CN114836845B - Flexible conductive polyurethane fiber and preparation method thereof - Google Patents
Flexible conductive polyurethane fiber and preparation method thereof Download PDFInfo
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- CN114836845B CN114836845B CN202210549132.4A CN202210549132A CN114836845B CN 114836845 B CN114836845 B CN 114836845B CN 202210549132 A CN202210549132 A CN 202210549132A CN 114836845 B CN114836845 B CN 114836845B
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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
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
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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
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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
- D01D5/12—Stretch-spinning methods
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention provides a flexible conductive polyurethane fiber and a preparation method thereof. The flexible conductive polyurethane fiber comprises a conductive core layer and an elastic skin layer, wherein the conductive core layer is a metal fiber with a two-dimensional bending structure or a metal fiber with a three-dimensional spiral structure, and the elastic skin layer is polyurethane fiber; the flexible conductive polyurethane fiber is obtained through coaxial spinning, and the diameter of the metal fiber is in the micron order. The preparation method combines the coaxial spinning, the drafting process and the twisting process, utilizes the coaxial spinning to prepare the conductive fiber with the sheath-core structure, generates a core layer with a special two-dimensional bending structure with a certain bending angle or a three-dimensional spiral structure with a special space configuration by changing the drafting proportion and the twist, and finally thins the skin layer and rapidly solidifies and forms the skin layer by rapid drafting of a drafting shaft in a coagulating bath. The conductive fiber obtained by the invention has the electrical signal which can be converted along with the strain, and has extremely high elastic performance.
Description
Technical Field
The invention relates to the technical field of flexible conductive fibers, in particular to a flexible conductive polyurethane fiber and a preparation method thereof.
Background
Conductive sensing fabrics are prepared by embedding or integrating conductive materials into elastic fabrics, which are widely used in elastic fabrics by virtue of their excellent elastic properties, and they are required to have both excellent conductivity similar to conductive materials and high elasticity and high flexibility similar to elastic fabrics. Therefore, the conductive sensing fabric can be widely applied to the fields of sensors, static resistance, electromagnetic radiation resistance and the like.
The traditional method for preparing the conductive sensing fabric is to weave the fiber into the spandex fabric, and then connect the conductive device with the spandex fabric to obtain the conductive sensing fabric. In addition, the conductive fiber can be prepared first and then woven into the conductive sensing fabric. At present, the method for preparing the conductive fiber generally comprises the steps of blending and spinning conductive particles and polyurethane resin or growing the conductive particles on the surface of the polyurethane fiber to prepare the conductive fiber, wherein the conductive particles in the conductive fiber obtained by the method are easy to be completely wrapped by the polyurethane resin to lose conductivity, and the conductive particles in the conductive fiber obtained by the method are easy to fall off to cause conductivity loss, so that the conductivity of the conductive sensing fabric is influenced. It can be seen that the preparation of high-performance elastic conductive fibers is critical to the preparation of conductive sensing fabrics.
In view of the foregoing, there is a need for an improved flexible conductive polyurethane fiber and a method for preparing the same, which solve the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a flexible conductive polyurethane fiber and a preparation method thereof, wherein a coaxial spinning process, a drafting process and a twisting process are combined, the coaxial spinning is utilized to prepare the conductive fiber with a sheath-core structure, a core layer with a two-dimensional bending structure with a special bending angle or a core layer with a three-dimensional spiral structure with a special spatial configuration is generated by changing the drafting proportion and the twist, and finally, the sheath layer is thinned and rapidly solidified and formed by rapid drafting of a drafting shaft in a coagulating bath, meanwhile, the core layer structure further tends to be stable, and metal wires with the special structure are uniformly distributed in the sheath layer material at the moment, so that the high-performance two-dimensional or three-dimensional flexible conductive polyurethane fiber is obtained.
