CN117684279A - Aramid micro-nanofiber aerogel material and preparation method thereof - Google Patents
Aramid micro-nanofiber aerogel material and preparation method thereof Download PDFInfo
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- CN117684279A CN117684279A CN202211079560.1A CN202211079560A CN117684279A CN 117684279 A CN117684279 A CN 117684279A CN 202211079560 A CN202211079560 A CN 202211079560A CN 117684279 A CN117684279 A CN 117684279A
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- liquid storage
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- aramid
- storage tank
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 92
- 239000004760 aramid Substances 0.000 title claims abstract description 60
- 229920003235 aromatic polyamide Polymers 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 31
- 239000004964 aerogel Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 93
- 238000009987 spinning Methods 0.000 claims abstract description 57
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- -1 halogen salt Chemical class 0.000 claims abstract description 20
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000003860 storage Methods 0.000 claims description 87
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 4
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 229910001622 calcium bromide Inorganic materials 0.000 claims description 2
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010041 electrostatic spinning Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000004108 freeze drying Methods 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 238000000352 supercritical drying Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 44
- 239000000835 fiber Substances 0.000 description 18
- 238000004140 cleaning Methods 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 150000002367 halogens Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002572 peristaltic effect Effects 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000578 dry spinning Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 210000003097 mucus Anatomy 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
-
- 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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
-
- 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
- D01D13/00—Complete machines for producing artificial threads
- D01D13/02—Elements of machines in combination
-
- 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
- D01F1/10—Other agents for modifying properties
-
- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The application discloses an aramid micro-nanofiber aerogel material and a preparation method thereof, wherein the preparation method comprises the following step S1 of preparing spinnability solution: and (3) at a preset temperature, placing halogen salt into a solvent, stirring until the halogen salt is uniformly dissolved, adding meta-aramid fiber, and stirring until the halogen salt is uniformly dissolved to obtain a spinnability solution. S2, spinning and collecting meta-aramid micro-nano fibers: spinning the spinnability solution into micro-nano fibers by using a centrifugal spinning method, wherein the micro-nano fibers are stacked and collected to obtain meta-aramid micro-nano fibers; s3, removing impurities in the meta-aramid micro-nano fiber. And carrying out ultrasonic cleaning on the collected meta-aramid micro-nano fibers, and then drying to obtain the aramid micro-nano fiber aerogel material. Compared with the existing electrostatic spinning method and air flow spinning method, the centrifugal spinning method has the advantages of high feeding rate and high production efficiency, does not need supercritical drying or liquid nitrogen freeze drying, and has lower energy consumption.
Description
Technical Field
The application relates to the field of aerogel material preparation, in particular to an aramid micro-nanofiber aerogel material and a preparation method thereof.
Background
Aerogel is the solid material with the lowest density in the world, and has the characteristics of large surface area, high porosity and the like. Therefore, the aerogel material has wide application prospect in the fields of heat insulation, sound insulation, filtration, adsorption, catalysis and the like. Meta-aramid is a high strength, heat resistant, chemically stable polymer whose repeating units contain benzene rings linked together by amide groups. The meta-aramid fiber has outstanding high temperature resistance, insulativity and flame retardance and is mainly applied to the fields of high temperature protective clothing, electric insulation, high temperature filtration and the like. Therefore, the meta-aramid fiber is prepared into the micro-nano fiber aerogel material, and the micro-nano fiber aerogel material is applied to the field and has a great application prospect. However, since meta-aramid has a high intramolecular hydrogen bond content, molecular chains are easily highly crosslinked by hydrogen bonds, and solubility in polar solvents is small. It is very difficult to prepare the common meta-aramid fiber into micro-nano fiber aerogel.
The prior method for preparing the meta-aramid nanofiber mainly comprises the steps of putting crude meta-aramid fiber into a solvent, soaking for 5 to 7 days, and thinning the diameter of the meta-aramid fiber to form the meta-aramid fiber.
The meta-aramid nanofiber obtained by the prior art is still short fiber, long nanofiber cannot be formed, subsequent processing for preparing the long nanofiber is complex and difficult, and practical application of the meta-aramid nanofiber is limited.
