CN115058784B - Preparation method of polytetrafluoroethylene flat filament with high quality density uniformity - Google Patents
Preparation method of polytetrafluoroethylene flat filament with high quality density uniformity Download PDFInfo
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- CN115058784B CN115058784B CN202210725682.7A CN202210725682A CN115058784B CN 115058784 B CN115058784 B CN 115058784B CN 202210725682 A CN202210725682 A CN 202210725682A CN 115058784 B CN115058784 B CN 115058784B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/42—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
- D01D5/426—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by cutting films
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/224—Selection or control of the temperature during stretching
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D10B2321/04—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons
- D10B2321/042—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of halogenated hydrocarbons polymers of fluorinated hydrocarbons, e.g. polytetrafluoroethene [PTFE]
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The application discloses a preparation method of polytetrafluoroethylene flat filaments 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; (IV) deoiling the calendered film; (V) uniformly cutting the deoiled calendered film to obtain initial polytetrafluoroethylene flat filaments; (six) carrying out hot drawing on the initial polytetrafluoroethylene flat filaments; and (seventh) performing heat setting on the flat filaments subjected to heat drawing to obtain polytetrafluoroethylene flat filaments. The mass density of the polytetrafluoroethylene flat filament prepared by the method ranges from 1.9g/cm to 2.03g/cm 3 The mass density coefficient of the modified ceramic material is 3.8% -5.4%.
Description
Technical Field
The application relates to a preparation method of polytetrafluoroethylene filaments, in particular to a preparation method of polytetrafluoroethylene flat filaments with high quality density uniformity.
Background
Industrial fumes are a major source of atmospheric pollution and have become a common problem worldwide. At present, an industrial smoke filtering material is mainly a film-covered needled felt, wherein the needled felt is mainly prepared by processing functional fibers and a reinforcing base cloth through a needling process, and the reinforcing base cloth is a woven cloth woven by Polytetrafluoroethylene (PTFE) filaments. The polytetrafluoroethylene has good chemical stability, is insoluble in a conventional solvent, is called as a plastic king, has excellent high and low temperature resistance (-260 ℃ to 260 ℃) and has the characteristics of non-adhesive surface, low friction coefficient and the like, and becomes an ideal material for preparing industrial smoke filtering material base cloth.
Because of extremely high melt viscosity (1010-1011 Pa.S), polytetrafluoroethylene filaments cannot be prepared by adopting a conventional melt extrusion method, a paste extrusion method or a cutting method is generally adopted at present, and polytetrafluoroethylene filaments for filter material base cloth are prepared by adopting a cutting method. Patent CN104294382a discloses a process for manufacturing high-strength low-elongation polytetrafluoroethylene filaments, which comprises the steps of standing polytetrafluoroethylene dispersion powder in an environment with the temperature lower than 15 ℃ for balance adjustment, and then adopting a conventional forming process to prepare high-strength low-elongation polytetrafluoroethylene flat filaments. Patent CN110528131a discloses a process for manufacturing high-strength low-friction polytetrafluoroethylene sewing thread, which comprises the steps of twisting initial polytetrafluoroethylene flat filaments obtained by cutting, and performing hot drawing to obtain single-strand sewing thread. Patent CN101713101a discloses a production method of polytetrafluoroethylene fiber filaments, which comprises the steps of firstly adhering and compounding a polytetrafluoroethylene film with a polyester film, then cutting the compounded double-layer film, and then removing the polyester film and thermally stretching the polytetrafluoroethylene film to prepare the polytetrafluoroethylene fiber filaments.
In the prior art, the preparation process of the polytetrafluoroethylene flat filament adopts the conventional polytetrafluoroethylene dispersion powder or directly processing or carrying out balance treatment on the powder, and then processing the polytetrafluoroethylene dispersion powder through the processes of paste preparation, preforming, extrusion molding, calendaring, slitting and the like to prepare the polytetrafluoroethylene flat filament. The relative friction strength among particles in the polytetrafluoroethylene dispersion powder raw material adopted in the prior art is lower in extrusion molding and calendaring processes, so that fibrils are formed and distributed unevenly, and further, the polytetrafluoroethylene structure in the flat filaments is uneven, and finally, the mass density of the flat filaments is uneven.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present application is directed to improving the mass density uniformity of polytetrafluoroethylene fibers.
In order to achieve the above object, the present application provides a method for preparing polytetrafluoroethylene flat filaments 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;
(IV) deoiling the calendered film;
(V) uniformly cutting the deoiled calendered film to obtain initial polytetrafluoroethylene flat filaments;
(six) carrying out hot drawing on the initial polytetrafluoroethylene flat filaments;
and (seventh) performing heat setting on the flat filaments subjected to heat drawing to obtain polytetrafluoroethylene flat filaments.
Further, in the step (one), 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.