In order to achieve the above-mentioned aim, the invention provides a flexible conductive polyurethane fiber, which comprises a conductive core layer and an elastic skin layer, wherein the conductive core layer is a metal fiber with a two-dimensional bending structure or a metal fiber with a three-dimensional spiral structure, and the elastic skin layer is polyurethane fiber; the flexible conductive polyurethane fiber is obtained through coaxial spinning, and the diameter of the metal fiber is in the micron order.
As a further improvement of the invention, the two-dimensional bending structure is preferably a wavy bending structure, the height of the wavy bending structure is 2-200 μm, and the distance between the peaks of adjacent waves is 1-100mm; the three-dimensional spiral structure is preferably a spring-shaped structure, the height of the spring-shaped structure is 2-200 mu m, and the distance between adjacent threads is 1-100mm; the diameter of the flexible conductive polyurethane fiber is 10-500 mu m.
In order to achieve the above object, the present invention further provides a method for preparing the flexible conductive polyurethane fiber, which comprises the following steps:
s1, dissolving polyurethane resin in a polar solvent according to a preset proportion, mechanically stirring uniformly at 20-30 ℃ and then vacuum defoaming to obtain spinning solution;
s2, transmitting the metal fiber into a core layer channel by utilizing coaxial spinning, filling the spinning solution obtained in the step S1 into a skin layer channel, and firstly keeping the first drawing speed of the metal fiber in the core layer channel and the extrusion speed of the spinning solution in the skin layer channel to be the same, so that the spinning solution is wrapped on the surface of the metal fiber; after a certain distance of drawing, drawing the metal fiber by adopting a second drawing speed smaller than the first drawing speed so as to bend the metal fiber to form a two-dimensional bending structure; drawing a certain distance, then entering a coagulating bath, and drawing the skin layer at a third drawing speed to obtain a two-dimensional flexible conductive polyurethane fiber; the third draft speed is greater than the first draft speed;
or twisting the metal fiber at a preset rotating speed while drawing to bend the metal fiber to form a three-dimensional spiral structure, so as to obtain the three-dimensional flexible conductive polyurethane fiber.
As a further improvement of the present invention, in step S2, the first draft speed is 1 to 5mm/S, the second draft speed is 0.5 to 4mm/S, and the third draft speed is 2 to 8mm/S.
As a further improvement of the present invention, the first draft speed has a draft distance of 0.1 to 5cm, the second draft speed has a draft distance of 0.1 to 10cm, and the third draft speed has a draft distance of 0.1 to 100cm.
As a further improvement of the present invention, in step S2, the preset rotational speed of the twisting process is 0.5-25r/min, and the elastic recovery of the metal fiber is 0-50%.
As a further improvement of the present invention, in step S2, the diameter of the metal fiber is 50-500 μm, and the metal fiber includes one or more of nickel wire, cobalt wire, iron wire, copper wire, zinc wire, gold wire, silver wire.
As a further improvement of the present invention, in step S1, the mass ratio of the polyurethane resin to the polar solvent is (20% -45%) (55% -80%).
As a further improvement of the present invention, in step S2, the temperature of the coagulation bath is 20-30 ℃, and the coagulation bath is one of simethicone, ethyl silicone oil and propyl silicone oil.
As a further improvement of the present invention, in step S1, the polar solvent includes one or more of tetrahydrofuran, N, dimethylformamide, N, dimethylacetamide.
