CN116063809A - High-air-permeability polytetrafluoroethylene fiber membrane material for sterilization and preparation method and application thereof - Google Patents
High-air-permeability polytetrafluoroethylene fiber membrane material for sterilization and preparation method and application thereof Download PDFInfo
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- CN116063809A CN116063809A CN202111282346.1A CN202111282346A CN116063809A CN 116063809 A CN116063809 A CN 116063809A CN 202111282346 A CN202111282346 A CN 202111282346A CN 116063809 A CN116063809 A CN 116063809A
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- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 128
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 128
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 128
- 239000000463 material Substances 0.000 title claims abstract description 85
- 239000012528 membrane Substances 0.000 title claims abstract description 53
- 239000000835 fiber Substances 0.000 title claims abstract description 44
- 230000001954 sterilising effect Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000004659 sterilization and disinfection Methods 0.000 title abstract description 26
- 230000035699 permeability Effects 0.000 claims abstract description 23
- 239000011148 porous material Substances 0.000 claims abstract description 15
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 65
- 239000011347 resin Substances 0.000 claims description 35
- 229920005989 resin Polymers 0.000 claims description 35
- 238000003490 calendering Methods 0.000 claims description 34
- 238000009998 heat setting Methods 0.000 claims description 28
- 238000005238 degreasing Methods 0.000 claims description 26
- 238000005096 rolling process Methods 0.000 claims description 26
- 239000006185 dispersion Substances 0.000 claims description 24
- 239000010687 lubricating oil Substances 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000003350 kerosene Substances 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000000903 blocking effect Effects 0.000 claims 1
- 244000005700 microbiome Species 0.000 claims 1
- 239000002184 metal Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to the field of sterilization filter materials, and discloses a polytetrafluoroethylene fiber membrane material for high-air-permeability sterilization, and a preparation method and application thereof. The pore diameter of the polytetrafluoroethylene fiber membrane material ranges from 0.03 to 0.5 mu m, the pressure is 7kPa, and the test area is 20cm 2 The air permeability under the condition is 3-5L/min. The polytetrafluoroethylene fiber membrane material can effectively reduce the pore diameter of the membrane and increase the air permeability of the membrane; is very suitable for the degerming filter material.
Description
Technical Field
The invention belongs to the field of sterilization filter materials, and particularly relates to a polytetrafluoroethylene fiber membrane material for high-air-permeability sterilization, and a preparation method and application thereof.
Background
Polytetrafluoroethylene is a high-performance material, and has wide application, and polytetrafluoroethylene powder, lubricant, compact, calendaring, double-layer simultaneous longitudinal stretching, transverse stretching and heat setting technology is adopted in patent ZL200510061828.9 (CN 1326935C) to prepare a polytetrafluoroethylene film with small pore diameter, so that the polytetrafluoroethylene film is applied to a sterilization filter material. The main principle is that the apparent density of the middle interface bonding layer is larger than that of the two sides when the two layers are stretched in the longitudinal direction at the same time, and the formation of small holes is facilitated in the transverse stretching process. For the gas flux test, the membrane prepared by the method has low ventilation, and high pressure is required in the application process to enable air to pass through, so that the operation cost is high and the safety is not high. It is difficult to prepare polytetrafluoroethylene fiber membrane for sterilization having high air permeability by the above method.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the polytetrafluoroethylene fiber membrane material for high-air-permeability sterilization, and the preparation method and the application thereof.
One of the objects of the present invention is to provide a polytetrafluoroethylene fiber membrane material having a pore size in the range of 0.03 to 0.5 μm under a pressure of 7kPa and a test area of 20cm 2 The air permeability under the condition is 3-5L/min. .
In a preferred embodiment of the present invention, the polytetrafluoroethylene fiber membrane material has a pore size in the range of 0.05 to 0.4 μm, preferably 0.1 to 0.25 μm.
In a preferred embodiment of the present invention, the polytetrafluoroethylene fiber membrane material has a test area of 20cm at a pressure of 7kPa 2 The air permeability under the conditions is preferably 3.5 to 4.8L/min.
