CN111672338A - Preparation method of polytetrafluoroethylene microporous film with ultrahigh porosity - Google Patents
Preparation method of polytetrafluoroethylene microporous film with ultrahigh porosity Download PDFInfo
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- CN111672338A CN111672338A CN202010416816.8A CN202010416816A CN111672338A CN 111672338 A CN111672338 A CN 111672338A CN 202010416816 A CN202010416816 A CN 202010416816A CN 111672338 A CN111672338 A CN 111672338A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
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Abstract
The invention discloses a preparation method of a polytetrafluoroethylene microporous film with ultrahigh porosity, which comprises the steps of mixing, screening, curing, compacting, calendering, thermal decomposition, stretching and heat setting, wherein the aperture of the prepared polytetrafluoroethylene microporous film with ultrahigh porosity is 1-5 mu m, the porosity is 80-90%, and the air permeability is 50-150 m3/(m2H) a tensile strength of 5 to 20N. The sacrificial agent selected by the invention generates gas after thermal decomposition and does not react with other agents, thereby not only contributing to an ultrahigh pore structure for the polytetrafluoroethylene film, but also not generating other substances due to high temperature, and ensuring the quality of the polytetrafluoroethylene film; the sacrificial agent is added for a plurality of times in a fractional manner, so that the sacrificial agent is mixed with other raw materials more uniformly, and the uniform pore distribution of the polytetrafluoroethylene film is ensured; poly (tetra) s prepared by the inventionThe vinyl fluoride film can be applied to the fields of precision electronic products, lighting equipment, waterproof mobile phones and the like; the operation is simple and easy to realize, and the method is suitable for mass production.
Description
Technical Field
The invention relates to the field of production and manufacturing of polytetrafluoroethylene films, in particular to a preparation method of a polytetrafluoroethylene film with ultrahigh porosity.
Background
Polytetrafluoroethylene (PTFE), known as "plastic king," has sealing properties, high lubricity and non-tackiness, electrical insulation properties, good aging resistance, excellent temperature resistance (capable of long-term operation at temperatures from plus 250 ℃ to minus 180 ℃), excellent chemical stability, and excellent corrosion resistance. The polytetrafluoroethylene membrane material is widely applied to industries such as national defense, aerospace, electronics, electrical, chemical engineering, medical treatment, textile and the like, so that the polytetrafluoroethylene membrane material becomes an irreplaceable product. But also brings great difficulty to the preparation of the microporous membrane material due to the excellent chemical stability.
The Chinese patent with the patent number of CN104906968A discloses a polytetrafluoroethylene membrane and a preparation method thereof, the polytetrafluoroethylene membrane is a superfine nanofiber membrane with a pore three-dimensional communicated structure formed by criss-cross beaded fiber filaments, has good waterproof performance, and has the porosity as high as more than 80%; however, the pore structure prepared by the technical scheme of the invention has the defect of uneven pore size distribution, so that the problems of uneven performance, low air permeability and the like of the polytetrafluoroethylene membrane are caused.
Disclosure of Invention
The invention provides a preparation method of a polytetrafluoroethylene film with ultrahigh porosity, which solves the technical problems and has excellent waterproofness, air permeability and tensile property.
The preparation method comprises the following specific steps:
mixing materials: placing polytetrafluoroethylene dispersion resin and extrusion aid in a mixer, starting the mixer, adding a small amount of sacrificial agent into the mixer for multiple times, and mixing the raw materials under high-speed rotation;
sieving: screening the mixed raw materials;
curing: placing the mixed raw material subjected to the sieving treatment in an oven for curing;
fourthly, pressing the blank: placing the cured raw materials into a blank pressing machine for prepressing at the pressing speed of 5-15 cm/min;
rolling: rolling the raw material pressed into the blank by using a rolling mill, wherein the temperature of the rolling roll is set to be 30-60 ℃ during rolling;
sixthly, thermal decomposition: carrying out thermal decomposition treatment on the base band obtained after calendering in a degreasing machine, removing the extrusion aid and the sacrificial agent, and further puffing the base band;
and (c) stretching treatment: stretching the base band after thermal decomposition, wherein the stretching treatment comprises longitudinal stretching and transverse treatment;
eighthly, heat setting: the setting time is 10-60 s, and the setting temperature is 340-450 ℃.
