CN102151493A - Method for preparing nano polytetrafluoroethylene microporous membrane - Google Patents
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Abstract
The invention discloses a method for preparing a nano polytetrafluoroethylene microporous membrane, which comprises: mixing high-molecular-weight polytetrafluoroethylene dispersion resin and lubricating oil according to a weight ratio of (4-6):1, extruding a pasty material in an extruder at 20 to 120 DEG C, calendering the pasty material into a belt in a calender, and transversely stretching the belt by 0 to 8 times; removing oil in an oven at 50 to 300 DEG C to obtain a dry membrane, and stretching at 335 to 390 DEG C; and finally, performing thermosetting to obtain the polytetrafluoroethylene microporous membrane with an average thickness of 1 to 300 micrometers, an average aperture smaller than or equal to 180 nanometers, a porosity more than or equal to 78 percent, a water pressure resistance more than or equal to 3kg/cm<2>, and a moisture permeability more than or equal to 10,000 grams of water per square meter per day. The obtained microporous membrane has high nano fiber content and high mechanical strength such as tensile strength. The super-small nano micropores can meet the application requirements for higher water pressure resistance or better filtering effect.
Description
Technical field
The present invention relates to a kind of preparation method of nanoscale microporous teflon membran.
Background technology
Fluorine resin especially polyflon has all obtained extensive use because of having excellent physical and mechanical performance and chemical stability in each fields such as chemical industry, mechano-electronic, space flight military project, new material and new forms of energy.Polytetrafluoroethyldispersion dispersion resin is adopted the paste extruding and extrudes also de-oiling, pass through unidirectional or biaxial tension again, can obtain according to the polytetrafluoroethylene (PTFE) poromerics that micropore is arranged, because its property, this material becomes a kind of high-end functional fluoropolymer material, for example as filter membrane, clothes film, man-made organ, wire-insulating material and encapsulant etc.
Microporous teflon membran is because of having good mechanical performance, water-proof breathable properties, and chemical stability, and late nineteen seventies is firm to be used to do wire cable insulating material, artificial blood vessel, band, filter membrane, and clothes film once coming out.Industrial common employing high-purity tetrafluoro second hydrocarbon monomer, the dispersion polymerization processes of carrying out polymerization or copolymerization prepares dispersion resin.Because poly-tetrafluoro dispersion resin can not carry out molten thermoplastic processing, but can push by paste, extrude, de-oiling, unidirectional again or biaxial tension becomes the excellent material with little porous.
At present, it is that the disclosed preparation method of United States Patent (USP) of US 3953566 and US 4187390 prepares that microporous teflon membran adopts the patent No. usually, this preparation method mainly may further comprise the steps: after polytetrafluoroethyldispersion dispersion resin and kerosene blend, paste is extruded, de-oiling, under the polytetrafluoroethylene (PTFE) fusing point, carry out unidirectional or biaxial tension again, promptly get microporous teflon membran.Higher or the filter effect better application requirement of water pressure resistance can not be satisfied greater than 200 nanometers in the aperture of the microporous teflon membran of this method gained.
The patent No. of big capital company be US 5234739 U.S. Patent Publication the preparation method of another kind of microporous teflon membran, it is with after polytetrafluoroethyldispersion dispersion resin and the kerosene blend, paste is extruded, de-oiling, more than the polytetrafluoroethylene (PTFE) fusing point, carry out the sintering typing more earlier, below the polytetrafluoroethylene (PTFE) fusing point, carry out unidirectional or biaxial tension then, obtain the microporous teflon membran of micropore multifilamentization.The aperture of the microporous barrier of this method gained is greater than 100 nanometers, how between 200 ~ 500 nanometers, can not satisfy the higher or filter effect better application requirement of water pressure resistance equally.
The patent No. be US 5814405 U.S. Patent Publication the preparation method of another microporous teflon membran: after polytetrafluoroethyldispersion dispersion resin and kerosene blend, paste is extruded, de-oiling, below the polytetrafluoroethylene (PTFE) fusing point, carry out longitudinal stretching again, more than the polytetrafluoroethylene (PTFE) fusing point, carry out the sintering typing more earlier, below the polytetrafluoroethylene (PTFE) fusing point, carry out cross directional stretch then, obtained the microporous teflon membran of micropore multifilamentization, the aperture of the microporous barrier of this method gained is greater than 200 nanometers, how about 1000 nanometers, also can not satisfy the higher or filter effect better application requirement of water pressure resistance.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of preparation method of nanoscale microporous teflon membran is provided.
