CN113279150B - Preparation method of conductive polytetrafluoroethylene porous membrane - Google Patents
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Abstract
The invention discloses a preparation method of a conductive polytetrafluoroethylene porous membrane, which comprises the steps of uniformly mixing polytetrafluoroethylene water dispersion emulsion, polyvinyl alcohol solution and conductive materials to prepare spinning solution, then preparing a nascent polytetrafluoroethylene nanofiber membrane by adopting an electrostatic spinning method, then soaking the nascent polytetrafluoroethylene nanofiber membrane in a solution containing conductive materials, extruding redundant dispersion medium and conductive materials on the surface of the membrane, then carrying out hot pressing treatment, and sintering to obtain the conductive polytetrafluoroethylene porous membrane. The method combines the electrostatic spinning process and the dipping process, leads the conductive material to be uniformly distributed on the surface and the inside of the finished product film by adding the conductive material into the electrostatic spinning solution and dipping the solution containing the conductive material, further has conductivity on the surface and the cross section of the finished product film, namely the film has isotropy on the conductivity, and the preparation method and the film structure are simple to regulate and control, and are easy for industrial production.
Description
Technical Field
The invention relates to the technical field of membranes, in particular to a preparation method of a conductive polytetrafluoroethylene porous membrane.
Background
Polytetrafluoroethylene (PTFE) has been widely used in the fields of environmental protection, filtration, construction, aerospace and the like due to its excellent thermal stability, chemical stability, extremely low friction coefficient and hydrophobic property, and particularly in high-temperature filtration materials, PTFE biaxially oriented films with high porosity and a microfibrillar pore structure prepared by a biaxial orientation process are widely used due to the advantages of high filtration efficiency, low resistance, easy surface cleaning and the like. The currently used method for preparing the polytetrafluoroethylene porous membrane is paste extrusion and biaxial tension.
However, since PTFE molecules have an unbranched linear structure with symmetric perfluorocarbons and a resistivity of 1022-1024 Ω · m, which makes PTFE membrane surfaces susceptible to electrostatic accumulation and potentially explosive when exposed to chemical dust or coal dust, it is particularly important to improve the conductivity of PTFE membrane materials to impart antistatic properties. Document CN106910924 mixes PTFE micropowder and conductive powder in water, and after filtering and drying, adds an ethanol solvent, and then performs rolling and heat treatment to obtain a hydrophobic and conductive PTFE film, which is complicated in preparation process. Document CN101831123 adopts PTFE dispersed emulsion with a mass concentration of 60% to mix with conductive powder, and after drying, the conductive PTFE porous membrane is prepared by rolling, rolling and stretching. The conductive PTFE films prepared by the two methods have insufficient load capacity of conductive materials in the films, and conductive particles cannot be contacted with each other, so that the electric conduction cannot be realized in the cross section direction of the films.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the technical problem of providing a preparation method of a conductive polytetrafluoroethylene porous membrane.
The technical scheme for solving the technical problem is to provide a preparation method of a conductive polytetrafluoroethylene porous membrane, which is characterized by comprising the following steps:
step 1, uniformly mixing polytetrafluoroethylene water dispersion emulsion, polyvinyl alcohol solution and conductive material to prepare spinning solution, and then preparing a nascent polytetrafluoroethylene nanofiber membrane by adopting an electrostatic spinning method;
step 2, dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 into a solution containing a conductive material, wherein the conductive material is simultaneously loaded on the surface and inside of the nascent polytetrafluoroethylene nanofiber membrane in the dipping process;
step 3, extruding the redundant dispersion medium and the conductive material on the surface of the film obtained in the step 2; then carrying out hot-pressing treatment on the film to ensure that each layer of conductive material in the film is better contacted;
and 4, sintering the membrane obtained in the step 3 to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous membrane.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method combines the electrostatic spinning process and the dipping process, leads the conductive material to be uniformly distributed on the surface and the inside of the finished product film by adding the conductive material into the electrostatic spinning solution and dipping the solution containing the conductive material, and further leads the finished product film to have conductivity on the surface (X and Y directions) and the cross section (Z direction), namely the film has isotropy on the conductivity, overcomes the defect that the traditional conductive film only has conductivity on the surface of the film, and has simple regulation and control of the preparation method and the film structure and easy industrial production.
