CN119615389A - Preparation method of ultra-high molecular weight polyethylene coarse denier fiber - Google Patents
Preparation method of ultra-high molecular weight polyethylene coarse denier fiber Download PDFInfo
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- CN119615389A CN119615389A CN202311172414.8A CN202311172414A CN119615389A CN 119615389 A CN119615389 A CN 119615389A CN 202311172414 A CN202311172414 A CN 202311172414A CN 119615389 A CN119615389 A CN 119615389A
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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
- D01D5/06—Wet spinning methods
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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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
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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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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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
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
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- 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
- D10B2321/02—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polyolefins
- D10B2321/021—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polyolefins polyethylene
- D10B2321/0211—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polyolefins polyethylene high-strength or high-molecular-weight polyethylene, e.g. ultra-high molecular weight polyethylene [UHMWPE]
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Abstract
The invention relates to the field of high polymer material preparation, in particular to a preparation method of ultra-high molecular weight polyethylene heavy denier fiber, and discloses a preparation method of ultra-high molecular weight polyethylene heavy denier fiber. Through the two cooling and preheating processes, the sheath-core structure of the fiber is firstly formed and eliminated, so that the solvent in the gel yarn is continuously separated out along with the preparation process, the conditions of yarn breakage and yarn breakage caused by the sheath-core structure of the gel yarn in the preparation process are avoided, the solid gel yarn with the sheath-core structure basically eliminated is obtained after the two cooling processes, the solid gel yarn is softened and melted by preheating, the stretchable gel yarn is prepared, and finally the ultra-high molecular weight polyethylene heavy denier fiber with large single filament number and good mechanical property is prepared.
Description
Technical Field
The invention relates to the field of preparation of high polymer materials, in particular to a preparation method of ultra-high molecular weight polyethylene heavy denier fiber.
Background
Since the advent of gel spinning technology, ultra-high molecular weight polyethylene fiber production technology has been developed in rapid progress, and currently, the main polyethylene fiber production technology in the world mainly comprises dry spinning and wet spinning.
The domestic wet process technology is relatively mature, and is popularized and applied to tens of enterprises in China, and the produced fiber has the characteristics of coarse fineness, good uniformity, high strength and high modulus, and is suitable for downstream enterprises. The dry method technology only realizes industrialization of chemical fiber at present, has the characteristics of fine denier, softness, good uniformity, high strength and high modulus, and is widely applied to downstream enterprises.
In terms of the current domestic development trend of technology and products, the wet product has relatively more solvent residues than the dry product, the fineness of the wet product is relatively larger, the fiber is harder, the fiber is not easy to fluff in the downstream processing process, the fiber is easy to process, and the fiber can be widely applied to the fields of military industry and civil use, but in the fields with higher requirements on solvent residues, such as medical equipment, the fiber needs further deep processing, and the solvent residues are removed. Therefore, the wet process technology is developed in the direction of fine denier in recent years, on one hand, the application field is expanded, and on the other hand, the improvement and enhancement are needed. The dry method technology adopts volatile solvents, so the residual quantity of the solvents in the product is relatively low, the fineness of the product is thin, the weight is light, and the dry method technology has the characteristics of high strength and high modulus, and can be widely applied to military industry and civil facilities. The fiber is soft, has high comfort, is easy to fuzz in the downstream processing process due to fine fineness, and is difficult to process. In recent years, dry technology has therefore been developed in the direction of coarse denier, mainly to improve its downstream workability.
CN112609250A discloses a method for preparing ultra-high molecular weight polyethylene heavy denier fiber monofilaments by a gel method, which comprises the steps of mixing ultra-high molecular weight polyethylene powder with white oil, preparing a spinning stock solution pre-swelling material, keeping a stirring state and heating, feeding the pre-swelling material into a double-screw extruder, feeding the pre-swelling material into a spinning component to form filaments through a spinneret plate, cooling the filaments by a cooling water tank to obtain ultra-high molecular weight gel filaments, standing for balancing, arranging the filaments in a cross lamination circular ring mode when the filaments fall into a barrel after the filaments are formed, extracting, drying and thermally stretching the gel filaments after balancing treatment, and finally winding to obtain the ultra-high molecular weight polyethylene heavy denier fiber monofilaments. The preparation method disclosed by the invention realizes 10 times of increase of single filament number under the condition of no decrease of strength, achieves 20-40 denier and has the diameter of 0.038-0.070 mm, and the method of combining the original multiple fine denier monofilaments into filaments is replaced by the coarse denier monofilaments, so that gaps among the fine denier monofilaments are effectively eliminated, and excellent strength and modulus are maintained. The method adopts wet technology, the diameter of a single hole of a spinneret plate is 1.5-2mm, a quenching forming mode is adopted, then the spinneret plate stands for a period of time, the internal stress of a precursor is eliminated, and high-power stretching is carried out.
