CN110424061B - Polytetrafluoroethylene colored film-cracked filament and preparation method thereof - Google Patents
Polytetrafluoroethylene colored film-cracked filament and preparation method thereof Download PDFInfo
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- CN110424061B CN110424061B CN201910702029.7A CN201910702029A CN110424061B CN 110424061 B CN110424061 B CN 110424061B CN 201910702029 A CN201910702029 A CN 201910702029A CN 110424061 B CN110424061 B CN 110424061B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/10—Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/22—Component parts, details or accessories; Auxiliary operations
- B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
- B29C43/10—Isostatic pressing, i.e. using non-rigid pressure-exerting members against rigid parts or dies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/36—Moulds for making articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
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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
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent 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
- D01F6/48—Monocomponent 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
- B29C43/10—Isostatic pressing, i.e. using non-rigid pressure-exerting members against rigid parts or dies
- B29C2043/106—Isostatic pressing, i.e. using non-rigid pressure-exerting members against rigid parts or dies using powder material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
- B29C2043/5808—Measuring, controlling or regulating pressure or compressing force
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
- B29C2043/5816—Measuring, controlling or regulating temperature
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Abstract
The invention discloses a polytetrafluoroethylene colored film-split filament and a preparation method thereof. The PTFE colored film-cracked filament has the advantages of rich color, bright color and good color fastness. Solves the problem of difficult PTFE coloring, improves the service performance and added value of PTFE, and enlarges the application range of high-technology PTFE fiber.
Description
Technical Field
The invention belongs to the field of fiber manufacturing, and particularly relates to a polytetrafluoroethylene colored film-split filament and a preparation method thereof.
Background
Polytetrafluoroethylene (PTFE) is a polar polymer compound, is a macromolecular linear structure, has an unbranched symmetric main chain structure, has high crystallinity, and is a perfluorinated linear polymer. Due to the special molecular structure, the high-temperature-resistant and high-viscosity-resistant polypropylene composite material has high chemical stability, extremely high and low temperature resistance, good non-adhesiveness and lubricity, excellent electrical insulation, aging resistance and other excellent performances. However, the molecular structure of the dye is also characterized by being not attacked by any substances outside, and the dye molecules cannot be combined with the structure of the dye to dye the dye, which is also the weak point of PTFE. The PTFE fibres currently on the market are mainly white and brown (obtained by sintering), because PTFE has poor compatibility with other substances, the solubility parameters are very low, and PTFE cannot be dyed by conventional dyeing methods.
Disclosure of Invention
The invention aims to overcome the defects and provide the polytetrafluoroethylene colored film-cracked filament.
The invention also aims to provide a preparation method of the polytetrafluoroethylene colored split film filament. The method adopts inorganic high-temperature resistant pigment fine powder, fully mixes the inorganic high-temperature resistant pigment fine powder with PTFE dispersion resin powder according to a certain proportion, blends the mixture with a lubricant, and carries out the working procedures of compression molding, calendering and the like. In the preparation method, because the inorganic high-temperature resistant pigment fine powder is added, the process conditions of each procedure are beneficially adjusted according to the specific factor, so that the performance of the prepared colored fiber is not reduced due to the addition of the pigment, the color of the fiber is various, the color fastness can completely meet the requirements of users, and the PTFE colored film split filament plays a greater role in various fields of military industry, civil use and the like.
The purpose of the invention is realized by the following modes:
a polytetrafluoroethylene colored film-split filament is prepared from inorganic high-temperature-resistant pigment fine powder and PTFE dispersion resin serving as raw materials through fully mixing, stirring and blending by using a lubricant, prepressing, pushing, rolling to form a film, drying and degreasing, heating and stretching, heat setting and twisting, and winding to obtain a finished product.
The weight ratio of the inorganic high-temperature resistant pigment fine powder to the PTFE dispersion resin is 0.3-1.0: 100.
the inorganic high-temperature resistant pigment fine powder resists the high temperature of more than 380 ℃, has the particle size of 25-50 mu m and is subjected to desalination treatment. This is due to the size of the pigment particles, which directly affects the color fastness of the colored filaments. The desalting treatment mainly removes metal ions in the pigment fine powder.
