CN103255634B - A kind of preparation method of polyacrylonitrile/pocompounde compounde micro-nano conductive fiber - Google Patents
A kind of preparation method of polyacrylonitrile/pocompounde compounde micro-nano conductive fiber Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, its step is as follows: polyacrylonitrile and polyethylene glycol are dissolved in dimethyl formamide by (1), spins polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming in electrostatic spinning apparatus; (2) polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in the water 10-60 minute of 40 DEG C-90 DEG C, obtains polyacrylonitrile porous micro nanometer fiber; (3) join in hydrochloric acid by aniline monomer, immerse polyacrylonitrile porous micro nanometer fiber, add the hydrochloric acid being dissolved with ammonium persulfate after stirring, reaction 0.5-3 hour, obtains the micro-nano conductive fiber of polyacrylonitrile/polyaniline.Polyethylene glycol used in the present invention is a kind of broad-spectrum water soluble polymer, does not pollute and cheap and easy to get, environmentally friendly to environment, and cost is low.
Description
Technical field
The invention belongs to composite conducting fiber and preparation field thereof, particularly a kind of polyacrylonitrile/pocompounde compounde micro-nano conductive fiber and preparation method thereof.
Background technology
The research group of Univ Pennsylvania USA MacDiarmid leader in 1976 has found that organic polymer polyacetylene has the electric conductivity of metalloid after doping, has from then on started the upsurge of research and development conducting polymer all over the world.In research subsequently, in succession find polyparaphenylene, polypyrrole, polyphenylene sulfide, polythiophene, poly-after adulterating, there is high electrical conductivity to multiple conjugated structure macromolecules such as styrene support, polyanilines.The research of conducting polymer not only has great theory value, and has very large using value.
Polyaniline is compared with other Structural electric Polymer, have that raw material is easy to get, prepares easy, good stability in air and water, charge storage ability is strong, electrical conductivity is high, also there is the features such as unique doping phenomenon, thus cause the broad interest of domestic and international researcher, and be considered to one of the most promising conducting polymer.Prepare conductive fiber with polyaniline, not only excellent conductivity is lasting, and by changing the concentration of dopant acid, be easy to the resistivity regulating fiber, this is the advantageous property not available for other conductive fiber; Except electric conductivity, polyaniline also has excellent microwave absorption performance, chemical property, optical property etc., has broad application prospects at many special dimensions.Therefore, in the research for application and development of polyaniline, preparing Conductive Polyaniline Fibers is one of research emphasis.
But because the strong rigidity of polyaniline chain and the strong interaction of interchain make it molten not insoluble, corresponding machinability, spinnability are also poor, limit its extensive use technically.Adsorpting polymerization method is exactly one of method realizing polyaniline machinability.Situ aggregation method is also known as " scene " adsorpting polymerization method, and during by this legal system for Conductive Polyaniline Fibers, the synthetic reaction of polyaniline is carried out on the surface of fiber.General technology first adsorbs a certain amount of aniline monomer on chemical fibre surface, then under certain reaction condition, adds oxidant and adulterant, and aniline monomer oxidative polymerization occurs under the effect of oxidant and adulterant and generates electrically conductive polyaniline.The electrically conductive polyaniline generated is attached to fiber surface, thus makes fiber have electric conductivity.Adopting situ aggregation method to prepare Conductive Polyaniline Fibers and have the advantages such as preparation process condition easily realizes, cost-saving, filamentary conductive energy is excellent compared with the existing method preparing conductive fiber, is the new thought of one preparing conductive fiber.
Researcher has prepared in Conductive Polyaniline Fibers made some preliminary effects at employing situ aggregation method, but the research of this respect still exists many deficiencies.The method is adopted to be difficult to make fiber effectively adsorb electrically conductive polyaniline, adopt the method to prepare polyaniline composite conductive fabric and often occur that conducting polymer and matrix fiber are in conjunction with the problem such as insecure, Dispersion on surface is uneven, thus cause composite conductive fabric poor stability, electric conductivity low.Thus have impact on stability and the persistence of conductive fiber, the conductive effect therefore adopting this legal system to obtain fiber often differs greatly, and can not produce the fiber with stable, lasting conductive effect, thus cannot realize suitability for industrialized production.As long as thoroughly solve the absorption problem of fiber to electrically conductive polyaniline, it is used widely becoming a kind of new method preparing conductive fiber.
