CN114941179B - Method for preparing long-stagnant-space superfine hollow conductive long fiber through electrostatic spinning - Google Patents
Method for preparing long-stagnant-space superfine hollow conductive long fiber through electrostatic spinning Download PDFInfo
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- CN114941179B CN114941179B CN202210630531.3A CN202210630531A CN114941179B CN 114941179 B CN114941179 B CN 114941179B CN 202210630531 A CN202210630531 A CN 202210630531A CN 114941179 B CN114941179 B CN 114941179B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/0023—Electro-spinning characterised by the initial state of the material the material being a polymer melt
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/08—Addition of substances to the spinning solution or to the melt for forming hollow filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
Abstract
The invention belongs to the technical field of electrostatic spinning, and particularly provides a method for preparing long-dead-space superfine hollow conductive long fibers by electrostatic spinning. The method comprises the following steps: 1) Placing a mixture of polyethylene and graphene in a certain proportion in a feeding barrel, spinning by a single-screw extruder through a coaxial nozzle, and simultaneously filling mixed gas in a core layer inflating device into fibers; 2) Starting a motor and a circulating pump, wherein the motor drives a central rotating shaft through a connecting crawler belt to enable the multi-column tube type receiving device to continuously rotate, the controller controls an electric heating wire to adjust the temperature of heat conducting oil, and received fibers are subjected to segmented bonding at certain intervals to seal gas. Finally, the long-dead-space superfine hollow conductive long fiber is obtained, can shield long microwaves, is light in weight and long in dead-space time, and meets the conditions of convenience in moving and unfolding and suitability for war environments.
Description
Technical Field
The invention belongs to the technical field of electrostatic spinning, and particularly provides a method for preparing long-dead-space superfine hollow conductive long fibers by electrostatic spinning.
Background
In recent years, electronic information technology and radar detection technology are rapidly developed, electromagnetic radiation pollution is brought to life of people, and some important weaponry are threatened. To solve this problem, a wave-absorbing material and an electromagnetic shielding material may be used to absorb or transfer the generated electromagnetic waves. Wave-absorbing materials refer to materials that absorb or substantially attenuate electromagnetic wave energy received at their surfaces, thereby reducing the interference of electromagnetic waves. Electromagnetic shielding material refers to a class of materials that can confine electromagnetic radiation within a certain area by absorbing and reflecting incident electromagnetic waves. Most of the traditional wave-absorbing materials and electromagnetic shielding materials are materials containing magnetic metals, and the materials are usually high in density and narrow in absorption frequency band, so that the use environment is limited to a certain extent.
With the increasing requirements of people on electromagnetic wave absorbing materials and electromagnetic shielding materials, the ideal wave absorbing and electromagnetic shielding materials are light in weight, wide in absorbing frequency band and strong in shielding capacity. In the informatization war, the development of the long microwave radar technology is very rapid, the shielding research on the long microwave at home and abroad is very slow, and the battle environment is increasingly complex, such as airplanes, naval vessels and the like, except for the threat of fire and electronic interference on the ground or in the air, the long microwave radar technology is also under the strict monitoring of detectors such as radar, infrared, laser and the like. The common wave-absorbing material and electromagnetic shielding material have high density and heavy weight and cannot adapt to the battle environment. At present, a material which is convenient to move, can be quickly arranged, can stay in the air for a period of time so as to avoid the reconnaissance of enemies and can effectively shield long microwaves is also lacked. This patent is hereby presented.