In a preferred embodiment of the invention, the polytetrafluoroethylene fiber membrane material has an average pore size of 0.05 to 0.25 μm, preferably 0.1 to 0.2 μm.
In a preferred embodiment of the present invention, the polytetrafluoroethylene fiber membrane material has a microbial barrier in air of not less than 99.5%, preferably 99.55-99.95%.
The method for detecting the above-mentioned parameters according to the present invention may employ a method known in the art, for example, in the examples of the present invention, the method disclosed in coulter usa is used for detecting the pore diameter of micropores of the prepared aseptic film; performing a sterilization performance test on the prepared sterilization film by adopting a general standard method of WSB58-2003 biological protective clothing of general office health department; the prepared degerming film is ventilated by adopting the national standard GB/T5453-1997 methodPerformance test, test pressure of 7kPa and test area of 20cm 2 。
In a preferred embodiment of the present invention, the polytetrafluoroethylene fiber membrane material is prepared by mixing polytetrafluoroethylene dispersion resin and a liquid lubricant.
The weight ratio of the polytetrafluoroethylene dispersion resin to the liquid lubricant is selected in a wide range, and preferably the weight ratio of the polytetrafluoroethylene dispersion resin to the liquid lubricant is 1: (0.2-0.5).
The polytetrafluoroethylene dispersion resin may be selected from materials conventional in the art, and in a preferred embodiment of the invention, the polytetrafluoroethylene dispersion resin has a crystallinity of 98% to 99.9%.
Regarding the molecular weight of the polytetrafluoroethylene dispersion resin, the selection range is wide, and in a preferred embodiment of the present invention, the molecular weight is 200 ten thousand to 1000 ten thousand.
The liquid lubricant may be selected from those conventional in the art, and in a preferred embodiment of the present invention, is selected from petroleum ether and/or aviation kerosene.
The second object of the invention is to provide a preparation method of the polytetrafluoroethylene fiber membrane material, which comprises the steps of fully mixing polytetrafluoroethylene dispersion resin and lubricant, compacting and calendaring to obtain polytetrafluoroethylene base bands; stretching the polytetrafluoroethylene base band longitudinally under the condition of multi-layer overlapping, and then rolling to obtain a bonded degreasing base band; and transversely stretching and heat setting the degreasing base band to obtain the polytetrafluoroethylene fiber membrane material.
The biaxial stretching process of polytetrafluoroethylene has severe requirements on preparation conditions, and is usually carried out by mixing and standing, so that the aim of mixing is fulfilled, and further mechanical mixing is not usually adopted. Because the conventional stirring and mixing are adopted, uneven parts and sharp ends possibly existing on stirring paddles can lead to material fiber formation in advance, and bad points and the like can be formed on the fiber-forming part in the subsequent process, so that the sample performance is reduced. The inventor of the invention discovers that non-stirring mixing can not cause dead spots, and by adopting the specific method, the prepared material can reduce the pore diameter and increase the air permeability of the membrane, and meanwhile, the sterilization rate of the material can be improved.
In a preferred embodiment of the present invention, the method of thoroughly mixing is non-stirring mixing, preferably the method of thoroughly mixing is that the container is rotated to drive the materials in the container to mix, and further preferably a low-speed roller is adopted as a mixing means, so that the above disadvantages can be effectively avoided, and compared with the standing mixing, the air permeability of the film can be further increased while the aperture is further reduced, and meanwhile, the sterilization rate of the materials can be further improved in combination with the subsequent specific rolling step of the present invention. According to the invention, the mixing time is chosen within a wide range, and in a preferred embodiment of the invention, the mixing time is 100-150 hours.
In a preferred embodiment of the invention, the number of overlapping layers of the polytetrafluoroethylene base tape before longitudinal stretching is 2-4, preferably two.
According to the invention, the pressure of the nip is selected within a wide range, and in a preferred embodiment of the invention, the pressure of the nip is 0.1-0.5MPa, preferably 0.3-0.4MPa.
