CN109750387B - Preparation method of oriented conductive hydrogel fiber material - Google Patents
Preparation method of oriented conductive hydrogel fiber material Download PDFInfo
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Abstract
An oriented conductive hydrogel fiber material and a preparation method thereof. Firstly, conductive particle dispersion liquid with different concentrations is obtained by adopting an ultrasonic dispersion method, and the dispersed conductive particles are in a uniform dispersion state from a mutual agglomeration or entanglement state so as to meet the requirements of subsequently enhancing the strength and the conductivity of a matrix. And then compounding the conductive particles into a gelable organic polymer solution to form a composite electrospinning precursor solution meeting the electrospinning concentration and viscosity, and electrospinning by adopting a liquid rotary receiving disc to prepare the polymer composite conductive particle hydrogel fiber with the oriented micro-nano fiber structure. The method is different from the design of single physical factor introduction of the traditional hydrogel, the oriented micro-nano fiber structure, the sensitive variable conductivity and the mechanical strength are simultaneously introduced into a hydrogel system, the hydrogel fiber material with excellent performance is prepared, and a new preparation technology is provided for material preparation in the fields of biomedical bracket materials, flexible electrode materials, biosensors and the like.
Description
Technical Field
The invention belongs to the field of materials, and particularly provides a method for preparing an oriented conductive hydrogel fiber material.
Background
The hydrogel material has the characteristics of excellent biocompatibility, degradability, flexibility and the like, and is widely applied to the fields of biomedical bracket materials, flexible electrodes or biosensors and the like. In the aspect of designing biomedical scaffold materials, the scaffold materials with human-like tissue structure characteristics tend to be designed and prepared. The scaffold material can be well matched with human tissues in terms of mechanical properties, and the requirements of implantation are met. Meanwhile, the design and preparation of the scaffold material also take the functional characteristics of corresponding tissues, such as the conductive performance of nerve tissues and muscle tissues, into consideration to the greatest extent. Therefore, the design and preparation of the conductive hydrogel material with good biocompatibility have important significance. Moreover, the realization of the conductive function not only well simulates the characteristics of the tissues in vivo, but also plays an important role in stem cell regulation and tissue repair. Flexible electrodes, biosensors and the like often use small changes of input and output electric signals as a standard for activity evaluation, so that a precise conductive system is constructed to improve the transmission speed and the sensing precision. However, the application of the traditional hydrogel material is also greatly limited because the traditional hydrogel material cannot effectively guide the distribution of the conductive particles on a macroscopic scale, and the sensitivity of the conductive material is further influenced.
Disclosure of Invention
The invention aims to provide a preparation process of oriented conductive hydrogel fibers, and the oriented conductive hydrogel fibers prepared by the invention have mechanical properties similar to those of extracellular matrix and good electric signal conduction capability, and can guide oriented growth and differentiation of cells. Through the control of the preparation process, the conductive particles can be well arranged in the hydrogel fiber in an orientation mode. The preparation of the high-conductivity oriented hydrogel fiber can be realized by regulating and controlling the concentration and the arrangement mode of the conductive particles.
A preparation method of oriented conductive hydrogel fiber is characterized in that one or more polymer solutions of polymer sodium alginate, chitosan, acrylamide, gelatin, fibrin and collagen which can be gelatinized are used as a matrix, and conductive particles such as carbon nano tubes (carbon fibers), graphene, silver nano-particles, polypyrrole (PPy), Polyaniline (PANI), Polythiophene (PEDOT) particles and the like are doped for electrostatic spinning. The orientation preparation of the hydrogel fiber and the regulation and control of the diameter of the fiber are carried out by a method of rotating a receiving disc with adjustable rotating speed, and the mechanical strength and the conductivity of the hydrogel fiber are regulated by doping conductive particles with different concentrations. The method is beneficial to simultaneously introducing the oriented fiber structure and the conductive performance into a hydrogel system, and the oriented fibers with the diameter equivalent to that of the conductive particles can guide the conductive particles (fibers) to be oriented and arranged into a mutual lap joint mode, so that the hydrogel material with excellent performance is obtained, and ideas are provided for the fields of construction of biomedical engineering scaffolds, flexible electrodes, sensor materials and the like.