The beneficial effects of the invention are as follows:
(1) The invention utilizes coaxial spinning to prepare conductive fibers with a sheath-core structure, changes the drawing speed of a core layer by changing the drawing speeds of different drawing shafts, further changes the structure of a core layer metal wire, firstly keeps the drawing speed of the metal wire to be the same as the extrusion speed of spinning solution in a sheath channel, uniformly wraps the spinning solution on the surface of the metal wire, then slows down the drawing speed of the metal wire before the sheath fiber is not solidified and molded, enables the metal wire to be in an overfeeding state to deform to a certain extent, generates a core layer with a two-dimensional bending structure with a special bending angle, and at the moment, the sheath layer is not solidified and molded, the core layer with the special structure is wrapped by the flow of sheath trickle, and finally, the sheath layer is thinned and rapidly solidified and molded by the rapid drawing of the drawing shafts in a coagulating bath, so that the high-performance two-dimensional flexible conductive polyurethane fiber is obtained. In addition, when the metal wire is drawn, the metal wire is twisted to a certain degree, the core layer with certain twist is deformed in an overfeeding state, the core layer with a three-dimensional spiral structure with a special space configuration is generated, and the skin layer is further drawn to obtain the high-performance three-dimensional flexible conductive polyurethane fiber. In the drawing process of the coagulation bath, on one hand, the core layer structure is further changed to obtain a more stable special two-dimensional or three-dimensional special structure; on the other hand, the orientation of polyurethane molecular chains changes in the continuous drafting process of the cortical fiber, the molecular chains tend to be tidy, the arrangement among different molecular chains is tidier, the cortical structure is more stable, and the crimping degree of the fiber can be improved. The whole preparation process is in a dynamic drawing process, and the morphology and the structure of the core layer and the skin layer can be continuously adjusted in the continuous drawing process, so that the prepared skin-core structure tends to be more stable. The invention selects the metal wires as the conductive material instead of the conductive particles, firstly, the defect of poor conductive performance caused by uneven distribution or complete package of the conductive particles is fundamentally avoided, and simultaneously, the coaxial spinning is combined, so that the metal wires with special structures are uniformly distributed in the skin material, and the conductivity of the metal wires is further improved; and due to the special structure of the metal wire, the flexibility and the elasticity of the skin-core structure are improved.
(2) The invention combines coaxial spinning, drafting process and twisting process based on the forming principle of solvent fast evaporation phase transition, changes the existence form of core layer metal wire by changing the drafting proportion of the drafting process and the twisting degree of the twisting process, and obtains the high-performance flexible conductive fiber with special structure, and the obtained conductive fiber has electric signal changeable along with strain and extremely high elastic performance. Meanwhile, the preparation method has the advantages of simple process, controllable parameters, simple operation and obvious feasibility. In addition, the wires used are of the order of micrometers, which are more easily deformed to give a particular structure.
(3) The invention is based on the compatibility (similar solubility parameter) between the normal temperature coagulation bath and the polar solvent, and utilizes the molding principle of phase transition caused by rapid solvent evaporation to mold the polyurethane resin of the skin layer, thereby further changing the existence form of the space of the core layer and further regulating and controlling the elasticity and the conductivity of the flexible conductive fiber.
Drawings
Fig. 1 is a schematic diagram of a preparation flow of the two-dimensional flexible conductive polyurethane fiber of the present invention.
Fig. 2 is a schematic diagram of a preparation flow of the three-dimensional flexible conductive polyurethane fiber of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention due to unnecessary details, only structures and/or processing steps closely related to aspects of the present invention are shown in the drawings, and other details not greatly related to the present invention are omitted.
In addition, it should be further noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention provides a flexible conductive polyurethane fiber, which comprises a conductive core layer and an elastic skin layer. The conductive core layer is made of metal fibers with a two-dimensional bending structure or metal fibers with a three-dimensional spiral structure, and the elastic skin layer is made of polyurethane fibers; the flexible conductive polyurethane fiber is obtained through coaxial spinning, and the diameter of the metal fiber is in the micron order.
The two-dimensional bending structure is preferably a wavy bending structure, the height of the wavy bending structure is 2-200 mu m, and the distance between adjacent waves is 1-100mm (namely the distance between adjacent wave crests); the three-dimensional spiral structure is preferably a spring-like structure, the height of the spring-like structure is 2-200 mu m, and the distance between adjacent threads is 1-100mm; the diameter of the flexible conductive polyurethane fiber is 10-500 mu m, the skin layers are uniformly distributed on the surface of the core layer, and the core layer is completely wrapped. The height of the wavy curved structure and the spring-like structure is mainly dependent on the diameter of the cortical fiber.
