CN110592687B - Fiber spinning method - Google Patents
Fiber spinning method Download PDFInfo
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- CN110592687B CN110592687B CN201910912891.0A CN201910912891A CN110592687B CN 110592687 B CN110592687 B CN 110592687B CN 201910912891 A CN201910912891 A CN 201910912891A CN 110592687 B CN110592687 B CN 110592687B
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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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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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
- 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
- D01D10/02—Heat treatment
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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
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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
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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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
- D01F1/10—Other agents for modifying properties
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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
- D01F6/54—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 polymers of unsaturated nitriles
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a fiber spinning method, which belongs to the field of fibers and comprises the following steps: 1) dissolving polyacrylonitrile polymer in a solvent to form a second spinning solution; 2) mixing and stirring the inorganic particles and the second spinning solution uniformly, and modifying the surface of the inorganic particles to form a micelle with dots in the spinning solution so as to form the first spinning solution; 3) conveying the first spinning solution into a first liquid conveying channel, conveying the second spinning solution into a second liquid conveying channel, and applying an electric field perpendicular to the flowing direction of the first spinning solution to the first liquid conveying channel to enable charged micelles in the first spinning solution to gather at the edge of the first liquid conveying channel; 4) mixing a first spinning solution in a first liquid conveying channel and a second spinning solution in a second liquid conveying channel at a nozzle opening, wherein a charged micelle in the first spinning solution is positioned in the middle of the two spinning solutions after the two spinning solutions are mixed, and the mixed spinning solutions are sprayed out from a nozzle to form a nascent fiber; 5) and carrying out post-treatment on the nascent fiber.
Description
Technical Field
The present invention relates to the field of fiber spinning.
Background
Polyacrylonitrile or acrylonitrile copolymer with acrylonitrile content greater than 85 wt%. The second monomer is usually nonionic monomer, such as methyl acrylate, methyl methacrylate, etc., and the third monomer is ionic monomer, such as sodium propylene sulfonate and 2-methylene-1, 4-succinic acid, etc.
The fiber method comprises dry spinning and wet spinning, and in some spinning, the spinning solution is added with inorganic material for reinforcement, but the inorganic material in the inorganic reinforced fiber is uniformly dispersed in the fiber body, so that the rigidity of the inorganic material is weakened, and the reinforcement performance is limited.
Disclosure of Invention
The invention aims to solve the problems in the background art and discloses a fiber spinning method, which comprises the following steps:
1) dissolving polyacrylonitrile polymer in a solvent to form a second spinning solution;
2) mixing and stirring the inorganic particles with the metal layer covered on the surface and the second spinning solution uniformly, and modifying the surface of the inorganic particles to form charged micelles in the spinning solution so as to form the first spinning solution;
3) conveying the first spinning solution into a first liquid conveying channel, conveying the second spinning solution into a second liquid conveying channel, and applying an electric field perpendicular to the flowing direction of the first spinning solution to the first liquid conveying channel to enable charged micelles in the first spinning solution to gather at the edge of the first liquid conveying channel;
4) mixing a first spinning solution in a first liquid conveying channel and a second spinning solution in a second liquid conveying channel at a nozzle opening, wherein a charged micelle in the first spinning solution is positioned in the middle of the two spinning solutions after the two spinning solutions are mixed, and the mixed spinning solutions are sprayed out from a nozzle to form a nascent fiber;
5) and carrying out post-treatment on the nascent fiber.
As an improvement, the preparation method of the inorganic particles comprises the following steps: firstly, forming a suspension gas by inorganic nano-particles and inert gas, and then introducing the suspension gas into a vacuum melting furnace, wherein the vacuum melting furnace contains iron vapor, and the iron vapor is condensed and covered on the surfaces of the inorganic nano-particles when meeting the inorganic nano-particles and is precipitated.
As an improvement, the solvent in the first step adopts dimethylacetamide, and the molecular weight of polyacrylonitrile is 6000-10000.
As an improvement, the flow rates of the first spinning solution and the second spinning solution are the same or have an error of not more than 10%.