CN101575745A discloses a thick and polyester fiber and a method for producing the same. The denier per filament of the fiber ranges from 7 to 20dtex, and the macro denier polyethylene fiber does not include polyester fibers having a total number of filaments of one. The production method comprises the steps of carrying out melt extrusion on the dried polyester chips, carrying out extrusion shaping by a round or special-shaped spinneret plate, carrying out side blowing air cooling solidification, carrying out oil feeding and interlacing treatment, and finally carrying out coiling molding by a coiling device to directly obtain the finished product of high-orientation polyester Fiber (FDY), or obtaining the semi-finished product of pre-orientation polyester fiber (POY), and carrying out high-order processing on the semi-finished product of pre-orientation polyester fiber (POY) to obtain the finished product. In addition, the production method of the product is simple, has strong operability and can meet the requirement of further processing.
CN101899722a discloses a method for preparing high-strength high-modulus coarse denier polyvinyl alcohol monofilament fiber by solid-phase alcoholysis spinning method, which is characterized in that polyvinyl alcohol with low alcoholysis degree is used for spinning under plasticization of a small amount of water, and coarse denier fiber is prepared at lower temperature, so that the problems that the plasticizer is used for extraction and the wet spinning method can not produce coarse denier (more than or equal to 1000D) fiber are avoided, a small amount of water is added to be in a molten state, the single screw is used for extrusion, metering is carried out by a metering pump, then extrusion is carried out by a spinneret, a small amount of water is removed by heating, the fiber is dried and stretched in multiple stages (10-16 times), and high-temperature tension heat setting is carried out, thus obtaining fiber with high strength and modulus, overcoming the defects of the prior art and products sold in market, and meeting the requirements of civil engineering for toughening, cracking resistance and the like of concrete. The method adopts a container which is easy to be used for swelling polyethylene, then is conveyed into one of two containers which are alternately used for stirring, is output through an output port at the bottom of the container, and has concentration gradient in the container and sedimentation at the bottom, so that suspension cannot be output uniformly and continuously, and uniformity of products in subsequent procedures cannot be ensured.
CN102154749A discloses a preparation method of coarse and ultra-high molecular weight polyethylene fiber yarn, which comprises the steps of spraying polyethylene solution through a spinneret plate, then entering into a coagulating bath of 100-150 ℃ for quenching to obtain gel fiber, wherein the spinneret plate comprises 20-50 groups of spinneret holes, each group of spinneret holes consists of 15-35 spinneret holes with the diameter of 0.7-1.0mm, and then extracting, drying and subsequently hot stretching the gel fiber. The invention has simple operation and low requirement on equipment, the single fiber diameter of the prepared coarse and ultra-high molecular weight polyethylene fiber yarn is 0.7-1.0mm, and the fiber yarn has high strength and is suitable for manufacturing high-strength ropes.
The dry process technology can realize high-speed stretching in the processing process due to the characteristic of volatile solvent, so that the fineness of the fiber is relatively thin, the single filament fineness of the current domestic dry spinning product is basically 0.8-1.3dtex, and the current dry spinning technology needs to be subjected to large-scale process adjustment in order to obtain the product with higher single filament fineness.
Disclosure of Invention
The invention aims to solve the problem of excessively fine denier of ultra-high molecular weight polyethylene fibers prepared by dry spinning, and provides a preparation method of ultra-high molecular weight polyethylene heavy denier fibers, which can firstly generate and then eliminate a sheath-core structure of the fibers by twice cooling and then preheating, so that the conditions of yarn breakage and yarn breakage in the preparation process are avoided, and finally the ultra-high molecular weight polyethylene heavy denier fibers with large denier per filament and good mechanical properties are prepared.
In order to achieve the above purpose, the first aspect of the invention provides a preparation method of an ultra-high molecular weight polyethylene heavy denier fiber, wherein a spinning solution is extruded by equipment to obtain gel filaments, the gel filaments are cooled twice, and then preheated, drawn, oiled and wound to obtain a precursor, and the precursor is subjected to multistage drawing to obtain the ultra-high molecular weight polyethylene heavy denier fiber.
In a second aspect, the present invention provides an ultra high molecular weight polyethylene macrodenier fiber produced by the process described above.