Disclosure of Invention
The present application aims to overcome or at least partially solve or alleviate the above-mentioned problems.
According to one aspect of the present application, there is provided a method for preparing an aramid micro-nanofiber aerogel material, comprising the steps of:
s1, preparing a spinnability solution:
and (3) at a preset temperature, placing halogen salt into a solvent, stirring until the halogen salt is uniformly dissolved, adding meta-aramid fiber, and stirring until the halogen salt is uniformly dissolved to obtain a spinnability solution.
S2, spinning and collecting meta-aramid micro-nano fibers:
spinning the spinnability solution into micro-nano fibers by using a centrifugal spinning method, wherein the micro-nano fibers are stacked and collected to obtain meta-aramid micro-nano fibers;
s3, removing impurities in the meta-aramid micro-nano fiber:
and carrying out ultrasonic cleaning on the collected meta-aramid micro-nano fibers, and then drying to obtain the aramid micro-nano fiber aerogel material.
The halogen salt is at least one selected from lithium chloride, calcium chloride, lithium bromide, sodium bromide, calcium bromide and potassium bromide.
The solvent is at least one selected from dimethylacetamide, dimethylformamide, dimethyl sulfoxide and N-methylpyrrolidone.
The mass ratio of meta-aramid to solvent to halogen salt is 1: 5-10:0.3-0.6.
The preset temperature is 50-80 ℃; the drying temperature is 100-150 ℃, the drying time is 20-40 minutes, and the ultrasonic cleaning time is 5-30 minutes.
The spinning and collecting meta-aramid micro-nano fiber comprises:
(1) Injecting the spinnability solution into a liquid storage tank, wherein the liquid storage tank is driven by a motor to rotate at a high speed, the rotating direction is not limited, the spinnability solution can rotate positively or reversely, and the spinnability solution is sprayed out from a needle arranged at the lower part of the liquid storage tank to form micro-nano fibers;
(2) And starting an air supply unit, blowing the micro-nano fibers to a collection unit by using the air supply unit, and stacking and collecting the obtained meta-aramid micro-nano fibers.
The air supply unit is arranged above the liquid storage tank; the device is used for providing air flow perpendicular to the direction of spraying spinnability solution, and the air flow provided by the air supply unit and the air flow generated by the rotation of the liquid storage tank can generate action resultant force obliquely downwards on the micro-nano fiber, wherein the included angle between the direction of the action resultant force and the horizontal direction is 30-45 degrees;
the rotation speed of the liquid storage tank is 2500-10000 revolutions per minute;
the air outlet speed of the air supply unit is 1-4 m/s.
The air humidity provided by the air supply unit is controlled to be 20% -60% RH; the temperature is 1-40 ℃.
The invention also provides a device for preparing the aramid micro-nano fiber aerogel material, which comprises an air supply unit, a spinning unit and a collecting unit which are arranged from top to bottom;
the air supply unit comprises a fan, a dehumidifier and an air box, wherein the dehumidifier is connected with a pipeline, the pipeline is arranged at the top end of the air box, the fan is arranged at the upper end of the interior of the air box, and the lower end of the air box is an open mouth;
the spinning unit is arranged below the air supply unit and comprises more than two liquid storage tanks, a motor is connected above each liquid storage tank, an air cover is arranged on the periphery of each liquid storage tank, the motor and the air cover are coaxially arranged, and the motor and the air cover are arranged on corresponding sliding rails;
the collecting unit is arranged below the spinning unit and comprises a rolling shaft, a conveying belt and a porous collecting plate, the porous collecting plate is arranged on the conveying belt and located below the air cover, and the rolling shaft is arranged at two ends of the conveying belt.
The air cover is placed in an inverted funnel shape, the fan blows dry air into the air cover vertically from right above, the diameter of an upper end opening of the air cover is smaller than that of a lower end opening, and the diameter of the upper end opening of the air cover is larger than that of the liquid storage tank in a rotating mode.