As an improvement, the inorganic particles are silicon nitride or silicon carbide, and the particle size of the inorganic particles is 50-500 nm.
As an improvement, the first spinning solution is prepared as follows:
taking 100 parts of second spinning solution, mixing and stirring 1-2 parts of sodium carboxymethylcellulose and the second spinning solution to fully mix the sodium carboxymethylcellulose and the second spinning solution; and secondly, adding 5-10 parts of inorganic particles with metal covered on the surfaces into the second spinning solution, stirring by using ultrasonic waves, carrying out surface modification on the nanoparticles by using sodium carboxymethyl cellulose to form negative electricity on the metal on the surfaces of the nanoparticles, and uniformly dispersing the negatively charged nanoparticles in the spinning solution to further form a first spinning solution.
As an improvement, the first spinning solution passes through an electric field in the spinning process, the direction of the electric field is perpendicular to the flowing direction of the first spinning solution, under the action of the electric field, the charged nanoparticles of the first spinning solution move towards one side of the first liquid conveying channel and are gathered at one side, and the first spinning solution and the second spinning solution with the gathered nanoparticles are mixed and enable the nanoparticles to be gathered in the middle of the mixed spinning solution.
As a refinement, the post-treatment comprises heat treatment and a drawing operation.
As an improvement, the heat treatment comprises passing through a first temperature zone and a second temperature zone, wherein the temperature of the first temperature zone is 1-5 ℃ higher than the glass transition temperature of polyacrylonitrile, and the temperature of the second temperature zone is 5-8 ℃ lower than the melting temperature.
Drawings
FIG. 1 is a schematic view of a nozzle;
FIG. 2 is a cross-sectional view taken along line A-A1 of FIG. 1
FIG. 3 is a schematic cross-sectional view of a composite fiber;
FIG. 4 is a schematic cross-sectional view of a composite fiber;
FIG. 5 is a schematic illustration of components of a filter media;
FIG. 6 is a drawing of a process for spinning and staple fiber preparation
The labels in the figure are: 1-a first liquid conveying channel, 11-a first liquid inlet, 2-a second liquid conveying channel, 21-a second liquid inlet, 3-a nozzle opening, 4-inorganic charged particles, 5-a first electrode plate, 6-a second electrode plate, 7-a metering pump, 8-a polyacrylonitrile fiber matrix, 9-an inorganic belt, 10-a first fiber net, 11-a second fiber net and 12-short fibers.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
Example 1: this example discloses a composite fiber, as shown in fig. 3, which comprises a polyacrylonitrile fiber matrix 8 and an inorganic band 9, fig. 3 is an enlarged view of the fiber viewed from the side, and it can be seen that an inorganic band 9 is formed in the middle of the fiber, the inorganic band 9 is composed of inorganic nanoparticles, the inorganic nanoparticles are aggregated with each other, and the surface of the inorganic nanoparticles is covered with metal. The inorganic tape extends along the length of the composite fiber in the radial direction of the composite fiber, and as shown in fig. 4, the width of the inorganic tape is the radial length of the composite fiber and is located at the center of the radial cross section of the fiber.
In a preferred embodiment, the inorganic nanoparticles are silicon carbide or silicon nitride, the particle size is 50-200 nm, the silicon carbide and silicon nitride have high rigidity and low thermal expansion coefficient, and can provide high strength for the fibers, the particle size enables the silicon carbide or silicon nitride to be densely gathered, the strength of the fibers is improved, and the strength of the fibers is reduced if the inorganic particles are too loose.
In a preferred embodiment, the metal coated on the surface of the inorganic nanoparticles is a mixture of one or more of iron, aluminum, copper and silver, especially iron or aluminum, so that the cost is low and the surface is easy to form negative electricity. The mass content of the composite fiber inorganic tape of the present example is 1% to 5%, preferably 5%.
The embodiment also discloses a short fiber prepared from the composite fiber, the length of the short fiber is 5 mm-50 mm, the diameter of the short fiber is 5-20 μm, and the short fiber is prepared by cutting or stretch breaking the composite fiber.