Through the technical scheme, the invention has the following beneficial effects:
(1) According to the invention, through specific procedures, particularly the two-time cooling and preheating processes, the skin-core structure of the fiber is firstly generated and then eliminated, so that the solvent in the gel silk is continuously separated out along with the preparation process, and the conditions of silk breakage and silk breakage in the process caused by the skin-core structure of the gel silk in the preparation process are avoided;
The method comprises the steps of cooling for quenching and rapid forming to form gel yarn with a sheath-core structure with solidified outside and soft inside, cooling for high-speed cold air and deep cooling to solidify and form the gel yarn and accelerate the precipitation of a large amount of solvent in the gel yarn, cooling for two times to obtain solid gel yarn with the sheath-core structure basically eliminated, and preheating and softening to soften the solid gel yarn to enable the solvent to volatilize more fully and improve the spinnability of the gel yarn.
(2) After the solvent is separated out, the solvent can be returned to the module for reuse, so that the recycling of the solvent is realized.
(3) The ultra-high molecular weight polyethylene coarse denier fiber prepared finally has large single filament number and good mechanical property.
Drawings
FIG. 1 is a schematic diagram of one embodiment of a fiber spinning system of the present invention.
Description of the reference numerals
1. Metering pump 2, coagulation bath 3, cold drawing machine 4, yarn guiding drying cold box 5, cold drawing machine 6, yarn guiding machine 7, preheating channel 8, yarn guiding machine 9, preheating drying drawing box 10, cold drawing machine 11, drawing hot box 12, cold drawing machine 13, oiling machine 14, winding machine
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a preparation method of ultra-high molecular weight polyethylene heavy denier fiber, which comprises the steps of extruding spinning solution through equipment to obtain gel yarn, cooling the gel yarn twice, preheating, drafting, oiling and winding to obtain precursor yarn, and carrying out multistage stretching on the precursor yarn to obtain the ultra-high molecular weight polyethylene heavy denier fiber.
According to the invention, through specific procedures, particularly the two-time cooling and preheating processes, the skin-core structure of the fiber is firstly eliminated, so that the solvent in the gel silk is continuously separated out along with the preparation process, the condition of broken silk and broken silk in the process caused by the skin-core structure of the gel silk is avoided, the solid gel silk with the skin-core structure basically eliminated is obtained after the two-time cooling, and the solid gel silk is softened and melted by preheating, so that the stretchable gel silk is prepared.
According to the invention, the spinning solution comprises ultra-high molecular weight polyethylene and a solvent.
According to the invention, the content of the ultra-high molecular weight polyethylene is 5-10wt% and the content of the solvent is 90-95wt%, based on the total mass of the spinning solution.
In the invention, when the content of the ultra-high molecular weight polyethylene and the solvent meets the above range, broken filaments and broken filaments are not easy to occur in the processing process, the performance of the finally prepared heavy denier fiber is further improved, and the balance between the single filament number and the processing difficulty can be realized.
Further, the content of the ultra-high molecular weight polyethylene is 6-7wt% and the content of the solvent is 93-94wt% based on the total mass of the spinning solution.
In a particularly preferred embodiment of the present invention, the ultra-high molecular weight polyethylene has a swelling temperature of 95-100 ℃, preferably 96-98 ℃.
According to the invention, the ultra-high molecular weight polyethylene has a viscosity average molecular weight of 100-1000 ten thousand g/mol.
In the invention, when the viscosity average molecular weight of the ultra-high molecular weight polyethylene meets the above range, the branching degree is low, the fluidity is good, and the breakage is not easy to occur in the processing process.
Further, the viscosity average molecular weight of the ultra-high molecular weight polyethylene is 400 ten thousand-500 ten thousand g/mol.
According to the invention, the solvent is selected from compounds containing benzene rings.
According to the invention, the solvent has a boiling point of 180-200 ℃, preferably 185-195 ℃.
According to the present invention, the solvent is at least one selected from decalin, tetrahydronaphthalene and toluene, preferably decalin.
In the present invention, the decalin is a decalin commonly used in the art, and in a particularly preferred embodiment, the decalin is a trans decalin, and is an isomer of decalin.
According to the invention, the apparatus comprises a twin-screw extruder, a metering pump, a spinning beam and a spinneret.
According to the invention, the extrusion process comprises the steps that the spinning solution is changed into a molten melt through the double-screw extruder, accurately metered through the metering pump, flows through the spinning box body and finally is extruded from the spinneret plate.
According to the invention, the melt temperature is 140-150 ℃.
In the invention, when the gel yarn meets the temperature in the range, more solvent is flashed off at the moment of leaving the spinneret plate, so that the solvent content in the gel yarn is lower.
Further, the melt temperature is 145-148 ℃.
In the present invention, the temperature of the spinning beam is not limited, and in a particularly preferred embodiment, the spinning beam is 160 to 200 ℃, preferably 170 to 190 ℃.
