CN117328154B - Method and equipment for continuously producing liquid crystal polyester fiber - Google Patents
Method and equipment for continuously producing liquid crystal polyester fiber Download PDFInfo
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- CN117328154B CN117328154B CN202311580567.6A CN202311580567A CN117328154B CN 117328154 B CN117328154 B CN 117328154B CN 202311580567 A CN202311580567 A CN 202311580567A CN 117328154 B CN117328154 B CN 117328154B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 123
- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 122
- 239000000835 fiber Substances 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000009987 spinning Methods 0.000 claims abstract description 50
- 238000011282 treatment Methods 0.000 claims abstract description 31
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 238000004804 winding Methods 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 58
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 20
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 20
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 20
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 12
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 10
- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical compound C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 238000010583 slow cooling Methods 0.000 claims description 7
- LEDMBFYDMKOSPL-UHFFFAOYSA-N 1-(2-hydroxyphenyl)cyclohexa-3,5-diene-1,2-diol Chemical compound OC1C=CC=CC1(O)C1=CC=CC=C1O LEDMBFYDMKOSPL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 18
- 239000000126 substance Substances 0.000 abstract description 2
- 230000008676 import Effects 0.000 description 18
- 238000002074 melt spinning Methods 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000004970 Chain extender Substances 0.000 description 5
- 229920000106 Liquid crystal polymer Polymers 0.000 description 5
- 239000000155 melt Substances 0.000 description 4
- -1 polyoxyethylene Polymers 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000004974 Thermotropic liquid crystal Substances 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000008041 oiling agent Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241001646851 Coleus Species 0.000 description 1
- 235000021508 Coleus Nutrition 0.000 description 1
- 229920000271 Kevlar® Polymers 0.000 description 1
- 239000004976 Lyotropic liquid crystal Substances 0.000 description 1
- 241001134446 Niveas Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229920000508 Vectran Polymers 0.000 description 1
- 239000004979 Vectran Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004761 kevlar Substances 0.000 description 1
- 229940070765 laurate Drugs 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003384 small molecules Chemical group 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
Classifications
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- 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
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
- D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
Abstract
The invention provides a method and equipment for continuously producing liquid crystal polyester fibers, and belongs to the field of chemical fiber manufacturing. The method comprises the following steps: step (1): vacuum drying is carried out on the liquid crystal polyester chip for 6-8 hours at the temperature of 120-150 ℃; step (2): melting and plasticizing the dried liquid crystal polyester slice at the temperature of 290-360 ℃, and then sequentially passing the obtained molten liquid crystal polyester slice through a metering unit, a spinning unit at the temperature of 290-360 ℃ and a spinneret plate to spray filament bundles; step (3): the sprayed tows are subjected to gradient cooling and drafting, and the drafted tows are subjected to high-temperature treatment, oiling by an oil tanker and winding to obtain the liquid crystal polyester fiber, so that the problems that the liquid crystal polyester fiber product is degraded in performance, high in manufacturing cost and unfavorable for industrial mass production due to the existing two-step process are solved.
Description
Technical Field
The invention belongs to the field of chemical fiber manufacturing, and particularly relates to a method and equipment for continuously producing liquid crystal polyester fibers.
Background
A Liquid Crystal Polymer (LCP) material is a new material developed in the 60 s of the 20 th century, and its molecular chain generally contains rigid rod-like groups, and is capable of forming a liquid crystal phase in a solution or molten state, corresponding to a lyotropic liquid crystal polymer and a thermotropic liquid crystal polymer, respectively. High performance fibers such as Kevlar fibers developed by DuPont in 1972 and Vectran fibers produced by Coleus in 1990 can be obtained by spinning using its liquid crystalline properties. The liquid crystal polyester fiber is a typical thermotropic liquid crystal polymer, has the outstanding characteristics of high strength, high modulus, high temperature resistance, wear resistance, strong dimensional stability, low moisture absorption and the like, and can be applied to the fields of aerospace, national defense, military industry, marine ropes and the like.
The prior production process of the liquid crystal polyester fiber adopts a two-step method, specifically, the primary fiber is prepared by melt spinning, and then the primary fiber is subjected to heat treatment to obtain the high-performance liquid crystal polyester fiber. The invention CN 115398048A of kogawa, ltd, discloses a liquid crystal polyester fiber and a method for producing the same, which comprises a step of preheating a spun yarn of the liquid crystal polyester fiber at 80 to 220 ℃ and a step of solid-phase polymerizing the spun yarn after the preheating step at 230 ℃ or more, wherein the spun yarn is transported at an elongation ratio of 1.000 to 1.200 times and heat-treated at least in the step of solid-phase polymerization.