Furthermore, the diameter of the fiber on the surface of the hydrogel material is between hundreds of nanometers and hundreds of micrometers, the hydrogel material has the characteristic that the filling and guiding conductive particles form orientation arrangement among single fibers, and the fiber have good arrangement orientation;
the preparation method of the oriented fiber conductive hydrogel material is characterized by comprising the following steps:
(1) dispersion of conductive particle suspension: respectively adding conductive particles with different gradient masses and a dispersant with proper concentration into deionized water for magnetic stirring, and then carrying out ultrasonic dispersion on the conductive particle suspension in a cell crusher to obtain uniform dispersion liquid of conductive particles with different concentrations;
(2) preparing an electrospinning precursor solution: dissolving a certain mass of gellable macromolecules and an appropriate proportion of an electrospinning auxiliary agent PEO in the dispersion prepared in the step (1), and magnetically stirring;
(3) preparation of receiving solution: preparing corresponding receiving solution for gelation, uniformly placing the receiving solution in a rotating receiving disc, and adjusting the rotating speed of the receiving disc to 20-60 r/min;
(4) electrospinning: sucking the precursor liquid into an electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting a proper propulsion speed, connecting the positive electrode of a high-voltage power supply with a spinning nozzle, connecting the negative electrode of the high-voltage power supply with a receiving disc, adjusting the distance between an electrospinning needle head and the receiving disc to be 3-10cm, adjusting the voltage to be 3-10kV, and obtaining a single conductive oriented composite fiber filament with the diameter of hundreds of nanometers to hundreds of micrometers, wherein the arrangement of the fiber filament has good orientation.
Further, the concentration of the conductive particles in the dispersion liquid in the step (1) is 0.1mg/mL-10 mg/mL; the addition amount of the dispersing agent is 1wt% -20wt% of the mass of the conductive particles.
Further, the concentration of the electrospinning auxiliary agent PEO in the step (2) is 0.02wt% to 1 wt%.
Further, the receiving liquid in the step (3) is an aqueous solution of the corresponding crosslinking agent of the electrospun macromolecules.
Further, the propelling speed in the step (4) is 0.2 mL/h-4 mL/h.
The invention has the beneficial effects that: according to the invention, conductive particles with different concentrations are compounded into a high molecular solution, and the conductive hydrogel fiber is obtained by rotating liquid electrostatic spinning, so that the conductive particles can form oriented ordered arrangement in the hydrogel fiber, and the conductivity and tensile resistance of the hydrogel fiber are greatly improved. The hydrogel fiber has a micro/nano oriented fiber structure, makes up for the shortage of the traditional hydrogel in physical properties, expands the application range of the hydrogel and provides a good idea for the fields of biomedical materials, sensors and the like.
Drawings
FIG. 1: a sodium alginate-carbon nanotube composite oriented conductive hydrogel fiber optic mirror image;
FIG. 2: SEM image of sodium alginate-carbon nanotube composite oriented conductive hydrogel fiber;
Detailed Description
Example 1: sodium alginate-carbon nanotube composite oriented conductive hydrogel fiber
Adding carbon nanotubes with different masses and Pluronic F-127 with the mass of 5% of the carbon nanotubes into deionized water, magnetically stirring, and placing the mixture in an ice bath for ultrasonic dispersion with the dispersion power of 300W and the dispersion time of 30-120min to obtain a carbon nanotube dispersion liquid with the concentration of 0.2-5 mg/ml. And mixing 1% of sodium alginate and 0.2% of PEO in the dispersion liquid, and magnetically stirring for 1 hour to obtain the electrospinning precursor liquid. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; 50ml of 0.5mol/l CaCl2The solution is uniformly placed in a rotating liquid receiving disc, and the rotating speed of the receiving disc is adjusted to 50 revolutions per minute. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electro-spinning for 1h, and collecting fiber bundles to obtain the carbon nanotube-sodium alginate composite oriented fiber hydrogel doped with 0.2-5 mg/ml. FIG. 1 is a photograph of carbon nanotube-sodium alginate composite oriented fibers at 1mg/ml under a light mirror. FIG. 2 is a photograph of 1mg/ml carbon nanotube-sodium alginate composite oriented fiber under a scanning electron microscope.
Example 2: sodium alginate-Polythiophene (PEDOT) composite oriented conductive hydrogel fiber
Adding Polythiophene (PEDOT) with different masses into deionized water, magnetically stirring, and ultrasonically dispersing with dispersion power of 300W for 30-120min to obtain solution with a concentration of 0.2mg/mlml-5mg/ml PEDOT dispersion. And mixing 1% of sodium alginate and 0.2% of PEO in the dispersion liquid, and magnetically stirring for 1 hour to obtain the electrospinning precursor liquid. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; 50ml of 0.5mol/l CaCl2The solution is uniformly placed in a rotating liquid receiving disc, and the rotating speed of the receiving disc is adjusted to 50 revolutions per minute. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electro-spinning for 1h, and collecting fiber bundles to obtain the PEDOT-sodium alginate composite oriented fiber hydrogel doped with 0.2-5 mg/ml.