The desalting treatment is a conventional desalting method, and aims to separate inorganic salt crystals. The PTFE dispersion resin is resin powder obtained by taking PTFE resin powder with the crystallinity of 98 percent and the average particle size of 200-300 mu m, screening the PTFE resin powder by using a filter screen with 8-20 meshes under the condition of being lower than 19 ℃, and removing agglomerated particles.
The weight ratio of the lubricant to the PTFE dispersion resin is 10-22: 100. the lubricant is not suitable for being used in too large proportion, otherwise, excessive internal gaps can be caused, the shrinkage rate of the prefabricated product is large, and the breakdown voltage is low; the ratio should not be too small, or the resistance is large when pressing, and the product is likely to crack.
Preferably the lubricant is paraffin oil, petroleum ether, white kerosene, jet fuel, most preferably jet fuel. In particular, the aviation kerosene has good lubricating property, is easy to permeate into inorganic high-temperature-resistant pigment fine powder and PTFE dispersion resin, can be completely volatilized in a drying and degreasing process, and has no residue in products.
The blending conditions of the lubricant are as follows: stirring at ambient temperature below 19 deg.C for 1-2 hr, and aging at 25-30 deg.C for 5-24 hr. The blending conditions of the aviation kerosene are preferably as follows: stirring at ambient temperature below 19 deg.C for 1-1.5 hr, and aging at 25-30 deg.C for 20-24 hr. The control of the environmental temperature and the curing temperature can prevent the phase change of PTFE and ensure the lubricant to fully and uniformly permeate.
The oil removal temperature in the drying and degreasing process is 290-310 ℃. The oil removing temperature of the invention is lower than that of the conventional PTFE filament, thus not only ensuring the full volatilization of the lubricant, but also not influencing the color brightness of the filament.
The preparation method of the polytetrafluoroethylene colored film-cracked filament specifically comprises the following steps:
(1) selection of pigment: taking inorganic high-temperature-resistant pigment fine powder which can resist the high temperature of more than 380 ℃, has the particle size of 25-50 mu m and is subjected to desalination treatment;
(2) treatment of the dispersed resin: sieving PTFE dispersion resin with the crystallinity of 98 percent and the average grain diameter of 200-300 mu m by using a filter screen with 8-20 meshes under the condition of being lower than 19 ℃ to remove agglomerated particles;
(3) mixing raw materials: fully stirring and uniformly mixing the pigment obtained by the treatment in the step (1) and the step (2) and PTFE dispersion resin, and then mixing with a lubricant;
the proportion of PTFE dispersion resin, lubricant and pigment is 100: 10-22: 0.3-1.0, mixing with lubricant at a temperature below 19 deg.C, stirring for 1-2 hr, and aging at 25-30 deg.C for 5-24 hr;
(4) pre-pressing and pushing: pouring the cured prefabricated powder into a prepressing machine for prepressing, wherein the pressure of the prepressing machine is 5.5-6 MPa, the prepressing time is 15-20 min, placing the prepressed molded product on a pushing machine for pushing, wherein the pressure of the pushing machine is 8-9 MPa, the temperature of a material cavity during pushing is 30-35 ℃, the temperature of a pushing opening die is 50-60 ℃, the ambient temperature is 20-25 ℃, the temperature of a water tank is 40-60 ℃, the compression ratio of the opening die is 130-150, the length-diameter ratio is 40-45, and the cone angle is 30-35 degrees; prepressing and pushing the mixture to prepare a cylindrical PTFE mold blank;
(5) rolling and film forming: the cylindrical PTFE film blank enters a fishtail-shaped guide plate and is made into a rolled film under the action of a rolling roller of a rolling machine; preferably, the diameter of a calendering roller is 1500mm, the width is 300mm, the speed is 1.5-12 m/min, the hot water temperature in a calendering roller is 50-80 ℃, the width of a calendered film is 16-25 cm, and the thickness is 0.25-0.45 mm;
(6) drying and degreasing: removing the lubricant from the PTFE nascent fiber; the oil removal temperature is 290 ℃ and 310 ℃, and the oil removal time is 3-6 seconds;
(7) first heating and stretching: heating and stretching the base band degreased in the step (6) in a stretching oven, stretching at the stretching temperature of 310-;
(8) slitting and heating and stretching for the second time: cutting a formed and wound strip PTFE film belt, wherein a cutting device is in a tension state, and the tension is controlled to be 80-120%; cutting by a coaxial blade cutting method, wherein the thickness of the blade is 0.12-0.25 mm, the blade is cut into 5-30 mm flat filaments, the linear speed of cutting is controlled to be 1.8-2.0 m/min, and two edge filaments on two sides of the cutting are recycled; then the cut flat filament enters an oven to be heated and stretched for the second time, the temperature is controlled at 350 ℃, the input speed is 2-6 m/min, the stretching multiple is 6-10 times, the output speed is 16-60 m/min, and the flat filament is wound after being output;
(9) heat setting and twisting: the flat filament after the second heating, stretching and winding is twisted again through heat setting, the heat setting temperature is controlled at 370 ℃ plus, the setting time is 0.5-1.2 min, the flat filament after the setting enters a twisting machine to be twisted into finished filaments, the twisting direction is S twist, the twist degree is 200 plus 1200 twist/m, and the feeding output speed is 35-40 m/min;
(10) winding a finished product: and winding the finished yarn subjected to heat setting and twisting on a winding shaft to a paper tube.
