CN115110168A - Method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity - Google Patents

Method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity Download PDF

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CN115110168A
CN115110168A CN202210727236.XA CN202210727236A CN115110168A CN 115110168 A CN115110168 A CN 115110168A CN 202210727236 A CN202210727236 A CN 202210727236A CN 115110168 A CN115110168 A CN 115110168A
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polytetrafluoroethylene
mass density
vertical oscillation
dispersion powder
fibers
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CN115110168B (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)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (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 granules in the powder; secondly, mixing the vibrated polytetrafluoroethylene dispersion powder and the extrusion-assisting oil agent in proportion to prepare paste and standing; thirdly, performing, extruding and rolling the paste after standing to obtain a rolled film; fourthly, the rolled film is subjected to hot drawing after oil removal to obtain a sintered film; and (V) splitting, carding and winding the sintered film to obtain the polytetrafluoroethylene split fiber with high mass density uniformity. The mass density range of the polytetrafluoroethylene fiber prepared by the method is 1.5-2.1 g/cm 3 Coefficient of variation of mass density of>15% reduction to<8%,The quality density uniformity of the fiber is improved.

Description

Method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity
Technical Field
The invention relates to a preparation method of polytetrafluoroethylene fibers, in particular to a preparation method of polytetrafluoroethylene split fibers with high mass density uniformity.
Background
The fluorine atoms on the molecular chain surface of Polytetrafluoroethylene (PTFE) are arranged in a spiral shape, which gives the PTFE excellent chemical stability, and except for molten alkali metal and self-fluorinated substance, it is insoluble in any other solvent, and is called "plastic king". In addition, the polytetrafluoroethylene also 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 the polytetrafluoroethylene have wide application in the field of industrial dust removal, especially in the field of waste incineration smoke dust filtration.
The polytetrafluoroethylene fiber for preparing the industrial dedusting filter material is prepared by adopting a film splitting technology. The patent CN106381537A discloses a method for manufacturing PTFE short fibers, which is based on the conventional polytetrafluoroethylene split 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 the polytetrafluoroethylene split fiber. Patent CN207973830U discloses a system for preparing polytetrafluoroethylene short fibers by using materials with different molecular weights, which performs flow configuration design on specific equipment in a polytetrafluoroethylene short fiber forming process. In the prior art, a lot of efforts are made on the aspects of forming technology and fiber performance improvement of polytetrafluoroethylene split fibers, but an effective solution is lacked for the problem that the polytetrafluoroethylene split fibers have uneven drafting acting force on polytetrafluoroethylene molecular chains in a sintered film in the hot drafting process, so that the mass density of the fibers is uneven.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problem to be solved by the present invention is how to improve the uniformity of mass density of polytetrafluoroethylene fibers.
In order to achieve the above object, the present invention provides a method for manufacturing a polytetrafluoroethylene fiber having a high uniformity of mass density, comprising the steps of:
firstly, carrying out vertical oscillation pretreatment on granular polytetrafluoroethylene dispersion powder to adjust the elongation of granules in the powder;
secondly, mixing the vibrated polytetrafluoroethylene dispersion powder and the extrusion-assisting oil agent in proportion to prepare paste and standing;
thirdly, performing, extruding and rolling the paste after standing to obtain a rolled film;
fourthly, the rolled film is subjected to hot drawing after oil removal to obtain a sintered film;
and (V) splitting, carding and winding the sintered film to obtain the polytetrafluoroethylene split fiber with high mass density uniformity.
Further, in the step (one), the vertical oscillation pretreatment is carried out in a vertical oscillation device which 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 from top to bottom is 0.8 to 4.0, preferably 0.8 to 3.2.
Further, in the step (II), the extrusion assisting oil agent is aviation kerosene.
Further, in the step (II), uniformly mixing the 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 to 200. mu.m.