Disclosure of Invention
In view of the above situation, the present invention provides a method for preparing a long-dead-space ultrafine hollow conductive long fiber by electrostatic spinning, so as to meet the requirements of shielding long microwaves and long dead-space time. The preparation principle of the invention is as follows: by taking high molecules such as polyethylene and the like as base materials, adding auxiliary materials such as graphene, carbon nanotubes and the like and changing the using amount, the electromagnetic wave absorption peak of the obtained composite material gradually moves to a low-frequency region, and meanwhile, the peak intensity of the absorption peak is increased, so that long microwaves can be effectively absorbed and shielded; by applying the electrostatic spinning principle, the mixed material is subjected to melt electrostatic spinning through coaxial electrostatic spinning equipment, and low-molecular-weight gas is encapsulated inside the fibers one by one, so that the average density of the fibers is basically consistent with the air density at the applied height, and the fibers can float in the air for a long time, thereby achieving the purpose of long-time air stagnation. Wherein be provided with feedstock channel and inflation channel in the coaxial shower nozzle, the mixture gets into feedstock channel by the feed inlet, and gas gets into inflation channel by the inflation inlet, and the two meet in spout department, and feeding lid and shell are linked together by the screw thread, and the clearance of being convenient for dismantle, fast assembly, after the equipment, also can guarantee its axiality. The long-dead-space superfine hollow conductive long fiber material prepared by the method has light weight, long dead-space time and capability of shielding long microwaves, can hide sensitive targets in a certain area in the military field, and provides more options for the development of stealth technology.
The invention provides a method for preparing long-stagnation-space superfine hollow conductive long fiber by electrostatic spinning, which is realized by adopting the following technical scheme:
(1) Polyethylene and one or more of graphene, carbon nano tubes and conductive graphite are blended according to a certain proportion, and a certain amount of polyvinyl alcohol is added into the mixed material as a dispersing agent to prevent the agglomeration of the polyvinyl alcohol and the graphene, the carbon nano tubes and the conductive graphite. And (3) placing the mixed materials into a feeding barrel, and heating the materials to a molten state by a single-screw extruder to prepare a spinning melt. Helium and nitrogen are placed in a core layer inflating device according to a certain proportion, a pressure gauge on a pipeline of the core layer inflating device is observed, a pressure reducing valve is adjusted to ensure smooth inflation of mixed gas, the density of fibers can be close to that of air due to the inflation of the mixed gas, the purpose of long dead space is achieved, and the mixing proportion and the inflation quantity of the two gases can be adjusted according to needs.
(2) By adopting a coaxial electrostatic spinning technology, mixed materials are spun by a single-screw extruder through a coaxial nozzle, mixed gas in a core layer inflating device is inflated into fibers through the coaxial nozzle, and the single-screw extruder is grounded. The coaxial nozzle comprises a feeding cover, a shell and a discharging pipe. The feeding cover is a hollow cylinder part with a certain wall thickness, the lower end of the feeding cover is internally provided with a thread and is connected with the shell, so that the feeding cover is convenient to disassemble and clean and can be quickly assembled, and the coaxiality of the feeding cover can be ensured after the feeding cover is assembled. Be provided with feedstock channel in the shell, form feedstock channel between shell and the inside solid position, inside solid position has certain radian with feed inlet contact department, and the mixture flow direction circumference of being convenient for gets into feedstock channel. The outer part of the shell is provided with an inflation inlet, the shell is connected with the inner solid part and is provided with an inflation channel, and the shell and the inner solid part are connected at two positions and are positioned at symmetrical positions so as to ensure that the inner solid part is firm. The mixed material enters the feeding channel from the feeding hole, the mixed gas enters the inflation channel from the inflation inlet, and the mixed gas and the inflation channel are converged at the nozzle. The discharge port is located outside the gas outlet, the nozzle is in threaded connection with the discharge pipe, and the gas outlet, the discharge port, the discharge pipe and the nozzle are arranged coaxially.
(3) The receiving device adopts a multi-column tube type receiving device, and mainly comprises a non-metal bracket, a central rotating shaft, a hollow column tube, an oil inlet, a circulating pump, an electric heating wire, a thermometer and a controller.
The receiving device is integrally in a long cage shape with a micro-drum in the middle, 12 hollow column tubes are uniformly distributed on the outer surface of the cage, the length of one section of fiber containing gas is set to be 8-12cm, and the length can be adjusted through the spacing distance between the column tubes. The column tube material of the receiving device is metal, and has good thermal conductivity.
The central rotating shaft of the receiving device is arranged on the non-metal bracket through a bearing, and the material of the central rotating shaft and the motor connecting track is rubber. The motor drives the central rotating shaft through the crawler belt to enable the receiving device to rotate, and therefore continuous receiving of fibers is achieved. The negative pole of the high-voltage electrostatic generator is connected with the central rotating shaft, the other end of the high-voltage electrostatic generator is grounded, and an electrostatic field is formed between the spinning device and the receiving device.