According to the invention, the single hole diameter of the spinneret plate is 0.5-2mm, preferably 1.2-1.5mm.
According to the invention, the aspect ratio of the spinneret plate is 4-10:1, preferably 6-8:1.
According to the invention, the spinneret plate is provided with the spray head, and the stretching multiplying power of the spray head is 5-20 times.
According to the invention, when the stretching multiplying power in the range is satisfied, the content of the solvent in the gel yarn can be controlled to be kept in a proper range, when the stretching multiplying power of the spray head is smaller than the range, more solvent exists in the gel yarn, and when the stretching multiplying power of the spray head is larger than the range, the phenomena of yarn breakage and yarn breakage are easy to occur, so that the performance of the final fiber is affected.
Further, the stretching multiplying power of the spray head is 10-15 times.
According to the invention, the extrusion rate is 2.5-5m/min, preferably 3-3.5m/min.
In the present invention, the component pressure in the spinneret is a pressure common in the art, and in a particularly preferred embodiment, the component pressure in the spinneret is 0 to 1.8MPa, preferably 0.5 to 1MPa.
According to the invention, the twice cooling comprises a first cooling and a second cooling, wherein the first cooling is solution cooling, and the second cooling is cold air cooling.
According to the invention, the cooling of the solution is carried out in a coagulation bath, the temperature of the gel filaments as they are drawn out of the coagulation bath being 40 ℃ or less, preferably 20 ℃ or less.
In the invention, the solution is cooled to be rapidly formed by quenching, the gel filaments pulled out of the coagulation bath are in an unstable state with solidified surfaces and soft interiors, and are close to a skin-core structure, and the solvent is continuously precipitated on the surfaces of the gel filaments along with the cooling of the surfaces of the gel filaments.
In the present invention, the quenching solution in the coagulation bath is a conventional solution incompatible with the spinning aid, preferably selected from water, a solvent included in the spinning solution, and a solution insoluble in the solvent, so as to facilitate the subsequent recovery and utilization of the solvent.
According to the invention, the cold air cooling is performed in a guide wire cold drawing machine, a guide wire drying cold box and a cold drawing machine, and an air knife is arranged in the guide wire drying cold box.
According to the invention, the high-speed air flow generated by the cold air cooling air knife is used for deep cooling the gel silk and drying the solvent separated out from the surface of the gel silk, so that the solvent content in the gel silk is greatly reduced, the skin-core structure is basically eliminated, and the solid gel silk is obtained.
According to the invention, the air outlet temperature of the air knife is-10 ℃ to 10 ℃.
According to the application, the air outlet temperature of the specific air knife can enable the yarn to be rapidly and deeply solidified to form stable gel yarn, and a large amount of solvent in the gel yarn is accelerated to be precipitated.
Further, the air outlet temperature of the air knife is-5 ℃ to 0 ℃.
According to the invention, the outlet wind speed of the air knife is 50-100m/s.
According to the application, the outlet wind speed of the specific air knife can remove the quenching solvent brought out of the coagulating bath from the surface of the fiber, and meanwhile, the solvent separated out of the gel silk due to cold shrinkage can be dried.
Further, the outlet wind speed of the air knife is 70-75m/s.
According to the invention, the draft ratio of the cold draft machine is 0.8-1.2 times.
In the invention, the gel yarn can shrink in the aspect of long diameter after being subjected to cryogenic treatment, and the specific drawing multiplying power of the cold drawing machine can prevent yarn breakage and yarn breakage in the production process.
Further, the draft ratio of the cold draft machine is 0.9-1 times.
According to the invention, the preheating is carried out in a preheating shaft, the temperature of the preheating being 40-100 ℃.
In the invention, the solidified gel yarn can be preheated and softened by the preheating, so that the subsequent solvent volatilization and directional stretching are facilitated, and the spinnability of the gel yarn is improved.
Further, the preheating temperature is 70-80 ℃.
According to the invention, the drafting is carried out in a preheating drying drafting box and a drafting hot box, wherein the drafting machine in the preheating drying drafting box is a hot drafting machine provided with a hot drafting roller.
According to the invention, the temperature of the preheating drying drafting oven is 60-150 ℃, preferably 100-140 ℃.
In the invention, the hot drawing roller is positioned in the preheating drying drawing box, and the temperature of the hot drawing roller are the same in the later stage.
According to the invention, the draft ratio of the hot draft machine is 1 to 1.5 times, preferably 1 to 1.2 times.
According to the invention, the temperature of the drawing hot box is 100-140 ℃, preferably 120-130 ℃.