The spinning unit further comprises: a needle, a needle mounting tube and a can body fixing cover;
the needle head is detachably arranged on the needle head mounting tube;
the needle head mounting tube is in threaded connection with the liquid storage tank;
the tank body fixing cover is wrapped outside the liquid storage tank;
the needle passes through a needle hole preset in the tank body fixing cover and extends to the outside of the tank body fixing cover;
the inner ring of the liquid storage tank is in a regular polygon shape, and the installation position of the needle head installation tube corresponds to the position of the top point of the inner ring of the liquid storage tank.
According to the invention, the meta-aramid fiber is completely dissolved by using the mixed solution of the halogen salt and the solvent to form a solution with spinnability, and then the solution is spun into the ultra-long micro-nano fiber by using a centrifugal spinning method, and then the ultra-long micro-nano fiber is stacked to form the meta-aramid fiber micro-nano fiber aerogel. Compared with the existing electrostatic spinning method and air flow spinning method, the invention adopts the centrifugal spinning method, the highest feeding rate can reach 3072ml/h, and the invention has the advantage of high production efficiency, does not need supercritical drying or liquid nitrogen freeze drying, and has lower energy consumption.
In the spinning process, more factors affecting the spinnability of the solution, such as the temperature and humidity of the spinning environment, are considered, and in order to stabilize efficient production, the humidity and the temperature are controlled in the actual production process, and the temperature is preferably 25 ℃ at room temperature, so that the stability and the continuity of the prepared material in the production process are ensured.
The above, as well as additional objectives, advantages, and features of the present application will become apparent to those skilled in the art from the following detailed description of a specific embodiment of the present application when read in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the present application will be described in detail hereinafter by way of example and not by way of limitation with reference to the accompanying drawings. The same reference numbers will be used throughout the drawings to refer to the same or like parts or portions. It will be appreciated by those skilled in the art that the drawings are not necessarily drawn to scale. In the accompanying drawings:
FIG. 1 is a schematic structural view of an apparatus for preparing an aramid micro-nanofiber aerogel material according to one embodiment of the present application;
FIG. 2 is a partial schematic view of a spinning unit according to one embodiment of the present application;
FIG. 3 is a partial schematic view of a feed unit in connection with a spinning unit according to one embodiment of the present application;
FIG. 4 is a schematic structural view of a spinning unit according to one embodiment of the present application;
FIG. 5 is a scanning electron microscope image of meta-aramid micro-nanofiber before cleaning impurities;
fig. 6 is a scanning electron microscope image of meta-aramid micro-nanofiber aerogel obtained after cleaning, impurity removal and drying.
Detailed Description
Referring to fig. 1, an apparatus for preparing an aramid micro-nanofiber aerogel material includes an air supply unit 1, a spinning unit 2 and a collecting unit 3 arranged from top to bottom;
the air supply unit 1 comprises fans, a dehumidifier 10 and an air box 11, wherein the dehumidifier 10 is connected with a pipeline 12, the pipeline 12 is arranged at the top end of the air box 11, the fans are arranged at the upper end of the interior of the air box 11, the air outlet of each pipeline 12 is correspondingly provided with a fan, and the lower end of the air box 11 is open;
the spinning unit 2 is arranged below the air supply unit 1 and comprises more than two liquid storage tanks 20, a motor 21 is connected above each liquid storage tank 20, an air cover 22 is arranged on the periphery of each liquid storage tank 20, each motor 21, the air cover 22, an air outlet of the pipeline 12 and a fan are coaxially arranged, and the motor 21 and the air cover 22 are arranged on corresponding sliding rails 23;
the collecting unit 3 is arranged below the spinning unit 2 and comprises a roller 30, a conveyor belt 31 and a porous collecting plate 32, the porous collecting plate 32 is arranged on the conveyor belt, the porous collecting plate 32 is arranged below the air cover 22, and the roller 30 is arranged at two ends of the conveyor belt 31.
The invention can make the dry air flow all flow to the spinning area which needs to be kept dry by arranging the dehumidifier and the pipeline, and improves the use efficiency of the dry air flow. According to the invention, the air flow required to be dried flows perpendicular to the plane of the rotary liquid storage tank, so that the fibers are ensured to be uniformly landed on the porous collecting plate, and therefore, an air box is required to be arranged, and the influence of the air flow outside the air box on the drying air flow perpendicular to the plane is prevented; and simultaneously, moist air outside the air box is prevented from entering a spinning area to influence the dry spinning environment.