Example 3: chitosan-graphene composite oriented conductive hydrogel fiber
Adding different masses of graphene and SDS (sodium dodecyl sulfate) with the mass of 5% of the graphene into deionized water, carrying out magnetic stirring, and then placing the mixture into an ice bath for ultrasonic dispersion, wherein the dispersion power is 200W, and the dispersion time is 30-120min, so as to obtain 0.2-5 mg/ml of graphene dispersion liquid. And mixing 5% of chitosan and 0.2% of PEO in the dispersion liquid, magnetically stirring, and dissolving to obtain the electrospinning precursor liquid. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; uniformly placing 15% NaOH-30% anhydrous ethanol in a rotating liquid receiving disc, and adjusting the rotating speed of the receiving disc to 30 revolutions per minute. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electrospinning for 1h, and collecting fiber bundles to obtain the graphene-chitosan composite oriented fiber hydrogel doped with 0.2-5 mg/ml.
Example 4: chitosan-carbon nanotube composite oriented conductive hydrogel fiber
Adding different masses of graphene and Pluronic F-127 with the mass of 5% of the graphene into deionized water, carrying out magnetic stirring, and then placing the mixture into an ice bath for ultrasonic dispersion, wherein the dispersion power is 200W, and the dispersion time is 30-120min, so as to obtain 0.2-5 mg/ml of carbon nano tube dispersion liquid. And mixing 5% of chitosan and 0.2% of PEO in the dispersion liquid, magnetically stirring, and dissolving to obtain the electrospinning precursor liquid. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; uniformly placing 15% NaOH-30% anhydrous ethanol in a rotating liquid receiving disc, and adjusting the rotating speed of the receiving disc to 30 revolutions per minute. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electro-spinning for 1h, and collecting fiber bundles to obtain the carbon nanotube-chitosan composite oriented fiber hydrogel doped with 0.2-5 mg/ml.
Example 5: fibrin-polypyrrole (PPy) composite oriented conductive hydrogel fiber
Adding polypyrrole with different masses into a deionized water solution, performing magnetic stirring, performing ultrasonic dispersion, wherein the dispersion power is 200W, the dispersion time is 30-120min, obtaining 0.2-5 mg/ml polypyrrole dispersion liquid, then blowing and beating 4% of collagen by using a liquid-moving gun until the collagen is dissolved in the dispersion liquid, adding the prepared 1% of PEO solution, placing on a rotating disc, mixing for 20-30 min, and fully mixing the two to obtain the electrospinning precursor solution. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; mixing 5-10units/ml 0.5mol/LCaCl2The solution is uniformly placed in a rotating liquid receiving disc, and the rotating speed of the receiving disc is adjusted to be 30 revolutions per minute. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electro-spinning for 1h, and collecting fiber bundles to obtain the polypyrrole/fibrin composite oriented fiber hydrogel doped with 0.2-5 mg/ml.
Example 6: sodium alginate/polyacrylamide-carbon nanofiber composite oriented conductive hydrogel fiber
Adding carbon nanofibers with different masses and Pluronic F-127 with the mass of 5% of the carbon nanofibers into deionized water, carrying out magnetic stirring, and then placing the carbon nanofibers into an ice bath for ultrasonic dispersion, wherein the dispersion power is 200W, and the dispersion time is 30-120min, so that carbon nanofiber dispersion liquid with the mass of 0.2-5 mg/ml is obtained. Mixing with the above dispersion solution 1%And carrying out magnetic stirring on sodium alginate, 8% acrylamide and 0.1% PEO for 1h to obtain the electrospinning precursor solution. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; 50ml of 0.08% ammonium persulfate, 0.04% N-N' methylenebisacrylamide, 0.2% tetramethylethylenediamine and 0.5mol/L CaCl2The solution is evenly mixed and placed in a rotating liquid receiving disc under the irradiation of ultraviolet light, and the rotating speed of the receiving disc is adjusted to be 30 r/min. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electro-spinning for 1h, collecting the fiber bundle, and carrying out ultraviolet consolidation and solidification for 1h to obtain the carbon nanofiber-sodium alginate/polyacrylamide composite oriented fiber hydrogel doped with 0.2-5 mg/ml.
