CN117779220A - Continuous fiber preparation method and device - Google Patents
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- CN117779220A CN117779220A CN202311854040.8A CN202311854040A CN117779220A CN 117779220 A CN117779220 A CN 117779220A CN 202311854040 A CN202311854040 A CN 202311854040A CN 117779220 A CN117779220 A CN 117779220A
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Abstract
The present disclosure provides a continuous fiber preparation method comprising the following steps. And providing a reaction die, wherein the reaction die comprises a first channel, a second channel and a third channel, and the first channel, the second channel and the third channel are mutually communicated at the crossing position to form a Y-shaped channel. And injecting the first solution containing the positive electricity material and the second solution containing the negative electricity material into the reaction mould from the inlet of the first channel and the inlet of the second channel in a one-to-one correspondence manner respectively, and converging at the crossing position, so that the positive electricity material and the negative electricity material undergo electrostatic complexing reaction to obtain fibers, and the fibers flow out from the outlet of the third channel. The fibers are drawn at the outlet of the third channel to produce continuous fibers. In another aspect of the present disclosure, an apparatus for implementing the foregoing fiber continuous manufacturing method is also presented.
Description
Technical Field
The disclosure belongs to the technical field of fiber material science, and particularly relates to a fiber continuous preparation method and device.
Background
High performance and bio-based elastic fibers have become one of the hot spots of research today, such as carbon fibers, glass fibers, collagen fibers, cellulose fibers, and the like. With the deep research of the fiber, the high-performance bio-based fiber is expected to be applied to various fields of textile industry, building construction, automobile manufacturing, biomedical engineering and the like. At the same time, the search and development of alternative biodegradable fibers is of great importance. In this regard, polysaccharides, particularly cellulose, chitosan, sodium alginate, and the like, have received increasing attention due to their biocompatibility, biodegradability, low cost, non-toxicity, innocuity, and reproducibility.
The method for preparing the fiber filaments by assembling the green polymers with good biocompatibility and preparing the composite fibers by utilizing the two-dimensional nano sheets mainly comprises wet spinning, dry spinning and electrostatic complex spinning. In the wet spinning process, the fiber needs to be solidified in an organic solvent coagulating bath, and the spinning solution has higher concentration and poorer fluidity, which is not beneficial to the high orientation of the polymer chains. The polymer solution used for dry spinning has higher viscosity, and the polymer chains have stronger entanglement, so that the orientation degree of the polymer chains is lower, bubbles in the spinning solution with lower fluidity are difficult to remove in the spinning process, a large number of defects such as holes are generated in the prepared fiber, and the mechanical properties of the cellulose filaments are greatly reduced. While interfacial complexation based on electrostatic action produces fibers in which electrostatic attraction between component interfaces of opposite charge combine to form a high aspect ratio material structure, the stretching process performed on the reactive interfaces can induce alignment of molecules along the fiber axis.
However, the method for preparing the fiber based on the interfacial electrostatic complexation in the related art is generally to draw the fiber in a vertical direction where two reaction droplets transversely meet the interface, and the fiber obtained by the method may have a non-uniform structure and be easily broken, and the length and continuous collection of the fiber are limited, so that it is difficult to meet the practical requirements. It is important how to use the electrostatic complexation between interfaces to achieve continuous collection and preparation of fibers.
Disclosure of Invention
In view of the above, the present disclosure provides a continuous fiber preparation method, which includes the following steps.
Step S1: and providing a reaction die, wherein the reaction die comprises a first channel, a second channel and a third channel, and the first channel, the second channel and the third channel are mutually communicated at the crossing position to form a Y-shaped channel.
Step S2: and injecting the first solution containing the positive electricity material and the second solution containing the negative electricity material into the reaction mould from the inlet of the first channel and the inlet of the second channel in a one-to-one correspondence manner respectively, and converging at the crossing position, so that the positive electricity material and the negative electricity material generate electrostatic complexing reaction to obtain fibers, and the fibers flow out from the outlet of the third channel.
