CN103255634A - Preparation method of polyacrylonitrile/polyaniline compound micro-nano conductive fiber - Google Patents
Preparation method of polyacrylonitrile/polyaniline compound micro-nano conductive fiber Download PDFInfo
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Abstract
The invention discloses a preparation method of a polyacrylonitrile/polyaniline compound micro-nano conductive fiber. The preparation method comprises the following steps of: (1) dissolving polyacrylonitrile and polyethylene glycol into dimethylformamide; standing, de-foaming, and spinning a polyacrylonitrile/polyethylene glycol micro-nano fiber in an electrostatic spinning device; (2) placing the polyacrylonitrile/polyethylene glycol micro-nano fiber into water of 40-90 DEG C for 10-60 minutes to obtain a polyacrylonitrile porous micro-nano fiber; and (3) adding an aniline monomer into hydrochloric acid; uniformly agitating and immersing the polyacrylonitrile porous micro-nano fiber in the solution; and adding hydrochloric acid dissolved with ammonium persulfate to react for 0.5-3 hours to obtain the polyacrylonitrile/polyaniline compound micro-nano conductive fiber. The polyethylene glycol used in the preparation method disclosed by the invention is a water-soluble polymer which has a wide application range, has no pollution to an environment, and is cheap and easy to obtain, environment-friendly and low in cost.
Description
Technical field
The invention belongs to composite conducting fiber and preparation field thereof, particularly a kind of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber and preparation method thereof.
Background technology
The MacDiarmid of Univ Pennsylvania USA leader's in 1976 research group has found that the organic polymer polyacetylene has the electric conductivity of metalloid after mixing, and has from then on started the upsurge of research and development conducting polymer all over the world.In research subsequently, find polyparaphenylene, polypyrrole, polyphenylene sulfide, polythiophene in succession, poly-multiple conjugated structure macromolecules such as styrene support, polyaniline had high electrical conductivity after doping.The research of conducting polymer not only has great value in theory, and has very big using value.
Polyaniline is compared with other structural conductive polymer, have that raw material is easy to get, prepares easy, the good stability in empty G﹠W, the charge storage ability is strong, electrical conductivity is high, also have unique characteristics such as doping phenomenon, thereby cause domestic and international researcher's extensive interest, and be considered to one of the most promising conducting polymer.Prepare conductive fiber with polyaniline, not only excellent conductivity is lasting, and passes through to change the concentration of dopant acid, the resistivity that is easy to regulate fiber, and this is the not available advantageous property of other conductive fiber; Except electric conductivity, polyaniline also has good electromagnetic microwave absorbent properties, chemical property, optical property etc., has broad application prospects at many special dimensions.Therefore, in the research for application and development of polyaniline, preparation layer/polyaniline conductive fiber is one of research emphasis.
But because the strong interaction of the strong rigidity of polyaniline chain and interchain makes it molten not insoluble, corresponding machinability, spinnability are also poor, have limited its extensive use technically.The adsorpting polymerization method is exactly one of method that realizes the polyaniline machinability.Situ aggregation method claims " scene " adsorpting polymerization method again, and when being equipped with the layer/polyaniline conductive fiber with this legal system, the synthetic reaction of polyaniline is to carry out on the surface of fiber.General technology is to adsorb a certain amount of aniline monomer earlier on the chemical fibre surface, adds oxidant and adulterant then under certain reaction condition, and aniline monomer oxidative polymerization takes place under the effect of oxidant and adulterant generates electrically conductive polyaniline.The electrically conductive polyaniline that generates is attached to fiber surface, thereby makes fiber have electric conductivity.Adopting situ aggregation method to prepare the layer/polyaniline conductive fiber and compare with the method for existing preparation conductive fiber and have preparation process condition and realize, save advantages such as cost, fiber electric conductivity be good easily, is a kind of new thought for preparing conductive fiber.
The researcher has made some preliminary effects aspect the layer/polyaniline conductive fiber adopting situ aggregation method to prepare, but still there are many deficiencies in the research of this respect.Adopt the method to be difficult to make fiber to adsorb electrically conductive polyaniline effectively, adopt the method to prepare the polyaniline composite conductive fabric and tend to occur conducting polymer and be combined insecure, problem such as the surface dispersion is inhomogeneous with matrix fiber, thereby cause composite conductive fabric poor stability, electric conductivity low.Thereby influenced stability and the persistence of conductive fiber, therefore the conductive effect that adopts this legal system to get fiber often differs greatly, and can not produce the fiber with stable, lasting conductive effect, thereby can't realize suitability for industrialized production.As long as thoroughly solved the absorption problem of fiber to electrically conductive polyaniline, it will become a kind of new method of preparation conductive fiber and be used widely.