As disclosed in invention CN 106591997B of new material science and technology, inc. Of nivea, a method for improving the heat treatment efficiency of thermotropic liquid crystal polyarylate fiber comprises the following steps: (1) Respectively drying the TLCP spinning slice and the small molecule chain extender; (2) Placing the dried TLCP spinning slice and the small molecular chain extender together in a high-speed mixer with a heating temperature control system according to the mass ratio of 99:1-90:10 for high-speed mixing to obtain the TLCP slice with the small molecular chain extender adhered on the surface; (3) And directly feeding the TLCP slices with the small molecular chain extender adhered on the surfaces from a screw feed inlet of a melt spinning machine, and carrying out melt spinning at the temperature of 250-350 ℃ to obtain the TLCP nascent fibers containing the small molecular chain extender.
The invention CN 106087177B of Sichuan national institute of textile science discloses a continuous solid-phase polycondensation heat treatment method for liquid crystal polyester fibers, wherein a heat treatment device comprises two or more heated chambers, the fibers sequentially pass through a low-temperature region and a high-temperature heated chamber, the heated chambers are provided with heating rollers and filament dividing guide rollers in inert gas protection atmosphere, a constant tension regulator and the filament dividing guide rollers are arranged between the chambers, and the liquid crystal polyester fibers with the strength higher than 20cN/dtex can be prepared, so that the performance of the nascent fibers is improved.
The prior art can realize the preparation of the liquid crystal polyester fiber, but the production adopts a two-step method, namely, the polyester resin is melt-spun to obtain coiled primary fiber, and then the coiled primary fiber is unwound, heat treated and coiled to obtain the finished fiber. However, the two-step method has the following problems that, on one hand, in the step of preparing the coiled nascent fiber in the first step, the melt spinning is usually subjected to the processes of cooling, oiling, coiling into a yarn cylinder and the like, and the oiling agent in the step is subjected to the subsequent second-step high-temperature heat treatment and is partially decomposed, so that the performance of the fiber is adversely affected, and even the fiber bundle is required to be oiled again after the second-step heat treatment so as to ensure the cohesion and smoothness of the fiber bundle; on the other hand, the two-step method has low production efficiency and high production cost, and is not beneficial to the application and development of the liquid crystal polyester fiber.
Therefore, how to avoid the defects of complicated and complex process flow, low production efficiency, high manufacturing cost and the like of the existing liquid crystal polyester fiber is a problem to be solved.
Disclosure of Invention
The present invention is directed to a method and apparatus for continuously producing liquid crystal polyester fiber, which solve the problems of the prior art. According to the method, one-step melt spinning and heat treatment procedures of the liquid crystal polyester chips can be completed through specially designed continuous production equipment, so that the production flow is simplified, the production efficiency is greatly improved, the liquid crystal polyester fibers with the strength of 15-22 cN/dtex are obtained, and the problems that the conventional two-step process brings about performance degradation to liquid crystal polyester fiber products, the manufacturing cost is high, and industrial mass production is not facilitated are solved.
The technical scheme of the invention is as follows:
the present invention provides a method for continuously producing a liquid crystal polyester fiber, the method comprising the steps of:
step (1): vacuum drying is carried out on the liquid crystal polyester chip for 6-8 hours at the temperature of 120-150 ℃;
step (2): melting and plasticizing the dried liquid crystal polyester slice at the temperature of 290-360 ℃, and then sequentially passing the obtained molten liquid crystal polyester slice through a metering unit, a spinning unit at the temperature of 290-360 ℃ and a spinneret plate to spray filament bundles;
step (3): and (3) carrying out gradient cooling on the sprayed tows, simultaneously carrying out drafting, and carrying out high-temperature treatment, oiling on an oil tanker and winding on the drafted tows to obtain the liquid crystal polyester fiber.
Further, in the step (1), the monomers composing the liquid crystal polyester chip are any one of the following combinations a-f: a, p-hydroxybenzoic acid and 2-hydroxy-6-naphthoic acid; b, p-hydroxybenzoic acid, terephthalic acid, isophthalic acid and biphenol; c, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid and hydroquinone; d, p-hydroxybenzoic acid, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid and biphenol; e, p-hydroxybenzoic acid, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid and hydroquinone; f, p-hydroxybenzoic acid, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid, biphenol and hydroquinone.
