CN115110168B - Manufacturing method of polytetrafluoroethylene fiber with high quality density uniformity - Google Patents

Manufacturing method of polytetrafluoroethylene fiber with high quality density uniformity Download PDF

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CN115110168B
CN115110168B CN202210727236.XA CN202210727236A CN115110168B CN 115110168 B CN115110168 B CN 115110168B CN 202210727236 A CN202210727236 A CN 202210727236A CN 115110168 B CN115110168 B CN 115110168B
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polytetrafluoroethylene
film
mass density
vertical oscillation
fiber
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CN115110168A (en
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徐玉康
薛士临
陈迎妹
陈银青
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Lingfulong New Material Technology Jiangsu Co ltd
Suzhou University
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Lingfulong New Material Technology Jiangsu Co ltd
Suzhou University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/48Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/42Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
    • D01D5/423Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by fibrillation of films or filaments

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

The invention discloses a method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity, which comprises the following steps: firstly, carrying out vertical oscillation pretreatment on granular polytetrafluoroethylene dispersion powder to adjust the elongation of particles in the powder; mixing the oscillated polytetrafluoroethylene dispersion powder with an auxiliary oil extrusion agent in proportion to prepare paste, and standing; thirdly, performing preforming, extrusion forming and calendaring on the paste after standing to obtain a calendared film; fourthly, carrying out hot drawing after degreasing on the rolled film to obtain a sintered film; fifthly, the sintered film is subjected to film splitting, carding and winding to obtain the polytetrafluoroethylene film splitting fiber with high quality density uniformity. The mass density range of the polytetrafluoroethylene fiber obtained by the method is 1.5-2.1 g/cm 3 The variation coefficient of the mass density is formed by>15% decrease to<8, the uniformity of the mass density of the fiber is improved.