Example 7: sodium alginate/collagen-nano silver wire composite oriented conductive hydrogel fiber
Adding silver nanowires with different masses into 0.5mol/L acetic acid aqueous solution, performing magnetic stirring, performing ultrasonic dispersion, wherein the dispersion power is 200W, the dispersion time is 30-120min, obtaining 0.2-5 mg/ml silver nanowire dispersion, dissolving 0.5% collagen in the dispersion, performing magnetic stirring until the collagen is dissolved, and then adjusting the pH value of the solution to be about 6.5 by using NaOH. Mixing 2% of sodium alginate and 0.1% of PEO in the collagen solution, magnetically stirring, and dissolving to obtain the electrospinning precursor solution. Sucking the precursor liquid into a 1ml electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting the propulsion speed to be 1-2ml/h, connecting the anode of a high-voltage power supply with a spinning nozzle, connecting the cathode of the high-voltage power supply with a receiving disc, and adjusting the distance between an electrospinning needle head and the receiving disc to be 5-8 cm; 50ml of 0.5mol/LCaCl2(the pH is adjusted to about 4 by dilute hydrochloric acid) the solution is uniformly placed in a rotating liquid receiving disc, and the rotating speed of the receiving disc is adjusted to 30 r/min. And finally, switching on a high-voltage power supply, adjusting the voltage to be 4-7kV, electro-spinning for 1h, and collecting fiber bundles to obtain the nano silver wire-sodium alginate/collagen composite oriented fiber hydrogel doped with 0.2-5 mg/ml.
Claims (4)
1. A preparation method of an oriented conductive hydrogel fiber material is characterized in that one or more polymer solutions of polymer sodium alginate, chitosan, fibrin and collagen which can be gelatinized are used as a matrix, and carbon nano tubes, carbon fibers, graphene, silver nano, polypyrrole PPy, polyaniline PANI and polythiophene PEDOT conductive particles are doped for electrostatic spinning; meanwhile, polyethylene oxide (PEO) is added as an electrospinning auxiliary agent; the hydrogel fiber is subjected to oriented preparation and fiber diameter size regulation and control by a rotating receiving disc method with adjustable rotating speed, and the mechanical strength and conductivity of the hydrogel fiber are regulated by doping conductive particles with different concentrations, so that a hydrogel material with excellent performance is obtained; the preparation method comprises the following steps:
(1) dispersion of conductive particle suspension: respectively adding conductive particles with different gradient masses and a dispersant with proper concentration into deionized water for magnetic stirring, and then carrying out ultrasonic dispersion on the conductive particle suspension in a cell crusher to obtain uniform dispersion liquid of conductive particles with different concentrations; the concentration of the conductive particles in the dispersion liquid is 0.1mg/mL-10 mg/mL; the addition amount of the dispersing agent is 1 to 20 weight percent of the mass of the conductive particles;
(2) preparing an electrospinning precursor solution: dissolving a certain mass of colloid-forming polymer and PEO in a proper proportion into the dispersion prepared in the step (1), and carrying out magnetic stirring;
(3) preparation of receiving solution: preparing corresponding receiving solution for gelation, uniformly placing the receiving solution in a rotating receiving disc, and adjusting the rotating speed of the receiving disc to 20-60 r/min;
(4) electrospinning: sucking the precursor liquid into an electrospinning needle cylinder, fixing the electrospinning needle cylinder on a propulsion pump, setting a proper propulsion speed, connecting the positive electrode of a high-voltage power supply with a spinning spray head, connecting the negative electrode of the high-voltage power supply with a receiving disc, adjusting the distance between an electrospinning needle head and the receiving disc to be 3-10cm, adjusting the voltage to be 3-10kV, and obtaining a single conductive oriented composite fiber filament with the diameter of hundreds of nanometers to hundreds of micrometers, wherein the arrangement of the fiber filament has good orientation;
the diameter of the fiber on the surface of the hydrogel material is between hundreds of nanometers and hundreds of micrometers, the hydrogel material has the characteristic that the filling and guiding conductive particles form orientation arrangement among single fibers, and the fiber has good arrangement orientation.
2. The method for preparing an oriented conductive hydrogel fiber material according to claim 1, wherein the concentration of the electrospinning aid PEO in the step (2) is 0.02wt% to 1 wt%.
3. The method for preparing an oriented conductive hydrogel fiber material of claim 1, wherein the receiving liquid in step (3) is an aqueous solution of electrospun polymeric corresponding cross-linking agent.
4. The method of claim 1, wherein the advancing speed in step (4) is 0.2mL/h to 4 mL/h.
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