On the other hand, the polyaniline material of nanostructured is due to its special nanometer size effect, and controlled electrochemistry, optical property, arouse great concern in Nano-function thin films field, become the hot fields of nanometer technology and material science research gradually.Existing researcher adopts " scene " adsorpting polymerization method at micro nanometer fiber Surface Creation polyaniline, prepare nano polyaniline composite conducting fiber, as first patent 200810059548.8 adopts method of electrostatic spinning to prepare polymethyl methacrylate (PMMA) nanofiber, then by in-situ polymerization thereon composite polyphenylene amine (PANI) obtain PMMA/PANI nanofiber laminated film; First patent 201110269757.7 utilizes method of electrostatic spinning to obtain the micro nanometer fiber of ordered arrangement; Then use ordered arrangement micro nanometer fiber as template, wrap up one deck conducting polymer at template fiber surface in-situ polymerization, obtain the conductive polymer micro-nano rice composite fibre of ordered arrangement coaxial configuration; Patent 00510076659.6 make use of electrostatic spinning and in situ chemical oxidative polymerization method has prepared 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/pocompounde compounde micro-nano conductive fiber.The method will thoroughly solve the absorption problem of nanofiber matrix to electrically conductive polyaniline.
The invention provides a kind of preparation method of polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, specifically comprise the steps:
(1) polyacrylonitrile and polyethylene glycol are dissolved in 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 standing and defoaming in electrostatic spinning apparatus;
(2) polyacrylonitrile in step (1)/polyethylene glycol micro nanometer fiber is placed in the water 10-60 minute of 40 DEG C-90 DEG C, obtains polyacrylonitrile porous micro nanometer fiber;
(3) aniline monomer of 2-10 weight portion is joined in the hydrochloric acid of 200 weight portions, the polyacrylonitrile porous micro nanometer fiber of 2-10 weight portion is immersed after stirring, be under the condition of 0-40 DEG C in temperature, add the hydrochloric acid being dissolved with ammonium persulfate of 80-100 weight portion, the quality of ammonium persulfate accounts for the 3-15% of hydrochloric acid quality, reaction 0.5-3 hour, obtains the micro-nano conductive fiber of polyacrylonitrile/polyaniline.
In described step (1), the molecular weight of polyethylene glycol is 4000-20000, and the molecular weight of polyacrylonitrile is 50000-100000, and spinning voltage is 10-20KV, and 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: first adopt method of electrostatic spinning to prepare polyacrylonitrile/polyethylene glycol micro nanometer fiber, then the polyethylene glycol in micro nanometer fiber is obtained polyacrylonitrile porous micro nanometer fiber with water-soluble taking off, finally adopt " scene " adsorpting polymerization method that aniline monomer is polymerized in the surface and hole of the micro-nano porous fibre of polyacrylonitrile, obtain polyacrylonitrile/layer/polyaniline conductive micro nanometer fiber.Improve polyaniline content in the fibre, really solve effective absorption problem of polyaniline.Fiber has stable, lasting conductive effect.By controlling the ratio of polyacrylonitrile and polyethylene glycol, spinning process condition, field test study reaction condition can the pattern of fiber and electric conductivity.Polyethylene glycol used in the present invention is a kind of broad-spectrum water soluble polymer, does not pollute and cheap and easy to get, environmentally friendly to environment, and cost is low.
Detailed description of the invention
Embodiment 1
By molecular weight be 50,000 polyacrylonitrile 30 grams and the molecular weight polyethylene glycol 10 grams that is 6000 be dissolved in 460 grams of dimethyl formamides and be mixed with the spinning solution that mass fraction is 8%, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming.Spinning voltage is 10KV, and spinning solution rate of flow of fluid is 0.5ml/h, and collecting distance is 15cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in 40 DEG C of water 60 minutes, gets rid of the polyethylene glycol in fiber, obtain polyacrylonitrile porous micro nanometer fiber.4 grams of aniline monomers are joined in the aqueous hydrochloric acid solution of the 1mol/L of 200 grams, polyacrylonitrile porous micro nanometer fiber 6 grams is immersed after stirring, control temperature 0 DEG C, the hydrochloric acid 1mol/L aqueous solution 100 grams being dissolved with 10 grams of ammonium persulfates is slowly added, react 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