Description

Manufacturing method of polytetrafluoroethylene fiber with high quality density uniformity
Technical Field
The invention relates to a preparation method of polytetrafluoroethylene fibers, in particular to a preparation method of polytetrafluoroethylene film-broken fibers with high mass density uniformity.
Background
The fluorine atoms on the surface of the molecular chain of Polytetrafluoroethylene (PTFE) are arranged in a spiral manner, so that the polytetrafluoroethylene has excellent chemical stability, and is insoluble in any other solvent except molten alkali metal and self-fluoride, and is called as "plastic king". In addition, the polytetrafluoroethylene has excellent high and low temperature resistance and can work for a long time in an environment of-260 ℃ to 260 ℃. The excellent corrosion resistance and excellent thermal stability make polytetrafluoroethylene widely applied in the field of industrial dust removal, especially in the field of dust filtration in garbage incineration.
Polytetrafluoroethylene fiber collection for preparing industrial dedusting filter materialThe preparation method comprises the step of preparing the product by a splitting film technology. Patent CN106381537A discloses a method for manufacturing PTFE short fibers, which is based on the conventional polytetrafluoroethylene film-broken fiber forming technology and adopts the density of 2.178-2.18 g/cm 3 The polytetrafluoroethylene dispersion powder is used as a raw material to improve the softness of polytetrafluoroethylene split fibers. Patent CN207973830U discloses a system for preparing polytetrafluoroethylene short fibers by using materials with different molecular weights, and the patent performs flow configuration design on specific equipment in the polytetrafluoroethylene short fiber forming process. In the prior art, a lot of efforts are made on the forming technology of polytetrafluoroethylene membrane split fibers and the improvement of fiber performance, but an effective solution is lacking for the problem that uneven fiber mass density is caused by uneven stretching force of polytetrafluoroethylene molecular chains in a sintered membrane in the process of hot stretching the polytetrafluoroethylene membrane split fibers.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention is directed to improving the mass density uniformity of polytetrafluoroethylene fibers.
In order to achieve the above object, the present invention provides a method for manufacturing polytetrafluoroethylene fiber with high mass density uniformity, comprising the steps of:
firstly, carrying out vertical oscillation pretreatment on granular polytetrafluoroethylene dispersion powder to adjust the elongation of particles in the powder;
mixing the oscillated polytetrafluoroethylene dispersion powder with an auxiliary oil extrusion agent in proportion to prepare paste, and standing;
thirdly, performing preforming, extrusion forming and calendaring on the paste after standing to obtain a calendared film;
fourthly, carrying out hot drawing after degreasing on the rolled film to obtain a sintered film;
fifthly, the sintered film is subjected to film splitting, carding and winding to obtain the polytetrafluoroethylene film splitting fiber with high quality density uniformity.
Further, in the step (one), vertical oscillation pretreatment is performed in an upper vertical oscillation device and a lower vertical oscillation device, wherein the device comprises an upper cover, a vertical oscillation groove, a vertical oscillation piston, a piston driving device and a base; the piston driving device arranged on the base can drive the vertical vibration piston to move up and down, so as to drive the vertical vibration groove to vibrate.
Further, in the step (I), the vertical oscillation frequency is 10-250 times/min, the vertical oscillation amplitude is 1-200 mm, the vertical oscillation time is 1-300 min, and the vertical oscillation environment temperature is-40-50 ℃.
Further, the elongation of the particles in the polytetrafluoroethylene dispersion powder pretreated by vertical oscillation up and down is 0.8 to 4.0, preferably, the elongation is 0.8 to 3.2.
In the step (II), the oil extrusion assisting agent is aviation kerosene.
Further, in the step (II), uniformly mixing polytetrafluoroethylene dispersion powder and aviation kerosene according to the mass ratio of 100:10-30 to obtain a paste, and standing the paste in an environment with the temperature of 45-60 ℃ for 15-60 hours.
Further, in the step (III), the thickness of the rolled film is 100 μm to 200. Mu.m.
In the step (IV), the rolled film is subjected to thermal drafting through a box body with the temperature of 200-250 ℃ to evaporate aviation kerosene, and then the box body with the temperature of 390 ℃ to obtain a sintered film; wherein, the input speed of the hot drawing is 4-6 m/min, and the output speed is 30-60 m/min.
Further, in the step (five), the input speed of the sintering film is 30-60 m/min, the winding speed of the polytetrafluoroethylene fiber bundle is 30-60 m/min, and the mass density of the polytetrafluoroethylene fiber is 1.5-2.1 g/cm 3 The coefficient of variation of the mass density is<8%。
Further, the granular polytetrafluoroethylene dispersion powder includes conventional granular polytetrafluoroethylene dispersion powder and granular polytetrafluoroethylene dispersion powder modified physically or chemically.