The water pressure resistance of the nanoscale microporous teflon membran that obtains with the method is higher, can satisfy the application of high requirement.
For solving above technical problem, a kind of technical scheme that the present invention takes is: a kind of preparation method of nanoscale microporous teflon membran is characterized in that this preparation method comprises the steps:
(1), with number-average molecular weight greater than 5*10
6, standard specific gravity is less than 2.165g/cm
3Polytetrafluoroethyldispersion dispersion resin and boiling point at the lubricating oil between 50 ℃ ~ 300 ℃ by weight after 4 ~ 6:1 mixes, under 20 ℃ ~ 120 ℃, extrude paste by the pushing machine, adopt calender that described paste is made belt, 0 ~ 8 times of cross directional stretch, de-oiling is a dry film in 50 ℃ ~ 300 ℃ baking oven then;
(2), step (1) gained dry film is stretched under 335 ℃ ~ 390 ℃, carry out thermal finalization at last, promptly obtain average thickness between 1 ~ 300 micron, average pore size is smaller or equal to 180 nanometers, porosity is more than or equal to 78%, water pressure resistance is more than or equal to 3 kilograms/square centimeter, and moisture permeability is more than or equal to the microporous teflon membran in 10000 gram water/square meter/skies.
Preferably, described polytetrafluoroethyldispersion dispersion resin standard specific gravity is 2.14 ~ 2.16g/cm
3
In the step (1), polytetrafluoroethyldispersion dispersion resin preferably mixes in relatively mild mode with lubricating oil.
In the step (2), when described stretching can be for longitudinal stretching, draw ratio was 1 ~ 200; Described stretching also can be cross directional stretch, and draw ratio is 5 ~ 50; Described stretching can also be biaxial tension, and wherein the cross directional stretch multiple is 1 ~ 200, and the longitudinal stretching multiple is 5 ~ 50.
According to the nanoscale microporous teflon membran of method for preparing, its average pore size is 10 ~ 180 nanometers, and porosity is 78% ~ 97%.Preferably, average pore size 30 ~ 100 nanometers of described nanoscale microporous teflon membran, porosity is 82% ~ 92%, and water pressure resistance is more than or equal to 5 kilograms/square centimeter, and moisture permeability is more than or equal to 15000 gram water/square meter/skies.
Preferably, the thickness of described nanoscale microporous teflon membran is between 1 ~ 200 micron, and air penetrability was smaller or equal to 18 seconds.
The present invention compared with prior art has the following advantages: the nanofiber content height of the nanoscale microporous teflon membran that preparation in accordance with the present invention obtained, its physical mechanical strength such as tension stress etc. are higher, through intensity is all above 300 kilograms/square centimeter after the stretching of carrying out draw direction under 335 ℃ ~ 390 ℃, its extra small nanometer micropore can satisfy the higher or filter effect better application requirement of water pressure resistance.
The specific embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment, but the invention is not restricted to these embodiment.
Embodiment 1
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.155 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. Exxon Mobile senior lubricant (trade mark Isopar K), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into the belt of about 0.08 cm of thickness.With behind 3 times of this wet band cross directional stretch in 220 ℃ baking oven de-oiling obtain dry film.With this dry film 10 times of longitudinal stretchings under 340 ℃ hot conditions, and then under 360 ℃ hot conditions 10 times of cross directional stretch, under 390 ℃ of high temperature, finalize the design at last, promptly obtain nanoscale microporous teflon membran of the present invention.After testing, the average pore size of gained nanoscale microporous teflon membran is 60 ~ 80nm, and porosity is 85% ~ 90%, and hot strength (laterally reaching vertically) is all greater than 500 kg/ cm
2, water pressure resistance is greater than 5kg/ cm
2, moisture permeability is greater than 15kg water/cm
2/ day, air penetrability is 9 ~ 11 seconds.
Embodiment 2
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.155 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. ExxonMobile senior lubricant (trade mark IsoparK), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into belt, the about 0.2cm of thickness.With behind 3.8 times of this wet band cross directional stretch in 220 ℃ baking oven de-oiling obtain dry film.With this dry film 30 times of longitudinal stretchings under 340 ℃ hot conditions, and then under 360 ℃ hot conditions 15 times of cross directional stretch, under 390 ℃ of high temperature, finalize the design at last, promptly obtain nanoscale microporous teflon membran of the present invention.After testing, the average pore size of gained nanoscale microporous teflon membran is 45 ~ 60nm, and porosity is 88% ~ 92%, and hot strength (laterally reaching vertically) is all greater than 700kg/cm
2, water pressure resistance is greater than 5 kg/ cm
2, moisture permeability is greater than 15kg water/cm
2/ day, air penetrability is 6 ~ 8 seconds.