Step S3: the fibers are drawn at the outlet of the third channel to produce continuous fibers.
According to an embodiment of the disclosure, the positive electrode material comprises a first polymer material and/or a first nanomaterial, wherein the first polymer material comprises at least one of polyvinylamine, polyethyleneimine, chitosan quaternary ammonium salt, chitosan, chitin, and the first nanomaterial comprises at least one of iron oxide nanoplatelets, zinc oxide nanoplatelets, silicon nanoplatelets, gold nanoplatelets.
According to an embodiment of the disclosure, the negative electrode material comprises a second polymer material and/or a second nanomaterial, wherein the second polymer material comprises at least one of polyacrylic acid, polymethyl acid, sodium polystyrene sulfonate, sodium alginate, and sodium carboxymethyl cellulose, and the second nanomaterial comprises at least one of graphene oxide, montmorillonite, and carbon nanotubes.
According to an embodiment of the present disclosure, the reaction rate of the electrostatic complexation is controlled by the injection fluxes of the first solution and the second solution and the inclination angle of the reaction mold.
According to the embodiment of the disclosure, the injection fluxes of the first solution and the second solution are the same, and the range of the injection fluxes is 0.1-3 ml/min;
according to the embodiment of the disclosure, the inclination angle of the reaction mold in the electrostatic complexation reaction ranges from 0 ° to 90 °.
According to embodiments of the present disclosure, the rate of the pulling operation is 0-12 rad/min.
According to an embodiment of the present disclosure, the material of the reaction mold is hydrogel.
According to an embodiment of the present disclosure, in step S1, a method of providing a reaction mold includes the following steps.
Step S101: and dissolving the polymer monomer, an initiator and a crosslinking agent in distilled water to obtain a mixed aqueous solution, and then adding a coagulant to obtain a reaction solution.
Step S102: pouring the reaction solution into a planar container, putting into a Y-shaped template, and stripping the Y-shaped template after polymerization qualification to obtain the reaction die.
Step S103: the reaction mold is rinsed, soaked in water to expand the reaction mold.
According to embodiments of the present disclosure, the mass ratio of the polymer monomer to the initiator is 1:1 to 1:6.
According to an embodiment of the present disclosure, the polymer monomer comprises acrylamide, the initiator comprises ammonium persulfate, and the crosslinking agent comprises N, N' -methylenebisacrylamide.
In another aspect of the present disclosure, an apparatus for implementing the aforementioned fiber continuous preparation method is presented, comprising an injection unit, a reaction unit, and a collection unit.
According to an embodiment of the present disclosure, the injection unit comprises two identical syringes containing a first solution and a second solution, respectively, and a syringe propulsion assembly. The reaction unit comprises a reaction die and an inclined assembly; wherein the reaction die is configured to include a first channel, a second channel, and a third channel, the first channel, the second channel, and the third channel being in communication with one another at intersecting locations to form a Y-shaped channel; the axial direction of the inclination component is orthogonal to the direction of the third channel, and the inclination component is suitable for adjusting the inclination angle of the reaction die; the reaction unit is adapted to receive the first solution and the second solution and to cause an electrostatic complexing reaction, thereby obtaining a fiber. The collecting unit includes a plurality of roller assemblies so that the fiber is continuously drawn by the roller assemblies to be continuously produced.
According to an embodiment of the present disclosure, the roller assembly at the end of the collecting unit is adapted to collect fibers.
According to embodiments of the present disclosure, a first solution and a second solution of oppositely charged materials are subjected to an in situ electrostatic complexation reaction between interfaces by a reaction die having a Y-shaped channel, thereby spontaneously assembling to form complex fibers. And then, the fiber is continuously generated through traction, the oriented assembly of a high molecular chain and a nano sheet is facilitated through traction and stretching, and the prepared fiber has high orientation degree and is beneficial to the high-strength toughening of the fiber. The fiber continuous preparation method provided by the disclosure is carried out in an aqueous solution, is nontoxic and environment-friendly, and has low requirements on reaction conditions and cost.