(2) The membrane material with a uniform nanofiber microporous structure is prepared by adopting an emulsion electrostatic spinning technology, the diameters of fibers are intensively distributed between 200nm and 300nm, the specific surface area of the membrane is larger, more conductive materials can be loaded, the loading amount is high, good contact among conductive material particles can be realized, the conductivity of the membrane is improved, and the isotropy is realized.
(3) In the dipping process, the conductive material is simultaneously loaded on the surface and inside of the nascent polytetrafluoroethylene nanofiber membrane, and the bonding performance of the conductive material and the membrane can be obviously improved after sintering.
(4) The method only adopts fiber-grade polyvinyl alcohol solution as a spinning carrier, and after sintering, polyvinyl alcohol can be decomposed to remove only polytetrafluoroethylene fibers and conductive materials. The used reagent is green and environment-friendly, the environmental pollution is greatly reduced, and the treatment and recovery cost of the solvent is avoided.
(5) The conductive polytetrafluoroethylene porous membrane prepared by the method has excellent comprehensive properties such as thermal stability, chemical stability and the like, has isotropic conductive performance, has stronger dredging effect on accumulated charges in a dust environment, and ensures the use safety.
Drawings
FIG. 1 is a surface electron micrograph of a conductive polytetrafluoroethylene porous film produced in example 1 of the present invention;
FIG. 2 is a cross-sectional electron micrograph of a conductive polytetrafluoroethylene porous film obtained in example 1 of the present invention;
FIG. 3 is a surface electron micrograph of a conductive polytetrafluoroethylene porous film obtained in example 2 of the invention;
FIG. 4 is a cross-sectional electron micrograph of a conductive polytetrafluoroethylene porous film obtained in example 2 of the invention.
Detailed Description
Specific examples of the present invention are given below. The specific examples are only intended to illustrate the invention in further detail and do not limit the scope of protection of the claims of the present application.
The invention provides a preparation method (method for short) of a conductive polytetrafluoroethylene porous membrane, which is characterized by comprising the following steps:
step 1, uniformly mixing polytetrafluoroethylene water dispersion emulsion, polyvinyl alcohol solution and conductive material to prepare spinning solution, and then preparing a nascent polytetrafluoroethylene nanofiber membrane by adopting an electrostatic spinning method;
preferably, in step 1, the polytetrafluoroethylene aqueous dispersion emulsion is a commercial polytetrafluoroethylene aqueous dispersion emulsion, and is a suspension obtained by dispersing polytetrafluoroethylene in water containing a certain surfactant, and the solid content is 60wt%.
Preferably, in the step 1, the mass fraction of the polytetrafluoroethylene in the spinning solution is 30-37.5 wt%; the mass fraction of the polyvinyl alcohol in the spinning solution is 3.75-5 wt%; the mass fraction of the conductive material in the spinning solution is 0.375wt% -1.875 wt%.
Preferably, in step 1, the process of the electrospinning method is: and (3) carrying out electrostatic spinning on the spinning solution for 3-6 h under the conditions that the voltage is 18-28 kv, the extrusion rate is 0.36-1.08 ml/h and the collection distance is 7-14 cm.
The conductive material is at least one of graphene oxide, a single-walled carbon nanotube, a multi-walled carbon nanotube, a hydroxylated carbon nanotube or graphite; the particle size of the conductive material is nano-scale, and the conductive material can be uniformly dispersed in an aqueous solution within a certain concentration range;
step 2, dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 in a solution containing a conductive material at room temperature for 20-40 min; in the dipping process, the conductive material is simultaneously loaded on the surface and the interior of the nascent polytetrafluoroethylene nanofiber membrane, and the bonding performance of the conductive material and the membrane can be obviously improved after sintering.
Preferably, in the step 2, the solution containing the conductive material is obtained by dispersing the conductive material in a dispersion medium by ultrasonic treatment for 15-30 min under the condition that the frequency is 20-40 KHz; the solid content of the conductive material in the solution containing the conductive material is 3-7 wt%; the dispersion medium is water, methanol, ethanol, ammonia water, N-methyl pyrrolidone, N-dimethylformamide or isopropanol;
preferably, in step 2, the immersion is carried out while continuously oscillating under ultrasonic conditions with a frequency of 15 to 25 KHz.