Further, in the step (1), the melting point of the liquid crystal polyester chip is 270-340 ℃.
Further, in the step (2), the liquid crystal polyester chips are melted in a single screw extruder.
Further, in the step (2), the rotation speed of the single screw extruder is 10-40r/min, the diameter is 25-35 mm, and the length-diameter ratio is 24-28:1.
Further, in the step (2), the specification of an internal spinneret plate of the spinning unit is 10-40 holes, the aperture is 0.1-0.3 mm, and the length-diameter ratio of the spinneret plate is 1.5-6.
Further, in the step (2), the temperature of the spinning unit is preferably set to 295 ℃ to 355 ℃.
Further, in the step (3), 3 slow coolers are adopted for gradient cooling, the length of each slow cooler is 50-100mm, and the temperature of each slow cooler is adjustable within the range of room temperature to 350 ℃.
In the slow cooler, the slow cooler is hollow cylindrical. The ejected tows pass through the high-temperature hollow cylinder to move downwards, so that the fibers have longer drafting distance and time, finer fibers can be prepared, and on the other hand, the structural difference between the fiber skin layer and the core layer can be reduced. If the height of the slow cooler is too large, the energy consumption is high and the improvement of the fiber performance is insignificant, and if the height of the slow cooler is too small, the improvement effect of the fiber performance is insignificant.
Further, in the step (3), 3 slow coolers are arranged from top to bottom in a gradient cooling mode, and the temperature interval is set to 280-350 ℃, 200-260 ℃ and 100-150 ℃ in sequence.
Further, in the step (3), when the tows undergo gradient cooling, the tows are drawn by a godet, and the drawing ratio is set to be 10-200.
Further, in step (3), the high temperature treatment includes a two-stage heat treatment. Specifically, the first-stage heat treatment temperature is set to 180-230 ℃, and the tension of the tows is controlled to 40-300 cN; the second-stage heat treatment temperature is set to be 230-330 ℃, and the tension of the filament bundles is controlled to be 40-300 cN.
Further, in the step (3), the two-stage heat treatments are respectively carried out in a hot box, and the hot box is filled with nitrogen atmosphere, so that degradation of fiber tows at high temperature is reduced.
Further, in the step (3), a plurality of hot rolls are arranged in the hot box to heat the tows. Specifically, the hot box of the first-stage heat treatment comprises 2 to 6 hot rolls, and the hot box of the second-stage heat treatment comprises 4 to 8 hot rolls.
Further, in the step (3), the oil agent comprises the following components in percentage by weight: 60% of polyether, 12% of sodium dodecyl benzene sulfonate, 10% of polyethylene glycol laurate, 10% of polyoxyethylene trimethylol tri-fatty acid ester, 5% of castor oil polyoxyethylene ester and 3% of polyoxyethylene alkyl phosphate potassium salt.
Further, in the step (3), the winding speed is set to be 50-300 m/min.
In the preparation method of the invention, the purpose of drying the liquid crystal polyester chips in advance is to remove the moisture of the chips so as to reduce the thermal degradation in the melt spinning process.
In the preparation method of the invention, the melting point of the liquid crystal polyester chip is 270-340 ℃, and capillary rheological test analysis is carried out on the chip, so that the chip can be melted and extruded within the temperature range above the melting point, but in order to ensure stable viscosity, good fluidity and reduced thermal degradation of materials in the spinning process, the spinning temperature is generally set to 290-360 ℃, preferably 295-355 ℃.
In the invention, the spinning temperature is higher, and the glass transition temperature is high due to the rigid structures such as benzene rings, naphthalene rings and the like of the liquid crystal polyester chip, if the spinning melt is extruded from the spinning hole at about 300 ℃ and is directly contacted with room temperature air, the surface of the melt trickle can be rapidly cooled, so that the fiber has an obvious sheath-core structure on one hand, and on the other hand, the fiber is difficult to realize high-power drawing to prepare the fine fiber. For this reason, the invention sets 3 slow coolers with adjustable length and temperature below the spinneret plate, so that the melt trickle is slowly cooled after exiting the spinneret plate, and the draft ratio is increased while the sheath-core structure of the fiber is weakened. Wherein the temperature of 3 slow coolers from top to bottom is set to 280-350 ℃, 200-260 ℃ and 100-150 ℃. The filament linear density range of the prepared liquid crystal polyester fiber is about 5-15 dtex, and the filament diameter of the liquid crystal polyester fiber is about 20-40 mu m under an optical microscope.
