CN114606594B - Stretchable elastic conductive polymer-based hydrogel fiber and preparation method thereof - Google Patents
Stretchable elastic conductive polymer-based hydrogel fiber and preparation method thereof Download PDFInfo
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- 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
- D01F6/50—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 polyalcohols, polyacetals or polyketals
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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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- 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
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
Abstract
The invention relates to a stretchable elastic conductive polymer-based hydrogel fiber and a preparation method thereof. The method comprises the following steps: dissolving an elastic polymer matrix, an aniline monomer and an acid solution in deionized water, and then mixing with a sodium alginate solution and an initiator solution to obtain a spinning solution; carrying out wet spinning, namely carrying out instant freezing on the obtained hydrogel fiber, then carrying out in-situ polymerization and crosslinking reaction, thawing to obtain the hydrogel fiber with a skin-core structure, and dissolving the skin. The preparation process of the method is simple, the operation is easy, the mould is not needed in the hydrogel fiber forming process, the mould removing process is avoided, the spinning process is continuous, and the preparation method is obviously superior to the traditional template method.
Description
Technical Field
The invention belongs to the field of flexible wearable electronic devices, and particularly relates to a stretchable and elastic conductive polymer-based hydrogel fiber and a preparation method thereof.
Background
The hydrogel is a novel soft material with water as a matrix and is formed by crosslinking under the actions of chemistry or physics and the like. The hydrogel has soft and stretchable performance and biocompatibility, is considered as one of carrier candidates of next-generation wearable equipment, and has potential application value in the aspects of wearable sensing, energy storage, biomedical detection devices and the like. The braiding property of the fibrous hydrogel makes the fibrous hydrogel have unique advantages in wearable devices, such as good integration with clothes, excellent air permeability and the like, so that the development of the flexible stretchable elastic conductive hydrogel fiber has important significance.
The traditional conductive hydrogel fiber is mainly doped in the fiber or coated on the surface of the hydrogel fiber by the traditional conductive materials such as carbon materials, metal nano particles, conductive polymers and the like, so that the prepared conductive hydrogel fiber has poor stretchability, and the conductivity is remarkably reduced and is not easy to recover in the stretching process. The conductive polymer such as polyaniline, polypyrrole and the like can be polymerized and crosslinked in situ in the elastomer polymer material, so as to prepare the stretchable elastic hydrogel. However, continuous preparation of stretchable elastic conductive polymer-based hydrogel fibers has not been reported yet, and continuous preparation of hydrogel fibers has important significance for advancing practical progress thereof. Therefore, development of a new method for continuously preparing stretchable elastic conductive polymer-based hydrogel fibers is needed.
For example, chinese patent CN110938894a discloses an anti-freezing, self-repairing conductive nanocomposite hydrogel fiber and a preparation method thereof, the prepared fiber has no stretchability, and the method has no environmental protection property because aniline monomer bath is adopted for in-situ polymerization of conductive polymers. Chinese patent CN110157013a discloses a preparation method of high-stretchability polyaniline-based flexible conductive hydrogel, which cannot realize continuous preparation of fibrous conductive hydrogel. Chinese patent CN109880127a discloses a preparation method of a high-strength triple-network polypyrrole-based conductive composite hydrogel material, and the method adopts a die method to obtain the hydrogel, so that continuous preparation of fibrous hydrogel cannot be tested.
Disclosure of Invention
The invention aims to solve the technical problem of providing a stretchable elastic conductive polymer-based hydrogel fiber and a preparation method thereof, so as to overcome the defects that the polymer-based hydrogel fiber in the prior art cannot be continuously produced and has poor mechanical properties.
The invention provides a preparation method of stretchable elastic conductive polymer-based hydrogel fiber, which comprises the following steps:
(1) Dissolving an elastic polymer matrix, an aniline monomer and an acid solution in deionized water, and mixing the obtained mixed solution with a sodium alginate solution and an initiator solution to obtain a spinning solution;
(2) Carrying out wet spinning on the spinning solution obtained in the step (1), and extruding the spinning solution into a coagulating bath in which divalent or trivalent non-oxidant metal salt is dissolved to obtain hydrogel fibers;
(3) Instantly freezing the hydrogel fiber in the step (2), then carrying out in-situ polymerization and crosslinking reaction, thawing to obtain the hydrogel fiber with a skin-core structure, and dissolving the skin to obtain the stretchable elastic conductive polymer-based hydrogel fiber.
The elastic polymer matrix in the step (1) comprises one or more of polyvinyl alcohol, polyacrylamide, poly (N, N-dimethylacrylamide) and agar.
The concentration of the elastic polymer matrix in the mixed solution in the step (1) is 1-20wt%.
The concentration of the aniline monomer in the mixed solution in the step (1) is 0.025-5 mol/L.