Step 3, extruding the redundant dispersion medium and the conductive material on the surface of the film obtained in the step 2 through an electric roller press; then, the membrane is subjected to hot pressing treatment by a hot press, so that each layer of conductive material in the membrane can be in good contact, the contact area is larger, the combination is tighter, and the conductivity of the membrane is improved;
preferably, in the step 3, the distance between two rollers of the electric roller press is 0.4-0.5 mm, the rotating speed of the rollers is 200-300 rpm, and the temperature is 20-30 ℃;
preferably, in the step 3, the temperature of a hot pressing plate of the hot press is 160-180 ℃, the pressure is 15-20 MPa, and the hot pressing time is 3-8 min;
and 4, sintering the membrane obtained in the step 3 to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous membrane.
Preferably, in step 4, the sintering process is: and (3) placing the film obtained in the step (3) in a muffle furnace, heating the film from room temperature to 360-380 ℃ at a heating rate of 0.8-1.5 ℃/min (preferably 1 ℃/min), and then preserving the heat for 3-6 h.
Example 1
Step 1, uniformly stirring 10g of polytetrafluoroethylene water dispersion emulsion (with the solid content of 60 wt%), 10g of polyvinyl alcohol aqueous solution (with the solid content of 10 wt%) and 0.2g of graphene oxide to obtain a spinning solution; performing electrostatic spinning on the spinning solution for 3 hours under the conditions that the voltage is 20kv, the extrusion rate is 0.48ml/h and the collection distance is 10cm to obtain a nascent polytetrafluoroethylene nanofiber membrane;
2, performing ultrasonic treatment on graphite for 15min under the condition of 20KHz to obtain graphite-containing ethanol dispersion liquid, wherein the content of graphite is 3wt%; dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 in an ethanol dispersion liquid containing graphite for 20min, and keeping the dispersion liquid to oscillate under the ultrasonic condition of 20KHz while dipping;
step 3, taking out the film, and extruding redundant ethanol and conductive materials on the surface of the film through an electric roller press, wherein the distance between two rollers of the electric roller press is 0.5mm, the rotating speed of the rollers is 200rpm, and the temperature is 25 ℃; and then, carrying out hot pressing treatment on the membrane by using a hot press, wherein the temperature of a hot pressing plate is 180 ℃, the pressure is 20MPa, and the hot pressing time is 5min.
And 4, heating the film obtained in the step 3 from room temperature to 360 ℃ at the heating rate of 1 ℃/min, sintering at the temperature for 3 hours to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous film.
As can be seen from fig. 1, the surface of the conductive film has been uniformly covered with graphene oxide and graphite.
As can be seen from fig. 2, the graphene oxide and the graphite are uniformly distributed between the electrospun fibers and filled in the conductive film.
As can be seen from fig. 1 and 2, the surface and the inside of the conductive film both contain graphene oxide and graphite having excellent conductivity, so that the conductive film has good conductivity on both the surface and the cross section.
Example 2
Step 1, uniformly stirring 15g of polytetrafluoroethylene water dispersion emulsion (with the solid content of 60 wt%), 10g of polyvinyl alcohol aqueous solution (with the solid content of 10 wt%) and 0.4g of hydroxylated carbon nanotube to obtain a spinning solution; carrying out electrostatic spinning on the spinning solution for 5 hours under the conditions that the voltage is 20kv, the extrusion rate is 0.72ml/h and the collection distance is 10cm, thus obtaining a nascent polytetrafluoroethylene nanofiber membrane;
2, performing ultrasonic treatment on graphite for 20min under the condition of 20KHz frequency to obtain graphite-containing ethanol dispersion liquid, wherein the content of graphite is 3wt%; dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 in an ethanol dispersion liquid containing graphite for 20min, and keeping the dispersion liquid oscillating under the ultrasonic condition of 20KHz while dipping;
step 3, taking out the film, and extruding redundant ethanol and conductive materials on the surface of the film through an electric roller press, wherein the distance between two rollers of the electric roller press is 0.5mm, the rotating speed of the rollers is 300rpm, and the temperature is 30 ℃; then, carrying out hot pressing treatment on the membrane by using a hot press, wherein the temperature of a hot pressing plate is 180 ℃, the pressure is 20MPa, and the hot pressing time is 5min;
and 4, heating the film obtained in the step 3 from room temperature to 370 ℃ at the heating rate of 1 ℃/min, sintering for 4 hours at the temperature to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous film.