Embodiment 3
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.155 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. Exxon Mobile senior lubricant (trade mark Isopar K), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into the belt of the about 0.07cm of thickness, this wet band de-oiling in 250 ℃ baking oven is obtained dry film.With this dry film 2 times of longitudinal stretchings under 345 ℃ hot conditions, and then under 360 ℃ hot conditions 15 times of cross directional stretch, under 390 ℃ of high temperature, finalize the design at last, promptly obtain nanoscale microporous teflon membran of the present invention.After testing, the average pore size of gained nanoscale microporous teflon membran is 100 ~ 110 nanometers, and porosity is 83% ~ 88%, and hot strength (laterally reaching vertically) is all greater than 300 kg/ cm
2, water pressure resistance is greater than 5kg/ cm
2, moisture permeability is greater than 15 kg water/cm
2/ day, air penetrability is 11 ~ 12 seconds.
Embodiment 4
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.155 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. Exxon Mobile senior lubricant (trade mark Isopar K), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into the belt of about 0.06 cm of thickness.The band de-oiling in 250 ℃ baking oven of will wetting then obtains dry film, with this dry film 10 times of cross directional stretch under 360 ℃ hot conditions, finalizes the design under 390 ℃ of high temperature at last, promptly obtains nanoscale microporous teflon membran of the present invention.After testing, the average pore size of gained nanoscale microporous teflon membran is 150 ~ 160 nanometers, porosity 80% ~ 85%, and hot strength (laterally) is greater than 300 kg/ cm
2, water pressure resistance is greater than 3 kg/ cm
2, moisture permeability is greater than 10 kg water/cm
2/ day, air penetrability is 15 ~ 16 seconds.
Embodiment 5
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.16 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. Exxon Mobile senior lubricant (trade mark Isopar K), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into the belt of the about 0.08cm of thickness.With 2 times of this wet band cross directional stretch, de-oiling obtains dry film in 220 ℃ baking oven then.With this dry film 5 times of longitudinal stretchings under 340 ℃ hot conditions, 10 times of cross directional stretch under 360 ℃ hot conditions are finalized the design under 390 ℃ of high temperature at last again, promptly obtain nanoscale microporous teflon membran of the present invention.After testing, between average pore size 90 ~ 110 nanometers of gained nanoscale microporous teflon membran, porosity 82% ~ 86%, hot strength (laterally reaching vertically) is all greater than 400 kg/ cm
2, water pressure resistance is greater than 3 kg/ cm
2, moisture permeability is greater than 15 kg water/cm
2/ day, air penetrability is 11 ~ 13 seconds.
The comparative example A
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.16 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. ExxonMobile senior lubricant (trade mark IsoparK), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into the belt of the about 0.08cm of thickness, with 2 times of this wet band cross directional stretch, de-oiling obtains dry film in 220 ℃ baking oven then.With this dry film 5 times of longitudinal stretchings under 300 ℃ hot conditions, and then under 300 ℃ hot conditions 10 times of cross directional stretch, under 390 ℃ of high temperature, finalize the design at last, the average pore size that obtains the nanoscale microporous teflon membran is 220 ~ 250 nanometers, porosity 82% ~ 86%, hot strength (laterally reaching vertically) is all less than 300kg/cm
2, water pressure resistance is less than 3 kg/ cm
2, moisture permeability is greater than 10 kg water/cm
2/ day, air penetrability is 13 ~ 15 seconds.
Comparative Examples B
With number-average molecular weight〉5 x 10
6, standard specific gravity is about 2.155 g/cm
3Polytetrafluoroethyldispersion dispersion resin mix mutually with the weight ratio of 5:1 with boiling point 180-200 ℃ U.S. Exxon Mobile senior lubricant (trade mark Isopar K), the gentle back that stirs is pressed into earlier cylinder in advance, extrude paste at 50 ℃ of following high pressure again, and roll into the belt of about 0.08 cm of thickness.This wet band de-oiling in 250 ℃ baking oven is obtained dry film, with this dry film 10 times of cross directional stretch under 250 ℃ hot conditions, under 390 ℃ of high temperature, finalize the design at last, the average pore size of the nanoscale microporous teflon membran that obtains is 250 ~ 300 nanometers, porosity is 80% ~ 85%, and hot strength (laterally reaching vertically) is all less than 300 kg/ cm
2, water pressure resistance is less than 3 kg/ cm
2, moisture permeability is greater than 10 kg water/cm
2/ day, air penetrability is 18 ~ 19 seconds.