Referring to fig. 1 and 2, four slide rails 23 are arranged in parallel, two ends of the four slide rails 23 are arranged on a slide rail bracket 24, and the slide rails 23 can move on the slide rail bracket 24. The whole spinning unit can move on the sliding rails 23 according to the requirements, the motor 21 and the air cover 22 can move on the respective sliding rails 23 according to the requirements, the motor 21 moves back and forth on the middle two sliding rails 23, the air cover 22 moves on the sliding rails 23 on the two sides, the motor 21 drives the liquid storage tanks 20 to move back and forth, so that the distance between the front liquid storage tanks 20 and the rear liquid storage tanks 20 is adjusted, meanwhile, the motor 21 and the sliding rails 23 of the air cover 22 can also move on the sliding rail supports 24, so that the distance between the left liquid storage tank 20 and the right liquid storage tanks 20 is adjusted, and the liquid storage tanks are fixed through bolts after the position is determined. If the distance between adjacent reservoirs is too close, the spinnability solutions that have not been completely dried may become entangled together to form mucus, thereby ultimately affecting the structure and state of the micro-nanofiber material.
Preferably, the fan blows dry air vertically into the air hood from directly above, the upper end opening diameter of the air hood 11 being smaller than the diameter of the lower end opening, the upper end opening diameter of the air hood 11 being larger than the reservoir rotation diameter.
The invention sets the air cover into an inverted funnel shape with a small upper part and a large lower part, and prevents spun fibers from flowing upwards. According to the fluid dynamics principle, when the openings at the upper end and the lower end are consistent in size, the pressure is consistent, and when the air flow in the vertical direction and the air flow on the plane of the rotary liquid storage tank meet, local turbulence is generated, and part of fibers can flow upwards due to the local turbulence, so that the collection of the fibers is not facilitated. Meanwhile, the structure with small upper part and large lower part can ensure that the flow direction of the air in the plane direction of the rotary liquid storage tank is downward when reaching the air cover wall, so that the influence of turbulence is reduced.
Preferably, the upper end opening diameter of the air cap 11 is 30 to 60cm; the diameter of the opening at the lower end of the air cover 11 is 65-120 cm, the diameter of the opening at the lower end is 5-30cm larger than that of the opening at the upper end, the diameter of the opening at the upper end of the air cover 11 is 10-30cm larger than the rotating diameter of the liquid storage tank, the rotating radius of the liquid storage tank is the distance from the center of the liquid storage tank to the outermost end of the needle, and the rotating diameter of the liquid storage tank is 2 times the rotating radius of the liquid storage tank.
The invention uses the air cover to avoid the mutual influence between the air flow fields respectively formed by the spinning units. The fiber spun by each spinning unit falls on a porous collecting plate under the lower port of the air cover, and the width is consistent with the diameter of the lower port of the air cover, so that the width dimension of the fiber collection is controlled.
Referring to fig. 3, the feeding unit 4 can add a spinnability solution into the spinning unit 2, and the spinning unit 2 can spray the spinnability solution stored in the interior by using centrifugal force generated by rotation of itself, and finally continuously generate a filament-shaped micro-nanofiber material.
Specifically, the feeding unit 4 is mainly composed of a feed pipe 40, a feed pipe port 41, and a peristaltic pump. Peristaltic pumps are primarily used to pump the spinnable solution into the reservoir 20, and the feed tube 40 is primarily used to deliver the spinnable solution. The input rate of the spinnability solution can be controlled by the power parameters of the peristaltic pump. The spinnability solution is added to a peristaltic pump that pumps the spinnability solution into the feed tube 40, along the feed tube 40 to the feed port 41, and from the feed port 41 into the reservoir 20. Wherein the material guiding pipe orifice 41 is arranged inside the liquid storage tank 20 in a non-contact way. Since the liquid storage tank 20 is rotated at a high speed, the material guide nozzle 41 is fixed. Therefore, if the spinning unit 2 is in contact with the feed port 41, severe friction must be generated, which causes not only safety hazards but also noise. Since the material guiding pipe 41 and the liquid storage tank 20 are arranged in a non-contact way in the embodiment, potential safety hazards are greatly reduced, and the service lives of the material feeding unit 4 and the liquid storage tank 20 are prolonged.