The central rotating shaft is of a hollow structure, and hot oil is introduced into the central rotating shaft. The heat conducting oil enters from the oil inlet hole on the left side and flows to each hollow column tube distributed on the circumference through the flow channel, the oil outlet hole is connected with the central rotating shaft through the bent tube, and the central rotating shaft is provided with a circulating pump so that the heat conducting oil circulates between each hollow column tube and the central rotating shaft. And a power line of the circulating pump is connected with the controller through the slip ring. The electric heating wire is connected with the controller through a slip ring arranged on a central rotating shaft, the thermometer is arranged on the central rotating shaft, and transmits a temperature signal to the controller through the slip ring, the controller automatically controls the electric heating wire wound on the rotating shaft to automatically heat the heat conducting oil, so that the heat conducting oil is kept in a certain temperature range and can reach the melting point of the material all the time, the received hollow fibers are subjected to segmented bonding at a certain distance, and a one-section and one-section hollow structure is formed to store gas in the fibers.
The invention provides a method for preparing long-stagnation-space superfine hollow conductive long fiber by electrostatic spinning, which has the following advantages and outstanding effects:
(1) Aiming at the current situation of lack of long microwave absorbing materials, the invention originally proposes to use the coaxial electrostatic spinning principle to develop a long hollow superfine hollow conductive long fiber capable of absorbing long microwaves so as to meet the strong demand of military weaponry or sensitive areas on long microwave stealth.
(2) The invention innovatively fills the fibers with low-density inert mixed gas, so that the fibers can float in the air for a long time, meet the requirement of long-time microwave stealth on military weaponry or sensitive areas, and adapt to war environments. The volume of the gas sealed in the fiber is regulated and controlled by controlling the diameter, the number, the position, the rotating speed, the temperature and the like of the column tubes in the multi-column tube type receiving device, so that the dead time of the fiber is adjusted.
(3) Most of the traditional wave-absorbing materials and electromagnetic shielding materials contain magnetic metal materials, and the materials are usually high in density and narrow in absorption frequency band, so that the use environment is limited to a certain extent. The surface of the graphene sheet layer contains a large number of dangling bonds, defects and functional groups, and the inside of the graphene sheet layer also contains rich interfaces, so that a strong polarization effect can be generated, and electromagnetic shielding is facilitated. The long hollow superfine hollow conductive long fiber prepared by the invention takes high molecules such as polyethylene and the like as base materials and graphene and the like as fillers, and is prepared by an electrostatic spinning method, so that the average density of the fiber can be adjusted. The requirements of shielding long microwave, light weight and long dead time are met, and the requirements are adapted to the conditions of war environment.
(4) The materials and gas names mentioned in the technical scheme can be replaced according to the needs so as to achieve the purpose of the invention.
Description of the drawings:
FIG. 1 is a schematic diagram of an apparatus for preparing a long hollow ultra-fine hollow conductive long fiber by electrospinning according to the present invention.
Fig. 2 is a schematic structural view of a coaxial showerhead.
In fig. 1: the device comprises a nonmetal support 1, a high-voltage electrostatic generator 2, a bearing 3, an oil inlet 4, a single-screw extruder 5, a feeding barrel 6, a coaxial sprayer 7, a pressure reducing valve 8, a pressure gauge 9, a core layer inflating device 10, hollow fibers 11, a controller 12, a thermometer 13, a central rotating shaft 14, a connecting crawler 15, a motor 16, a bent pipe 17, a sliding ring 18, an oil outlet 19, an electric heating wire 20, a circulating pump 21, a hollow column pipe 22 and a multi-column pipe receiving device 23.
In fig. 2: feed inlet 22, feed cover 23, feed channel 24, inflation inlet 25, spout 26, discharge pipe 27, inflation channel 28, shell 29, junction 30.