Preferably, the pore diameter of the polytetrafluoroethylene microporous film with the ultrahigh porosity is 1-5 μm, the porosity is 80% -90%, and the air permeability is 50-150 m3/(m2H) a tensile strength of 5 to 20N.
Preferably, the extrusion aid is one of kerosene, glycerol or lubricating oil, and the amount of the extrusion aid is 10-40% of the mass of the polytetrafluoroethylene dispersion resin.
Preferably, the sacrificial agent is one or more of ammonium salt or urea, the particle size of the sacrificial agent is 1-1500 mu m, and the using amount of the sacrificial agent is 1-10% of the mass of the polytetrafluoroethylene dispersion resin.
Preferably, the sacrificial agent also includes one or more of other solid powders that can be decomposed and volatilized into gases at high temperatures.
Preferably, the mixer is a double-cone mixer, the rotating speed of the mixer is 20-80 r/min, and the mixing time is 20-60 min.
Preferably, the sieve mesh size is 5-30 meshes.
Preferably, the curing temperature is 30-80 ℃, and the curing time is 6-15 h.
Preferably, the longitudinal stretching temperature is 150-240 ℃, and the multiple is 2-10 times; the stretching temperature of the transverse stretching is 60-250 ℃, and the multiple is 5-30.
Preferably, the number of times of addition of the sacrificial agent is 3, and the amount of each addition is 1/3 of the total amount of the sacrificial agent.
The beneficial effects of the invention include:
1) the sacrificial agent selected by the invention generates gas after thermal decomposition and does not react with other agents, namely polytetrafluoroethylene
The film contributes to an ultrahigh pore structure, other substances cannot be generated due to high temperature, and the quality of the polytetrafluoroethylene film is ensured;
2) in the mixing step, the method of adding the sacrificial agent for a plurality of times in fractional times is adopted, so that the sacrificial agent is mixed with other raw materials more uniformly, and the uniform pore distribution of the polytetrafluoroethylene film is ensured;
3) the polytetrafluoroethylene film prepared by the invention has the porosity of 80-90% and the air permeability of 50-150 m3/(m2H), the tensile strength is 5-20N, the performance is far superior to that of the existing polytetrafluoroethylene film products, and the polytetrafluoroethylene film can be applied to the fields of precision electronic products, lighting devices, waterproof mobile phones and the like;
4) the polytetrafluoroethylene film prepared by the technical scheme of the invention has the width of 200-2100 mm, is simple to operate and easy to realize, and is suitable for mass production.
Drawings
FIG. 1 is a scanning electron micrograph of a microporous polytetrafluoroethylene membrane prepared in example 1;
FIG. 2 is a scanning electron microscope image of a polytetrafluoroethylene microporous membrane prepared by the prior art.
Detailed Description
The present invention will be described in detail with reference to specific examples.
In the examples of the present invention, the polytetrafluoroethylene dispersion resin was commercially available and had an average particle diameter of 550. + -. 150. mu.m.
The sacrificial agent selected for use in embodiments of the present invention is preferably understood to include one or more other solid powders that decompose to a gas at high temperatures.
The porosity testing method in the embodiment of the invention is mercury intrusion method; the air permeability test method refers to GB/T36138-2018 polytetrafluoroethylene flat-plate microfiltration membrane for degerming; the waterproof effect test method is in accordance with GB/T4744-2013 detection and evaluation of textile waterproof performance-hydrostatic pressure method; the test method of the tensile test refers to GB/T36138-2018 polytetrafluoroethylene flat-plate type microfiltration membrane for degerming.
Example 1
In the embodiment, the extrusion aid is preferably kerosene, the amount of the extrusion aid is 30% of the mass of the polytetrafluoroethylene dispersion resin, and the sacrificial agent is preferably ammonium chloride.