Drawings
FIG. 1 is a flow chart of a method of continuously preparing fibers in an embodiment of the present disclosure;
FIG. 2 is a schematic view of an apparatus structure of a fiber continuous production method in an embodiment of the present disclosure;
FIG. 3 is a schematic view of a reaction die structure of a fiber continuous manufacturing method in an embodiment of the present disclosure;
FIG. 4 is a fiber fracture interfacial electron microscopy image prepared in example 1 of the present disclosure;
FIG. 5 is a stress-strain plot of the fiber prepared in example 1 of the present disclosure;
FIG. 6 is a fiber fracture interfacial electron microscopy image prepared in example 2 of the present disclosure;
FIG. 7 is a stress-strain plot of the fibers prepared in example 2 of the present disclosure;
FIG. 8 is a fiber fracture interfacial electron microscopy image prepared in example 3 of the present disclosure;
FIG. 9 is a stress-strain plot of the fiber prepared in example 3 of the present disclosure;
FIG. 10 is a fiber fracture interfacial electron microscopy image prepared in example 4 of the present disclosure;
fig. 11 is a stress-strain graph of the fiber prepared in example 4 of the present disclosure.
In the drawings and the specification, the reference numerals have the following meanings:
1. an injection unit;
2. a reaction unit;
21. a reaction mold;
211. a first channel;
212. a second channel;
213. a third channel;
22. a tilting assembly;
3. and a collecting unit.
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same.
The endpoints of the ranges and any values disclosed in this disclosure are not limited to the precise range or value, and such range or value should be understood to encompass values approaching those range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, and are to be considered as specifically disclosed in this disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. The terms "comprises," "comprising," and/or the like, as used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components.
All terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art unless otherwise defined. It should be noted that the terms used herein should be construed to have meanings consistent with the context of the present specification and should not be construed in an idealized or overly formal manner.
It is to be noted that unless otherwise defined, technical or scientific terms used in the present disclosure should be taken in a general sense as understood by one of ordinary skill in the art to which the present disclosure pertains. If, throughout, reference is made to "first," "second," etc., the description of "first," "second," etc., is used merely for distinguishing between similar objects and not for understanding as indicating or implying a relative importance, order, or implicitly indicating the number of technical features indicated, it being understood that the data of "first," "second," etc., may be interchanged where appropriate.
In the present disclosure, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; may be mechanically connected, may be electrically connected or may communicate with each other; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the terms in this disclosure will be understood by those of ordinary skill in the art as the case may be.
In the description of the present disclosure, it should be understood that the terms "longitudinal," "length," "circumferential," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate an orientation or a positional relationship based on that shown in the drawings, merely to facilitate description of the present disclosure and to simplify the description, and do not indicate or imply that the subsystem or element being referred to must have a particular orientation, be configured and operated in a particular orientation, and thus should not be construed as limiting the present disclosure.
Like elements are denoted by like or similar reference numerals throughout the drawings. Conventional structures or constructions will be omitted when they may obscure the understanding of this disclosure. And the shape, size and position relation of each component in the figure do not reflect the actual size, proportion and actual position relation. In addition, in the present disclosure, any reference signs placed between parentheses shall not be construed as limiting the disclosure.
Similarly, in the foregoing description of exemplary embodiments of the disclosure, various features of the disclosure are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure and aiding in the understanding of one or more of the various disclosed aspects. The description of the reference to the terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to be based on the fact that those skilled in the art can implement the technical solutions, and when the technical solutions are contradictory or cannot be implemented, the combination of the technical solutions should be considered as not existing, and not falling within the protection scope of the present disclosure.
In order to break through the limitations of interfacial complexation drawing between two droplets on fiber length and continuous collection in the related art, a continuous preparation method is designed in the present disclosure, wherein electrostatic complexation occurs between two oppositely charged component interfaces, and fiber is obtained in the direction of the reaction plane. Firstly, a hydrogel mold with a Y-shaped channel is designed and prepared, in the process of respectively and continuously injecting reaction solution from two inlets, shearing action is utilized to induce high molecular orientation assembly, in-situ complexing reaction occurs through electrostatic action after the reaction solution is converged to a crossing position, and finally continuous preparation is realized through a collecting device.