According to the invention, the draft ratio of the draft hot box is 1-2 times, preferably 1.2-1.5 times.
According to the invention, the multi-stage stretching comprises primary stretching, secondary stretching and tertiary stretching, and the total stretching multiplying power of the multi-stage stretching is 7-10 times.
According to the invention, the primary stretching has a magnification of 3-6 times, preferably 4-5 times, and the primary stretching has a temperature of 138-142 ℃, preferably 140-142 ℃.
According to the invention, the secondary stretching has a magnification of 1.2-1.6 times, preferably 1.3-1.5 times, and the secondary stretching has a temperature of 142-145 ℃, preferably 143-144 ℃.
According to the invention, the three-stage stretching magnification is 1-1.4 times, preferably 1.05-1.2 times, and the temperature of the three-stage stretching is 144-148 ℃, preferably 145-148 ℃.
In a second aspect, the present invention provides an ultra high molecular weight polyethylene macrodenier fiber produced by the process described above.
According to the invention, the solvent content of the ultra-high molecular weight polyethylene heavy denier fiber is 900-14500ppm, the single filament fineness is 1-51dtex, the breaking strength is more than or equal to 30cN/dtex, and the Young modulus is more than or equal to 1200cN/dtex.
In the present invention, the solvent content increases the linear density of the fiber, thereby increasing the weight per unit length of the fiber. The solvent in the later-stage fiber can be volatilized slowly, so that the linear density of the fiber is reduced, the coarse denier fiber with large single filament number is easily obtained by the solvent content, but the solvent content is only one of the influencing factors of the single filament number.
Further, the solvent content of the ultra-high molecular weight polyethylene heavy denier fiber is 3000-10000ppm, the single filament fineness is 1.5-3.8dtex, the breaking strength is more than or equal to 35cN/dtex, and the Young modulus is more than or equal to 1300cN/dtex.
Fig. 1 is a schematic structure diagram of a fiber spinning system, a metering pump 1 is used for metering a polyethylene spinning solution, the metering pump is used for extruding the polyethylene spinning solution through a specific spinneret plate, the extruded gel yarn enters a coagulation bath 2 for rapid cooling, the cooled gel yarn is cooled twice in a yarn guide cold drawing machine 3, a yarn guide drying cold box 4 and a cold drawing machine 5, the cooled gel yarn flows through a yarn guide machine 6 and enters a preheating channel 7 for preheating and heating, flows through a yarn guide machine 8 and enters a preheating drying drawing box 9, flows through a cold drawing machine 10 and enters a drawing hot box 11 for drawing and the refined stripping of a solvent, the refined stripped gel yarn flows through a cold drawing machine 12 and enters an oiling machine 13 for oiling, and is coiled in a coiling machine 14 to obtain a precursor, and the prepared precursor is subjected to multistage drawing to finally prepare the ultra-high molecular weight polyethylene coarse denier fiber.
The present invention will be described in detail by examples.
The diameter detection method of gel silk adopts Cai Kang microscope CKC2000, ocular 10 times and granularity analysis software DL-3000. Gel yarn samples are taken from the outlet of the spray head, the outlet of the coagulating bath, the outlet of the guide yarn drying cold box, the outlet of the preheating channel, the outlet of the preheating drying drafting box, the outlet of the drafting hot box, the outlet of the winding part and the outlet of the winding part of the finished fiber, and the diameter of the monofilament is measured under the 250 times of visual field.
The method for detecting the mass ratio of the ultra-high molecular weight polyethylene to the solvent in the gel silk comprises the steps of taking 100g of a bundle silk gel silk sample from a spray nozzle outlet, a coagulating bath outlet, a silk guide drying cold box outlet, a preheating channel outlet, a preheating drying drafting box outlet, a drafting hot box outlet, a winding outlet and a finished fiber winding outlet, drying for 3 hours under the vacuum condition of 140 ℃ (the temperature is higher than the glass transition point of the polyethylene, the polyethylene is molten, the internal solvent is not easy to volatilize, the measurement result is distorted), cooling to normal temperature after taking out, weighing, marking as m 1, the solvent content is 100-m 1, calculating according to the following formula,
Solvent:
The method for detecting the single filament number of the gel yarn and the ultra-high molecular weight polyethylene heavy denier fiber comprises the steps of testing by using GB/T/19975-2005, measuring the linear density of the bundle yarn, and calculating the single filament number, wherein the single filament number=the number of the single filament number and the number of holes of a spinneret plate of the bundle yarn fiber obtained by testing.
The method for detecting the solvent content adopts the method for detecting the mass ratio of the ultra-high molecular weight polyethylene in the gel silk to the solvent, and the average value is obtained by measuring three times.