On the other hand, the polyaniline material of nanostructured is because its special nanometer size effect, and controlled electrochemistry, optical property, caused people's very big concern in the novel nano field of functional materials, become the hot fields of nanometer technology and material science research gradually.Existing researcher adopts " scene " adsorpting polymerization method to generate polyaniline on the micro nanometer fiber surface, preparation nano polyaniline composite conducting fiber, at first adopt method of electrostatic spinning to prepare polymethyl methacrylate (PMMA) nanofiber as patent 200810059548.8, then by in-situ polymerization thereon composite polyphenylene amine (PANI) obtain PMMA/PANI nanofiber laminated film; Patent 201110269757.7 at first utilizes method of electrostatic spinning to get the micro nanometer fiber of arranging in order; With arranging micro nanometer fiber in order as template, at template fiber surface in-situ polymerization parcel one deck conducting polymer, arranged the conductive polymer micro-nano rice composite fibre of coaxial configuration in order then; Patent 00510076659.6 has utilized electrostatic spinning and in-situ chemical oxidation polymerization method to prepare ultra-hydrophobic conductive macromolecular nano fiber.But above method all exists the limited problem of effective absorption of electrically conductive polyaniline.
Summary of the invention
The present invention will provide a kind of " scene " adsorpting polymerization to prepare the method for polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber.This method will thoroughly solve the nanofiber matrix to the absorption problem of electrically conductive polyaniline.
The invention provides the preparation method of a kind of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber, specifically comprise the steps:
(1) polyacrylonitrile and polyethylene glycol are dissolved in the dimethyl formamide, be mixed with the spinning solution that mass fraction is 7-14%, the mass ratio of polyethylene glycol and polyacrylonitrile is 15-35:85-65, spins polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming in electrostatic spinning apparatus;
(2) polyacrylonitrile in the step (1)/polyethylene glycol micro nanometer fiber is placed 40 ℃-90 ℃ water 10-60 minute, obtain polyacrylonitrile porous micro nanometer fiber;
(3) aniline monomer with the 2-10 weight portion joins in the hydrochloric acid of 200 weight portions, immerse the polyacrylonitrile porous micro nanometer fiber of 2-10 weight portion after stirring, be under 0-40 ℃ the condition in temperature, the hydrochloric acid that is dissolved with ammonium persulfate that adds the 80-100 weight portion, the quality of ammonium persulfate accounts for the 3-15% of hydrochloric acid quality, reacted 0.5-3 hour, and obtained the micro-nano conductive fiber of polyacrylonitrile/polyaniline.
The molecular weight of polyethylene glycol is 4000-20000 in the described step (1), and the molecular weight of polyacrylonitrile is 50000-100000, and spinning voltage is 10-20KV, and the spinning solution rate of flow of fluid is 0.5-1.5ml/h, and collecting distance is 10-25cm.
The concentration of described hydrochloric acid is 0.5-2mol/L.
The invention has the beneficial effects as follows: at first adopt method of electrostatic spinning to prepare polyacrylonitrile/polyethylene glycol micro nanometer fiber, then the polyethylene glycol water in the micro nanometer fiber is dissolved and obtain polyacrylonitrile porous micro nanometer fiber, adopt " scene " adsorpting polymerization method to make aniline monomer polymerization in the surface of the micro-nano porous fibre of polyacrylonitrile and hole at last, obtain polyacrylonitrile/layer/polyaniline conductive micro nanometer fiber.Improve the content of polyaniline in fiber, really solved effective absorption problem of polyaniline.Fiber has stable, lasting conductive effect.Ratio by control polyacrylonitrile and polyethylene glycol, spinning process condition, on-the-spot adsorpting polymerization reaction condition can fiber pattern and electric conductivity.Polyethylene glycol used in the present invention is a kind of broad-spectrum water soluble polymer, and to not pollution and cheap and easy to get, environmentally friendly of environment, cost is low.