A preparation method of a polytetrafluoroethylene microporous film with ultrahigh porosity comprises the following steps:
mixing materials: adding 10 kg of polytetrafluoroethylene resin and an extrusion aid into a double-cone mixer, rotating clockwise for 15min, then rotating anticlockwise for 15min, and adding ammonium chloride powder every 5min in the mixing process, wherein the total amount of the ammonium chloride powder is 1% of the total mass of the polytetrafluoroethylene, the average particle size is 500 mu m, and the mixing temperature is 13 ℃; the rotating speed of the mixer is 80 r/min;
sieving: sieving the mixed raw materials, wherein the used sieve mesh specification is 16 meshes;
curing: placing the mixed raw material subjected to the sieving treatment in an oven for curing, wherein the curing temperature of the raw material is 35 ℃, and the curing time is 15 hours;
fourthly, green pressing: placing the cured raw materials into a blank briquetting machine for prepressing, wherein the briquetting speed is 10 cm/min,
rolling: rolling the raw material subjected to blank pressing by using a rolling mill, wherein the rolling temperature is 45 ℃;
sixthly, thermal decomposition: thermally decomposing the base band obtained after rolling in a degreasing machine, removing the extrusion aid and the sacrificial agent, further expanding the base band, fully volatilizing and decomposing the ammonium chloride in a drying oven at 110 ℃, and fully volatilizing the extrusion aid in the base band in a drying oven at 200 ℃;
and (c) stretching treatment: stretching the base band subjected to thermal decomposition, wherein the stretching treatment comprises longitudinal stretching and transverse stretching, the longitudinal stretching with the stretching ratio of 10 times is firstly carried out, and then the transverse stretching with the stretching ratio of 15 times is carried out;
eighthly, heat setting: the temperature of heat setting is 360 ℃, the time of heat setting is 40 s, and the cooling rate of heat setting is 20 ℃/min.
The obtained ultrahigh-porosity polytetrafluoroethylene microporous film has gas permeability of 130 m/(m) through top-bottom-up2H), the porosity is 88%, the tensile strength is 6N, and the effective width can reach about 2000 mm.
Fig. 1 and 2 are scanning electron micrographs of the polytetrafluoroethylene microporous membrane prepared in example 1 and the prior art, respectively, and as shown in fig. 1 and 2, under the same magnification of 300kx, it can be relatively intuitively observed that the pore size distribution and the pore size of the polytetrafluoroethylene microporous membrane prepared in example 1 are more uniform.
Example 2
In the embodiment, the extrusion aid is preferably kerosene with the dosage of 20% of the mass of the polytetrafluoroethylene dispersion resin, and the sacrificial agent is preferably urea.
A preparation method of a polytetrafluoroethylene microporous film with ultrahigh porosity comprises the following steps:
mixing materials: adding 5 kg of polytetrafluoroethylene resin and an extrusion aid into a double-cone mixer, rotating clockwise for 20 min, then rotating anticlockwise for 20 min, and adding urea powder every 5min in the mixing process, wherein the total amount of the urea powder is 0.5% of the total mass of the polytetrafluoroethylene, the average particle size is 1000 microns, and the mixing temperature is 10 ℃; the rotating speed of the mixer is 40 r/min;
sieving: sieving the mixed raw materials, wherein the used sieve mesh specification is 10 meshes;
curing: placing the mixed raw material subjected to the sieving treatment in an oven for curing, wherein the curing temperature of the raw material is 40 ℃, and the curing time is 12 hours;
fourthly, green pressing: placing the cured raw materials into a blank briquetting machine for prepressing, wherein the briquetting speed is 10 cm/min,
rolling: rolling the raw material subjected to blank pressing by using a rolling mill, wherein the rolling temperature is 50 ℃;
sixthly, thermal decomposition: thermally decomposing the base band obtained after calendering in a degreasing machine, removing the extrusion aid and the sacrificial agent, further expanding the base band, fully volatilizing and decomposing the urea in a 160 ℃ oven, and fully volatilizing the extrusion aid in the base band in a 210 ℃ oven;
and (c) stretching treatment: stretching the base band subjected to thermal decomposition, wherein the stretching treatment comprises longitudinal stretching and transverse stretching, and the longitudinal stretching with the stretching ratio of 3 times is firstly carried out, and then the transverse stretching with the stretching ratio of 8 times is carried out;
eighthly, heat setting: the temperature of heat setting is 380 ℃, the time of heat setting is 30s, and the cooling rate of heat setting is 20 ℃/min.