The method for detecting breaking strength and Young's modulus of the ultra-high molecular weight polyethylene heavy denier fiber comprises the step of detecting by using a GB/T19975-2005 method.
Ultra-high molecular weight polyethylene (average particle size 250 μm, viscosity average molecular weight 425 ten thousand g/mol) was purchased from Shanghai-Bile Corp;
the solvent is decalin (> 98% industrial grade with cis-trans ratio of 2:8) and is purchased from medium energy chemical company;
deionized water and nitrogen were purchased from the southern company external network.
Example 1
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching ratio of a nozzle is 5 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath is 10 ℃, the air outlet temperature of the air knife is-10 ℃, the air outlet speed of the air knife is 50m/s, the draft ratio of the cold draft machine is 0.8 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 130 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 1.
TABLE 1
Example 2
The spinneret plate adopts a length-diameter ratio of 6:1, the number of holes is 70 holes, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt percent based on the total mass of the spinning solution, the content of the solvent is 94wt percent, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching multiplying power of a nozzle is 20 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath tank is 20 ℃, the air outlet temperature of the air knife is 10 ℃, the air outlet speed of the air knife is 80m/s, the draft ratio of the cold draft machine is 1 time, the preheating is carried out in a preheating channel, the preheating temperature is 70 ℃, the temperature of a preheating drying draft box is 60 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 120 ℃, and the draft ratio of the draft hot box is 1.6 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 5 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.6 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.2 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 2.
TABLE 2
Example 3
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.2mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching multiplying power of a nozzle is 8 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath tank is 10 ℃, the air outlet temperature of the air knife is 0 ℃, the air outlet speed of the air knife is 60m/s, the draft ratio of the cold draft machine is 0.9 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 80 ℃, the temperature of a preheating drying draft box is 120 ℃, the draft ratio of the hot draft machine is 1.2 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.5 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4.5 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.1 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 3.
TABLE 3 Table 3
Example 4
The length-diameter ratio of the spinneret plate is 3:1, the number of holes is 70, the diameter of a single hole is 2mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the solvent content is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.23MPa, the stretching multiplying power of a spray head is 5 times, and the extrusion rate of the spray head is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath tank is 10 ℃, the air outlet temperature of the air knife is-10 ℃, the air outlet speed of the air knife is 70m/s, the draft ratio of the cold draft machine is 0.8 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 135 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.4 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 4.
TABLE 4 Table 4
Example 5
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching ratio of a nozzle is 5 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath tank is 30 ℃, the air outlet speed of an air knife is 50m/s, the air outlet temperature of the air knife is-10 ℃, the draft ratio of a cold draft machine is 0.8 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 130 ℃, the draft ratio of a hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 5.
TABLE 5
Example 6
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching ratio of a nozzle is 5 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath tank is 10 ℃, the air outlet temperature of the air knife is-10 ℃, the air outlet speed of the air knife is 120m/s, the draft ratio of the cold draft machine is 0.8 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 130 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 6.
TABLE 6
Example 7
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching multiplying power of a nozzle is 10 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath is 10 ℃, the air outlet temperature of the air knife is-10 ℃, the air outlet speed of the air knife is 50m/s, the draft ratio of the cold draft machine is 0.8 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 130 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 7.
TABLE 7
Example 8
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 140 ℃, the assembly pressure is 1.25MPa, the stretching multiplying power of a nozzle is 10 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath is 10 ℃, the air outlet temperature of the air knife is-10 ℃, the air outlet speed of the air knife is 50m/s, the draft ratio of the cold draft machine is 0.8 times, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 130 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The analysis and detection results of the gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 8.
TABLE 8
Comparative example 1
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching ratio of a nozzle is 5 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel filaments when the gel filaments are pulled out of the gel bath tank is 10 ℃, the gel filaments are preheated in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying drafting box is 130 ℃, the drafting multiplying power of a hot drafting machine is 1.1 times, the temperature of a drafting hot box is 140 ℃, and the drafting multiplying power of the drafting hot box is 1.2 times, so that the filaments are obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The results of analysis and detection of gel silk/precursor silk/ultra-high molecular weight polyethylene heavy denier fiber are shown in table 9.
TABLE 9
The fiber is wound in the channel preheating box, and the solvent on the surface of the fiber is brought to the drawing roller, so that the occasional broken filament of the filament bundle is wound on the drawing roller due to the surface tension of the solvent on the drawing roller, thereby causing the conditions of winding and broken filament. Meanwhile, the secondary cooling is not performed, the residual quantity of the solvent in the fiber is greatly increased, the application requirement of the fiber cannot be met, and the recovery rate of the solvent is reduced.