The invention also discloses a filter material, as shown in fig. 5, which comprises a first fiber net 10 and a second fiber net 11, wherein the first fiber net 10 and the second fiber net 11 are respectively doped with the short fibers 12 of the invention, the first fiber net and the second fiber net are bonded in a bonding way, as shown in fig. 5, the short fibers in the first fiber net and the short fibers in the second fiber net are mutually entangled, the first fiber net and the second fiber net have good fluffiness and connection performance, the first fiber net and the second fiber net both adopt polyimide fibers, and the density of the first fiber net and the second fiber net is 30-200g/M2Compared with the traditional fiber, the short fiber of the invention has the advantages of strengthening inorganic belts in the short fiber of the inventionThe short fibers are not easy to break when being wound, and are not easy to separate, so that the short fibers can enhance the bonding strength between the first fiber net and the second fiber net and are not easy to tear, and the short fibers have certain rigidity, so that the short fibers can play a role of a framework in the first fiber net and the second fiber net, the fluffiness of the first fiber net and the second fiber net is improved, and the filtering effect is improved.
The composite fiber and the filter material thereof prepared by the invention have higher high temperature resistance, and the inorganic belt in the middle of the fiber plays a role of a framework, so that the surface part of the fiber begins to melt at higher temperature, such as approaching the melting temperature, but the middle inorganic belt can ensure that the composite fiber and the filter material keep enough rigidity and can exert performance.
The short fibers in the filter material prepared by the method have the function similar to that of a thread gluing, and due to the rigidity of the short fibers, the first fiber net and the second fiber net can be firmly attached without introducing new substances such as glue and the like, so that the problem that the glue blocks gaps to influence the filtration and the air permeability is solved.
Example 2: as shown in fig. 6, this example discloses a spinning method of the above composite fiber, in which the fiber is spun to have a layer of inorganic nano-ribbon in the middle, the inorganic nano-material is gathered in the middle of the fiber to form a reinforced layer, and the outer layer of the fiber does not contain inorganic material, so that the fiber has strong strength and maintains the softness of the fiber. Specifically, the spinning method of the fiber of the present invention is as follows:
1) dissolving polyacrylonitrile polymer with molecular weight of 6000-1000 in a dimethylacetamide solvent to form a second spinning solution, wherein the concentration of the second spinning solution is 30-40%;
2) preparing inorganic nano particles. The preparation method of the inorganic particles comprises the following steps: firstly, forming a suspension gas by inorganic nano-particles and inert gas, then introducing the suspension gas into a vacuum furnace, wherein the vacuum furnace contains iron vapor, the iron vapor is condensed and covered on the surfaces of the inorganic nano-particles when meeting the inorganic nano-particles and is precipitated, and the precipitated mixture also comprises part of acceptable impurities, such as iron nano-particles and the like,
3) taking 100 parts of second spinning solution, mixing and stirring 1-2 parts of sodium carboxymethylcellulose and the second spinning solution to fully mix the sodium carboxymethylcellulose and the second spinning solution; secondly, adding 5-10 parts of precipitated inorganic particles into the second spinning solution, stirring by using ultrasonic waves, carrying out surface modification on the nanoparticles by using sodium carboxymethyl cellulose to form negative electricity on the surface metal of the nanoparticles, and uniformly dispersing the negatively charged nanoparticles in the spinning solution to further form a first spinning solution;
4) conveying the first spinning solution into a first liquid conveying channel, conveying the second spinning solution into a second liquid conveying channel, applying an electric field perpendicular to the flowing direction of the first spinning solution to the first liquid conveying channel to enable charged micelles in the first spinning solution to gather at the edge of the first liquid conveying channel, and controlling the flow rates of the first spinning solution and the second spinning solution to enable the flow rates of the first spinning solution and the second spinning solution to be the same or not more than 10% of error;
4) mixing a first spinning solution in a first liquid conveying channel and a second spinning solution in a second liquid conveying channel at a nozzle opening, wherein a charged micelle in the first spinning solution is positioned in the middle of the two spinning solutions after the two spinning solutions are mixed, and the mixed spinning solutions are sprayed out from a nozzle to form a nascent fiber;
5) carrying out post-treatment on the nascent fiber, and enabling the nascent fiber to pass through a first temperature area and a second temperature area, wherein the temperature of the first temperature area is 1-5 ℃ higher than the glass transition temperature of polyacrylonitrile, and the temperature of the second temperature area is 5-8 ℃ lower than the melting temperature; and then performing conventional traction and the like.
