min-1Stirring for 30min at the rotating speed of (1) to uniformly mix the components to prepare a 5% chitosan solution. At 5000rpm min-1Was centrifuged for 5min in the centrifuge to give a spinning dope.
(2) 5g of sodium hydroxide was dissolved in 95ml of water, and the sodium hydroxide was dissolved by stirring. 50ml of sodium hydroxide solution and 50ml of absolute ethanol solution are mixed. The volume ratio of the sodium hydroxide solution to the absolute ethyl alcohol is 5: 5.
(3) And (3) putting the spinning solution into a 20ml syringe 2, extruding the spinning solution through the syringe 2, and entering a coagulating bath 4, wherein the coagulating bath 4 is the solution prepared in the step (2). By means of the drawing action the fibres enter the fibre freezing unit, pass through the freezing ring 9, ice crystals grow, the fibres freeze and are then collected by the collecting drum 11.
(4) And (4) freeze-drying the fiber obtained in the step (3), and removing the solvent to obtain the porous fiber with the skin-core structure.
The skin thickness of the produced fiber was different for different coagulation bath 4 concentrations, as shown in fig. 5. In FIG. 5, a and b are scanning electron micrographs of the prepared fiber when the volume ratio of the sodium hydroxide solution in the coagulation bath to the ethanol is 5:5, and the thickness of the skin layer is 10 μm as shown in b; c. d is a scanning electron microscope image of the prepared fiber when the volume ratio of the sodium hydroxide solution in the coagulating bath to the ethanol is 7:3, and the thickness of the skin layer is 20 mu m.
The embodiments described above are intended to facilitate the understanding and use of the utility model by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The utility model provides a device for continuous preparation has aerogel fibre of skin-core structure which characterized in that, the device include along fibre extrusion unit, fibre solidification unit, fibre freezing unit and the fibre collection unit that fibre direction of motion set gradually, the device still include with fibre solidification unit and the fibre draft unit of fibre freezing unit looks adaptation.
2. The apparatus for continuously preparing aerogel fiber with sheath-core structure according to claim 1, wherein the fiber extrusion unit comprises an injector (2) and an injector control mechanism adapted to the injector (2), and the injector control mechanism is an injection pump (1) or an air-controlled volume tank.
3. The apparatus for continuously preparing aerogel fibers having a sheath-core structure according to claim 1, wherein the fiber coagulation unit comprises a coagulation tank (3) and a coagulation bath (4) disposed in the coagulation tank (3).
4. The apparatus for continuously preparing aerogel fibers having a sheath-core structure according to claim 3, wherein said fiber drawing unit comprises a plurality of drawing wheels.
5. The apparatus for continuously preparing aerogel fiber with sheath-core structure according to claim 4, wherein the fiber drawing unit comprises at least two first drawing wheels (5), a second drawing wheel (6) and a third drawing wheel (7), the first drawing wheel (5) is located in the coagulating bath (4), the third drawing wheel (7) is located above the fiber freezing unit, and the second drawing wheel (6) is located between the first drawing wheel (5) and the third drawing wheel (7) and outside the coagulating tank (3).
6. An apparatus for continuously preparing aerogel fibers having a sheath-core structure according to claim 1, wherein the fiber freezing unit comprises a freezing tank (8), and liquid nitrogen is contained in the freezing tank (8).
7. The apparatus for continuously preparing aerogel fibers with a sheath-core structure according to claim 6, wherein the fiber freezing unit further comprises a freezing ring (9) disposed on the freezing tank (8), and a heat conducting rod (10) is disposed between the freezing ring (9) and the bottom of the freezing tank (8).
8. An apparatus for continuously preparing aerogel fibers having a sheath-core structure according to claim 6, wherein the fiber collecting unit comprises a collecting drum (11) and a motor (12) in driving connection with the collecting drum (11), and one end of the collecting drum (11) extends into the freezing tank (8).
9. The apparatus for continuously preparing aerogel fibers having a sheath-core structure according to claim 8, wherein the fiber collecting unit further comprises a slide table (13), and the motor (12) is disposed on the slide table (13).
10. An apparatus for continuously preparing aerogel fibers with a sheath-core structure according to claim 1, further comprising a multi-hole spinneret (14) adapted to the fiber extrusion unit.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121293130.0U CN215828937U (en) | 2021-06-10 | 2021-06-10 | Device for continuously preparing aerogel fibers with skin-core structures |
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| CN202121293130.0U CN215828937U (en) | 2021-06-10 | 2021-06-10 | Device for continuously preparing aerogel fibers with skin-core structures |
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