Compared with the prior art, the invention has the beneficial results that:
1. the invention solves the problem of difficult PTFE coloring, improves the service performance and added value of PTFE, and enlarges the application range of high-technology PTFE fiber.
2. The invention adopts the lubricant to carry out degreasing treatment at lower temperature, particularly preferably selects aviation kerosene as the lubricant, and the PTFE film belt can remove the lubricant completely and can keep the bright color of the product. Moreover, the aviation kerosene can be recycled, and the requirement of green production is met.
3. The inorganic high-temperature resistant pigment fine powder which is resistant to high temperature of over 380 ℃, has the particle size of 25-50 mu m and is subjected to desalination treatment is selected, so that the pigment can adapt to the process conditions of each procedure in the preparation process, the stability of the pigment in the preparation process is ensured, and the excellent performance of the product is ensured.
4. The invention uses inorganic high temperature resistant pigment fine powder as a coloring agent, combines a specific lubricating agent, and adopts a paste extrusion method to produce the polytetrafluoroethylene colored film-cracked filament by using polytetrafluoroethylene dispersed resin powder, and the obtained PTFE colored film-cracked filament has rich color, bright color and good color fastness.
Detailed Description
The present invention will be described in further detail with reference to the following examples, and it should be understood that the described examples are only a part of the examples of the present invention, and not all examples, and all other examples obtained by one of ordinary skill in the art without any inventive work based on the examples of the present invention are within the scope of the present invention.
Example 1
The preparation process of the polytetrafluoroethylene black film-cracked filament comprises the following steps:
(1) cobalt oxide black natural black pigment produced by Hunan Nuo Li New Material science and technology Limited is selected as the colored fiber colorant, and the purchased cobalt black pigment is firstly ground by adding water for 24 hr. The grinding apparatus is manufactured by Hengli grinding machines manufacturing Co., Ltd. Filtering the ground pigment with 400-mesh and 1280-mesh metal sieves, desalting (removing metal salt ions), and oven drying to obtain colorant with particle size of 25-50 μm and high temperature resistance of above 380 deg.C.
(2) DF204 polytetrafluoroethylene dispersion resin (with the crystallinity of 98 percent and the average particle size of 200-.
(3) The lubricant is aviation kerosene produced by China aviation fuel oil headquarters.
0.1 kg of the pretreated fine powder of the cobalt black pigment was poured into 20 kg of the dispersion resin and mixed, after uniform mixing, 2 kg of aviation kerosene was slowly poured into the mixture, and the mixture was stirred with a low-speed stirrer (50 rpm) at a temperature of less than 19 ℃ for 1 hr. Aging the mixed materials at room temperature (25-30 deg.C) for 20 hr.
(4) Pouring the cured prefabricated powder into a mixing material cylinder, lifting the mixture to the top of a prepress by a lifter, slowly pouring the mixture into a prepress die cavity, and completely pouring the material in the material cylinder so as to avoid color difference between batches. The pressure of the prepress is 5.5MPa, and the prepressing time is 20 min. And covering the extrusion cover on the mold cavity of the prepress, and horizontally placing the prepress on a pushing machine for pushing. The pressure of the pushing machine is 8.5MPa, the temperature of a pushing material cavity is 35 ℃, the temperature of a pushing opening die is 55 ℃, the ambient temperature is 20 ℃, the temperature of a water tank is 50 ℃, the compression ratio of the opening die is 130, the length-diameter ratio is 40, and the cone angle is 30 degrees. After prepressing and pushing, the mixture is formed into a cylindrical die blank with the diameter of 14.5 mm.