Further, in the step (IV), the rolled film is subjected to aviation kerosene evaporation through a box body with the temperature of 200-250 ℃, and then is subjected to hot drawing through a 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 (V), 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 split fibers is 1.5-2.1 g/cm 3 Coefficient of variation of mass density of<8%。
Further, the granular polytetrafluoroethylene dispersion powder includes a conventional granular polytetrafluoroethylene dispersion powder and a physically or chemically modified granular polytetrafluoroethylene dispersion powder.
The invention provides a method for manufacturing polytetrafluoroethylene fibers with high mass density uniformity, which comprises the steps of firstly carrying out vibration preprocessing on polytetrafluoroethylene dispersion powder by adopting an up-and-down vertical oscillation technology so as to adjust the elongation of particles in the powder, then adopting the polytetrafluoroethylene dispersion powder subjected to vibration preprocessing as a raw material, and processing the raw material through paste preparation, standing, preforming, extrusion forming and other processes to prepare the polytetrafluoroethylene split fibers with high mass density uniformity. Compared with the prior art, the invention has the beneficial effects that: 1) the invention adopts the vertical oscillation technology to preprocess the granular polytetrafluoroethylene dispersion powder so as to change the elongation of the granules in the dispersion powder, improve the uniformity of the drafting acting force borne by a polytetrafluoroethylene molecular chain in a sintered film in the hot drafting process, and further improve the quality density uniformity of polytetrafluoroethylene film split fibers, 2) the polytetrafluoroethylene fibers with high quality density uniformity prepared by the technical scheme of the invention are used for preparing industrial dust removal filter materials, can avoid the phenomena of fiber embedding into carding card clothing and fiber net hole breaking caused by non-uniform fiber quality density on a carding machine, and improve the uniformity of the polytetrafluoroethylene fiber carding net.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a schematic structural diagram of an up-down vertical oscillation device in a preferred embodiment of the present invention;
FIG. 2 is a schematic structural view of polytetrafluoroethylene particles in a preferred embodiment of the invention;
FIG. 3 is a process flow diagram in a preferred embodiment of the invention;
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
As shown in FIG. 3, in the embodiment of the method for producing polytetrafluoroethylene fibers having high uniformity of mass density according to the invention, an up-down vertical oscillation device is used as shown in FIG. 1. The device comprises an upper cover 1, a vertical oscillation groove 3, a vertical vibration piston 4, a piston driving device 5 and a base 6. The vertical vibration piston 4 is driven to move up and down by the piston driving device 5 disposed on the base 6, thereby driving the vertical vibration tank 3 to vibrate. When the PTEE dispersion powder is used, the PTEE dispersion powder is placed in the vertical oscillation tank 3, the upper cover 1 is covered, and after the oscillation frequency, the amplitude and the time are set, the vertical oscillation piston 4 is started to perform oscillation preprocessing in the first step. This application utilizes the cold flow nature of polytetrafluoroethylene powder granule, through the vertical oscillation granule from top to bottom for polytetrafluoroethylene elongation increases.
The elongation of the particles in this application is log2(a/b), as shown in fig. 2, where a is the major axis length of the ellipse to which the particles are fitted and b is the minor axis length of the ellipse to which the particles are fitted.
After the granular polytetrafluoroethylene dispersion powder vertically oscillates up and down, part of spherical particles extend (the relative sliding capacity among the spherical particles is strong, but the friction among the spherical particles is small, and fibrils are difficult to form); in order to form fibrils among the particles, the elongation of the particles is increased to increase the mutual frictional strength among the particles (namely, the relative slippage capacity among the particles is reduced), so that the amount of the fibrils is increased, and the subsequent acting force distribution is improved.
The relative slippage capacity among the particles is reduced along with the increase of the elongation of the particles, and when the relative slippage capacity is reduced to a certain degree, the number of fibrils among the dispersed particles is greatly reduced in the extrusion forming process, so that the number of fibrils among the particles in the extrusion forming body is reduced, the structural nonuniformity of the extrusion forming body is increased, and the uniformity of a final product is reduced. If the elongation of the particles is too large, the packing compactness among the particles is greatly increased, so that effective relative slippage among the particles cannot be formed in the extrusion forming process, and the structural nonuniformity of the end product is increased. I.e. the amount of fibrils between particles shows a tendency to increase and then decrease with increasing elongation of the particles.