The two-dimensional bending structure means that the metal fibers are in a wavy shape and are in the same plane, so that the structure is called as two-dimensional structure. The three-dimensional spiral structure is a spring shape in which metal fibers are spiral and are not in the same plane, and is called as three-dimensional.
As shown in fig. 1 and 2, the invention also provides a preparation method of the flexible conductive polyurethane fiber, which comprises the following steps:
s1, preparing a spinning solution:
stirring the polar solvent, adding the polyurethane resin into the polar solvent according to the mass ratio of the polyurethane resin to the polar solvent of (20% -45%) (55% -80%), mechanically stirring for 100-140min at 20-30 ℃, and carrying out vacuum defoaming treatment on the obtained solution at 20-30 ℃ after the polyurethane resin is completely dissolved and the spinning solution is a uniform-phase solution, thus obtaining the spinning solution.
Wherein the polar solvent comprises one or more of tetrahydrofuran, N, dimethylformamide, N, dimethylacetamide.
S2, preparing flexible conductive polyurethane fibers:
(1) Preparing two-dimensional flexible conductive polyurethane fibers:
and (3) spinning by adopting a coaxial spinning nozzle, transferring the conductive micron-sized metal fibers into a core layer channel I, filling the spinning solution obtained in the step (S1) into a skin layer channel II, firstly keeping the first drawing speed of the metal fibers in the core layer channel to be the same as the extrusion speed of the spinning solution in the skin layer channel, and starting a subsequent drawing shaft to start to operate while extruding the primary fibers so as to ensure that the spinning solution is wrapped on the surface of the metal fibers. After a certain distance of drawing, drawing the metal fiber at a second drawing speed smaller than the first drawing speed, keeping the metal fiber in an overfeeding state, bending the metal fiber to form a two-dimensional bending structure with a certain bending angle (the deformation process of the metal wire is easy to control), and performing the steps when the polyurethane resin is in an unshaped state. After the continuous drafting for a certain distance, the fiber with the sheath-core structure enters into a coagulating bath, and the sheath is stretched at a third drafting speed (higher than the first drafting speed and the second drafting speed), so that the polyurethane resin of the sheath is thinned and is easy to form, and the two-dimensional flexible conductive polyurethane fiber is obtained.
As shown in fig. 1, after coming out from the coaxial spinning nozzle, the sheath-core structure is formed after passing through a drafting shaft a, a drafting shaft b and a drafting shaft c in sequence. Specifically, the metal fiber is pulled out from the core layer channel I under the drafting action of the drafting shaft a, and the speed of the drafting shaft a is the first drafting speed; the speed of the drafting shaft b is the second drafting speed; the speed of the drawing axis c (in the coagulation bath) is the third drawing speed.
Wherein the first drafting speed is 1-5mm/s of drafting shaft a, the second drafting speed is 0.5-4mm/s of drafting shaft b, and the third drafting speed is 2-8mm/s of drafting shaft c. The first drawing speed is a drawing distance between the coaxial spinning nozzle and the drawing shaft a of 0.1-5cm, the second drawing speed is a drawing distance between the drawing shaft a and the drawing shaft b of 0.1-10cm, and the third drawing speed is a drawing distance between the drawing shaft b and the drawing shaft c of 0.1-100cm (the length is the length of the coagulation bath).
The diameter of the metal fiber is 50-500 μm, and the metal fiber comprises one or more of nickel wire, cobalt wire, iron wire, copper wire, zinc wire, gold wire and silver wire.
The temperature of the coagulating bath is 20-30 ℃, and the coagulating bath is one of dimethyl silicone oil, ethyl silicone oil and propyl silicone oil.