In a preferred embodiment of the invention, the preparation method comprises the following steps:
proportioning polytetrafluoroethylene dispersion resin and a liquid lubricant according to the weight ratio, and sealing; step b: rotating the sealed mixed material in the step a, fully mixing the resin powder subjected to the sealing treatment in the step a with a liquid lubricant, and standing to form a polytetrafluoroethylene material; step c: b, pressing the polytetrafluoroethylene material prepared in the step b into a blank through a pressed blank, extruding the prepared blank, and then calendaring into a polytetrafluoroethylene base band; step d: c, carrying out multi-layer overlapping on the polytetrafluoroethylene base band prepared in the step c, carrying out longitudinal stretching, and then rolling to obtain a bonded degreasing base band; step e: and d, transversely stretching the degreasing base band prepared in the step d, and then performing heat setting to obtain the polytetrafluoroethylene fiber membrane material.
According to the present invention, it is preferable that the polytetrafluoroethylene dispersion resin and the liquid lubricant are compounded in the weight ratio and then sealed, and the main function of the sealing in the present invention is to prevent the liquid lubricant from being volatilized and reduced.
The conditions for thorough mixing may be selected widely, and in a preferred embodiment of the present invention, the conditions for thorough mixing in the step b include: the temperature is 30-60 ℃, the time is 100-150h, the rotating speed is 10-200rpm, and the preferable rotating speed is 10-50rpm.
In a preferred embodiment of the present invention, the standing conditions in step b comprise: the temperature is 40-80 ℃ and the time is 10-20h.
In a preferred embodiment of the present invention, the conditions in step c include: the temperature of the pressed compact is 20-30 ℃, the extrusion temperature is 40-60 ℃, and the calendering temperature is 40-60 ℃.
In a preferred embodiment of the present invention, the conditions in the step d include: the temperature of the longitudinal stretching and/or rolling is 50-160 ℃, preferably 80-160 ℃, and the pressure of the rolling is 0.1-0.5MPa, preferably 0.3-0.4MPa.
In a preferred embodiment of the present invention, the conditions in step e include: the temperature of the transverse stretching is 80-170 ℃, and/or the heat setting temperature is 250-380 ℃, and/or the heat setting time is 20-80 seconds.
In a more preferred embodiment of the present invention, the preparation method comprises the steps of:
step a: mixing, namely mixing polytetrafluoroethylene dispersion resin with a liquid lubricant, and sealing in a sealing tank; step b: b, fully mixing, rotating the sealing tank in the step a for a period of time, fully mixing the resin powder subjected to the sealing treatment in the step a with the liquid lubricant, and standing for a period of time to form polytetrafluoroethylene materials; step c: compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank by a compacting machine, extruding a rod-shaped object by a pushing machine from the prepared blank, and calendaring the rod-shaped object into a polytetrafluoroethylene base band by a calendaring machine; step d: c, simultaneously longitudinally stretching and rolling two layers, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, simultaneously longitudinally stretching in an oven, and then immediately rolling and pressing by using two metal rolls in the oven to obtain a degreasing base band bonded together; step e: transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d, and then sintering and setting for a period of time to obtain a polytetrafluoroethylene fiber membrane material for high-permeability sterilization; polytetrafluoroethylene dispersion resin and liquid lubricant in a weight ratio of 1: (0.2-0.5) mixing; in the step b, the stirring temperature is 30-60 ℃ and the stirring time is 100-150h, and the stirring time is 10-20h and the stirring temperature is 40-80 ℃ when the mixture is kept stand; the blank pressing temperature in the step c is 20-30 ℃, the pushing temperature is 40-60 ℃ and the rolling temperature is 40-60 ℃; the temperature of the oven in the step d is 50-160 ℃, and the pressure of the two metal roll presses is 0.1-0.5MPa; the transverse stretching temperature in the step e is 80-170 ℃, the heat setting temperature is 250-380 ℃ and the heat setting time is 20-80 seconds.
According to the invention, in step d, the polytetrafluoroethylene base tapes prepared in step c are subjected to multi-layer overlapping, preferably in such a way that each layer of polytetrafluoroethylene base tapes is placed in parallel.
The invention further provides a polytetrafluoroethylene fiber membrane material, which is prepared by the preparation method. The pore diameter of the polytetrafluoroethylene membrane material prepared by the preferred method is 0.1-0.15 mu m, the air permeability is 3-5L/min@7kPa, and the microbial barrier property in the air is not less than 99.5%.