(5) The cylindrical PTFE film blank enters the fish tail-shaped guide plate, and is made into a calendered film with the thickness of 0.25 cm and the diameter of 16 cm under the action of a calendering roller with the width of 30 cm and the diameter of 150 cm on a calender. The speed of the calendering roller is 12m/min, the hot water temperature of the calendering roller is 60 ℃, and the surface temperature of the calendering roller is 70 ℃.
(6) Winding the rolled base band after rolling on a winding shaft, feeding the rolled base band into an oil removing tank after unwinding, removing the lubricant in the PTFE nascent fiber, wherein the temperature of the oil removing tank is 290 ℃, the feeding and output speed is 30m/min, and the oil removing time is 6 seconds; and (3) the deoiled and degreased base band passes through a cooling water roller to carry out flash cooling on the base band, the temperature of the base band discharged out of the box body is close to room temperature, and the deoiled calendered base band is flatly wound on the base band roller.
(7) Unreeling a base band roller, enabling the base band to enter an oven for heating and stretching, wherein the base band feeding speed is 4m/min, the oven temperature is 320 ℃, the output speed is 18m/min, the stretching ratio is 4 times, the film tape width is 4 cm, a strip PTFE film tape is stretched, cooled by a cooling water roller and then wound on a film tape shaft, and the wound film tape is thermally relaxed for 1hr in a heat preservation chamber with the room temperature of 40 ℃;
(8) unwinding a base band disc, and entering a slitting device, wherein the slitting device is in a tension state, and the tension is controlled to be 120%; the cutting adopts a coaxial blade cutting method, the base band is cut into 34 flat filaments with the width of 5mm, the linear speed of the cutting is controlled at 2.0m/min, the base band except two side filaments respectively enters an oven through a splitting device for secondary heating and stretching, the temperature of the oven is 350 ℃, the feeding speed is 2m/min, the output speed is 16m/min, the thickness of a blade is 0.15mm, the two side filaments are wound on a winding head below the cutting device, and the rest 32 flat filaments pass through a heating box and are respectively wound on a rear winding shaft after heating and stretching.
(9) And (3) thermally setting and twisting the cut and stretched flat filaments, wherein the length of a thermal setting area is 20 cm, the temperature is controlled at 370 ℃, the setting time is 1.2min, the cut and stretched flat filaments are twisted into finished filaments by a twisting machine after setting, the twisting direction is S twist, the twist degree is 450 twist/m, and the feeding output speed is 40m/min.
(10) The black polytetrafluoroethylene film-broken filament after shaping and twisting is wound on a paper tube and becomes a commercial filament after being inspected to be qualified for sale.
In parallel, 5 samples were taken for the following tests:
example 1 product PTFE Black film slit filament product Performance index test results
The above tests were carried out according to the standard GB/T35748-2017 "Poly (Central vinyl fluoride) filament".
Example 2
The preparation process of the polytetrafluoroethylene red film-cracked filament comprises the following steps:
(1) the cadmium red inorganic pigment produced by Hunan Nuo Li New Material science and technology Limited is selected as the colored fiber colorant, and the purchased cadmium red inorganic pigment is firstly ground by adding water for 24 hours. The grinding apparatus is manufactured by Hengli grinding machines manufacturing Co., Ltd. Filtering the ground pigment by a 400-mesh metal sieve and a 1280-mesh metal sieve, desalting (removing metal salt ions), and drying. The obtained colorant can resist high temperature above 380 deg.C, and has particle diameter of 25-50 μm.
(2) CGF216G type polytetrafluoroethylene dispersion resin (with the crystallinity of 98 percent and the average particle size of 200-300 mu m) produced by Zhonghao Chen photochemical research institute Co., Ltd is selected, the dispersion resin needs to be stored at the temperature below 19 ℃, and is firstly screened by a 20-mesh filter screen when being used under the condition of the temperature below 19 ℃ so as to remove agglomerated particles.
(3) The lubricant is aviation kerosene produced by Shenyang Wanfu lubricating oil Co., Ltd.