Besides the surface modification of step 3, the nanoparticles may also be surface modified by other conventional surfactants.
The first spinning solution described in this embodiment passes through an electric field in the spinning process, the direction of the electric field is perpendicular to the flowing direction of the first spinning solution, and under the action of the electric field, the charged nanoparticles of the first spinning solution move towards one side of the first liquid delivery channel and are collected at one side, as shown in fig. 1, the first spinning solution and the second spinning solution in which the nanoparticles are collected are mixed, and the nanoparticles are collected at the middle of the mixed spinning solution. As shown in fig. 2, which is a cross-sectional view of a-a1 observed, it can be seen that inorganic nanobelts are gathered in the middle of the dope in the nozzle opening after passing through the electric field and mixing with the second dope, so that the strength of the fiber is improved while maintaining the fiber flexibility. The invention can be used for preparing filter materials and reinforcing short fibers used between filter material layers.
The properties of the modified fiber prepared as described above are as follows:
example 3: the present embodiment discloses a spinning nozzle and a spinning apparatus for spinning the above composite fiber, as shown in fig. 1, the spinning nozzle includes:
a first liquid delivery passage 1 for delivering a first spinning solution to a nozzle opening 3, the first spinning solution having inorganic charged particles 4 dispersed therein, the inorganic charged particles being inorganic nanoparticles,
a second liquid delivery passage 2 which delivers the second spinning liquid to the nozzle opening 3;
a nozzle opening 3 for collecting the spinning solutions collected from the first and second liquid supply paths, respectively, and performing discharge spinning;
be equipped with the electric field of the first spinning liquid flow direction of perpendicular to on the first infusion way, the electric field can apply in first infusion way 1 and make inorganic charged particle 4 in the first infusion way gather towards the edge of first infusion way to make inorganic charged particle be located the centre of nozzle opening after the first spinning liquid in first infusion way and the second spinning liquid in second infusion way mix, and then make and be equipped with inorganic particle area in the middle of nozzle opening spun cellosilk, wherein the size and the length of electric field according to spinning needs automatically regulated with can be in first infusion way 1 with the edge that inorganic charged particle removed first infusion way 1 can.
In order to apply an electric field to the first infusion channel, as shown in fig. 1, a first electrode plate 5 and a second electrode plate 6 are provided on the spinning nozzle, and the first electrode plate and the second electrode plate are respectively connected with a positive electrode and a negative electrode of a power supply to form the electric field between the first electrode plate and the second electrode plate. The widths of the two electrode plates are equal to or larger than the widths of the first infusion channel and the second infusion channel so as to enable the charged particles in the first infusion channel to be in an electric field. The electrode plates can be made of the existing common materials such as iron, copper, aluminum and the like, and the thickness is set according to the convention requirement.
In a preferred embodiment, as shown in fig. 1, the first electrode sheet 5 is located at the outer layer of the first infusion channel, and the second electrode sheet is located at the outer side of the second infusion channel. In other embodiments, the two motor blades are only positioned on two sides of the first infusion channel.
As shown in fig. 1, the sectional area of the nozzle opening from the mixing point of the first spinning solution and the second spinning solution (the plane a-a1 in fig. 1) to the nozzle opening (the plane B-B1 in the figure) of the nozzle opening is reduced in sequence, and the O-electricity in the figure smoothly transitions the mixing point of the first spinning solution and the second spinning solution, and in a more preferred embodiment, the second liquid feeding channel smoothly transitions to the O-point, so that the first spinning solution and the second spinning solution can be smoothly mixed.
In spinning, the flow rates of the first and second spinning solutions need to be the same or nearly the same, so in a preferred embodiment, the first and second feed lines are provided with metering pumps 7 for controlling the flow rate of the second spinning solution, and the metering pumps 7 can be controlled to control the liquid flows through the first and second feed lines.