The product structure can control the feeding rate, so that the technical effect that the operation device 20 can produce continuous micro-nano fiber materials is ensured.
Optionally, the spinning unit 2 comprises: the needle 24, the needle mounting tube 25, the liquid storage tank 20, the tank body fixing cover 26, the sealing ring and the sealing gasket 27, wherein the needle 24 is detachably mounted on the needle mounting tube 25; the needle mounting tube 25 is in threaded connection with the reservoir 20; the sealing ring is arranged at the threaded connection part of the needle mounting tube 25 and the liquid storage tank 20; the tank body fixing cover 26 is wrapped outside the liquid storage tank 20; a sealing gasket 27 is arranged between the tank body fixing cover 26 and the liquid storage tank 20; and needle 24 passes through a needle hole preset in canister retainer cover 26 and extends to the outside of canister retainer cover 26.
Specifically, fig. 4 is a schematic view of a spinning unit 2 according to one embodiment of the present application. Referring to fig. 4, the spinning unit 2 mainly includes a needle 24, a needle mounting tube 25, a liquid storage tank 20 and a tank fixing cover 26, a seal ring, and a seal gasket 27. The corresponding number of needle mounting tubes 25 are detachably mounted in the threaded holes of the outer ring of the liquid storage tank 20, and sealing rings are placed at the bottoms of the threaded holes, so that the tightness of the spinnability solution pipeline is ensured, and liquid leakage is prevented. A needle 24 is detachably mounted on each needle mounting tube 25. The canister retainer cover 26 encloses the reservoir 20 and a plurality of needle apertures are also provided in the canister retainer cover 26 through which the needles 24 extend to the exterior of the canister retainer cover 26. Wherein, because the tank body fixing cover 26 wraps the liquid storage tank 20, the needle head mounting tube 25 and a part of the needle head 24, only the tip of the needle head 24 is exposed outside the tank body fixing cover 26, and therefore, the needle head 24 and the needle head mounting tube 25 are not separated in the process of rotating the spinning unit 2. The sealing gasket 27 is arranged between the tank body fixing cover 26 and the liquid storage tank 20, so that the tightness of a liquid storage tank formed by the joint of the tank body fixing cover 26 and the liquid storage tank 20 is ensured. The spinnability solution is stored in the liquid storage tank 20, and as the spinnability solution is continuously sprayed to the outside, the spinnability solution is continuously fed into the liquid storage tank 20 through the feeding unit 4, and the height of the spinnability solution in the liquid storage tank 20 is always kept constant.
During rotation of the liquid storage tank 20 driven by the motor 21, the spinnable solution stored in the liquid storage tank 20 may flow to the needle 24 through the needle mounting tube 25 by centrifugal force and be sprayed to the outside of the tank fixing cover 26 through the needle 24. The spinnability solution sprayed to the outside of the tank holding cover 26 becomes a filiform micro-nano fiber material gradually under the set humidity and temperature environment.
In addition, since the needle 24, the needle mounting tube 25 and the liquid storage tank 20 are designed in a three-phase separated structure, the needle 24 and the needle mounting tube 25 can be detached from the liquid storage tank 20 at any time, and the needle 24 can also be detached from the needle mounting tube 25 at any time. Thereby, the technical effects of facilitating cleaning of the needle mounting tube 25 and the liquid storage tank 20 and ensuring multiple uses of the needle mounting tube 25 and the liquid storage tank 20 are achieved.
Through the product structure, the technical effect that the needle 24 and the needle mounting tube 25 can not fall off can be guaranteed, and the spinning unit 2 can work normally is guaranteed.
Alternatively, the inner circumference of the liquid reservoir 20 is polygonal in shape, and the mounting position of the needle mounting tube 25 corresponds to the position of the vertex of the inner circumference of the liquid reservoir 20.