0.1 kg of the pretreated fine powder of the cadmium red pigment is poured into 20 kg of the dispersion resin to be mixed, after uniform mixing, 4 kg of aviation kerosene is slowly poured, and the mixture is stirred by a low-speed stirrer (the rpm is 50) at the temperature of below 19 ℃ for 1 hour. Mixing the raw materials at a temperature below 19 deg.C, stirring for 1.5hr, standing at room temperature (25-30 deg.C) for 20hr, and aging.
(4) Pouring the cured prefabricated powder into a mixing material cylinder, lifting the mixture to the top of a prepress by a lifter, slowly pouring the mixture into a prepress die cavity, and completely pouring the material in the material cylinder so as to avoid color difference between batches. The pressure of the prepress is 5.0MPa, and the prepressing time is 20 min. And covering the extrusion cover on the mold cavity of the prepress, and horizontally placing the prepress on a pushing machine for pushing. The pressure of the pushing machine is 8.5MPa, the temperature of a pushing material cavity is 35 ℃, the temperature of a pushing opening die is 55 ℃, the ambient temperature is 20-25 ℃, the temperature of a water tank is 50 ℃, the compression ratio of the opening die is 130, the length-diameter ratio is 40, and the cone angle is 35 degrees. After prepressing and pushing, the mixture is formed into a cylindrical die blank with the diameter of 14.5 mm.
(5) The cylindrical PTFE film blank enters the fish tail-shaped guide plate, and is made into a calendered film with the thickness of 0.4 cm and the diameter of 16 cm under the action of a calendering roller with the width of 30 cm and the diameter of 150 cm on a calender. The speed of the calendering roller is 12m/min, the hot water temperature of the calendering roller is 60 ℃, and the surface temperature of the calendering roller is 70 ℃.
(6) Winding the calendered base band after calendering on a winding shaft, feeding the calendered base band after unreeling into an oil removing box, removing a lubricant in PTFE (polytetrafluoroethylene) nascent fiber, wherein the temperature of the oil removing box is 310 ℃, the feeding and output speed is 35m/min, the oil removing time is 6 seconds, the base band after oil removing and degreasing passes through a cooling water roller, carrying out flash cooling on the base band, the temperature of the base band discharged from a box body is close to the room temperature, and the calendered base band after oil removing is smoothly wound on the base band roller.
(7) Unreeling a base band roller, enabling the base band to enter an oven for heating and stretching, wherein the base band feeding speed is 6m/min, the oven temperature is 320 ℃, the output speed is 18m/min, the stretching ratio is 5 times, the width of the film tape is 4 cm, the strip PTFE film tape is stretched, cooled by a cooling water roller and then wound on a film tape shaft, and the wound film tape is thermally relaxed for 1hr in a heat preservation chamber with the room temperature of 50 ℃;
(8) unwinding a base band disc, and entering a slitting device, wherein the slitting device is in a tension state, and the tension is controlled to be 120%; slitting adopts a coaxial blade cutting method, a base belt with the width of 8cm is cut into 34 flat filaments with the width of 5mm, the linear speed of slitting is controlled at 2.0m/min, the base belt enters an oven through a slitting device respectively for secondary heating and stretching except two side filaments, the temperature of the oven is 350 ℃, the feeding speed is 2m/min, the output speed is 16m/min, the thickness of a blade is 0.15mm, the two side filaments are wound on a winding head below the slitting device, and the rest 32 flat filaments pass through a heating box and are wound on a rear winding shaft respectively after being heated and stretched.
(9) And (3) thermally setting and twisting the cut and stretched flat filaments, wherein the length of a thermal setting area is 20 cm, the temperature is controlled at 340 ℃, the setting time is 1.2min, the cut and stretched flat filaments are twisted into finished filaments by a twisting machine after setting, the twisting direction is S twisting, the twisting degree is 450 twisting, and the feeding output speed is 40m/min.
(10) The red PTFE film-broken filament after shaping and twisting is wound on a paper tube and becomes a commercial filament after being inspected to be qualified.
In parallel, 5 samples were taken for the following tests:
example 2 product PTFE Red film cracked filament product Performance index test results
The above tests were carried out according to the standard GB/T35748-2017 "Poly (Central vinyl fluoride) filament".