FIG. 1 is a flow chart of a method of continuously preparing fibers in an embodiment of the present disclosure.
The present disclosure proposes a fiber continuous preparation method, as shown in fig. 1, comprising the following steps.
Step S1: providing a reaction die, wherein the reaction die comprises a first channel, a second channel and a third channel, and the first channel, the second channel and the third channel are mutually communicated at the crossing position to form a Y-shaped channel;
step S2: injecting a first solution containing positive electricity material and a second solution containing negative electricity material into a reaction mould from an inlet of a first channel and an inlet of a second channel in one-to-one correspondence respectively, and converging at a crossing position to enable the positive electricity material and the negative electricity material to generate electrostatic complexing reaction to obtain fibers, wherein the fibers flow out from an outlet of a third channel;
step S3: the fibers are drawn at the outlet of the third channel to produce continuous fibers.
According to embodiments of the present disclosure, a first solution and a second solution of oppositely charged materials are subjected to an in situ electrostatic complexation reaction between interfaces by a reaction die having a Y-shaped channel, thereby spontaneously assembling to form complex fibers. And then, the fiber is continuously generated through traction, the oriented assembly of a high molecular chain and a nano sheet is facilitated through traction and stretching, and the prepared fiber has high orientation degree and is beneficial to the high-strength toughening of the fiber. The fiber continuous preparation method provided by the disclosure is carried out in an aqueous solution, is nontoxic and environment-friendly, and has low requirements on reaction conditions and cost.
According to embodiments of the present disclosure, reference to positively and negatively charged materials in this disclosure means materials that carry positive and negative charges such that both electrostatically complex to give fibers.
According to an embodiment of the disclosure, the positive electrode material comprises a first polymer material and/or a first nanomaterial, wherein the first polymer material comprises at least one of polyvinylamine, polyethyleneimine, chitosan quaternary ammonium salt, chitosan, chitin, and the first nanomaterial comprises at least one of iron oxide nanoplatelets, zinc oxide nanoplatelets, silicon nanoplatelets, gold nanoplatelets.
According to an embodiment of the disclosure, the negative electrode material comprises a second polymer material and/or a second nanomaterial, wherein the second polymer material comprises at least one of polyacrylic acid, polymethyl acid, sodium polystyrene sulfonate, sodium alginate, and sodium carboxymethyl cellulose, and the second nanomaterial comprises at least one of graphene oxide, montmorillonite, and carbon nanotubes.
According to embodiments of the present disclosure, the reaction solution is suitable for use in an electrostatic complexation reaction between any one or more components comprising a positive charge material and any one or more components comprising a negative charge material, including an assembly between one or more first polymeric materials and one or more second polymeric materials, an assembly between one or more first polymeric materials and second nanomaterials, an assembly between a first nanomaterial and one or more second nanomaterials, and the like.
According to the embodiment of the disclosure, the method for preparing the fiber is based on the electrostatic action between the green polymer and/or the nano sheet material with positive charges and negative charges, and the mode ensures that the fiber has the advantages of the polymer, namely lower production cost, good biocompatibility, biodegradability and antibacterial wound healing promotion effect, and has important significance for the practical application in the field of biomedical materials
In some specific embodiments, the preparation method of the first solution and the second solution in step S2 includes dissolving and dispersing the high viscosity solution of the positive electric material or the negative electric material in ultrapure water, and stirring at room temperature to obtain the first solution or the second solution.
According to an embodiment of the present disclosure, the reaction rate of the electrostatic complexation is controlled by the injection fluxes of the first solution and the second solution and the inclination angle of the reaction mold.