The air permeability of the obtained polytetrafluoroethylene microporous film with ultrahigh porosity is 80 m3/(m2H), the porosity is 82%, the tensile strength is 13N, and the width can reach about 350 mm.
Example 3
In the embodiment, the extrusion aid is preferably kerosene with the dosage of 35% of the mass of the polytetrafluoroethylene dispersion resin, and the sacrificial agent is preferably ammonium bicarbonate and ammonium carbonate.
A preparation method of a polytetrafluoroethylene microporous film with ultrahigh porosity comprises the following steps:
mixing materials: adding 5 kg of polytetrafluoroethylene resin and an extrusion aid into a double-cone mixer, rotating clockwise for 20 min, then rotating counterclockwise for 20 min, and adding a sacrificial agent every 5min in the mixing process, wherein the sacrificial agent is mixed powder of ammonium bicarbonate and ammonium carbonate, the total amount of the ammonium bicarbonate is 0.5 percent of the total mass of the polytetrafluoroethylene, the average particle size is 200 mu m, the total amount of the ammonium carbonate is 0.5 percent of the total mass of the polytetrafluoroethylene, and the average particle size is 300 mu m; the mixing temperature is 18 ℃; the rotating speed of the mixer is 30 r/min;
sieving: sieving the mixed raw materials, wherein the used sieve mesh specification is 18 meshes;
curing: placing the mixed raw material subjected to the sieving treatment in an oven for curing, wherein the curing temperature of the raw material is 30 ℃, and the curing time is 15 hours;
fourthly, green pressing: placing the cured raw materials into a blank briquetting machine for prepressing, wherein the briquetting speed is 10 cm/min,
rolling: rolling the raw material subjected to blank pressing by using a rolling mill, wherein the rolling temperature is 30 ℃;
sixthly, thermal decomposition: thermally decomposing the base band obtained after rolling in a degreasing machine, removing the extrusion aid and the sacrificial agent, further expanding the base band, fully volatilizing and decomposing the ammonium bicarbonate and the ammonium carbonate in a 60 ℃ oven, and fully volatilizing the extrusion aid in the base band in a 230 ℃ oven;
and (c) stretching treatment: stretching the base band subjected to thermal decomposition, wherein the stretching treatment comprises longitudinal stretching and transverse stretching, and the longitudinal stretching with the stretching ratio of 3 times is firstly carried out, and then the transverse stretching with the stretching ratio of 13 times is carried out;
eighthly, heat setting: the temperature of heat setting is 380 ℃, the time of heat setting is 30s, and the cooling rate of heat setting is 20 ℃/min.
The air permeability of the obtained polytetrafluoroethylene microporous film with ultrahigh porosity is 140 m3/(m2H), the porosity is 86%, the tensile strength is 9N, and the width can reach about 1800 mm.
Example 4
In the embodiment, the extrusion aid is preferably kerosene with the dosage of 30% of the mass of the polytetrafluoroethylene dispersion resin, and the sacrificial agent is preferably ammonium bicarbonate.
A preparation method of a polytetrafluoroethylene microporous film with ultrahigh porosity comprises the following steps:
mixing materials: adding 5 kg of polytetrafluoroethylene resin and an extrusion aid into a double-cone mixer, rotating clockwise for 15min, then rotating counterclockwise for 15min, and adding ammonium bicarbonate powder every 5min in the mixing process, wherein the total amount of the ammonium bicarbonate powder is 1% of the total mass of the polytetrafluoroethylene, and the average particle size is 200 mu m; the mixing temperature is 18 ℃; the rotating speed of the mixer is 40 r/min;
sieving: sieving the mixed raw materials, wherein the used sieve mesh specification is 20 meshes;
curing: placing the mixed raw material subjected to the sieving treatment in an oven for curing, wherein the curing temperature of the raw material is 30 ℃, and the curing time is 15 hours;
fourthly, green pressing: placing the cured raw materials into a blank briquetting machine for prepressing, wherein the briquetting speed is 10 cm/min,
rolling: rolling the raw material subjected to blank pressing by using a rolling mill, wherein the rolling temperature is 30 ℃;
sixthly, thermal decomposition: thermally decomposing the base band obtained after rolling in a degreasing machine, removing the extrusion aid and the sacrificial agent, further expanding the base band, fully volatilizing and decomposing the ammonium bicarbonate in a 50 ℃ oven, and fully volatilizing the extrusion aid in the base band in a 230 ℃ oven;
and (c) stretching treatment: stretching the base band subjected to thermal decomposition, wherein the stretching treatment comprises longitudinal stretching and transverse stretching, and the longitudinal stretching with the stretching ratio of 5 times is firstly carried out, and then the transverse stretching with the stretching ratio of 13 times is carried out;
eighthly, heat setting: the temperature of heat setting is 380 ℃, the time of heat setting is 30s, and the cooling rate of heat setting is 20 ℃/min.