The specific embodiment
Embodiment 1
Be 50,000 polyacrylonitrile, 30 grams with molecular weight with molecular weight be that 6000 polyethylene glycol 10 grams are dissolved in that to be mixed with mass fraction in the 460 gram dimethyl formamides be 8% spinning solution, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming.Spinning voltage is 10KV, and the spinning solution rate of flow of fluid is 0.5ml/h, and collecting distance is 15cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed 40 ℃ of water 60 minutes, get rid of the polyethylene glycol in the fiber, obtain polyacrylonitrile porous micro nanometer fiber.4 gram aniline monomers are joined in the aqueous hydrochloric acid solution of 200 1mol/L that restrain, the back immersion polyacrylonitrile porous that stirs micro nanometer fiber 6 grams, 0 ℃ of control temperature, the hydrochloric acid 1mol/L aqueous solution 100 grams that are dissolved with 10 gram ammonium persulfates are slowly added, reacted 3 hours, obtain the micro-nano conductive fiber of polyacrylonitrile/polyaniline, the diameter of fiber is at 240nm, and the electrical conductivity of fiber is 5.8 S/cm.
Embodiment 2
Be 50,000 polyacrylonitrile, 45 grams with molecular weight with molecular weight be that 6000 polyethylene glycol 15 grams are dissolved in that to be mixed with mass fraction in the 440 gram dimethyl formamides be 12% spinning solution, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming.Spinning voltage is 10KV, and the spinning solution rate of flow of fluid is 0.5ml/h, and collecting distance is 15cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed 50 ℃ of water 50 minutes, get rid of the polyethylene glycol in the fiber, obtain polyacrylonitrile porous micro nanometer fiber.3 gram aniline monomers are joined in the aqueous sulfuric acid of 200 1mol/L that restrain, the back immersion polyacrylonitrile porous that stirs micro nanometer fiber 10 grams, 10 ℃ of control temperature, slow 100 grams of the sulfuric acid water 1mol/L solution that is dissolved with 8 gram ammonium persulfates are added slowly, reacted 0.5 hour, obtain the micro-nano conductive fiber of polyacrylonitrile/polyaniline, the diameter of fiber is at 360nm, and the electrical conductivity of fiber is 0.013 S/cm.
Embodiment 3
Be 100,000 polyacrylonitrile, 40 grams with molecular weight with molecular weight be that 8000 polyethylene glycol 10 grams are dissolved in that to be mixed with mass fraction in the 450 gram dimethyl formamides be 10% spinning solution, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming.Spinning voltage is 15KV, and the spinning solution rate of flow of fluid is 1ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed 80 ℃ of water 20 minutes, get rid of the polyethylene glycol in the fiber, obtain polyacrylonitrile porous micro nanometer fiber.5 gram aniline monomers are joined in the aqueous hydrochloric acid solution of 200 0.5mol/L that restrain, micro-nano porous fibre 10 grams of the back immersion polyacrylonitrile that stirs, 30 ℃ of control temperature, the hydrochloric acid 0.5mol/L aqueous solution 100 grams that are dissolved with 10 gram ammonium persulfates are slowly added, reacted 2 hours, obtain the micro-nano conductive fiber of polyacrylonitrile/polyaniline, the diameter of fiber is at 420nm, and the electrical conductivity of fiber is 0.44 S/cm.
Embodiment 4
Be 80,000 polyacrylonitrile, 35 grams with molecular weight with molecular weight be that 6000 polyethylene glycol 15 grams are dissolved in that to be mixed with mass fraction in the 450 gram dimethyl formamides be 10% spinning solution, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming.Spinning voltage is 20KV, and the spinning solution rate of flow of fluid is 0.8ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed 60 ℃ of water 40 minutes, get rid of the polyethylene glycol in the fiber, obtain polyacrylonitrile porous micro nanometer fiber.9 gram aniline monomers are joined in the aqueous hydrochloric acid solution of 200 1.5mol/L that restrain, micro-nano porous fibre 2 grams of the back immersion polyacrylonitrile that stirs, 10 ℃ of control temperature, 1.5mol/L aqueous hydrochloric acid solution 100 grams that are dissolved with 15 gram ammonium persulfates are slowly added, reacted 1.5 hours, obtain the micro-nano conductive fiber of polyacrylonitrile/polyaniline, the diameter of fiber is at 380nm, and the electrical conductivity of fiber is 1.7 S/cm.