The acid solution in the step (1) comprises one or more of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid solution with the concentration of 0.1-6 mol/L.
The concentration of the sodium alginate solution in the step (1) is 0.5-5 wt%.
The initiator in the step (1) comprises one or more of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide.
The concentration of the initiator solution in the step (1) is 0.025-5 mol/L.
The molar ratio of the aniline monomer to the initiator in the step (1) is 1:0.1-1:10.
The mixing in the step (1) is carried out at 0-4 ℃.
The extrusion speed in the step (2) is 0.5-2 ml/min.
The divalent non-oxidant metal salt in step (2) comprises CaCl 2 、BaCl 2 One or more of them.
The trivalent non-oxidant metal salt in step (2) comprises AlCl 3 。
The concentration of the divalent or trivalent non-oxidant metal salt in the coagulation bath in the step (2) is 1 to 20wt%.
The instantaneous freezing in the step (3) is as follows: the hydrogel fiber is pulled into a freezing solution for instantaneous freezing, wherein the freezing solution is dry ice or liquid nitrogen.
The temperature of the in-situ polymerization and crosslinking reaction in the step (3) is 0 to minus 80 ℃ and the time is 6 to 96 hours.
In the step (3), dissolving the skin as follows: dissolving the skin by using a citrate solution; the citrate comprises one or two of potassium citrate and sodium citrate, and the concentration of the citrate solution is 0.05-1.0 mol/L.
The invention also provides the stretchable and elastic conductive polymer-based hydrogel fiber prepared by the preparation method.
The invention also provides application of the stretchable elastic conductive polymer-based hydrogel fiber in wearable equipment.
The invention utilizes the principle that sodium alginate is rapidly gelled in a solution coagulating bath in which divalent (or trivalent) non-oxidative metal salt is dissolved, and the spinning solution containing sodium alginate is extruded into the coagulating bath to obtain the hydrogel fiber through wet spinning. Freezing the hydrogel fiber, and soaking the hydrogel fiber in citrate after low-temperature reaction to obtain the stretchable and elastic conductive polymer-based hydrogel fiber. The invention continuously prepares the conductive elastic hydrogel fiber which has excellent conductivity and stretchability.
Advantageous effects
(1) According to the invention, the sodium alginate hydrogel is rapidly formed by utilizing ion cross-linking induced by ion exchange between sodium alginate and divalent (or trivalent) non-oxidative metal salt cations, and the hydrogel fiber is prepared by utilizing the property through a wet spinning method. The preparation process is simple and easy to operate, the hydrogel fiber forming process does not need a die, the process of removing the die is avoided, the spinning process is continuous, and the preparation method is obviously superior to the traditional template method.
(2) The hydrogel fiber formed by the method disclosed by the invention is soaked in a simple citrate solution to dissociate sodium alginate gel, so that the brittle and tough transition of the fiber is realized, and the stretchability and elasticity of the hydrogel fiber are greatly improved.
Drawings
FIG. 1 is a sample view of a hydrogel fiber of the present invention.
FIG. 2 is a scanning electron microscope image of the hydrogel fibers of example 1.
FIG. 3 shows the mechanical and elastic properties of the hydrogel fibers of example 1.
Fig. 4 is a picture of the hydrogel fiber of example 1 as a wire-on line to illuminate an LED lamp.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The raw materials required by the embodiment of the invention are as follows: sodium alginate, N, N-methylene bisacrylamide, N, N, N ', N' -tetramethyl ethylenediamine are purchased from Allatin, polyvinyl alcohol (alcoholysis degree 98-99.8%), acrylamide, aniline, nitric acid, phosphoric acid, potassium persulfate, ammonium persulfate, sodium persulfate and hydrogen peroxide (30% aqueous solution) are purchased from national pharmaceutical chemicals Co. The raw materials and equipment used in the present invention are all commonly used raw materials and equipment unless otherwise specified.
The mechanical property testing method comprises the following steps: the mechanical properties of the prepared hydrogel fibers were tested at 23℃under 60% humidity using an MTS E42 stretcher, with a 20mm clamp spacing and a 10mm stretching rate -1 The number of samples was 5, the diameter of the hydrogel fiber was calculated by a microscope before the tensile test, and the relationship between the elongation at break and the tensile strength of the sample was obtained by the tensile test.
The conductivity test method comprises the following steps: the patent conductivity is obtained by using alternating current impedance spectrum test (Electrochemical Impedance Spectroscopy, EIS) test, an electrochemical workstation adopted by the test is Interface1000E of Gamry electrochemical instrument company in the United states, the experimental temperature is room temperature, and the frequency range is 0.01HZ-10 5 HZ, voltage disturbance was 5mV.