Detailed Description
Example 1:
in the apparatus of fig. 1, polyethylene was mixed with graphene in a ratio of 100:1, and adding 2 percent of polyvinyl alcohol as a dispersing agent into the mixed material. The single screw extruder 5 is grounded, the mixed material is placed in the feed barrel 6, and the mixed material is heated to a molten state by the single screw extruder 5 to prepare a spinning melt. The spinning melt enters the feed channel 24 from the feed opening 22 of the coaxial nozzle 7, and helium and nitrogen are simultaneously fed in a ratio of 1: the volume ratio of the core layer inflating device 10 is filled from an inflating port 25 of the coaxial nozzle 7 into an inflating channel 28, and the pressure gauge 9 is used for observing and adjusting the pressure reducing valve 8 to ensure that the core layer inflating device is smoothly filled into the hollow fibers 11. The spinning melt and the gas mixture join at the nozzle 26, emerge from the outlet pipe 27 and then fall onto the multi-column pipe receptacle 23. The multi-column tube type receiving device 23 is arranged on the non-metal support 1 through a bearing 3, the negative pole of the high-voltage electrostatic generator 2 is connected with the central rotating shaft 14, and the other end of the high-voltage electrostatic generator is grounded. 12 hollow column tubes 22 are uniformly distributed on the multi-column tube type receiving device 23. The heat conducting oil enters from the left oil inlet 4 and flows to each hollow column tube 22 distributed circumferentially through a flow channel, the oil outlet 19 is connected with the central rotating shaft 14 through the bent pipe 17, and the central rotating shaft 14 is provided with a circulating pump 21, so that the heat conducting oil circulates between each hollow column tube 22 and the central rotating shaft 14. The electric heating wire 20 is connected with the controller 12 through a slip ring 18 arranged on the central rotating shaft 14, the thermometer 13 is arranged on the central rotating shaft 14 and transmits a temperature signal to the controller 12 through the slip ring 18, the controller 12 controls the electric heating wire 20 to adjust the temperature of the heat conducting oil, and the received hollow fibers 11 can be bonded in a segmented mode at certain intervals to store gas in the hollow fibers 11. The central rotating shaft 14 is connected with the motor 16 through the connecting crawler belt 15, and the material of the connecting crawler belt 15 is selected from rubber, so that the central rotating shaft can be effectively insulated and can prevent heat from dissipating. The motor 16 drives the central rotating shaft 14 by the crawler belt 15 to rotate the multi-column tube type receiving device 23, so as to realize continuous receiving of the hollow fiber 11. After the hollow fibers 11 fall into the multi-column tubular receiving device 23, the mixed gas in the hollow fibers 11 can be sealed by continuously extruding the hollow fibers 11 at intervals. Finally obtaining the long hollow superfine hollow conductive long fiber.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (1)
1. A method for preparing long-stagnant-space superfine hollow conductive long fiber by electrostatic spinning is characterized by adopting the following technical scheme:
(1) Mixing polyethylene with one or more of graphene, carbon nano tubes and conductive graphite according to a certain proportion, adding a certain amount of polyvinyl alcohol serving as a dispersing agent into a mixed material, placing the mixed material into a feeding barrel, and heating the material to a molten state by a single-screw extruder to prepare a spinning melt; helium and nitrogen are placed in a core layer inflating device according to a certain proportion, a pressure gauge on a pipeline of the core layer inflating device is observed, a pressure reducing valve is adjusted, smooth inflation of mixed gas is guaranteed, and the mixing proportion and the inflation quantity of the two gases can be adjusted according to needs;
(2) By adopting a coaxial electrostatic spinning technology, mixed materials are spun by a single-screw extruder through a coaxial nozzle, and meanwhile, mixed gas in a core layer inflating device is inflated into fibers through the coaxial nozzle, and the single-screw extruder is grounded; the coaxial nozzle comprises a feeding cover, a shell and a discharging pipe; the feeding cover is a hollow cylinder part with a certain wall thickness, the lower end of the feeding cover is internally provided with threads and is connected with the shell, so that the feeding cover is convenient to disassemble and clean and can also ensure the coaxiality of the feeding cover; a feeding channel is arranged in the shell, the feeding channel is formed between the shell and the internal solid part, and the contact part of the