(2) Preparing three-dimensional flexible conductive polyurethane fibers:
and (2) spinning by adopting a coaxial spinning nozzle, transferring conductive micron-sized metal fibers into a core layer channel I, placing the metal fibers on a spiral twisting shaft, filling the spinning solution obtained in the step (S1) into a skin layer channel II, firstly keeping the first drawing speed of the metal fibers in the core layer channel and the extrusion speed of the spinning solution in the skin layer channel to be the same, starting a subsequent drawing shaft to start to operate while extruding the original fibers, and simultaneously operating the twisting shaft at a certain angular speed to ensure that the spinning solution is wrapped on the surface of the metal fibers. After a certain distance of drawing, drawing the metal fiber at a second drawing speed which is smaller than the first drawing speed, keeping the metal fiber in an overfeeding state in the twisting process, bending the metal fiber to form a spiral structure with a certain three-dimensional space configuration (the deformation process of the metal wire is easy to control), and carrying out the steps when the polyurethane resin is in an unshaped state. After the continuous drafting for a certain distance, the fiber with the sheath-core structure enters into a coagulating bath, and the sheath is stretched at a third drafting speed (higher than the first drafting speed and the second drafting speed), so that the polyurethane resin of the sheath is thinned and is easy to form, and the two-dimensional flexible conductive polyurethane fiber is obtained.
As shown in fig. 2, the difference from the preparation of the two-dimensional flexible conductive polyurethane fiber is that the twisting shaft α is added for twisting during the drawing process, and the rest steps and parameter settings are the same, and are not described herein.
Specifically, the angular velocity of the twisting shaft alpha is 0.5-25r/min, the elastic retraction rate of the metal fiber is 0-50%, the elastic retraction rate refers to the shrinkage of the metal wire which is changed into a spiral shape after twisting, and the elastic retraction rate is related to the twist degree of the metal wire.
The invention is described in detail below by means of several examples:
example 1
A preparation method of flexible conductive polyurethane fiber comprises the following steps:
s1, preparing a spinning solution:
stirring tetrahydrofuran, adding 30g of polyurethane resin into 70g of tetrahydrofuran solvent according to the mass ratio of the polyurethane resin to the tetrahydrofuran of 30 percent (70 percent), mechanically stirring for 120min at 25 ℃, and carrying out vacuum defoaming treatment on the obtained solution at the temperature of 25 ℃ after the polyurethane resin is completely dissolved and the spinning solution is a uniform phase solution to obtain the spinning solution.
S2, preparing flexible conductive polyurethane fibers (two dimensions):
spinning by adopting a coaxial spinning nozzle, transferring nickel wires with the diameter of 10 mu m into a core layer channel I, and spinning the nickel wires obtained in the step S1The yarn stock solution is filled into the cortex channel II, the first drafting speed of the nickel yarn in the core layer channel is kept the same as the extrusion speed of the spinning stock solution in the cortex channel, and the subsequent drafting shaft is started to start to operate while the primary fiber is extruded, so that the spinning stock solution is wrapped on the surface of the nickel yarn. After a certain distance of drawing, drawing the nickel wire at a second drawing speed smaller than the first drawing speed, keeping the nickel wire in an overfeeding state, bending the nickel wire to form a two-dimensional bending structure with a certain bending angle, and carrying out the steps when the polyurethane resin is in an unshaped state. After the fiber with the sheath-core structure is continuously drafted for a certain distance, the fiber enters into a silicone oil coagulation bath at room temperature, and the sheath is stretched at a third drafting speed (which is higher than the first drafting speed and the second drafting speed), so that the sheath polyurethane resin is thinned and is easy to form, and the two-dimensional flexible conductive polyurethane fiber is obtained. The solubility parameter of tetrahydrofuran was found to be 20.3J/cm 3 The solubility parameter of the silicone oil is 14.9-15.5J/cm 3 The solubility parameters of the two are not greatly deviated, so that the skin layer is easy to form.