Can find out that by above embodiment 1 to 5 adopt the temperature of polytetrafluoroethylene (PTFE) average fusing point more than 335 ℃ to carry out unidirectional or biaxial tension, both can prepare average pore size is 10 ~ 180 nanometers, the higher polytetrafluoroethylene film of water pressure resistance.
Polytetrafluoroethyldispersion dispersion resin that above embodiment adopted and lubricating oil can adopt as respective name products such as E.I.Du Pont Company, the big capital company of Japan, U.S. Exxon Mobile.
The method of testing of the data foundation among the above embodiment and the instrument that is adopted are respectively: the method for testing of mean pore size adopts Al Kut apertometer (Coulter Porometer) to detect according to ASTM standard E1298-89 method; Hot strength is to survey with tension intensity machine (Instron), and watertight method of testing adopts Mu Leng hydraulic pressure instrument (Mullen Tester) to detect according to ASTM standard D751-2006 method; The method of testing of moisture permeability is according to JIS standard L1099-B1 method; The method of testing of air penetrability adopts air permeable instrument (Gurley Densometer) detection in the song according to ASTM standard 0726-58 method.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit essence is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (10)
1. the preparation method of a nanoscale microporous teflon membran is characterized in that, this preparation method comprises the steps:
(1), with number-average molecular weight greater than 5*10
6, standard specific gravity is less than 2.165g/cm
3Polytetrafluoroethyldispersion dispersion resin and boiling point at the lubricating oil between 50 ℃ ~ 300 ℃ by weight after 4 ~ 6:1 mixes, under 20 ℃ ~ 120 ℃, extrude paste by the pushing machine, adopt calender that described paste is made belt, 0 ~ 8 times of cross directional stretch, de-oiling is a dry film in 50 ℃ ~ 300 ℃ baking oven then;
(2), step (1) gained dry film is stretched under 335 ℃ ~ 390 ℃, carry out thermal finalization at last, promptly obtain average thickness between 1 ~ 300 micron, average pore size is smaller or equal to 180 nanometers, porosity is more than or equal to 78%, water pressure resistance is more than or equal to 3 kilograms/square centimeter, and moisture permeability is more than or equal to the microporous teflon membran in 10000 gram water/square meter/skies.
2. the preparation method of nanoscale microporous teflon membran according to claim 1 is characterized in that: described polytetrafluoroethyldispersion dispersion resin standard specific gravity is 2.14 ~ 2.16g/cm
3
3. the preparation method of nanoscale microporous teflon membran according to claim 1 is characterized in that: in the step (2), the described longitudinal stretching that is stretched as, draw ratio are 1 ~ 200.
4. the preparation method of nanoscale microporous teflon membran according to claim 1 is characterized in that: in the step (2), the described cross directional stretch that is stretched as, draw ratio are 5 ~ 50.
5. the preparation method of polytetrafluoroethylene film according to claim 1 is characterized in that: in the step (2), describedly be stretched as biaxial tension, wherein the cross directional stretch multiple is 1 ~ 200, and the longitudinal stretching multiple is 5 ~ 50.
6. the nanoscale microporous teflon membran that adopts the preparation method of the described nanoscale microporous teflon membran of each claim in the claim 1 to 5 to prepare.
7. nanoscale microporous teflon membran according to claim 6 is characterized in that: the average pore size of described nanoscale microporous teflon membran is 10 ~ 180 nanometers, and porosity is 78% ~ 97%.
8. nanoscale microporous teflon membran according to claim 7 is characterized in that: average pore size 30 ~ 100 nanometers of described nanoscale microporous teflon membran, porosity 82% ~ 92%.
9. nanoscale microporous teflon membran according to claim 6 is characterized in that: the water pressure resistance of described nanoscale microporous teflon membran is more than or equal to 5 kilograms/square centimeter, and moisture permeability is more than or equal to 15000 gram water/square meter/skies.
10. nanoscale microporous teflon membran according to claim 6 is characterized in that: described nanoscale microporous teflon membran thickness between 1 ~ 200 micron, air penetrability was smaller or equal to 18 seconds.
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