According to the embodiment of the disclosure, the injection fluxes of the first solution and the second solution are the same, and the range of the injection fluxes is 0.1-3 ml/min;
according to the embodiment of the disclosure, the inclination angle of the reaction mold in the electrostatic complexation reaction ranges from 0 ° to 90 °.
In some embodiments, the implantation flux and tilt angle may be controlled using a single variable control method to control the rate of electrostatic complexation.
According to embodiments of the present disclosure, the rate of the pulling operation is 0-12 rad/min.
According to the embodiment of the disclosure, the continuous preparation is achieved by continuously injecting the reaction solution, continuously converging the reaction solution to generate a reaction interface, stretching and pulling the complex to obtain continuous fibers and collecting the continuous fibers.
According to an embodiment of the present disclosure, the material of the reaction mold is hydrogel.
According to the embodiment of the disclosure, the hydrogel has good hydrophilicity, so that the directional mobility of the reaction solution on the surface of the hydrogel is good, thereby inducing the self-assembly of the reaction solution to form fibers with high orientation degree of molecular chains, and meanwhile, the smooth characteristic of the hydrogel channel effectively prevents the superfine fibers from being cut off or adhered by the surfaces of other channels with roughness;
according to an embodiment of the present disclosure, in step S1, a method of providing a reaction mold includes the following steps.
Step S101: and dissolving the polymer monomer, an initiator and a crosslinking agent in distilled water to obtain a mixed aqueous solution, and then adding a coagulant to obtain a reaction solution.
Step S102: pouring the reaction solution into a planar container, putting into a Y-shaped template, and stripping the Y-shaped template after polymerization qualification to obtain the reaction die.
Step S103: the reaction mold is rinsed, soaked in water to expand the reaction mold.
In some specific embodiments, to obtain a polyacrylamide (PAAm) hydrogel reaction mold with Y-channels, 3D printed Y-resin is used as a template. 15g of acrylamide (AAm), 0.1g of N, N' -methylenebisacrylamide (MBAAm) and 0.3g of APS (ammonium persulfate) were dissolved in 100mL of distilled water to obtain a reaction solution, and 300. Mu.L of tetramethyl ethylenediamine (TEMED) was added at room temperature. PAAm hydrogels were synthesized by free radical polymerization for 5 min. And stripping the Y-shaped resin template, cutting to obtain a hydrogel reaction mold containing channels, flushing the obtained hydrogel reaction mold with excessive water to wash out unreacted components, and soaking the hydrogel reaction mold in water until the hydrogel reaction mold is fully expanded.
According to embodiments of the present disclosure, the mass ratio of the polymer monomer to the initiator is 1:1 to 1:6.
In some specific embodiments, the polymer monomer comprises acrylamide, the initiator comprises ammonium persulfate, and the crosslinker comprises N, N' -methylenebisacrylamide.
Fig. 2 is a schematic view of an apparatus structure of a fiber continuous manufacturing method in an embodiment of the present disclosure, and fig. 3 is a schematic view of a reaction mold structure of a fiber continuous manufacturing method in an embodiment of the present disclosure.
In another aspect of the present disclosure, an apparatus for implementing the aforementioned fiber continuous preparation method is presented, as shown in fig. 2, including an injection unit 1, a reaction unit 2, and a collection unit 3.
According to embodiments of the present disclosure, the injection unit 1 comprises two identical syringes and a syringe propulsion device, which in some specific embodiments may be a syringe pump. The syringe contains a first solution and a second solution, respectively. The reaction unit 2 includes a reaction die 21 and a tilting assembly 22; wherein, as shown in fig. 3, the reaction mold 21 is configured to include a first channel 211, a second channel 212, and a third channel 213, and the first channel 211, the second channel 212, and the third channel 213 communicate with each other at crossing positions to form a Y-shaped channel; the axial direction of the tilting assembly 22 is orthogonal to the direction of the third channel 213, and is suitable for adjusting the tilting angle of the reaction mold; the reaction unit 2 is adapted to receive the first solution and the second solution and to generate an electrostatic complexing reaction, thereby obtaining fibers. The collecting unit 3 includes a plurality of roller assemblies so that the fiber is continuously drawn by the roller assemblies to be continuously produced.