Wherein the drafting speed of the drafting shaft a is 5mm/s, the drafting speed of the drafting shaft b is 3mm/s, and the drafting speed of the drafting shaft c is 8mm/s. The distance between the coaxial spinning nozzle and the drafting shaft a is 3cm, the distance between the drafting shaft a and the drafting shaft b is 5cm, and the distance between the drafting shaft b and the drafting shaft c is 50cm.
Examples 2 to 5
The difference between the preparation method of the flexible conductive polyurethane fiber and the embodiment 1 is that in the step S2, the drawing speeds of the drawing axis a, the drawing axis b and the drawing axis c are different, and the other steps are substantially the same as those of the embodiment 1, and are not repeated here.
The flexible conductive polyurethane fibers (two-dimensional) prepared in examples 1 to 5 were subjected to performance test, and the results are shown in table 1, wherein the electrical conductivity refers to the electrical conductivity of the fibers when stretched by 1000%:
TABLE 1 Flexible conductive polyurethane fiber-related Properties prepared in examples 1-5
As can be seen from table 1, when the drawing speeds of the drawing axes a and c are unchanged, as the drawing speed of the drawing axis b is reduced (examples 1, 2, and 3, i.e., as the drawing speed ratio of the drawing axes a and b is increased), the extensibility (i.e., breaking strain) of the flexible conductive polyurethane fiber is gradually increased, because the nickel filaments are bent and deformed to different extents under the synergistic effect of different drawing speeds, and the heights of the obtained two-dimensional wavy bending structures and the distances between the peaks of adjacent waves are different, thereby affecting the extensibility of the flexible conductive polyurethane fiber. When the speed of the drawing shaft a and the drawing shaft b is unchanged, the extensibility (namely breaking strain) of the flexible conductive polyurethane fiber gradually increases along with the reduction of the speed of the drawing shaft c (examples 1, 4 and 5), because the tensile force applied to the skin fiber in the forming process is different when the drawing speed of the drawing shaft c is different, the skin structure is different, and meanwhile, the bending structure of the core layer is correspondingly changed in the process, so that the extensibility of the flexible conductive polyurethane fiber is different.
The two-dimensional flexible conductive polyurethane fibers prepared in examples 1-5 have small difference in conductivity and breaking strain, and have good overall effect.
Examples 6 to 8
The difference between the preparation method of the flexible conductive polyurethane fiber and the embodiment 1 is that in the step S2, the distances among the coaxial spinning nozzle, the drawing shaft a, the drawing shaft b and the drawing shaft c are different, and the other parts are substantially the same as the embodiment 1, and are not described herein. The distance between the coaxial spinning nozzle and the drawing shaft a is denoted as an outlet-a, the distance between the drawing shaft a and the drawing shaft b is denoted as a-b, and the distance between the drawing shaft b and the drawing shaft c is denoted as b-c.
The performance test was conducted on the preparation method of the flexible conductive polyurethane fibers prepared in examples 6 to 8, and the results are shown in Table 2, wherein the electrical conductivity refers to the electrical conductivity of the fibers when stretched by 1000%:
TABLE 2 Properties related to Flexible conductive polyurethane fibers prepared in examples 6-8
As can be seen from table 2, by varying the distance between the different draw axes, the effect on the conductivity, strain at break and stress at break of the flexible conductive polyurethane fibers is not great, since the two-dimensional bending structure of the fibers varies mainly depending on the fit of the draw ratio. And the forming process of the flexible conductive fiber is directly influenced by changing the length of the coagulating bath, so that the mechanical property of the flexible conductive fiber is influenced.
Examples 9 to 12
The difference between the preparation method of the flexible conductive polyurethane fiber and the preparation method of the embodiment 1 is that in the step S2, the angular velocity of the twisting shaft α and the elastic retraction rate of the nickel wire (depending on the twist of the nickel wire) are different, and the other is substantially the same as the embodiment 1, and the details are not repeated (the preparation of the embodiment 1 is that the two-dimensional flexible conductive polyurethane fiber, i.e. the nickel wire is not twisted, and the angular velocity of the twisting shaft α and the elastic retraction rate of the nickel wire are both 0).