Referring to fig. 4, the liquid storage tank 20 is divided into an inner ring and an outer ring, and the shape of the inner ring of the liquid storage tank 20 is a regular polygon. The liquid storage tank 20 is provided with a conductive threaded mounting hole, and the needle mounting tube 25 can be mounted on the outer ring of the liquid storage tank 20 through the threaded mounting hole. Wherein the mounting position of the needle mounting tube 25 corresponds to the position of the vertex of the inner ring of the liquid reservoir 20. Since the inner ring of the reservoir 20 is polygonal, the flow direction of the spinnability solution in the reservoir 20 is not normal, but is directed toward the apex, i.e., the needle mounting tube 25 corresponding to the apex. Therefore, during the spinning process of the filiform micro-nano fiber material, no spinnability solution is deposited on the inner wall of the liquid storage tank 20 and forms gel, and finally the thread mounting holes are blocked, so that the spinning unit 2 cannot work normally.
Through the product structure, the technical effects of preventing the spinnability solution from depositing on the inner wall of the liquid storage tank 20 and forming gel and further ensuring the normal operation of the spinning unit 2 are achieved.
The invention is further illustrated by the following specific examples:
example 1
The method for preparing the aramid micro-nanofiber aerogel material by adopting the device comprises the following steps:
s1, preparing a spinnability solution:
and (3) at the preset temperature of 75 ℃, putting halogen salt lithium chloride into solvent dimethylacetamide, stirring until the halogen salt lithium chloride is uniformly dissolved, adding meta-aramid fiber, and stirring until the meta-aramid fiber is uniformly dissolved to obtain spinnability solution. The mass ratio of meta-aramid to solvent to halogen salt is 1:7.5:0.45.
S2, spinning and collecting meta-aramid micro-nano fibers:
spinning the spinnability solution into micro-nano fibers by using a centrifugal spinning method, wherein the meta-aramid micro-nano fibers obtained by stacking and collecting the micro-nano fibers concretely comprise the following steps:
(1) Injecting the spinnability solution into a plurality of liquid storage tanks, rotating the liquid storage tanks at high speed under the drive of a motor, controlling the rotating speed to 4000 revolutions per minute, and spraying the spinnability solution from a needle head arranged at the lower part of the liquid storage tanks to form micro-nano fibers;
(2) Opening an air supply unit above the liquid storage tank, wherein the air supply speed is 3m/s, the air supply unit provides air flow perpendicular to the direction of spraying spinnability solution, the air humidity provided by the air supply unit is controlled at 40% RH, the temperature is controlled at 25 ℃, the air flow provided by the air supply unit and the air flow generated by the rotation of the liquid storage tank can generate inclined downward action resultant force on the micro-nano fibers, the included angle between the direction of the action resultant force and the horizontal direction is 30-45 degrees, and the micro-nano fibers fall onto a porous collecting plate under a lower port of an air cover through the action resultant force. The air fluid then flows out of the collection unit through the through holes in the porous collection plate. Wherein the air flow speed provided by the air supply unit is 1-3 m/s. The interval between adjacent liquid storage tanks is adjusted on the slide rail, and then the control of the wind speed is combined to obtain a micro-nano fiber material with uniform whole thickness;
s3, removing impurities in the meta-aramid micro-nano fiber.
And carrying out ultrasonic cleaning on the collected meta-aramid micro-nanofiber for 10 minutes to remove impurities, and drying at 120 ℃ for 30 minutes to obtain the aramid micro-nanofiber aerogel material.
Referring to fig. 5, the meta-aramid micro-nanofiber obtained by collection has a large amount of punctiform substances independent of the fiber before cleaning, and the punctiform substances are lithium chloride particles with the particle diameter of about 200nm and conform to the particle diameter of the dried lithium chloride particles. Meanwhile, before drying, the phenomenon of mutual adhesion among fibers (presumably the result that dimethylacetamide DMAc exists on the surfaces of the fibers) occurs, and a plurality of parallel fibers are mutually adhered into bundles, so that the fibers are densely and more messy in arrangement, and a plurality of fiber bundles are entangled in a staggered manner, and the porosity is low.