As can be seen from fig. 3, the surface of the conductive film has been uniformly covered with the hydroxylated carbon nanotubes and graphite.
As can be seen from fig. 4, the hydroxylated carbon nanotubes and graphite are uniformly distributed between the electrospun fibers and filled inside the conductive film.
As can be seen from fig. 3 and 4, the surface and the inside of the conductive film both contain hydroxylated carbon nanotubes and graphite having excellent conductivity, so that the conductive film has good conductivity on both the surface and the cross section.
Example 3
Step 1, uniformly stirring 20g of polytetrafluoroethylene water dispersion emulsion (with the solid content of 60 wt%), 12g of polyvinyl alcohol aqueous solution, 0.2g of hydroxylated carbon nanotube (with the solid content of 10 wt%) and 0.2g of graphene oxide to obtain spinning solution; carrying out electrostatic spinning on the spinning solution for 5 hours under the conditions that the voltage is 21.5kv, the extrusion rate is 0.72ml/h and the collection distance is 12cm, thus obtaining a nascent polytetrafluoroethylene nanofiber membrane;
2, performing ultrasonic treatment on graphite for 20min under the condition of 20KHz frequency to obtain graphite-containing ethanol dispersion liquid, wherein the content of graphite is 5wt%; dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 in an ethanol dispersion liquid containing graphite for 20min, and keeping the dispersion liquid oscillating under the ultrasonic condition of 20KHz while dipping;
step 3, taking out the film, and extruding redundant ethanol and conductive materials on the surface of the film through an electric roller press, wherein the distance between two rollers of the electric roller press is 0.5mm, the rotating speed of the rollers is 250rpm, and the temperature is 30 ℃; then, carrying out hot pressing treatment on the membrane by using a hot press, wherein the temperature of a hot pressing plate is 170 ℃, the pressure is 28MPa, and the hot pressing time is 5min;
and 4, heating the film obtained in the step 3 from room temperature to 370 ℃ at the heating rate of 1 ℃/min, sintering for 4 hours at the temperature to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous film.
Example 4
Step 1, uniformly stirring 20g of polytetrafluoroethylene water dispersion emulsion (with the solid content of 60 wt%), 12g of polyvinyl alcohol aqueous solution, 0.2g of hydroxylated carbon nanotube (with the solid content of 10 wt%) and 0.2g of graphene oxide to obtain spinning solution; carrying out electrostatic spinning on the spinning solution for 6 hours under the conditions that the voltage is 25kv, the extrusion rate is 0.95ml/h and the collection distance is 10cm, thus obtaining a nascent polytetrafluoroethylene nanofiber membrane;
2, performing ultrasonic treatment on graphite for 30min under the condition of 30KHz frequency to obtain graphite-containing ethanol dispersion liquid, wherein the content of graphite is 5wt%; dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 in an ethanol dispersion liquid containing graphite for 30min, and keeping the dispersion liquid to oscillate under the ultrasonic condition of 20KHz while dipping;
step 3, taking out the film, and extruding redundant ethanol and conductive materials on the surface of the film by using an electric roller press, wherein the distance between two rollers of the electric roller press is 0.5mm, the rotating speed of the rollers is 250rpm, and the temperature is 25 ℃; then, carrying out hot pressing treatment on the membrane by using a hot press, wherein the temperature of a hot pressing plate is 180 ℃, the pressure is 20MPa, and the hot pressing time is 8min;
and 4, heating the membrane obtained in the step 3 from room temperature to 380 ℃ at the heating rate of 1 ℃/min, sintering at the temperature for 6 hours to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous membrane.
The results of the tests according to examples 1-4 are shown in Table 1:
TABLE 1
As can be seen from Table 1, the electrical resistivity of the porous conductive polytetrafluoroethylene film measured by a digital multimeter was less than 60. Omega. Mm in both the X and Y directions, and less than 80. Omega. Mm in the Z direction, indicating that the film obtained by the present invention is excellent in electrical conductivity. The introduction of the conductive material can obviously improve the conductivity of the polytetrafluoroethylene film, but the mechanical property of the conductive film is slightly reduced, but the conductive film completely meets the application requirement of the film, mainly because the adhesion among polytetrafluoroethylene particles is influenced by the existence of conductive particles in the high-temperature sintering forming process, so that the fiber forming property is reduced.