The performance test was performed on the preparation methods of flexible conductive polyurethane fibers prepared in examples 9 to 12, and the results are shown in table 3, wherein the performance of the three-dimensional flexible conductive polyurethane fibers is shown in the specification, and the conductivity refers to the conductivity of the fibers when stretched by 1000%:
TABLE 3 Properties related to Flexible conductive polyurethane fibers prepared in examples 9-12
As can be seen from table 3, as the angular velocity and the elastic retraction rate of the nickel wire increase, the breaking strain of the three-dimensional flexible conductive polyurethane fiber increases, because the nickel wire deforms to obtain a three-dimensional spiral structure with different structures under different angular velocities and elastic retraction rates of the nickel wire, thereby affecting the ductility of the finally obtained fiber, indicating that the spatial structure of the nickel wire can be effectively changed by changing the angular velocity and the elastic retraction rate of the nickel wire, and further regulating and controlling the ductility of the sheath-core fiber.
The three-dimensional flexible conductive polyurethane fibers prepared in examples 9-12 have little difference in breaking strain and deviation in conductivity, but have better overall effect.
Examples 13 to 14
The difference between the preparation method of the flexible conductive polyurethane fiber and the embodiment 9 is that in the step S1, the mass ratio of the polyurethane resin to the tetrahydrofuran is different, and the other steps are substantially the same as those in the embodiment 9, and are not repeated here.
The performance test was performed on the preparation methods of flexible conductive polyurethane fibers prepared in examples 13 to 14, and the results are shown in table 4, where two dimensions refer to two-dimensional flexible conductive polyurethane fibers, three dimensions refer to three-dimensional flexible conductive polyurethane fibers, and conductivity refers to conductivity when the fibers are stretched by 1000%:
TABLE 4 Properties related to Flexible conductive polyurethane fibers prepared in examples 13-14
As can be seen from table 4, the increase or decrease of the polyurethane resin content in the spinning dope reduces the ductility of the flexible conductive polyurethane fiber, mainly because the viscosity of the spinning dope increases with the increase of the polyurethane resin content in the spinning dope, which generates a certain resistance to the deformation of the nickel wire, thereby making the two-dimensional or three-dimensional bending structure different and further affecting the ductility of the fiber; with the reduction of the polyurethane resin content in the spinning solution, the content of the sheath fiber wrapped on the nickel wire is different in the drafting process, and the two-dimensional or three-dimensional bending structure is influenced.
Examples 15 to 16
The difference between the preparation method of the flexible conductive polyurethane fiber and the embodiment 9 is that in the step S2, the diameter of the nickel wire is different, and the other is substantially the same as the embodiment 9, and the description thereof will not be repeated.
The performance test was performed on the preparation methods of flexible conductive polyurethane fibers prepared in examples 15 to 16, and the results are shown in table 5, where two dimensions refer to two-dimensional flexible conductive polyurethane fibers, three dimensions refer to three-dimensional flexible conductive polyurethane fibers, and conductivity refers to conductivity when the fibers are stretched by 1000%:
TABLE 5 Flexible conductive polyurethane fiber-related Properties prepared in examples 15-16
As is clear from table 5, as the diameter of the nickel wire increases, the breaking stress of the flexible conductive fiber increases, because the nickel wire is a reinforcing rigid fiber, which plays a role in reinforcing the sheath-core fiber.
Comparative example 1
The preparation method of the flexible conductive polyurethane fiber is different from that of the embodiment 1 in that in the step S2, the drawing speed of the drawing shaft a and the drawing shaft b is the same, and the drawing process ensures that the nickel wire is not deformed, so as to obtain the flexible conductive polyurethane fiber with a sheath-core structure. The conductivity of the obtained fiber (two-dimensional fiber) is 30S/m, the breaking strain is 1200%, the breaking stress is 27.15MPa, the performances of conductivity, breaking strain, breaking stress and the like are reduced, and further the core layer with a special structure is explained to ensure that the performance of the prepared sheath-core structure is better.