By molecular weight be 50,000 polyacrylonitrile 45 grams and the molecular weight polyethylene glycol 15 grams that is 6000 be dissolved in 440 grams of dimethyl formamides and be mixed with the spinning solution that mass fraction is 12%, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming.Spinning voltage is 10KV, and spinning solution rate of flow of fluid is 0.5ml/h, and collecting distance is 15cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in 50 DEG C of water 50 minutes, gets rid of the polyethylene glycol in fiber, obtain polyacrylonitrile porous micro nanometer fiber.3 grams of aniline monomers are joined in the aqueous sulfuric acid of the 1mol/L of 200 grams, polyacrylonitrile porous micro nanometer fiber 10 grams is immersed after stirring, control temperature 10 DEG C, slow 100 grams of the sulfuric acid water 1mol/L solution being dissolved with 8 grams of ammonium persulfates is added slowly, react 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
By molecular weight be 100,000 polyacrylonitrile 40 grams and the molecular weight polyethylene glycol 10 grams that is 8000 be dissolved in 450 grams of dimethyl formamides and be mixed with the spinning solution that mass fraction is 10%, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming.Spinning voltage is 15KV, and spinning solution rate of flow of fluid is 1ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in 80 DEG C of water 20 minutes, gets rid of the polyethylene glycol in fiber, obtain polyacrylonitrile porous micro nanometer fiber.5 grams of aniline monomers are joined in the aqueous hydrochloric acid solution of the 0.5mol/L of 200 grams, the micro-nano porous fibre of polyacrylonitrile 10 grams is immersed after stirring, control temperature 30 DEG C, the hydrochloric acid 0.5mol/L aqueous solution 100 grams being dissolved with 10 grams of ammonium persulfates is slowly added, react 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
By molecular weight be 80,000 polyacrylonitrile 35 grams and the molecular weight polyethylene glycol 15 grams that is 6000 be dissolved in 450 grams of dimethyl formamides and be mixed with the spinning solution that mass fraction is 10%, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming.Spinning voltage is 20KV, and spinning solution rate of flow of fluid is 0.8ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in 60 DEG C of water 40 minutes, gets rid of the polyethylene glycol in fiber, obtain polyacrylonitrile porous micro nanometer fiber.9 grams of aniline monomers are joined in the aqueous hydrochloric acid solution of the 1.5mol/L of 200 grams, the micro-nano porous fibre of polyacrylonitrile 2 grams is immersed after stirring, control temperature 10 DEG C, the 1.5mol/L aqueous hydrochloric acid solution 100 grams being dissolved with 15 grams of ammonium persulfates is slowly added, react 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
By molecular weight be 50,000 polyacrylonitrile 38 grams and the molecular weight polyethylene glycol 7 grams that is 6000 be dissolved in 465 grams of dimethyl formamides and be mixed with the spinning solution that mass fraction is 9%, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming.Spinning voltage is 15KV, and spinning solution rate of flow of fluid is 1ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in 60 DEG C of water 40 minutes, gets rid of the polyethylene glycol in fiber, obtain polyacrylonitrile porous micro nanometer fiber.10 grams of aniline monomers are joined in the aqueous hydrochloric acid solution of the 0.8mol/L of 200 grams, the micro-nano porous fibre of polyacrylonitrile 6 grams is immersed after stirring, control temperature 15 DEG C, the 0.8mol/L aqueous sulfuric acid 100 grams being dissolved with 12 grams of ammonium persulfates is slowly added, react 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
By molecular weight be 50,000 polyacrylonitrile 32.5 grams and the molecular weight polyethylene glycol 17.5 grams that is 8000 be dissolved in 450 grams of dimethyl formamides and be mixed with the spinning solution that mass fraction is 10%, in electrostatic spinning apparatus, spin polyacrylonitrile/polyethylene glycol micro nanometer fiber after standing and defoaming.Spinning voltage is 20KV, and spinning solution rate of flow of fluid is 1ml/h, and collecting distance is 20cm.Polyacrylonitrile/polyethylene glycol micro nanometer fiber is placed in 70 DEG C of water 40 minutes, gets rid of the polyethylene glycol in fiber, obtain polyacrylonitrile porous micro nanometer fiber.4 grams of aniline monomers are joined in the aqueous hydrochloric acid solution of the 1mol/L of 200 grams, polyacrylonitrile porous micro nanometer fiber 6 grams is immersed after stirring, control temperature 0 DEG C, the hydrochloric acid 1mol/L aqueous solution 100 grams being dissolved with 10 grams of ammonium persulfates is slowly added, react 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
A preparation method for polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in dimethyl formamide, be mixed with the spinning solution that mass fraction is 7%, the mass ratio of polyethylene glycol and polyacrylonitrile is 15:85, in electrostatic spinning apparatus, polyacrylonitrile/polyethylene glycol micro nanometer fiber is spun after standing and defoaming, the molecular weight of polyethylene glycol is 4000, and the molecular weight of polyacrylonitrile is 50000, and spinning voltage is 10KV, spinning solution rate of flow of fluid is 0.5 ml/h, and collecting distance is 25cm;