The invention also provides an application of the polytetrafluoroethylene fiber membrane material in a sterilization filter material.
Compared with the prior art, the invention has the beneficial effects that:
(1) The polytetrafluoroethylene fiber membrane material of the invention can increase the air permeability of the membrane while having lower membrane pore diameter, and has a pressure of 7kPa and a test area of 20cm 2 The air permeability under the condition is 3-5L/min, and the microbial barrier property in the air is more than 99.5%, so that the antibacterial material is very suitable for the antibacterial filter material.
(2) The conventional mechanical stirring after raw material proportioning can lead the materials to form fibers in advance, dead spots are formed at the fiber forming part in the subsequent process, and the sample performance is reduced, so in the conventional preparation method, the raw materials of the polytetrafluoroethylene composite membrane matrix are proportioned and then are kept stand, and the materials are mixed in a standing state without adopting further external force to assist in mixing. The inventor of the present invention has surprisingly found that by adopting non-stirring mixing in combination with the step of rolling after stretching, the obtained polytetrafluoroethylene fiber membrane material can effectively reduce the membrane pore diameter and simultaneously increase the membrane air permeability.
The invention has the advantages that the inventor considers that the invention possibly introduces non-stirring type mixing through researches, and combines the steps of rolling after stretching, wherein the non-stirring type mixing ensures the uniformity of the mixed materials, and the rolling ensures that the multi-layer film is fully bonded to form a uniform layer after being longitudinally stretched, thereby being beneficial to improving the uniformity of the film in other subsequent processes and further improving the air permeability.
(3) The preparation process is simple, the operation cost and the damage to the membrane caused by high-pressure operation are reduced, and the prepared high-air-permeability sterilization material has obvious economic and social benefits.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
In the following examples, some sources of the raw materials of the present invention are described in examples, and other raw materials are commercially available, unless otherwise specified.
Example 1
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.2, and sealing in a sealed tank;
b. b, fully mixing, namely rotating a sealing tank for 100 hours at 30 ℃ and 200rpm to fully mix resin powder with a liquid lubricant, and standing for 10 hours at 40 ℃ to form a polytetrafluoroethylene material;
c. compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank at 20 ℃ through a compacting machine, extruding a rod-shaped object at 40 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 40 ℃ through a calendaring machine;
d. c, longitudinally stretching and rolling the two layers simultaneously, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, longitudinally stretching the polytetrafluoroethylene base band in a baking oven at 50 ℃, and then rolling the polytetrafluoroethylene base band in the baking oven by using two metal rollers under the pressure of 0.1MPa to obtain a degreasing base band bonded together;
e. and d, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d at 80 ℃, and then heat setting for 20 seconds at 250 ℃ to obtain the polytetrafluoroethylene fiber membrane material M1 for high-air permeability sterilization.
Example 2
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.5, and sealing in a sealed tank;
b. b, fully mixing, namely rotating a sealing tank for 150 hours at 60 ℃ and standing for 20 hours at 80 ℃ after fully mixing resin powder and a liquid lubricant by 120rpm to form a polytetrafluoroethylene material;
c. compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank at 30 ℃ through a compacting machine, extruding a rod-shaped object at 60 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 60 ℃ through a calendaring machine;
d. c, simultaneously longitudinally stretching and rolling two layers, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, simultaneously longitudinally stretching in a 160 ℃ oven, and then immediately rolling with two metal rollers under the pressure of 0.5MPa in the oven to obtain a bonded degreasing base band;
e. and d, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d at 170 ℃, and then heat setting for 80 seconds at 380 ℃ to obtain the polytetrafluoroethylene fiber membrane material M2 for high-air permeability sterilization.