In summary, the flexible conductive polyurethane fiber and the preparation method thereof provided by the invention combine the coaxial spinning, the drafting process and the twisting process, prepare the conductive fiber with the sheath-core structure by utilizing the coaxial spinning, change the drafting speed of the core layer by changing the drafting speeds of different drafting shafts, further change the structure of the core layer metal wire, generate the core layer with a special two-dimensional bending structure with a certain bending angle or generate the core layer with a special three-dimensional spiral structure (twisting is needed), and finally thin and fast solidify the skin layer by the fast drafting of the drafting shafts in the coagulating bath, and the metal wire with the special structure is uniformly distributed in the skin layer material at the moment, thus obtaining the high-performance two-dimensional or three-dimensional flexible conductive polyurethane fiber; the obtained conductive fiber has an electric signal which can be converted along with the strain and has extremely high elastic performance; the preparation method has the advantages of simple process, controllable parameters, simple operation and obvious feasibility.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. A preparation method of flexible conductive polyurethane fiber is characterized in that: the method comprises the following steps:
s1, dissolving polyurethane resin in a polar solvent according to a preset proportion, mechanically stirring uniformly at 20-30 ℃ and then vacuum defoaming to obtain spinning solution;
s2, transmitting the metal fiber into a core layer channel by utilizing coaxial spinning, filling the spinning solution obtained in the step S1 into a skin layer channel, and firstly keeping the first drawing speed of the metal fiber in the core layer channel and the extrusion speed of the spinning solution in the skin layer channel to be the same, so that the spinning solution is wrapped on the surface of the metal fiber; after a certain distance of drawing, drawing the metal fiber by adopting a second drawing speed smaller than the first drawing speed so as to bend the metal fiber to form a two-dimensional bending structure; drawing a certain distance, then entering a coagulating bath, and drawing the skin layer at a third drawing speed to obtain a two-dimensional flexible conductive polyurethane fiber; the third draft speed is greater than the first draft speed;
or twisting the metal fiber at a preset rotating speed while drawing to bend the metal fiber to form a three-dimensional spiral structure, so as to obtain the three-dimensional flexible conductive polyurethane fiber;
the first drafting speed is 1-5mm/s, the second drafting speed is 0.5-4mm/s, and the third drafting speed is 2-8mm/s;
the first drafting speed has a drafting distance of 0.1-5cm, the second drafting speed has a drafting distance of 0.1-10cm, and the third drafting speed has a drafting distance of 0.1-100cm;
the preset rotating speed in the twisting process is 0.5-25r/min, and the elastic retraction rate of the metal fiber is 0-50%;
the two-dimensional bending structure is a wavy bending structure, the height of the wavy bending structure is 2-200 mu m, and the distance between the wave crests of adjacent waves is 1-100mm; the three-dimensional spiral structure is a spring-shaped structure, the height of the spring-shaped structure is 2-200 mu m, and the distance between adjacent threads is 1-100mm.
2. The method for preparing the flexible conductive polyurethane fiber according to claim 1, wherein: in step S2, the metal fiber includes one or more of nickel wire, cobalt wire, iron wire, copper wire, zinc wire, gold wire, and silver wire.
3. The method for preparing the flexible conductive polyurethane fiber according to claim 1, wherein: in the step S1, the mass ratio of the polyurethane resin to the polar solvent is (20% -45%) (55% -80%).
4. The method for preparing the flexible conductive polyurethane fiber according to claim 1, wherein: in the step S2, the temperature of the coagulating bath is 20-30 ℃, and the coagulating bath is one of dimethyl silicone oil, ethyl silicone oil and propyl silicone oil.
5. The method for preparing the flexible conductive polyurethane fiber according to claim 1, wherein: in step S1, the polar solvent includes one or more of tetrahydrofuran, N, dimethylformamide, N, dimethylacetamide.
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