Referring to fig. 6, as can be seen from a scanning electron microscope image of the meta-aramid micro-nanofiber aerogel obtained after the cleaning and the impurity removal and the drying, after the cleaning, the lithium chloride particles can be found to disappear, the fibers are changed from multi-heeled bundles into single independent distribution, and the adjacent fibers do not have parallel adhesion tendency, but form a loose grid staggered structure. At the same time, because of the relative independence between the fibers, finer fibers are identified, the structure is loose, the porosity is high, and the existence of very fine fiber filaments with a diameter of about 300-500nm can be found.
Example 2
S1, preparing a spinnability solution:
at the preset temperature of 50 ℃, the halogen salt calcium chloride is put into the solvents of dimethylacetamide and N-methylpyrrolidone, stirred until the halogen salt calcium chloride is uniformly dissolved, then meta-aramid fiber is added, and stirred until the halogen salt calcium chloride is uniformly dissolved, thus obtaining spinnability solution. The mass ratio of meta-aramid to solvent to halogen salt is 1:5:0.6. The mass ratio of the dimethylacetamide to the N-methylpyrrolidone is 2:1.
s2, spinning and collecting meta-aramid micro-nano fibers:
spinning the spinnability solution into micro-nano fibers by using a centrifugal spinning method, wherein the micro-nano fibers are stacked and collected to obtain meta-aramid micro-nano fibers;
(1) Injecting the spinnability solution into a liquid storage tank, rotating the liquid storage tank at a high speed under the drive of a motor, controlling the rotating speed to 2500 rpm, and spraying the spinnability solution from a needle head arranged at the lower part of the liquid storage tank to form micro-nano fibers;
(2) Starting an air supply unit, controlling the air humidity provided by the air supply unit to be 60% RH and the temperature to be 24 ℃, blowing the micro-nano fibers to a collecting unit at the lower port of an air cover by using the air supply unit, stacking and collecting the obtained meta-aramid micro-nano fibers.
S3, removing impurities in the meta-aramid micro-nano fiber.
And carrying out ultrasonic cleaning on the collected meta-aramid micro-nanofiber for 30 minutes to remove impurities, and drying at 150 ℃ for 20 minutes to obtain the aramid micro-nanofiber aerogel material.
Example 3
S1, preparing a spinnability solution:
and (3) at the preset temperature of 80 ℃, adding sodium bromide halide into N-methylpyrrolidone, stirring until the sodium bromide halide is uniformly dissolved, adding meta-aramid fiber, and stirring until the sodium bromide halide is uniformly dissolved to obtain spinnability solution. The mass ratio of meta-aramid to solvent to halogen salt is 1:10:0.3.
S2, spinning and collecting meta-aramid micro-nano fibers:
spinning the spinnability solution into micro-nano fibers by using a centrifugal spinning method, wherein the micro-nano fibers are stacked and collected to obtain meta-aramid micro-nano fibers;
(1) Injecting the spinnability solution into a liquid storage tank, rotating the liquid storage tank at a high speed under the drive of a motor, controlling the rotating speed to 10000 revolutions per minute, and spraying the spinnability solution from a needle arranged at the lower part of the liquid storage tank to form micro-nano fibers;
(2) Starting an air supply unit, controlling the air humidity provided by the air supply unit to be 20% RH and the temperature to be 26 ℃, blowing the micro-nano fibers to a collecting unit at the lower port of an air cover by using the air supply unit, stacking and collecting the obtained meta-aramid micro-nano fibers.
S3, removing impurities in the meta-aramid micro-nano fiber.
And carrying out ultrasonic cleaning on the collected meta-aramid micro-nanofiber for 5 minutes to remove impurities, and drying at 100 ℃ for 40 minutes to obtain the aramid micro-nanofiber aerogel material.
It is noted that unless otherwise indicated, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this application belongs.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The foregoing is merely a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present application should be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (10)
1. The preparation method of the aramid micro-nanofiber aerogel material is characterized by comprising the following steps of:
s1, preparing a spinnability solution:
and (3) at a preset temperature, placing halogen salt into a solvent, stirring until the halogen salt is uniformly dissolved, adding meta-aramid fiber, and stirring until the halogen salt is uniformly dissolved to obtain a spinnability solution.