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 is 0.8-4.0. Preferably, the elongation is 1.0-3.1.
In the step (II), the extrusion assisting oil 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 30-60 hours.
Further, in the step (III), the thickness of the rolled film is 200 μm to 400. Mu.m.
In the step (V), the rolled film after the oil removal treatment is conveyed to a cutting device, and the rolled film is uniformly cut to obtain 20-200 initial polytetrafluoroethylene flat filaments, wherein the width of the initial polytetrafluoroethylene flat filaments is 0.5-3 mm.
In the step (six), the initial polytetrafluoroethylene flat filaments are conveyed to a hot drawing device for hot drawing processing, the temperature is 250-380 ℃, the number of groups of drawing points is 3-5, the drawing multiple is 20-40 times, the input speed is 0.4-1.0 m/min, and the output speed is 10-40 m/min.
Further, in the step (seventh), the flat filaments after hot drawing are conveyed to a hot shaping box body for heat shaping processing, the temperature of the box body is 360-440 ℃, the input speed is 80-120 m/min, the output speed is 100-140 m/min, and the mass density of the polytetrafluoroethylene flat filaments is 1.9-2.03g/cm 3 The mass density coefficient of the modified ceramic material is 3.8% -5.4%.
Compared with the prior art, the application has the beneficial effects that:
1) According to the application, the vertical oscillation technology is adopted to carry out oscillation preprocessing treatment on the granular polytetrafluoroethylene dispersion powder, and the structural uniformity of the polytetrafluoroethylene flat filaments is improved by improving the interaction strength among particles in the dispersion powder, so that the mass density uniformity of the flat filaments is improved.
2) The preparation method of the polytetrafluoroethylene flat filament with high quality density uniformity has high production efficiency and can improve the yield.
The conception, specific structure, and technical effects of the present application will be further described with reference to the accompanying drawings to fully understand the objects, features, and effects of the present application.
Drawings
Fig. 1 is a schematic diagram of an up-down vertical oscillation device according to a preferred embodiment of the present application.
Fig. 2 is a schematic structural view of polytetrafluoroethylene particles in a preferred embodiment of the application.
FIG. 3 is a process flow diagram of a preferred embodiment of the present application.
Detailed Description
The following description of the preferred embodiments of the present application refers to the accompanying drawings, which make the technical contents thereof more clear and easy to understand. The present application may be embodied in many different forms of embodiments and the scope of the present application is not limited to only the embodiments described herein.
In the embodiment of the method for preparing polytetrafluoroethylene flat filaments with high mass density uniformity according to the present application, 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 application utilizes the cold fluidity of polytetrafluoroethylene powder particles, and increases the elongation of polytetrafluoroethylene by vertically oscillating the particles up and down.
In the present 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 preprocessing, wherein the vertical oscillation frequency is 50 times/min, the vertical oscillation amplitude is 10mm, the vertical oscillation time is 15min, the vertical oscillation environment temperature is 15 ℃, and the elongation of the particles in the polytetrafluoroethylene dispersion powder subjected to the vertical oscillation preprocessing is 1.0.
In this embodiment, 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.
Mixing the polytetrafluoroethylene dispersion powder subjected to oscillation preprocessing 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 55 ℃ for 50 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 250 mu m;
step four, passing the rolled film in the step three through a box body with the temperature of 240 ℃ to evaporate aviation kerosene, wherein the input speed is 10m/min, and the output speed is 10m/min;
and step five, conveying the deoiled rolled film in the step four to a cutting device, and uniformly cutting the stretched film by a cutting blade to obtain 80 initial polytetrafluoroethylene flat filaments. Wherein the width of the initial polytetrafluoroethylene flat filament is 1.5mm;
step six, conveying the flat filaments in the step five to a hot drawing device for hot drawing processing, wherein the temperature is 360 ℃, the number of groups of drawing points is 4 groups, the drawing multiple is 30 times, the input speed is 0.5m/min, and the output speed is 15m/min;
and step seven, conveying the flat filaments subjected to the hot drawing in the step six to a hot setting box body for hot setting processing to prepare polytetrafluoroethylene flat filaments with high density uniformity. The temperature of the box body is 400 ℃, the input speed is 90m/min, the output speed is 120m/min, the mass density is 1.9g/cm < 3 >, and the mass density variation coefficient is 5%.
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 50 times/min, the vertical oscillation amplitude is 10mm, the vertical oscillation time is 50min, the vertical oscillation environment temperature is 15 ℃, and the elongation of the particles in the polytetrafluoroethylene dispersion powder subjected to the vertical oscillation pretreatment is 2.2.