Example 1
Step one, adopting conventional granular polytetrafluoroethylene dispersion powder as a raw material, placing a certain amount of granular polytetrafluoroethylene dispersion powder in an up-down vertical oscillation device for up-down vertical oscillation preprocessing, wherein the up-down vertical oscillation frequency is 15 times/min, the up-down vertical oscillation amplitude is 2mm, the up-down vertical oscillation time is 30min, the up-down vertical oscillation environment temperature is 10 ℃, and the elongation of granules in the polytetrafluoroethylene dispersion powder subjected to the up-down vertical oscillation preprocessing is 0.8.
Step two, mixing the polytetrafluoroethylene dispersion powder subjected to oscillation preprocessing with aviation kerosene, uniformly mixing the polytetrafluoroethylene dispersion powder and the aviation kerosene according to the mass ratio of 100:20 to obtain a paste, and standing the paste in an environment with the temperature of 50 ℃ for 40 hours;
pouring the paste left standing in the step two into a preforming device, pressurizing to prepare a preforming body, and performing extrusion forming and calendering to obtain a calendered film with the thickness of 120 microns;
and step four, evaporating aviation kerosene from the calendered film in the step three through a box body with the temperature of 230 ℃, and performing hot drawing through a box body with the temperature of 390 ℃ to obtain a sintered film. Wherein the input speed of the hot drawing is 4m/min, and the output speed is 35 m/min;
and step five, feeding the sintered film obtained in the step four into a film splitting device, and then preparing the polytetrafluoroethylene split fiber with high quality density uniformity through carding by a carding needle roller and winding. The input speed of the sintered film is 35m/min, and the winding speed of the polytetrafluoroethylene fiber bundle is35m/min, the mass density of the polytetrafluoroethylene split fibers is 1.9g/cm 3 The coefficient of variation of mass density was 7%.
Example 2
Step one, adopting conventional granular polytetrafluoroethylene dispersion powder as a raw material, placing a certain amount of granular polytetrafluoroethylene dispersion powder in an up-down vertical oscillation device for up-down vertical oscillation preprocessing, wherein the up-down vertical oscillation frequency is 40 times/min, the up-down vertical oscillation amplitude is 2mm, the up-down vertical oscillation time is 60min, the up-down vertical oscillation environment temperature is 10 ℃, and the elongation of granules in the polytetrafluoroethylene dispersion powder subjected to the up-down vertical oscillation preprocessing is 2.0.
Step two, mixing the polytetrafluoroethylene dispersion powder subjected to oscillation preprocessing with aviation kerosene, uniformly mixing the polytetrafluoroethylene dispersion powder and the aviation kerosene according to the mass ratio of 100:20 to obtain a paste, and standing the paste in an environment with the temperature of 50 ℃ for 40 hours;
pouring the paste left standing in the step two into a preforming device, pressurizing to prepare a preforming body, and performing extrusion forming and calendering to obtain a calendered film with the thickness of 120 microns;
and step four, evaporating aviation kerosene from the calendered film in the step three through a box body with the temperature of 230 ℃, and performing hot drawing through a box body with the temperature of 390 ℃ to obtain a sintered film. Wherein the input speed of the hot drawing is 4m/min, and the output speed is 35 m/min;
and step five, feeding the sintered film obtained in the step four into a film splitting device, and then preparing the polytetrafluoroethylene split fiber with high quality density uniformity through carding by a carding needle roller and winding. The input speed of the sintered membrane 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 coefficient of variation in mass density was 4%.
Example 3
Step one, adopting conventional granular polytetrafluoroethylene dispersion powder as a raw material, placing a certain amount of granular polytetrafluoroethylene dispersion powder in an up-and-down vertical oscillation device to perform up-and-down vertical oscillation preprocessing treatment, wherein the up-and-down vertical oscillation frequency is 60 times/min, the up-and-down vertical oscillation amplitude is 2mm, the up-and-down vertical oscillation time is 100min, the up-and-down vertical oscillation environment temperature is 10 ℃, and the elongation of granules in the polytetrafluoroethylene dispersion powder subjected to the up-and-down vertical oscillation preprocessing treatment is 3.2.