The invention provides a method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity, which comprises the steps of firstly carrying out vibration pretreatment on polytetrafluoroethylene dispersion powder by adopting an up-down vertical oscillation technology to adjust the elongation of particles in the powder, and then adopting the polytetrafluoroethylene dispersion powder pretreated by the vibration pretreatment as a raw material to prepare polytetrafluoroethylene film-broken fibers with high mass density uniformity through the processes of paste preparation, standing, preforming, extrusion forming and the like. Compared with the prior art, the invention has the beneficial effects that: 1) The invention adopts vertical oscillation technology to preprocess granular polytetrafluoroethylene dispersion powder to change the extension of particles in the dispersion powder, improves the uniformity of stretching force born by polytetrafluoroethylene molecular chains in a sintering film in the hot stretching process, and further improves the uniformity of mass density of polytetrafluoroethylene film-broken fibers, and 2) polytetrafluoroethylene fibers with high uniformity of mass density, which are prepared by the technical scheme of the invention, are used for preparing industrial dust-removing filter materials, can avoid the phenomenon that fibers are embedded into carding card clothing and broken holes in fiber net on a carding machine due to uneven mass density of the fibers, and improves the uniformity of carding and forming of polytetrafluoroethylene fibers.
The conception, specific structure, and technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, features, and effects of the present invention.
Drawings
FIG. 1 is a schematic diagram showing the structure of an up-down vertical oscillation device according to a preferred embodiment of the present invention;
FIG. 2 is a schematic view of polytetrafluoroethylene particles in a preferred embodiment of the invention;
FIG. 3 is a process flow diagram of a preferred embodiment of the present invention;
Detailed Description
The following description of the preferred embodiments of the present invention refers to the accompanying drawings, which make the technical contents thereof more clear and easy to understand. The present invention may be embodied in many different forms of embodiments and the scope of the present invention is not limited to only the embodiments described herein.
In the embodiment of the method for producing polytetrafluoroethylene fiber having high mass density uniformity according to the present invention, as shown in fig. 3, an up-down vertical oscillation device is used as shown in fig. 1. The device comprises an upper cover 1, a vertical oscillating groove 3, a vertical oscillating piston 4, a piston driving device 5 and a base 6. The piston driving device 5 arranged on the base 6 can drive the vertical vibration piston 4 to move up and down, so as to drive the vertical vibration groove 3 to vibrate. When the vibration pretreatment device is used, PTEE dispersed powder is placed in a vertical vibration groove 3, an upper cover 1 is covered, and after the vibration frequency, amplitude and time are set, a vertical vibration piston 4 is started to perform vibration pretreatment in the first step. The cold fluidity of the polytetrafluoroethylene powder particles is utilized, and the polytetrafluoroethylene elongation is increased by vertically oscillating the particles up and down.
In this application, the elongation=log2 (a/b), as shown in fig. 2, a is the major axis length of the particle-fitted ellipse, and b is the minor axis length of the particle-fitted ellipse.
After the granular polytetrafluoroethylene dispersion powder is vertically oscillated up and down, part of spherical particles are elongated (the relative sliding capacity among the spherical particles is strong, but the inter-particle friction is small, and fibrils are difficult to form); in order to form fibrils between particles, the amount of fibrils is increased by increasing the elongation of the particles to increase the mutual frictional strength between the particles (i.e., decrease the relative sliding ability between the particles), thereby improving the subsequent force distribution.
The relative slip between the particles decreases with increasing elongation of the particles, and when the relative slip decreases to a certain extent, the number of inter-particle fibrils dispersed in the extrusion molding process decreases greatly, resulting in a decrease in the number of inter-particle fibrils in the extrusion molding, an increase in structural non-uniformity of the extrusion molding, and a decrease in the uniformity of the final product. If the elongation of the particles is too great, the packing density between the particles increases greatly, resulting in failure to form effective relative slip between the particles in the extrusion process, but rather in increased structural non-uniformity of the end product. That is, the amount of fibrils between particles shows a tendency to increase and decrease with increasing elongation of the particles.
Example 1
Firstly, taking conventional granular polytetrafluoroethylene dispersion powder as a raw material, placing a certain amount of granular polytetrafluoroethylene dispersion powder into an upper vertical oscillation device for vertical oscillation pretreatment, wherein the vertical oscillation frequency is 15 times/min, the vertical oscillation amplitude is 2mm, the vertical oscillation time is 30min, the vertical oscillation environment temperature is 10 ℃, and the elongation of the particles in the polytetrafluoroethylene dispersion powder subjected to the vertical oscillation pretreatment is 0.8.