Example 3
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.3, and sealing in a sealed tank;
b. b, fully mixing, namely rotating a sealing tank for 120h at 50 ℃ and 50rpm to fully mix resin powder with a liquid lubricant, and standing for 15h at 60 ℃ to form a polytetrafluoroethylene material;
c. compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank at 20 ℃ through a compacting machine, extruding a rod-shaped object at 50 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 50 ℃ through a calendaring machine;
d. c, simultaneously longitudinally stretching and rolling two layers, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, simultaneously longitudinally stretching in a 100 ℃ oven, and then immediately rolling with two metal rollers under the pressure of 0.3MPa in the oven to obtain a degreasing base band bonded together;
e. and d, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d at 120 ℃, and then heat setting for 60 seconds at 350 ℃ to obtain the polytetrafluoroethylene fiber membrane material M3 for high-air permeability sterilization.
Example 4
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.5, and sealing in a sealed tank;
b. b, fully mixing, namely rotating a sealing tank for 100 hours at 30 ℃ and 10rpm to fully mix resin powder with a liquid lubricant, and standing for 10 hours at 80 ℃ to form a polytetrafluoroethylene material;
c. compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank at 30 ℃ through a compacting machine, extruding a rod-shaped object at 60 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 40 ℃ through a calendaring machine;
d. c, simultaneously longitudinally stretching and rolling two layers, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, simultaneously longitudinally stretching in a baking oven at 120 ℃, and then immediately rolling with two metal rollers under the pressure of 0.4MPa in the baking oven to obtain a degreasing base band bonded together;
e. and d, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d at 100 ℃, and then heat setting for 40 seconds at 300 ℃ to obtain the polytetrafluoroethylene fiber membrane material M4 for high-air permeability sterilization.
Example 5
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.3, and sealing in a sealed tank;
b. b, fully mixing, namely rotating a sealing tank for 150 hours at 50 ℃ and 30rpm to fully mix resin powder with a liquid lubricant, and standing for 10 hours at 40 ℃ to form a polytetrafluoroethylene material;
c. compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank at 30 ℃ through a compacting machine, extruding a rod-shaped object at 0 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 40 ℃ through a calendaring machine;
d. c, simultaneously longitudinally stretching and rolling two layers, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, simultaneously longitudinally stretching in a 60 ℃ oven, and then immediately rolling with two metal rollers under the pressure of 0.3MPa in the oven to obtain a degreasing base band bonded together;
e. and d, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d at 140 ℃, and then heat setting for 50 seconds at 350 ℃ to obtain the polytetrafluoroethylene fiber membrane material M5 for high-air permeability sterilization.
Comparative example 1
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.3, standing for 120 hours in a sealed tank at 50 ℃ to ensure that the resin powder is fully mixed with the liquid lubricant, and then standing for 15 hours at 60 ℃ to form a polytetrafluoroethylene material;
b. pressing and calendaring, namely pressing the polytetrafluoroethylene material prepared in the step a into a cylindrical blank at 20 ℃ through a pressing machine, extruding a rod-shaped object at 50 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 50 ℃ through a calendaring machine;
c. the two layers are longitudinally stretched and rolled simultaneously, the two layers of the polytetrafluoroethylene base band prepared in the step b are overlapped, the longitudinal stretching is carried out simultaneously in a 100 ℃ oven, and then the two layers of the polytetrafluoroethylene base band are rolled and pressed under the pressure of 0.3MPa by two metal rollers in the oven, so that the degreasing base band bonded together is obtained;
d. and c, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step c at 120 ℃, and then heat setting for 60 seconds at 350 ℃ to obtain the polytetrafluoroethylene fiber membrane material M6 for high-air permeability sterilization.
Comparative example 2
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.3, and sealing in a sealed tank;
b. b, fully mixing, namely rotating a sealing tank for 120h at 50 ℃ and 50rpm to fully mix resin powder with a liquid lubricant, and standing for 15h at 60 ℃ to form a polytetrafluoroethylene material;
c. compacting and calendaring, namely compacting the polytetrafluoroethylene material prepared in the step b into a cylindrical blank at 20 ℃ through a compacting machine, extruding a rod-shaped object at 50 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 50 ℃ through a calendaring machine;
d. c, simultaneously stretching the two layers longitudinally, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step c, and simultaneously stretching longitudinally in a 100 ℃ oven to obtain a bonded degreasing base band;
e. and d, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step d at 120 ℃, and then heat setting for 60 seconds at 350 ℃ to obtain the polytetrafluoroethylene fiber membrane material M7 for high-air permeability sterilization.