Step two, mixing the polytetrafluoroethylene dispersion powder subjected to oscillation preprocessing with aviation kerosene, uniformly mixing the polytetrafluoroethylene dispersion powder and the aviation kerosene according to the mass ratio of 100:20 to obtain a paste, and standing the paste in an environment with the temperature of 50 ℃ for 40 hours;
pouring the paste left standing in the step two into a preforming device, pressurizing to prepare a preforming body, and performing extrusion forming and calendering to obtain a calendered film with the thickness of 120 microns;
and step four, evaporating aviation kerosene from the calendered film in the step three through a box body with the temperature of 230 ℃, and performing hot drawing through a box body with the temperature of 390 ℃ to obtain a sintered film. Wherein the input speed of the hot drawing is 4m/min, and the output speed is 35 m/min;
and step five, feeding the sintered film obtained in the step four into a film splitting device, and then preparing the polytetrafluoroethylene split fiber with high quality density uniformity through carding by a carding needle roller and winding. The input speed of the sintered membrane 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 coefficient of variation in mass density was 7.2%.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (10)

1. A method for producing a polytetrafluoroethylene fiber having a high mass density uniformity, comprising the steps of:
firstly, carrying out vertical oscillation pretreatment on granular polytetrafluoroethylene dispersion powder to adjust the elongation of granules in the powder;
secondly, mixing the vibrated polytetrafluoroethylene dispersion powder and the extrusion assisting oil agent in proportion to prepare paste and standing;
thirdly, performing, extruding and rolling the paste after standing to obtain a rolled film;
fourthly, the rolled film is subjected to hot drawing after oil removal to obtain a sintered film;
and (V) splitting, carding and winding the sintered membrane to obtain the polytetrafluoroethylene split fiber with high mass density uniformity.
2. The method for producing polytetrafluoroethylene fibers with high uniformity of mass density as set forth in claim 1, wherein in the step (one), the vertical oscillation pretreatment is performed in a vertical oscillation device; the upper and lower vertical oscillation devices comprise 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 fibers with high uniformity of mass density according to claim 2, wherein in 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. A process for producing polytetrafluoroethylene fibers having high uniformity of mass density as set forth in claim 3, wherein the polytetrafluoroethylene dispersion powder pretreated by vertical oscillation has an elongation of particles of 0.8 to 4.0.
5. A process for producing polytetrafluoroethylene fibers with high uniformity of mass density as set forth in claim 4, wherein in step (II), the extrusion aid is jet fuel.
6. The process for producing polytetrafluoroethylene fibers having high uniformity of mass density according to claim 5, wherein in the second step, the polytetrafluoroethylene dispersion powder and aviation kerosene are uniformly mixed in a mass ratio of 100:10 to 30 to obtain a paste, and the paste is left to stand in an environment at a temperature of 45 ℃ to 60 ℃ for 15 to 60 hours.
7. A process for producing polytetrafluoroethylene fibers having high uniformity of mass density as set forth in claim 6, wherein in step (III), the thickness of the calendered film is from 100 to 200 μm.
8. The method for producing polytetrafluoroethylene fibers having high uniformity of mass density according to claim 7, wherein in the fourth step, the rolled film is passed through a chamber at a temperature of 200 ℃ to 250 ℃ to evaporate kerosene, and then is subjected to hot drawing in a chamber at a 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.
9. The method for producing polytetrafluoroethylene fibers with high uniformity of mass density according to claim 8, wherein in step (V), the sintered film feeding 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 fibers is 1.5 to 2.1g/cm 3 Coefficient of variation of mass density of<8%。
10. A process for producing polytetrafluoroethylene fibers with high uniformity of mass density as set forth in claim 9, wherein the polytetrafluoroethylene dispersion powder in the form of particles includes a conventional polytetrafluoroethylene dispersion powder in the form of particles and a polytetrafluoroethylene dispersion powder in the form of particles that has been physically or chemically modified.
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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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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