Mixing the polytetrafluoroethylene dispersion powder subjected to the oscillation preprocessing treatment with aviation kerosene, uniformly mixing the polytetrafluoroethylene dispersion powder and aviation kerosene according to the mass ratio of 100:20 to obtain a paste, and standing the paste in an environment at 50 ℃ for 40 hours;
pouring the paste subjected to standing in the step two into a preforming device, pressurizing to prepare a preforming body, and performing extrusion molding and calendaring to obtain a calendared film with the thickness of 120 mu m;
and step four, passing the rolled film in the step three through a box body with the temperature of 230 ℃ to evaporate aviation kerosene, and then carrying out hot drawing through the box body with the temperature of 390 ℃ to obtain the sintered film. Wherein, the input speed of the hot drawing is 4m/min, and the output speed is 35m/min;
and fifthly, feeding the sintered film in the step four into a film splitting device, and then carding by a carding needle roller, and winding to prepare the polytetrafluoroethylene film splitting fiber with high quality density uniformity. The input speed of the sintering film is 35m/min, the winding speed of the polytetrafluoroethylene fiber bundle is 35m/min, and the mass density of the polytetrafluoroethylene split fiber is 1.9g/cm 3 The mass density variation coefficient is 7%.
Example 2
Firstly, taking conventional granular polytetrafluoroethylene dispersion powder as a raw material, placing a certain amount of granular polytetrafluoroethylene dispersion powder into an upper vertical oscillation device for vertical oscillation pretreatment, wherein the vertical oscillation frequency is 40 times/min, the vertical oscillation amplitude is 2mm, the vertical oscillation time is 60min, the vertical oscillation environment temperature is 10 ℃, and the elongation of the particles in the polytetrafluoroethylene dispersion powder subjected to the vertical oscillation pretreatment is 2.0.
Mixing the polytetrafluoroethylene dispersion powder subjected to the oscillation preprocessing treatment with aviation kerosene, uniformly mixing the polytetrafluoroethylene dispersion powder and aviation kerosene according to the mass ratio of 100:20 to obtain a paste, and standing the paste in an environment at 50 ℃ for 40 hours;
pouring the paste subjected to standing in the step two into a preforming device, pressurizing to prepare a preforming body, and performing extrusion molding and calendaring to obtain a calendared film with the thickness of 120 mu m;
and step four, passing the rolled film in the step three through a box body with the temperature of 230 ℃ to evaporate aviation kerosene, and then carrying out hot drawing through the box body with the temperature of 390 ℃ to obtain the sintered film. Wherein, the input speed of the hot drawing is 4m/min, and the output speed is 35m/min;
and fifthly, feeding the sintered film in the step four into a film splitting device, and then carding by a carding needle roller, and winding to prepare the polytetrafluoroethylene film splitting fiber with high quality density uniformity. The input speed of the sintering film is 35m/min, the winding speed of the polytetrafluoroethylene fiber bundle is 35m/min, and the mass density of the polytetrafluoroethylene split fiber is 1.95g/cm 3 The mass density variation coefficient is 4%.
Example 3
Firstly, taking conventional granular polytetrafluoroethylene dispersion powder as a raw material, placing a certain amount of granular polytetrafluoroethylene dispersion powder into an upper vertical oscillation device for vertical oscillation pretreatment, wherein the vertical oscillation frequency is 60 times/min, the vertical oscillation amplitude is 2mm, the vertical oscillation time is 100min, the vertical oscillation environment temperature is 10 ℃, and the elongation of particles in the polytetrafluoroethylene dispersion powder subjected to the vertical oscillation pretreatment is 3.2.
Mixing the polytetrafluoroethylene dispersion powder subjected to the oscillation preprocessing treatment with aviation kerosene, uniformly mixing the polytetrafluoroethylene dispersion powder and aviation kerosene according to the mass ratio of 100:20 to obtain a paste, and standing the paste in an environment at 50 ℃ for 40 hours;
pouring the paste subjected to standing in the step two into a preforming device, pressurizing to prepare a preforming body, and performing extrusion molding and calendaring to obtain a calendared film with the thickness of 120 mu m;
and step four, passing the rolled film in the step three through a box body with the temperature of 230 ℃ to evaporate aviation kerosene, and then carrying out hot drawing through the box body with the temperature of 390 ℃ to obtain the sintered film. Wherein, the input speed of the hot drawing is 4m/min, and the output speed is 35m/min;
and fifthly, feeding the sintered film in the step four into a film splitting device, and then carding by a carding needle roller, and winding to prepare the polytetrafluoroethylene film splitting fiber with high quality density uniformity. The input speed of the sintering film is 35m/min, the winding speed of the polytetrafluoroethylene fiber bundle is 35m/min, and the mass density of the polytetrafluoroethylene split fiber is 2.03g/cm 3 The mass density variation coefficient is 7.2%.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention without requiring creative effort by one of ordinary skill in the art. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.