Example 1
10g of polyvinyl alcohol was first dissolved in 90ml of water at room temperature to prepare a 10wt% PVA aqueous solution. Taking 10ml of PVA aqueous solution after complete dissolution, stirring in a beaker, sequentially adding nitric acid solution (6 mol/L,166.7 mu L), aniline monomer (91.3 mu L) and sodium alginate (0.1 g) into the solution, and uniformly stirring to obtain a transparent viscous solution which is recorded as solution A; secondly, preparing sodium alginate solution with the concentration of 2wt% and recording the sodium alginate solution as solution B; finally, a solution of 0.1mol/L ammonium persulfate was prepared and designated as solution C. The preparation is implemented as follows: according to the volume ratio of 2:1:1, respectively taking A, B, C solutions according to the proportion, and uniformly stirring to obtain a precursor solution of the hydrogel. The gel precursor solution was bubble removed, filled into a 2ml syringe and extruded into a calcium chloride (10 wt%) solution at a rate of 1.5ml/min using a syringe pump, after fiber formation, it was transferred to liquid nitrogen for 15min, after freezing was completed, it was transferred to a freezer for 48h at low temperature (-10 ℃). After the reaction is finished, the hydrogel fiber is taken out from a refrigerator and thawed for 30min, and after the hydrogel fiber is completely thawed, the post-treatment is carried out: soaking with deionized water for 24h, and soaking with 0.5mol/L sodium citrate solution for 48h to obtain conductive elastic hydrogel fiber (figure 1). Fig. 2 is an electron micrograph of a hydrogel fiber showing the successful preparation of the hydrogel fiber and its abundant porosity, which is advantageous for improving its tensile properties. Its mechanical strength is 380kPa, and its elastic deformation can be up to 330% (figure 3). The prepared fiber is immersed in a glycerin/phosphoric acid (1:1) mixed aqueous solution, after being immersed for 2 hours, the fiber is taken out and connected with a circuit through a wire, an LED bulb (figure 4) can be lightened to show that the fiber has good conductivity, and the prepared hydrogel fiber has good conductivity and has the conductivity of 26S/m.
Example 2
To 10ml of water were added 0.1g of acrylamide and 0.06wt% of N, N-methylenebisacrylamide and 0.25wt% of N, N, N ', N' -tetramethylethylenediamine with respect to the acrylamide monomer and stirred to form a uniform solution, followed by sequentially adding nitric acid solution (6 mol/L, 166.7. Mu.L), aniline monomer (182.6. Mu.L) and sodium alginate (0.1 g), and after stirring uniformly, a transparent viscous solution was obtained and was designated as solution A; secondly, preparing sodium alginate solution with the concentration of 2wt% and recording the sodium alginate solution as solution B; finally, preparing 0.2mol/L sodium persulfate solution which is marked as solution C. According to the volume ratio of 2:1:1, respectively taking A, B, C solutions according to the proportion, and uniformly stirring to obtain a precursor solution of the hydrogel. The gel precursor solution was bubble removed, filled into a syringe and extruded into a calcium chloride (20 wt%) solution at a rate of 2.0ml/min using a syringe pump, after fiber formation, it was transferred to dry ice for 30min, after freezing was completed, it was transferred to a freezer for a reaction at low temperature (-40 ℃) for 72h. After the reaction is finished, the hydrogel fiber is taken out from a refrigerator and thawed for 30min, and after the hydrogel fiber is completely thawed, the post-treatment is carried out: soaking the conductive elastic hydrogel fiber in deionized water for 24 hours, and then soaking the conductive elastic hydrogel fiber in 0.1mol/L potassium citrate solution for 48 hours to obtain the conductive elastic hydrogel fiber, wherein the breaking strength can reach 400KPa, and the breaking elongation can reach 350%.
Example 3
To 10ml of 10wt% polyvinyl alcohol solution were sequentially added phosphoric acid solution (6 mol/L, 166.7. Mu.L), aniline monomer (273.9. Mu.L) and sodium alginate (0.2 g), and after stirring uniformly, a transparent viscous solution was obtained and was designated as solution A; secondly, preparing sodium alginate solution with the concentration of 2wt% and recording the sodium alginate solution as solution B; finally, 0.3mol/L potassium persulfate solution is prepared and is marked as solution C. According to the volume ratio of 2:1:1, respectively taking A, B, C solutions according to the proportion, and uniformly stirring to obtain a precursor solution of the hydrogel. The gel precursor solution was bubble removed, filled into a syringe and extruded into a calcium chloride (15 wt%) solution at a rate of 0.5ml/min using a syringe pump, after fiber formation, it was transferred to liquid nitrogen for 15min, after freezing was completed, it was transferred to a freezer for a reaction at low temperature (-50 ℃) for 72h. After the reaction is finished, the hydrogel fiber is taken out from a refrigerator and thawed for 30min, and after the hydrogel fiber is completely thawed, the post-treatment is carried out: soaking for 24 hours by deionized water, and soaking for 48 hours by 0.25mol/L sodium citrate solution to finally obtain the conductive elastic hydrogel fiber, wherein the breaking strength can reach 350KPa, and the breaking elongation is 300%.