Example 3
The preparation process of the polytetrafluoroethylene blue film-cracked filament comprises the following steps:
(1) cobalt blue natural blue pigment produced by Hunan Nuoli New Material science and technology Limited is selected as the colored fiber colorant, and the purchased cobalt black pigment is ground by adding water for 24 hr. The grinding apparatus is manufactured by Hengli grinding machines manufacturing Co., Ltd. Filtering the ground pigment by a 400-mesh metal sieve and a 1280-mesh metal sieve, desalting (removing metal salt ions), and drying. The obtained colorant can resist high temperature above 380 deg.C, and has particle diameter of 25-50 μm.
(2) F104 type polytetrafluoroethylene dispersion resin (with the crystallinity of 98 percent and the average particle size of 200-.
(3) The lubricant is aviation kerosene produced by China aviation fuel oil headquarters.
0.1 kg of the pretreated fine powder of the cobalt blue pigment was poured into 20 kg of the dispersion resin and mixed, after uniform mixing, 3 kg of aviation kerosene was slowly poured into the mixture, and the mixture was stirred with a low-speed stirrer (50 rpm) at a temperature of less than 19 ℃ for 1 hr. Mixing the raw materials at a temperature below 19 deg.C, stirring for 2hr, standing at room temperature (25-30 deg.C) for 20hr, and aging.
(4) Pouring the cured prefabricated powder into a mixing material cylinder, lifting the mixture to the top of a prepress by a lifter, slowly pouring the mixture into a prepress die cavity, and completely pouring the material in the material cylinder so as to avoid color difference between batches. The pressure of the prepress is 5.5MPa, and the prepressing time is 20 min. And covering the extrusion cover on the mold cavity of the prepress, and horizontally placing the prepress on a pushing machine for pushing. The pressure of the pushing machine is 8.5MPa, the temperature of a pushing material cavity is 35 ℃, the temperature of a pushing opening die is 55 ℃, the ambient temperature is 20-25 ℃, the temperature of a water tank is 50 ℃, the compression ratio of the opening die is 130, the length-diameter ratio is 40, and the cone angle is 35 degrees. After prepressing and pushing, the mixture is formed into a cylindrical die blank with the diameter of 14.5 mm.
(5) The cylindrical PTFE film blank enters the fish tail-shaped guide plate, and is made into a calendered film with the thickness of 0.25 cm and the diameter of 16 cm under the action of a calendering roller with the width of 30 cm and the diameter of 150 cm on a calender. The speed of the calendering roller is 12m/min, the hot water temperature of the calendering roller is 60 ℃, and the surface temperature of the calendering roller is 70 ℃.
(6) Winding the calendered base band after calendering on a winding shaft, unreeling, then feeding into an oil removal tank, wherein the temperature of the oil removal tank is 310 ℃, the feeding and output speed is 30m/min, the oil removal time is 6 seconds, the base band after oil removal and degreasing passes through a cooling water roller, carrying out flash cooling on the base band, the temperature of the base band discharged from a box body is close to the room temperature, and the calendered base band after oil removal is flatly wound on the base band roller.
(7) Unreeling a base band roller, enabling the base band to enter an oven for heating and stretching, wherein the base band feeding speed is 4m/min, the oven temperature is 320 ℃, the output speed is 18m/min, the stretching ratio is 4 times, the width of the film tape is 4 cm, the strip PTFE film tape is stretched, cooled by a cooling water roller and then wound on a film tape shaft, and the wound film tape is thermally relaxed for 1hr in a heat preservation chamber with the room temperature of 40 ℃;
(8) unwinding a base band disc, and entering a slitting device, wherein the slitting device is in a tension state, and the tension is controlled to be 120%; slitting adopts a coaxial blade cutting method, a base belt with the width of 8cm is cut into 34 flat filaments with the width of 5mm, the linear speed of slitting is controlled at 1.8m/min, the base belt enters an oven through a slitting device respectively for secondary heating and stretching, the temperature of the oven is 330 ℃, the feeding speed is 2m/min, the output speed is 16m/min, the thickness of a blade is 0.15mm, two side filaments are wound on a winding head below the slitting device, and the rest 32 flat filaments pass through a heating box and are wound on a rear winding shaft respectively after being heated and stretched.