Claims (9)

1. A method for manufacturing polytetrafluoroethylene fiber with high quality density uniformity is characterized by comprising the following steps:
firstly, carrying out vertical oscillation pretreatment on granular polytetrafluoroethylene dispersion powder to adjust the elongation of particles in the powder;
the elongation of the particles in the polytetrafluoroethylene dispersion powder pretreated by vertical oscillation is 0.8-3.2;
the elongation = log2 (a/b), a being the major axis length of the particle-fitted ellipse, b being the minor axis length of the particle-fitted ellipse;
mixing the oscillated polytetrafluoroethylene dispersion powder with an auxiliary oil extrusion agent in proportion to prepare paste, and standing;
thirdly, performing preforming, extrusion forming and calendaring on the paste after standing to obtain a calendared film;
fourthly, carrying out hot drawing after degreasing on the rolled film to obtain a sintered film;
fifthly, the sintered film is subjected to film splitting, carding and winding to obtain the polytetrafluoroethylene film splitting fiber with high quality density uniformity.
2. The method for producing polytetrafluoroethylene fiber having high mass density uniformity according to claim 1 wherein, in the step (one), the vertical oscillation pretreatment is performed in a vertical oscillation device; the vertical oscillation device comprises an upper cover, a vertical oscillation groove, a vertical oscillation piston, a piston driving device and a base; the piston driving device arranged on the base can drive the vertical vibration piston to move up and down, so as to drive the vertical vibration groove to vibrate.
3. The method for producing polytetrafluoroethylene fiber having high uniformity of mass density according to claim 2, wherein in the step (one), the vertical oscillation frequency is 10 to 250 times/min, the vertical oscillation amplitude is 1 to 200mm, the vertical oscillation time is 1 to 300min, and the vertical oscillation ambient temperature is-40 to 50 ℃.
4. The method for producing polytetrafluoroethylene fiber having high mass density uniformity according to claim 1 wherein in step (two), the extrusion aid is aviation kerosene.
5. The method for producing polytetrafluoroethylene fiber having high mass density uniformity according to claim 4, wherein in the second step, polytetrafluoroethylene dispersion powder and aviation kerosene are uniformly mixed at a mass ratio of 100:10-30 to obtain a paste, and the paste is left to stand at a temperature of 45 ℃ to 60 ℃ for 15 to 60 hours.
6. The method for producing polytetrafluoroethylene fiber having high mass density uniformity according to claim 5 wherein in step (III), the thickness of the rolled film is 100 μm to 200. Mu.m.
7. The method for producing polytetrafluoroethylene fiber with high mass density uniformity according to claim 6, wherein in the step (four), the sintered film is obtained by passing a rolled film through a box at a temperature of 200 ℃ to 250 ℃ to evaporate aviation kerosene, and then passing the film through a box at a temperature of 390 ℃ to carry out hot drawing; wherein, the input speed of the hot drawing is 4-6 m/min, and the output speed is 30-60 m/min.
8. The method for producing polytetrafluoroethylene fiber having high mass density uniformity according to claim 7, wherein in the step (fifth), the sintered film input speed is 30 to 60m/min, the polytetrafluoroethylene fiber bundle winding speed is 30 to 60m/min, and the mass density of the polytetrafluoroethylene split fiber is 1.5 to 2.1g/cm 3 The coefficient of variation of the mass density is<8%。
9. The method for producing polytetrafluoroethylene fiber having high mass density uniformity according to claim 8 wherein the granular polytetrafluoroethylene dispersion powder comprises a conventional granular polytetrafluoroethylene dispersion powder and a physically or chemically modified granular polytetrafluoroethylene dispersion powder.
CN202210727236.XA 2022-06-24 2022-06-24 Manufacturing method of polytetrafluoroethylene fiber with high quality density uniformity Active CN115110168B (en)

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CN116288778A (en) * 2023-03-16 2023-06-23 南京英斯瑞德高分子材料股份有限公司 Manufacturing and preparing method for PTFE (polytetrafluoroethylene) membranous split filament synthetic fibers

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CN102051703A (en) * 2010-11-25 2011-05-11 辽宁省金氟龙环保新材料有限公司 Manufacturing method of film split polytetrafluoroethylene fibers
CN102071483A (en) * 2010-11-22 2011-05-25 宋朋泽 Preparation method of polytetrafluoroethylene chopped fiber
CN111793853A (en) * 2020-08-05 2020-10-20 扬州大学 Spinning method of PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) conductive fiber with high elongation
CN113046855A (en) * 2021-03-23 2021-06-29 苏州大学 Low linear density bundle-shaped polytetrafluoroethylene filament and preparation process and application thereof
CN113122950A (en) * 2021-03-16 2021-07-16 苏州大学 Rapid manufacturing method of polytetrafluoroethylene fiber

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102071483A (en) * 2010-11-22 2011-05-25 宋朋泽 Preparation method of polytetrafluoroethylene chopped fiber
CN102051703A (en) * 2010-11-25 2011-05-11 辽宁省金氟龙环保新材料有限公司 Manufacturing method of film split polytetrafluoroethylene fibers
CN111793853A (en) * 2020-08-05 2020-10-20 扬州大学 Spinning method of PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) conductive fiber with high elongation
CN113122950A (en) * 2021-03-16 2021-07-16 苏州大学 Rapid manufacturing method of polytetrafluoroethylene fiber
CN113046855A (en) * 2021-03-23 2021-06-29 苏州大学 Low linear density bundle-shaped polytetrafluoroethylene filament and preparation process and application thereof

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