According to the embodiment of the present disclosure, the first solution and the second solution are flowed in from the first channel 211 inlet and the second channel 212 inlet of the reaction mold 21, respectively, by the injection unit 1. After the reaction solutions are gathered at the crossing position, the reaction solutions are gathered in the third channel 213 to form fibers through continuous ion complexing self-assembly and flow out together, the fibers are pulled out from the outlet of the third channel 213 by forceps, and the fibers are collected by a roller device after being washed by a water bath.
According to an embodiment of the present disclosure, the roller assembly at the end of the collecting unit 3 is adapted to collect fibers.
It should be noted that the described embodiments are only some embodiments of the present disclosure, and not all embodiments. Based on the embodiments in this disclosure, other embodiments that may be obtained by one of ordinary skill in the art without making any inventive effort are within the scope of the present disclosure.
In the following examples, a unified reaction apparatus was employed in which the channel diameter of the hydrogel reaction mold obtained by reshaping of the reaction unit 2 was 3mm. The liquid injection device of injection unit 1 employs a commercially available LSP10-B syringe pump, two oppositely charged reaction solutions are added separately with two 10mL syringes, and the appropriate flux is controlled as needed. The speed of collecting the fiber by the collecting device 3 can be adjusted to be 0-12 rad/min.
Example 1
0.5g of Chitosan (CS) powder was added to 99.5g of a 1wt% acetic acid solution, and stirred sufficiently at room temperature until completely dissolved, to obtain a 0.5% mass fraction chitosan solution, as a first solution. 1g of Sodium Alginate (SA) is added into 99g of deionized water, and the mixture is fully stirred at room temperature until the sodium alginate is completely dissolved, so that a sodium alginate solution with the mass fraction of 1% is obtained and is used as a second solution.
The reaction solutions with different charges are respectively added by adopting a 10mL injector, the two reaction solutions are respectively injected from a first channel inlet and a second channel inlet of a reaction die by using an injection pump at a flow rate of 0.5mL/min, flow out through a third channel after converging at a crossing position, fiber is pulled out from an outlet of the third channel by using tweezers, and is hung to a roller assembly for continuous collection at a speed of 4.2rad/min after being cleaned by a water bath. And (5) airing the CS-SA fiber obtained by collecting the endmost roller assembly at room temperature.
The CS-SA fibers prepared in example 1 were subjected to electron microscopy and stress testing.
Fig. 4 and 5 are respectively fracture interface electron microscopy charts and stress strain charts of the fibers prepared in example 1 of the present disclosure.
As shown in FIG. 4 and FIG. 5, the CS-SA fiber prepared in example 1 had a diameter of 5 to 10. Mu.m, a uniform and non-fractured internal structure and a tensile strength of 503MPa.
Example 2
0.5g of Chitosan (CS) powder was added to 99.5g of a 1wt% acetic acid solution, and stirred sufficiently at room temperature until completely dissolved, to obtain a 0.5% mass fraction chitosan solution, as a first solution. 9g of sodium polystyrene sulfonate (PSSNa) was added to 91g of deionized water, and stirred sufficiently at room temperature until completely dissolved, to obtain a sodium polystyrene sulfonate aqueous solution with a mass fraction of 9%, and as a second solution.
The reaction solutions with different charges are respectively added by adopting a 10mL injector, the two reaction solutions are respectively injected from a first channel inlet and a second channel inlet of a reaction die by utilizing an injection pump at a flow rate of 0.5mL/min, flow out through a third channel after converging at a crossing position, fiber is pulled out from an outlet of the third channel by using tweezers, and is continuously collected at a speed of 4.2rad/min after being washed by a water bath, and the collected CS-PSSNa fiber is dried at room temperature.
Electron microscopy and stress testing were performed on the CS-PSSNa fibers prepared in example 2.
Fig. 6 and 7 are fracture interface electron microscopy and stress strain graphs, respectively, of the fiber prepared in example 2 of the present disclosure.