The air permeability of the obtained polytetrafluoroethylene microporous film with ultrahigh porosity is 100m3/(m2H), the porosity is 83 percent, the tensile strength is 7N, and the width can reach about 1800 mm.
The above-described preferred embodiments of the present invention are not intended to limit the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the claims of the present invention.
Claims (9)
1. A preparation method of a polytetrafluoroethylene microporous film with ultrahigh porosity comprises the following steps:
mixing materials: placing polytetrafluoroethylene dispersion resin and extrusion aid into a mixer, starting the mixer, adding a small amount of sacrificial agent into the mixer for multiple times, and mixing the raw materials;
sieving: screening the mixed raw materials;
curing: placing the mixed raw material subjected to the sieving treatment in an oven for curing;
fourthly, pressing the blank: placing the cured raw materials into a blank pressing machine for prepressing at the pressing speed of 5-15 cm/min;
rolling: rolling the raw material pressed into the blank by using a rolling mill, wherein the temperature of the rolling roll is set to be 30-60 ℃ during rolling;
sixthly, thermal decomposition: carrying out thermal decomposition treatment on the base band obtained after calendering in a degreasing machine, removing the extrusion aid and the sacrificial agent, and further puffing the base band;
and (c) stretching treatment: stretching the base band after thermal decomposition, wherein the stretching treatment comprises longitudinal stretching and transverse treatment;
eighthly, heat setting: the setting time is 10-60 s, and the setting temperature is 340-450 ℃.
2. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the ultra-high porosity polytetrafluoroethylene microporous film has a pore diameter of 1-5 mu m, a porosity of 80-90% and an air permeability of 50-150 m3/(m2H) a tensile strength of 5 to 20N.
3. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the extrusion aid is one of kerosene, glycerol or lubricating oil, and the amount of the extrusion aid is 10-40% of the mass of the polytetrafluoroethylene dispersion resin.
4. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the sacrificial agent is one or more of ammonium salt or urea, the particle size of the sacrificial agent is 1-1500 mu m, and the consumption of the sacrificial agent is 1-10% of the mass of the polytetrafluoroethylene dispersion resin.
5. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the mixer is a double-cone mixer, the rotating speed of the mixer is 20-80 r/min, and the mixing time is 20-60 min.
6. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: and the specification of the sieve pores during sieving is 5-30 meshes.
7. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the curing temperature is 30-80 ℃, and the curing time is 6-15 h.
8. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the longitudinal stretching temperature is 150-240 ℃, and the multiple is 2-10 times; the stretching temperature of the transverse stretching is 60-250 ℃, and the multiple is 5-30.
9. The method for preparing a microporous membrane of ultra-high porosity polytetrafluoroethylene according to claim 1, wherein the method comprises the following steps: the number of times of addition of the sacrificial agent was 3, and the amount of each addition was 1/3 of the total amount of the sacrificial agent.
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| CN115720422A (en) * | 2022-11-17 | 2023-02-28 | 歌尔微电子股份有限公司 | Waterproof membrane structure and preparation method thereof |
| CN115720422B (en) * | 2022-11-17 | 2024-09-10 | 歌尔微电子股份有限公司 | Waterproof film structure and preparation method thereof |
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Application publication date: 20200918 |