Comparative example 3
a. Mixing, namely mixing Japanese Dajin F106 polytetrafluoroethylene dispersion resin and kerosene according to a weight ratio of 1: mixing at a weight ratio of 0.3, standing for 120 hours in a sealed tank at 50 ℃ to ensure that the resin powder is fully mixed with the liquid lubricant, and then standing for 15 hours at 60 ℃ to form a polytetrafluoroethylene material;
b. pressing and calendaring, namely pressing the polytetrafluoroethylene material prepared in the step a into a cylindrical blank at 20 ℃ through a pressing machine, extruding a rod-shaped object at 50 ℃ through a pushing press, and calendaring the rod-shaped object into polytetrafluoroethylene base band at 50 ℃ through a calendaring machine;
c. and c, simultaneously stretching the two layers longitudinally, overlapping the two layers of the polytetrafluoroethylene base band prepared in the step b, and simultaneously stretching longitudinally in a 100 ℃ oven to obtain a bonded degreasing base band;
d. and c, transversely stretching and heat setting, namely transversely stretching the degreasing base band prepared in the step c at 120 ℃, and then heat setting for 60 seconds at 350 ℃ to obtain the polytetrafluoroethylene fiber membrane material M8 for sterilization.
Test case
Detecting the micropore diameter of the prepared sterilizing film by adopting a method disclosed by Coulter in the United states;
performing a sterilization performance test on the prepared sterilization film by adopting a general standard method of WSB58-2003 biological protective clothing of general office health department;
the air permeability of the prepared degerming film is tested by adopting the national standard GB/T5453-1997 method, the test pressure is 7kPa, and the test area is 20cm 2 。
The above test results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the degerming film prepared by the invention has very high air permeability and degerming rate on the basis of smaller pore diameter.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (12)
1. A polytetrafluoroethylene fibrous membrane material with pore diameter ranging from 0.03 to 0.5 mu m, pressure of 7kPa and test area of 20cm 2 The air permeability under the condition is 3-5L/min.
2. The polytetrafluoroethylene fiber membrane material according to claim 1 wherein:
the pore diameter of the polytetrafluoroethylene fiber membrane material ranges from 0.05 to 0.4 mu m, preferably from 0.1 to 0.25 mu m; and/or the number of the groups of groups,
the polytetrafluoroethylene fiber membrane material has a pressure of 7kPa and a test area of 20cm 2 The air permeability under the condition is 3.5-4.8L/min; and/or the number of the groups of groups,
the average pore diameter is 0.05 to 0.25. Mu.m, preferably 0.1 to 0.2. Mu.m;
and/or the microorganism blocking rate in the air is not less than 99.5%, preferably 99.55 to 99.95%.
3. A polytetrafluoroethylene fiber membrane material according to claim 1 or 2 wherein:
the polytetrafluoroethylene fiber membrane material is prepared by mixing polytetrafluoroethylene dispersion resin and a liquid lubricant;
preferably, the weight ratio of polytetrafluoroethylene dispersion resin to liquid lubricant is 1: (0.2-0.5).
4. A polytetrafluoroethylene fiber membrane material according to claim 3 wherein:
the crystallinity of the polytetrafluoroethylene dispersion resin is 98-99.9%, and/or the molecular weight is 200-1000 ten thousand; and/or the number of the groups of groups,
the liquid lubricant is selected from petroleum ether and/or aviation kerosene.
5. A process for producing the polytetrafluoroethylene fiber membrane material of any one of claims 1-4 comprising thoroughly mixing the components including polytetrafluoroethylene dispersion resin and lubricant, compacting, and calendaring to obtain polytetrafluoroethylene base tape; stretching the polytetrafluoroethylene base band longitudinally under the condition of multi-layer overlapping, and then rolling to obtain a bonded degreasing base band; and transversely stretching and heat setting the degreasing base band to obtain the polytetrafluoroethylene fiber membrane material.