Mixing the polytetrafluoroethylene dispersion powder subjected to oscillation preprocessing 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 55 ℃ for 50 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 250 mu m;
step four, passing the rolled film in the step three through a box body with the temperature of 240 ℃ to evaporate aviation kerosene, wherein the input speed is 10m/min, and the output speed is 10m/min;
and step five, conveying the deoiled rolled film in the step four to a cutting device, and uniformly cutting the stretched film by a cutting blade to obtain 80 initial polytetrafluoroethylene flat filaments. Wherein the width of the initial polytetrafluoroethylene flat filament is 1.5mm;
step six, conveying the flat filaments in the step five to a hot drawing device for hot drawing processing, wherein the temperature is 360 ℃, the number of groups of drawing points is 4 groups, the drawing multiple is 30 times, the input speed is 0.5m/min, and the output speed is 15m/min;
and step seven, conveying the flat filaments subjected to the hot drawing in the step six to a hot setting box body for hot setting processing to prepare polytetrafluoroethylene flat filaments with high density uniformity. The temperature of the box body is 400 ℃, the input speed is 90m/min, the output speed is 120m/min, the mass density is 1.95g/cm < 3 >, and the variation coefficient of the mass density is 3.8%.
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 10mm, the vertical oscillation time is 100min, the vertical oscillation environment temperature is 15 ℃, and the elongation of particles in the polytetrafluoroethylene dispersion powder subjected to the vertical oscillation pretreatment is 3.1.
Mixing the polytetrafluoroethylene dispersion powder subjected to oscillation preprocessing 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 55 ℃ for 50 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 250 mu m;
step four, passing the rolled film in the step three through a box body with the temperature of 240 ℃ to evaporate aviation kerosene, wherein the input speed is 10m/min, and the output speed is 10m/min;
and step five, conveying the deoiled rolled film in the step four to a cutting device, and uniformly cutting the stretched film by a cutting blade to obtain 80 initial polytetrafluoroethylene flat filaments. Wherein the width of the initial polytetrafluoroethylene flat filament is 1.5mm;
step six, conveying the flat filaments in the step five to a hot drawing device for hot drawing processing, wherein the temperature is 360 ℃, the number of groups of drawing points is 4 groups, the drawing multiple is 30 times, the input speed is 0.5m/min, and the output speed is 15m/min;
and step seven, conveying the flat filaments subjected to the hot drawing in the step six to a hot setting box body for hot setting processing to prepare polytetrafluoroethylene flat filaments with high density uniformity. The temperature of the box body is 400 ℃, the input speed is 90m/min, the output speed is 120m/min, the mass density is 2.03g/cm < 3 >, and the variation coefficient of the mass density is 5.4%.
The foregoing describes in detail preferred embodiments of the present application. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the application 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 preparation method of polytetrafluoroethylene flat filaments with high mass 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 0.8-4.0;
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;
(IV) deoiling the calendered film;
(V) uniformly cutting the deoiled calendered film to obtain initial polytetrafluoroethylene flat filaments;
(six) carrying out hot drawing on the initial polytetrafluoroethylene flat filaments;
and (seventh) performing heat setting on the flat filaments subjected to heat drawing to obtain polytetrafluoroethylene flat filaments.
2. The method for producing a polytetrafluoroethylene flat filament with 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 a polytetrafluoroethylene flat filament with high mass density uniformity 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 process for producing polytetrafluoroethylene flat filament with high density uniformity according to claim 3, wherein in the second step, the extrusion assisting oil agent is aviation kerosene.
5. The method for producing a polytetrafluoroethylene flat filament with high 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 30-60 hours.
6. The process for producing a polytetrafluoroethylene flat filament having high mass density uniformity according to claim 5, wherein in the step (III), the thickness of the rolled film is 200 μm to 400. Mu.m.
7. The method for producing a polytetrafluoroethylene flat filament with high density uniformity according to claim 6, wherein in the step (five), the rolled film after the degreasing treatment is fed to a cutting device, and the number of the initial polytetrafluoroethylene flat filaments is 20-200, and the width of the initial polytetrafluoroethylene flat filaments is 0.5-3 mm.
8. The method for producing a polytetrafluoroethylene flat filament with high density uniformity according to claim 7, wherein in the step (six), the initial polytetrafluoroethylene flat filament is fed to a hot drawing device for hot drawing at a temperature of 250 ℃ to 380 ℃, the number of groups of drawing points is 3 to 5, the drawing multiple is 20 to 40 times, the input speed is 0.4 to 1.0m/min, and the output speed is 10 to 40m/min.
9. The method for producing a polytetrafluoroethylene flat filament with high mass density uniformity according to claim 8, wherein in the step (seventh), the flat filament after heat drawing is transported to a heat-setting tank for heat-setting processing, the tank temperature is 360 ℃ to 440 ℃, the input speed is 80 to 120m/min, the output speed is 100 to 140m/min, and the mass density of the polytetrafluoroethylene flat filament is in the range of 1.9 to 2.03g/cm 3 The mass density coefficient of the modified ceramic material is 3.8% -5.4%.
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