Comparative example 2
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching ratio of a nozzle is 5 times, and the extrusion rate of the nozzle is 3.25m/min.
The air outlet speed of the air knife is 50m/s, the air outlet temperature of the air knife is-10 ℃, the draft ratio of the cold draft machine is 0.8 times, the preheating is carried out in a preheating channel, the preheating temperature is 100 ℃, the temperature of a preheating drying draft box is 130 ℃, the draft ratio of the hot draft machine is 1.1 times, the temperature of a draft hot box is 140 ℃, and the draft ratio of the draft hot box is 1.2 times, so that the filament is obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The gel yarn cannot be normally produced, the tension of the gel yarn is extremely low under the high temperature condition, and the gel yarn is directly broken under the influence of the high-speed wind direction of an air knife, so that the stretching condition cannot be maintained.
Comparative example 3
The length-diameter ratio of the spinneret plate is 6:1, the number of holes is 70, the diameter of a single hole is 1.5mm, the content of the ultra-high molecular weight polyethylene is 6wt% based on the total mass of the spinning solution, the content of the solvent is 94wt%, the swelling temperature of the ultra-high molecular weight is 98 ℃, the melt temperature is 145 ℃, the assembly pressure is 1.25MPa, the stretching ratio of a nozzle is 5 times, and the extrusion rate of the nozzle is 3.25m/min.
The temperature of the gel silk when the gel silk is pulled out of the gel bath tank is 10 ℃, the air outlet speed of the air knife is 50m/s, the air outlet temperature of the air knife is-10 ℃, the draft multiplying power of the cold draft machine is 0.8 times, the temperature of the draft hot box is 140 ℃, and the draft multiplying power of the draft hot box is 1.2 times, so that the precursor silk is obtained.
And then carrying out a multi-stage stretching process on the precursor, wherein the primary stretching magnification is 4 times, the primary stretching temperature is 140 ℃, the secondary stretching magnification is 1.5 times, the secondary stretching temperature is 144 ℃, the tertiary stretching magnification is 1.05 times, and the tertiary stretching temperature is 145 ℃.
The device cannot stably run, and the gel silk is directly broken. The main reason is that the gel silk is not softened, is in a skin-core structure state, is not dissolved in the inside, and causes the breakage of the gel silk once being drafted in a later drafting hot box.
The properties of the ultra high molecular weight polyethylene macro-denier fibers prepared in the examples and the comparative examples were tested and the results are shown in table 10.
Table 10
| Solvent content (ppm) | Breaking strength (cN/dtex) | Young's modulus (cN/dtex) | |
| Example 1 | 5000 | 34.1 | 1330 |
| Example 2 | 3500 | 35.3 | 1315 |
| Example 3 | 4800 | 33.6 | 1302 |
| Example 4 | 14000 | 29.8 | 1205 |
| Example 5 | 7000 | 33.5 | 1258 |
| Example 6 | 4800 | 34.7 | 1305 |
| Example 7 | 900 | 36.8 | 1360 |
| Example 8 | 1200 | 35.1 | 1325 |
| Comparative example 1 | 15000 | 28.9 | 1159 |
| Comparative example 2 | - | - | - |
| Comparative example 3 | - | - | - |
"-" Indicates that the preparation was not successful and could not be detected.
The ultra-high molecular weight polyethylene heavy denier fiber prepared by the invention has large single filament number and good mechanical property compared with the comparative example.
In example 1, compared with example 4, the single filament fineness can be increased by using a larger spinneret aperture, but the solvent residue in the fiber is increased, and the spinnability of the fiber is decreased.
Compared with the embodiment 1 and the embodiment 5, the temperature of the condensing bath is high, which is not beneficial to the rapid precipitation of the solvent, and the residual quantity of the solvent of the precursor fiber and the subsequent finished fiber is increased, and the single filament fineness can meet the requirement, but the spinnability of the product is poor due to the high residual quantity of the solvent, the loss of the solvent is increased, the performance index is reduced, and the maximization of the product cost is not beneficial.
In comparison with example 1 and example 6, the speed of the air knife is increased, which is beneficial to solvent recovery, the precipitation and volatilization of the solvent on the surface of the fiber are increased by the increase of the air speed, and the breaking strength of the product is improved by the product, but the mutation rate of the fiber is increased due to the excessively high air speed, so that the quality index of the product is reduced.
In example 1, compared with example 7, the spray head stretching ratio is increased, the mass ratio of the solvent to the ultra-high molecular weight polyethylene in the prepared coarse denier fiber is reduced, and finally the solvent content in the fiber is low, so that the recovery of the solvent is facilitated, but the spray head stretching ratio is increased, the fineness of the fiber is also reduced, and the preparation of the monofilament with large fineness is not facilitated.