Embodiment 5
Be 50,000 polyacrylonitrile, 38 grams with molecular weight with molecular weight be that 6000 polyethylene glycol 7 grams are dissolved in that to be mixed with mass fraction in the 465 gram dimethyl formamides be 9% spinning solution, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming.Spinning voltage is 15KV, and the spinning solution rate of flow of fluid is 1ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed 60 ℃ of water 40 minutes, get rid of the polyethylene glycol in the fiber, obtain polyacrylonitrile porous micro nanometer fiber.10 gram aniline monomers are joined in the aqueous hydrochloric acid solution of 200 0.8mol/L that restrain, micro-nano porous fibre 6 grams of the back immersion polyacrylonitrile that stirs, 15 ℃ of control temperature, 0.8mol/L aqueous sulfuric acid 100 grams that are dissolved with 12 gram ammonium persulfates are slowly added, reacted 2 hours, obtain the micro-nano conductive fiber of polyacrylonitrile/polyaniline, the diameter of fiber is at 280nm, and the electrical conductivity of fiber is 0.25 S/cm.
Embodiment 6
Be 50,000 polyacrylonitrile, 32.5 grams with molecular weight with molecular weight be that 8000 polyethylene glycol 17.5 grams are dissolved in that to be mixed with mass fraction in the 450 gram dimethyl formamides be 10% spinning solution, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming.Spinning voltage is 20KV, and the spinning solution rate of flow of fluid is 1ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed 70 ℃ of water 40 minutes, get rid of the polyethylene glycol in the fiber, obtain polyacrylonitrile porous micro nanometer fiber.4 gram aniline monomers are joined in the aqueous hydrochloric acid solution of 200 1mol/L that restrain, the back immersion polyacrylonitrile porous that stirs micro nanometer fiber 6 grams, 0 ℃ of control temperature, the hydrochloric acid 1mol/L aqueous solution 100 grams that are dissolved with 10 gram ammonium persulfates are slowly added, reacted 3 hours, obtain the micro-nano conductive fiber of polyacrylonitrile/polyaniline, the diameter of fiber is at 300nm, and the electrical conductivity of fiber is 7.6 S/cm.
Embodiment 7
The preparation method of a kind of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in the dimethyl formamide, be mixed with mass fraction and be 7% spinning solution, the mass ratio of polyethylene glycol and polyacrylonitrile is 15:85, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming, the molecular weight of polyethylene glycol is 4000, and the molecular weight of polyacrylonitrile is 50000, and spinning voltage is 10KV, the spinning solution rate of flow of fluid is 0.5 ml/h, and collecting distance is 25cm;
(2) polyacrylonitrile in the step (1)/polyethylene glycol micro nanometer fiber is placed 40 ℃ water 10 minutes, obtain polyacrylonitrile porous micro nanometer fiber;
(3) 2 gram aniline monomers are joined in the 200 gram hydrochloric acid, the concentration of hydrochloric acid is 0.5mol/L, back immersion 2 gram polyacrylonitrile porous micro nanometer fibers stir, be under 0 ℃ the condition in temperature, add 80 and restrain the hydrochloric acid that is dissolved with ammonium persulfate, the quality of ammonium persulfate accounts for 3% of hydrochloric acid quality, reacts 0.5 hour, obtains the micro-nano conductive fiber of polyacrylonitrile/polyaniline.
Embodiment 8
The preparation method of a kind of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in the dimethyl formamide, be mixed with mass fraction and be 14% spinning solution, the mass ratio of polyethylene glycol and polyacrylonitrile is 35:85, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming, the molecular weight of polyethylene glycol is 20000, and the molecular weight of polyacrylonitrile is 100000, and spinning voltage is 20KV, the spinning solution rate of flow of fluid is 1.5ml/h, and collecting distance is 25cm;
(2) polyacrylonitrile in the step (1)/polyethylene glycol micro nanometer fiber is placed 90 ℃ water 60 minutes, obtain polyacrylonitrile porous micro nanometer fiber;
(3) 10 gram aniline monomers are joined in the 200 gram hydrochloric acid, the concentration of hydrochloric acid is 2 mol/L, back immersion 10 gram polyacrylonitrile porous micro nanometer fibers stir, be under 40 ℃ the condition in temperature, add 100 and restrain the hydrochloric acid that is dissolved with ammonium persulfate, the quality of ammonium persulfate accounts for 15% of hydrochloric acid quality, reacts 3 hours, obtains the micro-nano conductive fiber of polyacrylonitrile/polyaniline.