internal solid part and the feeding hole has a certain radian; the outer part of the shell is provided with an inflation inlet, the shell is connected with the inner solid part and is provided with an inflation channel, and the shell and the inner solid part are connected at two positions and are positioned at symmetrical positions; the mixed material enters the feeding channel from the feeding hole, the mixed gas enters the inflation channel from the inflation inlet, and the mixed gas and the inflation channel are converged at the nozzle; the discharge port is positioned outside the gas outlet, the nozzle is in threaded connection with the discharge pipe, and the gas outlet, the discharge port, the discharge pipe and the nozzle are coaxially arranged;
(3) The receiving device adopts a multi-column tube type receiving device and mainly comprises a non-metal bracket, a central rotating shaft, a hollow column tube, an oil inlet, a circulating pump, an electric heating wire, a thermometer and a controller;
the receiving device is integrally in a long cage shape with a micro-drum in the middle, 12 hollow column tubes are uniformly distributed on the outer surface of the cage, the length of a section of fiber containing gas is set to be 8-12cm, and the length can be adjusted through the spacing distance between the column tubes; the column tube material of the receiving device is metal; the central rotating shaft of the receiving device is arranged on the non-metal bracket through a bearing, and the material of the central rotating shaft and the motor connecting track is rubber; the motor drives the central rotating shaft through the crawler belt to enable the receiving device to rotate, so that continuous receiving of fibers is realized; the negative pole of the high-voltage electrostatic generator is connected with the central rotating shaft, the other end of the high-voltage electrostatic generator is grounded, and an electrostatic field is formed between the spinning device and the receiving device; the central rotating shaft is of a hollow structure, and hot oil is introduced into the central rotating shaft; heat conducting oil enters from the left oil inlet hole and flows to each hollow column tube distributed circumferentially through the flow channel, the oil outlet hole is connected with the central rotating shaft through the bent tube, and the central rotating shaft is provided with a circulating pump so that the heat conducting oil circulates between each hollow column tube and the central rotating shaft; the power line of the circulating pump is connected with the controller through the slip ring; the electric heating wire is connected with the controller through a slip ring arranged on the central rotating shaft, the thermometer is arranged on the central rotating shaft and transmits a temperature signal to the controller through the slip ring, and the controller automatically controls the electric heating wire wound on the rotating shaft to automatically heat the heat conducting oil so as to keep the heat conducting oil within a certain temperature range; and carrying out sectional bonding on the received hollow fibers at certain intervals to form a section-by-section hollow structure so as to seal gas in the fibers.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757425A (en) * | 2017-03-08 | 2017-05-31 | 中原工学院 | A kind of electrospinning device and its method for preparing hyperbranched hollow structure eider down |
| CN112030269A (en) * | 2020-09-04 | 2020-12-04 | 安徽瑜合警用装备有限公司 | Special lasting electric heating self-heating composite functional fiber material for military police and preparation method and application thereof |
| CN112962173A (en) * | 2021-03-05 | 2021-06-15 | 莱西市寰球新能源技术中心 | Communication and electronic radiation-proof material |
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| TWI374037B (en) * | 2008-08-21 | 2012-10-11 | Univ Taipei Medical | Bio-acceptable conduits and method providing the same |
| KR20140125416A (en) * | 2012-02-16 | 2014-10-28 | 코넬 유니버시티 | Ordered porious nanofibers, methods, and applications |
| US11312828B2 (en) * | 2019-05-14 | 2022-04-26 | National Tsinghua University | Method of fabricating patterned cellulose nanocrystal composite nanofibers and nano thin films and their applications |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757425A (en) * | 2017-03-08 | 2017-05-31 | 中原工学院 | A kind of electrospinning device and its method for preparing hyperbranched hollow structure eider down |
| CN112030269A (en) * | 2020-09-04 | 2020-12-04 | 安徽瑜合警用装备有限公司 | Special lasting electric heating self-heating composite functional fiber material for military police and preparation method and application thereof |
| CN112962173A (en) * | 2021-03-05 | 2021-06-15 | 莱西市寰球新能源技术中心 | Communication and electronic radiation-proof material |
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