6. The method of manufacturing according to claim 5, wherein:
the conditions of thorough mixing included: the fully mixing method is non-stirring mixing, preferably rotating the container to drive the materials in the container to mix; and/or mixing time is 100-150h; and/or the number of the groups of groups,
the overlapped layers of the polytetrafluoroethylene base band before longitudinal stretching are 2-4 layers; and/or the number of the groups of groups,
the rolling pressure is 0.1-0.5MPa.
7. The preparation method according to claim 5 or 6, characterized by comprising the steps of:
step a: proportioning polytetrafluoroethylene dispersion resin and a liquid lubricant according to the weight ratio, and sealing;
step b: rotating the sealed mixed material in the step a, fully mixing the resin powder subjected to the sealing treatment in the step a with a liquid lubricant, and standing to form a polytetrafluoroethylene material;
step c: b, pressing the polytetrafluoroethylene material prepared in the step b into a blank through a pressed blank, extruding the prepared blank, and then calendaring into a polytetrafluoroethylene base band;
step d: c, carrying out multi-layer overlapping on the polytetrafluoroethylene base band prepared in the step c, carrying out longitudinal stretching, and then rolling to obtain a bonded degreasing base band;
step e: and d, transversely stretching the degreasing base band prepared in the step d, and then performing heat setting to obtain the polytetrafluoroethylene fiber membrane material.
8. The method of manufacturing according to claim 7, wherein:
the conditions for thorough mixing in step b include: the temperature is 30-60 ℃, the time is 100-150h, the rotating speed is 10-200rpm, and the preferable rotating speed is 10-50rpm; and/or the number of the groups of groups,
the standing condition in the step b comprises: the temperature is 40-80 ℃ and the time is 10-20h; and/or the number of the groups of groups,
the conditions in step c include: the temperature of the pressed compact is 20-30 ℃, the extrusion temperature is 40-60 ℃, and the calendering temperature is 40-60 ℃.
9. The method of manufacturing according to claim 7, wherein:
the conditions in step d include: the temperature of the longitudinal stretching and/or rolling is 50-160 ℃, preferably 80-160 ℃, and the pressure of the rolling is 0.1-0.5MPa.
10. The method of manufacturing according to claim 7, wherein:
the conditions in step e include:
the temperature of the transverse stretching is 80-170 ℃, and/or the heat setting temperature is 250-380 ℃, and/or the heat setting time is 20-80 seconds.
11. A polytetrafluoroethylene fiber membrane material prepared by the preparation method of any one of claims 5-10.
12. Use of a polytetrafluoroethylene fiber membrane material according to any one of claims 1-4, 11 as a sterilizing filter material.
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| CN1052797A (en) * | 1989-12-07 | 1991-07-10 | 大金工业株式会社 | Make the method and the half sintering polytetrafluoroethylfilm sandwich construction goods of multilayer polytetrafluoroethylporous porous membrane |
| WO1994028059A1 (en) * | 1993-05-21 | 1994-12-08 | E.I. Du Pont De Nemours And Company | Porous polytetrafluoroethylene and preparation |
| CN1775847A (en) * | 2005-12-05 | 2006-05-24 | 浙江理工大学 | Method for preparing PTFE film material for air degerming |
| CN108912359A (en) * | 2018-06-12 | 2018-11-30 | 苏州优可发新材料科技有限公司 | A kind of high bubble pressure microporous teflon membran and preparation method thereof |
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2021
- 2021-11-01 CN CN202111282346.1A patent/CN116063809A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052797A (en) * | 1989-12-07 | 1991-07-10 | 大金工业株式会社 | Make the method and the half sintering polytetrafluoroethylfilm sandwich construction goods of multilayer polytetrafluoroethylporous porous membrane |
| WO1994028059A1 (en) * | 1993-05-21 | 1994-12-08 | E.I. Du Pont De Nemours And Company | Porous polytetrafluoroethylene and preparation |
| CN1775847A (en) * | 2005-12-05 | 2006-05-24 | 浙江理工大学 | Method for preparing PTFE film material for air degerming |
| CN108912359A (en) * | 2018-06-12 | 2018-11-30 | 苏州优可发新材料科技有限公司 | A kind of high bubble pressure microporous teflon membran and preparation method thereof |
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