(9) And (3) thermally setting and twisting the cut and stretched flat filaments, wherein the length of a thermal setting area is 20 cm, the temperature is controlled at 340 ℃, the setting time is 1.2min, the cut and stretched flat filaments enter a twisting machine after being set, twisting finished filaments are twisted, the twisting direction is S twisting, the twisting degree is 450 twisting/m, and the feeding output speed is 40m/min.
(10) The blue polytetrafluoroethylene film-broken filaments after shaping and twisting are wound on a paper tube and become commercial filaments after being inspected to be qualified for sale.
In parallel, 5 samples were taken for the following tests:
example 3 product PTFE blue film slit filament product Performance index test results
The above tests were carried out according to the standard GB/T35748-2017 "Poly (Central vinyl fluoride) filament".
Claims (3)
1. A preparation method of polytetrafluoroethylene colored film-split filaments is characterized by comprising the following steps:
(1) selection of pigment: taking inorganic high-temperature resistant pigment fine powder which resists high temperature of more than 380 ℃, has particle size of 25-50 mu m and is subjected to desalination treatment;
(2) treatment of the dispersed resin: sieving PTFE dispersion resin with the crystallinity of 98 percent and the average grain diameter of 200-300 mu m by using a filter screen with 8-20 meshes under the condition of being lower than 19 ℃ to remove agglomerated particles;
(3) mixing raw materials: fully stirring and uniformly mixing the pigment obtained by the treatment in the step (1) and the step (2) and PTFE dispersion resin, and then mixing with a lubricant;
the weight ratio of the PTFE dispersion resin to the lubricant to the pigment is 100: 10-22: 0.3-1.0, mixing with lubricant at a temperature below 19 deg.C, stirring for 1-2 hr, and aging at 25-30 deg.C for 5-24 hr;
(4) pre-pressing and pushing: pouring the cured prefabricated powder into a prepressing machine for prepressing, wherein the pressure of the prepressing machine is 5.5-6 MPa, the prepressing time is 15-20 min, placing the prepressed molded product on a pushing machine for pushing, the pressure of the pushing machine is 8-9 MPa, the material cavity temperature during pushing is 30-35 ℃, the pushing die temperature is 50-60 ℃, the ambient temperature is 20-25 ℃, the water tank temperature is 40-60 ℃, the die compression ratio is 130-150, the length-diameter ratio is 40-45, and the cone angle is 30-35°(ii) a Prepressing and pushing the mixture to prepare a cylindrical PTFE film blank;
(5) rolling and film forming: the cylindrical PTFE film blank enters a fishtail-shaped guide plate and is made into a rolled film under the action of a rolling roller of a rolling machine;
(6) drying and degreasing: removing the lubricant from the calendered film; the oil removal temperature is 290 ℃ and 310 ℃, and the oil removal time is 3-6 seconds;
(7) first heating and stretching: the rolled film degreased in the step (6) is put into a stretching oven for heating and stretching, the stretched film is stretched at the stretching temperature of 310-;
(8) slitting and heating and stretching for the second time: cutting the strip PTFE film belt, wherein the cutting device is in a tension state, and the tension is controlled to be 80-120%; cutting by a coaxial blade cutting method, wherein the thickness of the blade is 0.12-0.25 mm, the blade is cut into flat filaments with the thickness of 5-30 mm, the linear speed of cutting is controlled to be 1.8-2.0 m/min, and two flat filaments on two sides of the cutting are recycled; then the cut flat filament enters an oven to be heated and stretched for the second time, the temperature is controlled at 350 ℃, the input speed is 2-6 m/min, the stretching multiple is 6-10 times, the output speed is 16-60 m/min, and the flat filament is wound after being output;
(9) heat setting and twisting: the flat filament after the second heating, stretching and winding is twisted again through heat setting, the heat setting temperature is controlled at 370 ℃ plus, the setting time is 0.5-1.2 min, the flat filament after the setting enters a twisting machine to be twisted into finished filaments, the twisting direction is S twist, the twist degree is 200 plus 1200 twist/m, and the feeding output speed is 35-40 m/min;
winding a finished product: the finished yarn after heat setting and twisting is wound on a paper tube through a winding shaft.
2. The process for preparing a colored polytetrafluoroethylene film-split filament according to claim 1, wherein the lubricant is jet fuel.
3. The colored polytetrafluoroethylene split filament produced by the process for producing a colored polytetrafluoroethylene split filament according to any one of claims 1 to 2.
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