Example 4
To 10ml of 7wt% polyvinyl alcohol solution were added nitric acid solution (6 mol/L, 166.7. Mu.L), aniline monomer (365.2. Mu.L) and sodium alginate (0.05 g) in this order, and after stirring well, a clear viscous solution was obtained and was designated as solution A; secondly, preparing sodium alginate solution with the concentration of 2wt% and recording the sodium alginate solution as solution B; finally, preparing 0.4mol/L hydrogen peroxide solution which is denoted as solution C. According to the volume ratio of 2:1:1, respectively taking A, B, C solutions according to the proportion, and uniformly stirring to obtain a precursor solution of the hydrogel. The gel precursor solution was bubble removed, filled into a syringe and extruded into a calcium chloride (15 wt%) solution at a rate of 1.0ml/min using a syringe pump, and after fiber formation, it was transferred to dry ice for 30min, and after freezing was completed, it was transferred to a freezer for a reaction at low temperature (-80 ℃) for 96h. After the reaction is finished, the hydrogel fiber is taken out from a refrigerator and thawed for 30min, and after the hydrogel fiber is completely thawed, the post-treatment is carried out: soaking the conductive elastic hydrogel fiber in deionized water for 24 hours, and then soaking the conductive elastic hydrogel fiber in 1.0mol/L sodium citrate solution for 48 hours to obtain the conductive elastic hydrogel fiber, wherein the breaking strength is 400KPa and 200%.
Claims (9)
1. A preparation method of stretchable elastic conductive polymer-based hydrogel fiber comprises the following steps:
(1) Dissolving an elastic polymer matrix, an aniline monomer and an acid solution in deionized water, and mixing the obtained mixed solution with a sodium alginate solution and an initiator solution to obtain a spinning solution, wherein the elastic polymer matrix comprises one or more of polyvinyl alcohol, polyacrylamide, poly (N, N-dimethylacrylamide) and agar;
(2) Carrying out wet spinning on the spinning solution obtained in the step (1), and extruding the spinning solution into a coagulating bath in which divalent or trivalent non-oxidant metal salt is dissolved to obtain hydrogel fibers;
(3) Instantly freezing the hydrogel fiber in the step (2), then carrying out in-situ polymerization and crosslinking reaction, and thawing to obtain the hydrogel fiber with a skin-core structure, and dissolving the skin by adopting a citrate solution to obtain the stretchable elastic conductive polymer-based hydrogel fiber.
2. The method according to claim 1, wherein the concentration of the elastic polymer matrix in the mixed solution in the step (1) is 1 to 20wt%.
3. The method according to claim 1, wherein the concentration of the aniline monomer in the mixed solution in the step (1) is 0.025 to 5mol/L; the acid solution comprises one or more of hydrochloric acid, sulfuric acid, phosphoric acid and nitric acid solutions with the concentration of 0.1-6 mol/L.
4. The preparation method according to claim 1, wherein the concentration of the sodium alginate solution in the step (1) is 0.5-5 wt%; the initiator comprises one or more of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide; the concentration of the initiator solution is 0.025-5 mol/L, and the molar ratio of the initiator to the aniline monomer is 1:0.1-1:10; the mixing is carried out at 0-4 ℃.
5. The method according to claim 1, wherein the extrusion speed in the step (2) is 0.5 to 2ml/min; divalent non-oxidant metal salts include CaCl 2 、BaCl 2 One or more of the following; trivalent non-oxidizer metal salts include AlCl 3 The method comprises the steps of carrying out a first treatment on the surface of the The concentration of the divalent or trivalent non-oxidant metal salt in the coagulation bath is 1 to 20wt%.
6. The method according to claim 1, wherein the instantaneous freezing in step (3) is: the hydrogel fiber is pulled into a freezing solution for instantaneous freezing, wherein the freezing solution is dry ice or liquid nitrogen; the temperature of in-situ polymerization and crosslinking reaction is 0 to minus 80 ℃ and the time is 6 to 96 hours.
7. The method according to claim 1, wherein the citrate in the step (3) comprises one or two of potassium citrate and sodium citrate, and the concentration of the citrate solution is 0.05-1.0 mol/L.
8. A stretchable, elastic, electrically conductive polymer-based hydrogel fiber prepared by the method of claim 1.
9. Use of the stretchable, elastic conductive polymer-based hydrogel fiber of claim 8 in a wearable device.
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