Compared with example 8, the example 7 is compared with the example 8, the temperature of the spinning melt is reduced, the rapid flash evaporation of the solvent is not facilitated, the content of the solvent in the gel silk is increased, the mass ratio of the solvent to the ultra-high molecular weight polyethylene in the prepared coarse denier fiber is increased, and the solvent residue in the final fiber is increased.
Comparative example 1 did not undergo the second cooling step, comparative example 2 did not undergo the first cooling step, and comparative example 3 did not undergo the preheating step.
The results of the table show that the invention can lead the sheath-core structure of the fiber to be firstly appeared and then eliminated in the preparation process by adopting twice cooling and preheating, so that the solvent in the gel yarn is continuously separated out along with the preparation process, the condition of yarn breakage and yarn breakage in the process caused by the sheath-core structure of the gel yarn in the preparation process is avoided, and finally, the prepared ultra-high molecular weight polyethylene heavy denier fiber has large filament number, low solvent content in the fiber and good mechanical property, and simultaneously, the recycling of the solvent can be realized.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575742A (en) * | 2008-05-05 | 2009-11-11 | 宁波荣溢化纤科技有限公司 | Preparation method of ultra-high molecular weight polyethylene fiber |
| CN101748533A (en) * | 2009-12-17 | 2010-06-23 | 北京特斯顿新材料技术发展有限公司 | Draft process and equipment thereof for polyethylene fibres with superhigh molecular weight |
| US20110269359A1 (en) * | 2007-06-08 | 2011-11-03 | Honeywell International Inc. | Ultra-high strength uhmw pe fibers and products |
| CN104404640A (en) * | 2014-12-26 | 2015-03-11 | 常熟绣珀纤维有限公司 | Ultra-high-molecular-weight polyethylene protofilament drafting method |
| CN106591969A (en) * | 2016-12-27 | 2017-04-26 | 吉林大学 | Polyetheretherketone hollow fiber preparation method |
| CN111270329A (en) * | 2018-12-05 | 2020-06-12 | 北京同益中新材料科技股份有限公司 | Coarse monofilament ultra-high molecular weight polyethylene fiber and preparation method and application thereof |
| CN111592709A (en) * | 2020-06-24 | 2020-08-28 | 上海化工研究院有限公司 | Special material for medium-high-strength polyethylene fibers and preparation method of melt spinning fibers |
| CN112609250A (en) * | 2020-12-07 | 2021-04-06 | 青岛信泰科技有限公司 | Method for preparing ultra-high molecular weight polyethylene coarse denier fiber monofilament by gel method |
| CN114481343A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Fiber spinning method and polyethylene spinning fiber |
-
2023
- 2023-09-12 CN CN202311172414.8A patent/CN119615389A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110269359A1 (en) * | 2007-06-08 | 2011-11-03 | Honeywell International Inc. | Ultra-high strength uhmw pe fibers and products |
| CN101575742A (en) * | 2008-05-05 | 2009-11-11 | 宁波荣溢化纤科技有限公司 | Preparation method of ultra-high molecular weight polyethylene fiber |
| CN101748533A (en) * | 2009-12-17 | 2010-06-23 | 北京特斯顿新材料技术发展有限公司 | Draft process and equipment thereof for polyethylene fibres with superhigh molecular weight |
| CN103608502A (en) * | 2011-06-30 | 2014-02-26 | 霍尼韦尔国际公司 | Ultra-high strength UHMW PE fibers and products |
| CN104404640A (en) * | 2014-12-26 | 2015-03-11 | 常熟绣珀纤维有限公司 | Ultra-high-molecular-weight polyethylene protofilament drafting method |
| CN106591969A (en) * | 2016-12-27 | 2017-04-26 | 吉林大学 | Polyetheretherketone hollow fiber preparation method |
| CN111270329A (en) * | 2018-12-05 | 2020-06-12 | 北京同益中新材料科技股份有限公司 | Coarse monofilament ultra-high molecular weight polyethylene fiber and preparation method and application thereof |
| CN111592709A (en) * | 2020-06-24 | 2020-08-28 | 上海化工研究院有限公司 | Special material for medium-high-strength polyethylene fibers and preparation method of melt spinning fibers |
| CN114481343A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Fiber spinning method and polyethylene spinning fiber |
| CN112609250A (en) * | 2020-12-07 | 2021-04-06 | 青岛信泰科技有限公司 | Method for preparing ultra-high molecular weight polyethylene coarse denier fiber monofilament by gel method |
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