Embodiment 9
The preparation method of a kind of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in the dimethyl formamide, be mixed with mass fraction and be 10% spinning solution, the mass ratio of polyethylene glycol and polyacrylonitrile is 35:65, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming, the molecular weight of polyethylene glycol is 10000, and the molecular weight of polyacrylonitrile is 80000, and spinning voltage is 15 KV, the spinning solution rate of flow of fluid is 1 ml/h, and collecting distance is 20 cm;
(2) polyacrylonitrile in the step (1)/polyethylene glycol micro nanometer fiber is placed 80 ℃ water 50 minutes, obtain polyacrylonitrile porous micro nanometer fiber;
(3) 5 gram aniline monomers are joined in the 200 gram hydrochloric acid, the concentration of hydrochloric acid is 2mol/L, back immersion 5 gram polyacrylonitrile porous micro nanometer fibers stir, be under 20 ℃ the condition in temperature, add 100 and restrain the hydrochloric acid that is dissolved with ammonium persulfate, the quality of ammonium persulfate accounts for 10 % of hydrochloric acid quality, reacts 1.5 hours, obtains the micro-nano conductive fiber of polyacrylonitrile/polyaniline.
Embodiment 10
The preparation method of a kind of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in the dimethyl formamide, be mixed with the spinning solution that mass fraction is 12 %, the mass ratio of polyethylene glycol and polyacrylonitrile is 20:80, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming, the molecular weight of polyethylene glycol is 8000, and the molecular weight of polyacrylonitrile is 60000, and spinning voltage is 12 KV, the spinning solution rate of flow of fluid is 1 ml/h, and collecting distance is 15cm;
(2) polyacrylonitrile in the step (1)/polyethylene glycol micro nanometer fiber is placed 80 ℃ water 50 minutes, obtain polyacrylonitrile porous micro nanometer fiber;
(3) 8 gram aniline monomers are joined in the 200 gram hydrochloric acid, the concentration of hydrochloric acid is 1mol/L, back immersion 7 gram polyacrylonitrile porous micro nanometer fibers stir, be under 30 ℃ the condition in temperature, add 85 and restrain the hydrochloric acid that is dissolved with ammonium persulfate, the quality of ammonium persulfate accounts for 10% of hydrochloric acid quality, reacts 2.5 hours, obtains the micro-nano conductive fiber of polyacrylonitrile/polyaniline.
Claims (3)
1. the preparation method of polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber is characterized in that its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in the dimethyl formamide, be mixed with the spinning solution that mass fraction is 7-14%, the mass ratio of polyethylene glycol and polyacrylonitrile is 15-35:85-65, spins polyacrylonitrile/polyethylene glycol micro nanometer fiber after the standing and defoaming in electrostatic spinning apparatus;
(2) polyacrylonitrile in the step (1)/polyethylene glycol micro nanometer fiber is placed 40 ℃-90 ℃ water 10-60 minute, obtain polyacrylonitrile porous micro nanometer fiber;
(3) aniline monomer with the 2-10 weight portion joins in the hydrochloric acid of 200 weight portions, immerse the polyacrylonitrile porous micro nanometer fiber of 2-10 weight portion after stirring, be under 0-40 ℃ the condition in temperature, the hydrochloric acid that is dissolved with ammonium persulfate that adds the 80-100 weight portion, the quality of ammonium persulfate accounts for the 3-15% of hydrochloric acid quality, reacted 0.5-3 hour, and obtained polyacrylonitrile/polyaniline composite micro-nano rice conductive fiber.
2. the preparation method of polyacrylonitrile according to claim 1/polyaniline composite micro-nano rice conductive fiber, it is characterized in that: the molecular weight of polyethylene glycol is 4000-20000 in the described step (1), the molecular weight of polyacrylonitrile is 50000-100000, spinning voltage is 10-20KV, the spinning solution rate of flow of fluid is 0.5-1.5ml/h, and collecting distance is 10-25cm.
3. the preparation method of polyacrylonitrile according to claim 1/polyaniline composite micro-nano rice conductive fiber, it is characterized in that: the concentration of described hydrochloric acid is 0.5-2mol/L.
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| CN103965513A (en) * | 2014-04-29 | 2014-08-06 | 中原工学院 | Method for preparing polyaniline nanofiber/cellulose diacetate composite conductive material |
| CN103981693A (en) * | 2014-06-03 | 2014-08-13 | 陕西科技大学 | Polyaniline (PANI)-alkaline aramid fiber (ARF) composite conductive fiber and preparation method thereof |
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