Nothing in this specification is said to apply to the prior art.
Claims (9)
1. A method for preparing a conductive polytetrafluoroethylene porous membrane is characterized by comprising the following steps:
step 1, uniformly mixing polytetrafluoroethylene water dispersion emulsion, polyvinyl alcohol solution and conductive material to prepare spinning solution, and then preparing a nascent polytetrafluoroethylene nanofiber membrane by adopting an electrostatic spinning method;
step 2, dipping the nascent polytetrafluoroethylene nanofiber membrane obtained in the step 1 into a solution containing a conductive material, wherein the conductive material is simultaneously loaded on the surface and inside of the nascent polytetrafluoroethylene nanofiber membrane in the dipping process;
step 3, extruding the redundant dispersion medium and the conductive material on the surface of the film obtained in the step 2; then carrying out hot-pressing treatment on the film to ensure that each layer of conductive material in the film is better contacted;
the conductive material is at least one of graphene oxide, a single-walled carbon nanotube, a multi-walled carbon nanotube, a hydroxylated carbon nanotube or graphite; the particle size of the conductive material is nano-scale;
and 4, sintering the membrane obtained in the step 3 to remove polyvinyl alcohol, and sintering and molding polytetrafluoroethylene to obtain the conductive polytetrafluoroethylene porous membrane.
2. The method for producing an electrically conductive polytetrafluoroethylene porous membrane according to claim 1, characterized in that in step 1, the mass fraction of polytetrafluoroethylene in the spinning solution is 30 to 37.5wt%; the mass fraction of the polyvinyl alcohol in the spinning solution is 3.75 to 5wt%; the mass fraction of the conductive material in the spinning solution is 0.375wt% -1.875 wt%.
3. The method for preparing a conductive polytetrafluoroethylene porous membrane according to claim 1, wherein the electrospinning process in step 1 is: and (3) carrying out electrostatic spinning on the spinning solution for 3 to 6 hours under the conditions that the voltage is 18 to 28kv, the extrusion rate is 0.36 to 1.08ml/h, and the collection distance is 7 to 14cm.
4. The method for producing the electrically conductive polytetrafluoroethylene porous membrane according to claim 1, wherein in step 2, the nascent polytetrafluoroethylene nanofiber membrane of step 1 is immersed in a solution containing an electrically conductive material at room temperature for 20 to 40min.
5. The method for preparing the conductive polytetrafluoroethylene porous membrane according to claim 1, wherein in step 2, the solution containing the conductive material is obtained by dispersing the conductive material in a dispersion medium under the condition that the frequency is 20 to 40KHz and ultrasonic waves are applied for 15 to 30min; the solid content of the conductive material in the solution containing the conductive material is 3 to 7wt%; the dispersion medium is water, methanol, ethanol, ammonia water, N-methyl pyrrolidone, N-dimethylformamide or isopropanol.
6. The method for producing an electrically conductive polytetrafluoroethylene porous film according to claim 1, wherein in step 2, the film is immersed while being continuously oscillated under an ultrasonic condition at a frequency of 15 to 25khz.
7. The method for preparing an electrically conductive polytetrafluoroethylene porous membrane according to claim 1, wherein in step 3, the excess dispersion medium and electrically conductive material on the surface of the membrane obtained in step 2 are extruded by an electric roll press; the distance between two rollers of the electric roller press is 0.4 to 0.5mm, the rotation speed of the rollers is 200 to 300rpm, and the temperature is 20 to 30 ℃.
8. The method for producing an electrically conductive polytetrafluoroethylene porous film according to claim 1, wherein in step 3, a hot press is used for hot pressing, the temperature of a hot press plate is 160 to 180 ℃, the pressure is 15 to 20MPa, and the hot pressing time is 3 to 8min.
9. The method for preparing a conductive polytetrafluoroethylene porous membrane according to claim 1, wherein in the step 4, the sintering process is: and (3) placing the film obtained in the step (3) in a muffle furnace, heating the film from room temperature to 360-380 ℃ at a heating rate of 0.8-1.5 ℃/min, and then preserving heat for 3-6 h.
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