As shown in FIG. 6 and FIG. 7, the CS-PSSNa fiber prepared in example 2 has a diameter of 5-10 μm and a uniform internal structure, and the fracture in FIG. 6 is generated by the influence of high-energy electron beams in the scanning electron microscope test, and the tensile strength of the fiber is about 321.4MPa.
Example 3
28.5g of a 40% Polyethyleneimine (PEI) solution is added to 71.5g of deionized water, and the mixture is fully stirred at room temperature until the mixture is uniformly mixed to obtain an 11.4% by mass polyethyleneimine aqueous solution, and the pH of the polyethyleneimine aqueous solution is adjusted to 2-3 by using hydrochloric acid so that the solution is positively charged and is used as a first solution. 0.3g of sodium carboxymethyl cellulose is added into 99.7g of deionized water, and the mixture is fully stirred at room temperature until the sodium carboxymethyl cellulose is completely dissolved, so that CMC solution with the mass fraction of 0.3% is obtained and is used as a second solution.
The reaction solutions with different charges are respectively added by adopting a 10mL injector, the two reaction solutions are respectively injected from a first channel inlet and a second channel inlet of a reaction die by utilizing an injection pump at a flow rate of 0.5mL/min, flow out through a third channel after converging at a crossing position, fiber is pulled out from an outlet of the third channel by using tweezers, and is continuously collected at a speed of 4.2rad/min after being washed by a water bath, and the collected PEI-CMC fiber is dried at room temperature.
Electron microscopy and stress testing were performed on the PEI-CMC fiber prepared in example 3.
Fig. 8 and 9 are fracture interface electron microscopy and stress strain graphs, respectively, of the fiber prepared in example 3 of the present disclosure.
As shown in FIG. 8 and FIG. 9, the PEI-CMC fiber prepared in example 3 has a diameter of 5-15 μm and a uniform internal structure, and the fracture in FIG. 8 is generated by the influence of high-energy electron beams in the scanning electron microscope test, and the tensile strength of the fiber is about 227.5MPa.
Example 4
28.5g of 40% Polyethyleneimine (PEI) solution is added into 71.5g of deionized water, and the mixture is fully stirred at room temperature until the mixture is uniformly mixed, so that 11.4% by mass of polyethyleneimine aqueous solution is obtained, pH of the aqueous solution is regulated to 2-3 by hydrochloric acid, and the aqueous solution is positively charged and is used as a first solution. 9g of sodium polystyrene sulfonate (PSSNa) was weighed into 91g of deionized water, and stirred sufficiently at room temperature until completely dissolved, to obtain a sodium polystyrene sulfonate aqueous solution with a mass fraction of 9%, and used as a second solution.
The reaction solutions with different charges are respectively added by adopting a 10mL injector, the two reaction solutions are respectively injected from a first channel inlet and a second channel inlet of a reaction die by utilizing an injection pump at a flow rate of 0.5mL/min, flow out through a third channel after converging at a crossing position, fiber is pulled out from an outlet of the third channel by using tweezers, and is continuously collected at a speed of 4.2rad/min after being washed by a water bath, and the collected PEI-PSSNa fiber is dried at room temperature.
Electron microscopy and stress testing were performed on the PEI-PSSNa fiber prepared in example 4.
Fig. 10 and 11 are respectively fracture interface electron microscopy and stress strain graphs of the fiber prepared in example 4 of the present disclosure.
As shown in FIG. 10 and FIG. 11, the PEI-PSSNa fiber prepared in example 4 has a diameter of 20-30 μm and a uniform internal structure, and the fracture in FIG. 10 is generated by the influence of a high-energy electron beam in a scanning electron microscope test, and the tensile strength of the fiber is about 150MPa.
While the foregoing is directed to embodiments of the present disclosure, other and further details of the invention may be had by the present application, it is to be understood that the foregoing description is merely exemplary of the present disclosure and that no limitations are intended to the scope of the disclosure, except insofar as modifications, equivalents, improvements or modifications may be made without departing from the spirit and principles of the present disclosure.