(2) polyacrylonitrile in step (1)/polyethylene glycol micro nanometer fiber is placed in the water 10 minutes of 40 DEG C, obtains polyacrylonitrile porous micro nanometer fiber;
(3) 2 grams of aniline monomers are joined in 200 grams of hydrochloric acid, the concentration of hydrochloric acid is 0.5mol/L, 2 grams of polyacrylonitrile porous micro nanometer fibers are immersed after stirring, be under the condition of 0 DEG C in temperature, add the hydrochloric acid that 80 grams are 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
A preparation method for polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in dimethyl formamide, be mixed with the spinning solution that mass fraction is 14%, the mass ratio of polyethylene glycol and polyacrylonitrile is 35:85, in electrostatic spinning apparatus, polyacrylonitrile/polyethylene glycol micro nanometer fiber is spun after standing and defoaming, the molecular weight of polyethylene glycol is 20000, and the molecular weight of polyacrylonitrile is 100000, and spinning voltage is 20KV, spinning solution rate of flow of fluid is 1.5ml/h, and collecting distance is 25cm;
(2) polyacrylonitrile in step (1)/polyethylene glycol micro nanometer fiber is placed in the water 60 minutes of 90 DEG C, obtains polyacrylonitrile porous micro nanometer fiber;
(3) 10 grams of aniline monomers are joined in 200 grams of hydrochloric acid, the concentration of hydrochloric acid is 2 mol/L, 10 grams of polyacrylonitrile porous micro nanometer fibers are immersed after stirring, be under the condition of 40 DEG C in temperature, add the hydrochloric acid that 100 grams are 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
A preparation method for polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in dimethyl formamide, be mixed with the spinning solution that mass fraction is 10%, the mass ratio of polyethylene glycol and polyacrylonitrile is 35:65, in electrostatic spinning apparatus, polyacrylonitrile/polyethylene glycol micro nanometer fiber is spun after 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, spinning solution rate of flow of fluid is 1 ml/h, and collecting distance is 20 cm;
(2) polyacrylonitrile in step (1)/polyethylene glycol micro nanometer fiber is placed in the water 50 minutes of 80 DEG C, obtains polyacrylonitrile porous micro nanometer fiber;
(3) 5 grams of aniline monomers are joined in 200 grams of hydrochloric acid, the concentration of hydrochloric acid is 2mol/L, 5 grams of polyacrylonitrile porous micro nanometer fibers are immersed after stirring, be under the condition of 20 DEG C in temperature, add the hydrochloric acid that 100 grams are 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
A preparation method for polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in 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, polyacrylonitrile/polyethylene glycol micro nanometer fiber is spun after 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, spinning solution rate of flow of fluid is 1 ml/h, and collecting distance is 15cm;
(2) polyacrylonitrile in step (1)/polyethylene glycol micro nanometer fiber is placed in the water 50 minutes of 80 DEG C, obtains polyacrylonitrile porous micro nanometer fiber;
(3) 8 grams of aniline monomers are joined in 200 grams of hydrochloric acid, the concentration of hydrochloric acid is 1mol/L, 7 grams of polyacrylonitrile porous micro nanometer fibers are immersed after stirring, be under the condition of 30 DEG C in temperature, add the hydrochloric acid that 85 grams are 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. a preparation method for polyacrylonitrile/pocompounde compounde micro-nano conductive fiber, is characterized in that, its step is as follows:
(1) polyacrylonitrile and polyethylene glycol are dissolved in 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 standing and defoaming in electrostatic spinning apparatus;
(2) polyacrylonitrile in step (1)/polyethylene glycol micro nanometer fiber is placed in the water 10-60 minute of 40 DEG C-90 DEG C, obtains polyacrylonitrile porous micro nanometer fiber;
(3) aniline monomer of 2-10 weight portion is joined in the hydrochloric acid of 200 weight portions, the polyacrylonitrile porous micro nanometer fiber of 2-10 weight portion is immersed after stirring, be under the condition of 0-40 DEG C in temperature, add the hydrochloric acid being dissolved with ammonium persulfate of 80-100 weight portion, the quality of ammonium persulfate accounts for the 3-15% of hydrochloric acid quality, reaction 0.5-3 hour, obtains polyacrylonitrile/pocompounde compounde micro-nano conductive fiber.
2. the preparation method of polyacrylonitrile/pocompounde compounde micro-nano conductive fiber according to claim 1, it is characterized in that: in described step (1), the molecular weight of polyethylene glycol is 4000-20000, the molecular weight of polyacrylonitrile is 50000-100000, spinning voltage is 10-20KV, 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/pocompounde compounde micro-nano conductive fiber according to claim 1, is characterized in that: the concentration of described hydrochloric acid is 0.5-2mol/L.
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