As shown in figure 1, a first liquid inlet 11 is arranged on the first liquid conveying channel, a second liquid inlet 21 is arranged on the second liquid conveying channel, a first spinning solution flows into the first liquid inlet, and a second spinning solution flows into the second liquid inlet.
The invention also discloses spinning equipment, which comprises a spinning equipment body and the fiber spinning nozzle, wherein the spinning equipment body is used for conveying spinning solution to the fiber spinning nozzle, and the spinning equipment body is conventional technology and not shown in the figure.
Claims (5)
1. A fiber spinning method is characterized by comprising the following steps:
1) dissolving polyacrylonitrile polymer in dimethylacetamide to form a second spinning solution;
2) mixing and stirring the inorganic nano-particles with the surface covered with the metal layer and the second spinning solution uniformly, modifying the surface of the inorganic nano-particles to form charged micelles in the spinning solution so as to form the first spinning solution,
3) conveying a first spinning solution into a first liquid conveying channel, and conveying a second spinning solution into a second liquid conveying channel, wherein the flow rates of the first spinning solution and the second spinning solution are the same or have an error of not more than 10%;
applying an electric field perpendicular to the flowing direction of the first spinning solution to the first liquid conveying channel to enable charged micelles in the first spinning solution to gather at the edge of the first liquid conveying channel;
4) mixing a first spinning solution in a first liquid conveying channel and a second spinning solution in a second liquid conveying channel at a nozzle opening, wherein a charged micelle in the first spinning solution is positioned in the middle of the two spinning solutions after the two spinning solutions are mixed, and the mixed spinning solutions are sprayed out from a nozzle to form a nascent fiber;
5) post-treating the nascent fiber;
the preparation method of the inorganic nano-particles with the metal layers covered on the surfaces comprises the following steps: firstly, forming suspended gas by inorganic nano-particle silicon nitride or silicon carbide and inert gas, and then introducing the suspended gas into a vacuum melting furnace, wherein the vacuum melting furnace contains iron vapor, and the iron vapor is condensed and covered on the surface of the inorganic nano-particle when meeting the inorganic nano-particle and is precipitated;
the first spinning solution was prepared as follows:
taking 100 parts of second spinning solution, mixing and stirring 1-2 parts of sodium carboxymethylcellulose and the second spinning solution to fully mix the sodium carboxymethylcellulose and the second spinning solution; secondly, adding 5-10 parts of inorganic nano particles with metal layers covered on the surfaces into the second spinning solution, stirring by using ultrasonic waves, carrying out surface modification on the inorganic nano particles by using sodium carboxymethyl cellulose to form negative electricity on the surface metal of the inorganic nano particles, and uniformly dispersing the inorganic nano particles with the negative electricity in the spinning solution to further form a first spinning solution;
the first spinning solution passes through an electric field in the spinning process, the direction of the electric field is perpendicular to the flowing direction of the first spinning solution, under the action of the electric field, charged inorganic nanoparticles of the first spinning solution move towards one side of the first liquid conveying channel and are gathered at one side, and the first spinning solution and the second spinning solution, on which the inorganic nanoparticles are gathered, are mixed to enable the inorganic nanoparticles to be gathered at the middle of the mixed spinning solution.
2. The method for spinning a fiber according to claim 1, wherein the molecular weight of polyacrylonitrile is 6000-10000.
3. The method of spinning a fiber according to claim 2, wherein the inorganic nanoparticles have a particle size of 50 to 500 nm.
4. A method for spinning fibres as claimed in claim 3 in which said post-treatment includes heat treatment and drawing operations.
5. A method for spinning fibers as claimed in claim 4, wherein said heat treatment comprises passing through a first temperature zone and a second temperature zone, the first temperature zone being at a temperature 1 ℃ to 5 ℃ above the glass transition temperature of polyacrylonitrile and the second temperature zone being at a temperature 5 ℃ to 8 ℃ below the melting temperature.
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| CN201910912891.0A CN110592687B (en) | 2019-09-25 | 2019-09-25 | Fiber spinning method |
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