Claims (10)
1. A continuous fiber preparation method comprising:
providing a reaction die, wherein the reaction die comprises a first channel, a second channel and a third channel, and the first channel, the second channel and the third channel are mutually communicated at the crossing position to form a Y-shaped channel;
injecting a first solution containing a positive electric material and a second solution containing a negative electric material into the reaction mould from the inlet of the first channel and the inlet of the second channel in a one-to-one correspondence manner respectively, and converging at the crossing position to enable the positive electric material and the negative electric material to generate electrostatic complexing reaction to obtain fibers, wherein the fibers flow out from the outlet of the third channel;
the fibers are drawn at the outlet of the third channel to produce the fibers continuously.
2. The continuous production method for a fiber according to claim 1, wherein,
the positive electrode material comprises a first high polymer material and/or a first nano material, wherein the first high polymer material comprises at least one of polyvinylamine, polyethyleneimine, chitosan quaternary ammonium salt, chitosan and chitin, and the first nano material comprises at least one of ferric oxide nano-sheets, zinc oxide nano-sheets, silicon nano-sheets and gold nano-sheets;
the negative electrode material comprises a second high polymer material and/or a second nano material, wherein the second high polymer material comprises at least one of polyacrylic acid, polymethyl acid, sodium polystyrene sulfonate, sodium alginate and sodium carboxymethyl cellulose, and the second nano material comprises at least one of graphene oxide, montmorillonite and carbon nano tubes.
3. The continuous production method of a fiber according to claim 1, wherein a reaction rate of the electrostatic complexation is controlled by injection fluxes of the first solution and the second solution and an inclination angle of the reaction mold.
4. The continuous production method for a fiber according to claim 3, wherein,
the injection flux of the first solution and the injection flux of the second solution are the same, and the range of the injection flux is 0.1-3 ml/min;
the inclination angle of the reaction die in the electrostatic complexation reaction is in the range of 0-90 degrees.
5. The continuous fiber production method according to claim 1, wherein the pulling operation is performed at a rate of 0 to 12rad/min.
6. The continuous fiber production method according to claim 1, wherein the material of the reaction die is hydrogel.
7. The continuous fiber production method according to claim 6, wherein the method of providing a reaction mold comprises:
dissolving a polymer monomer, an initiator and a crosslinking agent in distilled water to obtain a mixed aqueous solution, and then adding a coagulant to obtain a reaction solution;
pouring the reaction solution into a planar container, putting into a Y-shaped template, and stripping the Y-shaped template after polymerization qualification to obtain the reaction mold;
the reaction mold is rinsed, soaked in water to expand the reaction mold.
8. The continuous production method for a fiber according to claim 7, wherein,
the mass ratio of the polymer monomer to the initiator is 1:1-1:6;
the polymer monomer comprises acrylamide, the initiator comprises ammonium persulfate, and the cross-linking agent comprises N, N' -methylene bisacrylamide.
9. An apparatus for carrying out the continuous fiber production process of any of claims 1 to 8, comprising:
an injection unit (1) comprising two identical syringes containing a first solution and a second solution respectively and a syringe propulsion assembly;
a reaction unit (2) adapted to receive said first solution and said second solution and to undergo an electrostatic complexation reaction, thereby obtaining a fiber, comprising:
a reaction die (21) configured to include a first channel (211), a second channel (212), and a third channel (213), the first channel (211), the second channel (212), and the third channel (213) communicating with each other at intersecting positions to form a Y-shaped channel;
a tilting assembly (22), wherein the axial direction of the tilting assembly (22) is orthogonal to the direction of the third channel, and is suitable for adjusting the tilting angle of the reaction die (21);
a collecting unit (3) comprising a plurality of roller assemblies, so that the fibers are continuously pulled by the roller assemblies to be continuously produced.
10. The device according to claim 9, wherein a roller assembly at the end of the collecting unit (3) is adapted to collect the fibers.
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