S2, spinning and collecting meta-aramid micro-nano fibers:
spinning the spinnability solution into micro-nano fibers by using a centrifugal spinning method, wherein the micro-nano fibers are stacked and collected to obtain meta-aramid micro-nano fibers;
s3, removing impurities in the meta-aramid micro-nano fiber:
and carrying out ultrasonic cleaning on the collected meta-aramid micro-nano fibers, and then drying to obtain the aramid micro-nano fiber aerogel material.
2. The method according to claim 1, wherein the halogen salt is at least one selected from the group consisting of lithium chloride, calcium chloride, lithium bromide, sodium bromide, calcium bromide and potassium bromide; or/and the solvent is at least one selected from dimethylacetamide, dimethylformamide, dimethyl sulfoxide and N-methylpyrrolidone.
3. The preparation method according to claim 2, wherein the mass ratio of meta-aramid, solvent and halogen salt is 1: 5-10:0.3-0.6.
4. The method according to claim 3, wherein the preset temperature is 50 to 80 ℃; the drying temperature is 100-150 ℃, and the drying time is 20-40 minutes; the ultrasonic cleaning time is 5-30 minutes.
5. The method of any one of claims 1-4, wherein spinning and collecting meta-aramid micro-nanofibers comprises: (1) Injecting the spinnability solution into a liquid storage tank, rotating the liquid storage tank at a high speed under the drive of a motor, and spraying the spinnability solution from a needle arranged at the lower part of the liquid storage tank to form micro-nano fibers;
(2) And opening the air supply unit, enabling the micro-nano fibers to float down to the collecting unit through the action and resultant force generated by the air supply unit and the rotary liquid storage tank, and stacking and collecting the obtained meta-aramid micro-nano fibers.
6. The method according to claim 5, wherein the air supply unit is disposed above the liquid storage tank; the device is used for providing air flow perpendicular to the direction of spraying spinnability solution, and the air flow provided by the air supply unit and the air flow generated by the rotation of the liquid storage tank can generate action resultant force obliquely downwards on the micro-nano fiber, wherein the included angle between the direction of the action resultant force and the horizontal direction is 30-45 degrees;
the rotation speed of the liquid storage tank is 2500-10000 revolutions per minute;
the air outlet speed of the air supply unit is 1-4 m/s.
7. The preparation method according to claim 5, wherein the air humidity provided by the air supply unit is controlled to be 20% -60% RH, and the temperature is 1-40 ℃.
8. An apparatus for use in the production process according to any one of claims 1 to 7, comprising a wind supply unit, a spinning unit and a collecting unit arranged from top to bottom;
the air supply unit comprises a fan, a dehumidifier and an air box, wherein the dehumidifier is connected with a pipeline, the pipeline is arranged at the top end of the air box, the fan is arranged at the upper end of the interior of the air box, and the lower end of the air box is an open mouth;
the spinning unit is arranged below the air supply unit and comprises more than two liquid storage tanks, a motor is connected above each liquid storage tank, an air cover is arranged on the periphery of each liquid storage tank, the motor and the air cover are coaxially arranged, and the motor and the air cover are arranged on corresponding sliding rails;
the collecting unit is arranged below the spinning unit and comprises a rolling shaft, a conveying belt and a porous collecting plate, the porous collecting plate is arranged on the conveying belt and located below the air cover, and the rolling shaft is arranged at two ends of the conveying belt.
9. The apparatus of claim 8, wherein the air hood is placed in an inverted funnel shape, the fan blows dry air vertically into the air hood from directly above, an upper end opening diameter of the air hood is smaller than a lower end opening diameter, and an upper end opening diameter of the air hood is larger than a rotation diameter of the liquid storage tank.
10. The apparatus according to claim 9 or 8, wherein the spinning unit further comprises: a needle, a needle mounting tube and a can body fixing cover;
the needle head is detachably arranged on the needle head mounting tube;
the needle head mounting tube is in threaded connection with the liquid storage tank;
the tank body fixing cover is wrapped outside the liquid storage tank;
the needle passes through a needle hole preset in the tank body fixing cover and extends to the outside of the tank body fixing cover;
the inner ring of the liquid storage tank is in a regular polygon shape, and the installation position of the needle head installation tube corresponds to the position of the top point of the inner ring of the liquid storage tank.
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