In the preparation method of the invention, the drafting process is realized by the speed difference between the rollers, the tension is regulated by the speed difference, the drafting ratio between the rollers is measured by the tension measuring device, and the drafting ratio = the ratio of the speeds of two adjacent rollers.
After passing through the slow cooler, the fiber tows enter the heating roller through the godet, and are subjected to high-temperature heat treatment under the action of tension, and as the melting point of the liquid crystal polyester is raised to a certain extent after heat treatment, the heat treatment is performed by two-stage gradient heating, and the heating roller is placed in a hot box in nitrogen atmosphere, so that high-temperature degradation is reduced as much as possible.
In the preparation method, when the fiber tows subjected to the high-temperature heat treatment are oiled on the oil tanker, the oiling amount is controlled by controlling the rotating speed of the oil tanker.
The strength of the liquid crystal polyester fiber prepared by the method is 15-22 cN/dtex, the modulus is 75-105 GPa, and the elongation at break is 2-4%.
The invention also provides equipment for continuously producing the liquid crystal polyester fiber, which is used for implementing the method, and comprises the following units in sequence according to the material processing direction:
and a melting plasticizing unit: the method comprises the steps of (1) carrying out melt extrusion on a liquid crystal polyester slice at a temperature above the melting point of the liquid crystal polyester slice to form molten liquid crystal polyester;
metering unit: the method is used for accurately calculating the discharge amount of the molten liquid crystal polyester, so that the subsequent spinning is continuously and stably performed.
Spinning unit: spinning the molten liquid crystal polyester and spraying out a silk bundle;
and (3) a slow cooling unit: the device is used for carrying out gradient cooling on the tows;
and a heat treatment unit: for subjecting the tow to a high temperature treatment;
oiling unit: the method comprises the steps of (1) carrying out oil tanker oiling on the tows subjected to high-temperature treatment;
a winding unit: for winding the tows to form the liquid crystal polyester fiber.
Further, the melt plasticizing unit includes a single screw extruder. The single-screw extruder comprises a screw motor, a screw outer sleeve, a screw and a flange;
further, the metering unit comprises a metering pump motor, a metering pump and a metering pump heat-preserving cover.
Further, the spinning unit comprises a spinning component and a spinning component heat insulation cover, and a spinneret plate is arranged at the tail end of the spinning component.
Further, 3 slow coolers are arranged on the slow cooling unit from top to bottom, and the adjustable length range of each slow cooler is 50-100mm.
Further, the heat treatment unit comprises two heat boxes, and a plurality of heat rollers are arranged in each heat box. Preferably, the primary heat box is provided with 2 to 6 heat rolls, and the secondary heat box is provided with 4 to 8 heat rolls.
Further, the hot box is provided with one or more N 2 And (5) an inlet and an outlet.
Further, one or more godet rolls are arranged between the spinning unit and the heat treatment unit.
Further, one or more godet rollers are arranged between the heat treatment unit and the oil tanker oiling unit.
Further, one or more godet rolls are arranged between the oiling unit and the winding unit.
The invention has the beneficial effects that:
1. the preparation method of the liquid crystal polyester fiber is simple to operate, the technological conditions are easy to control, and the melt spinning and heat treatment procedures are continuously and efficiently completed by a one-step method, so that the production flow of the liquid crystal polyester fiber is shortened, the production efficiency is greatly improved, the production cost is reduced, and the liquid crystal polyester fiber has wide application prospect and important economic value.
2. In the method, the liquid crystal polyester fiber obtained through melt spinning is subjected to gradient cooling, and can be directly subjected to online high-temperature heat treatment without being wound into nascent fibers, so that the liquid crystal polyester fiber can be prepared through a one-step method. The one-step continuous production solves the problem of uneven internal and external properties of the winding tube caused by high-temperature heat treatment of the primary fiber in the traditional two-step method, and also avoids the degradation of fiber properties caused by partial decomposition of the oiling agent at the subsequent high temperature in the primary fiber production.
3. In the method, 3 slow coolers are adopted for gradient cooling, so that tows sprayed by melt spinning are slowly cooled in three temperature intervals in sequence, and finally are cooled by air. The arrangement has the advantages that the fiber sheath-core structure can be weakened, the draft ratio can be increased, the filament linear density range of the finally prepared liquid crystal polyester fiber is about 5-15 dtex, and the filament diameter of the finally prepared liquid crystal polyester fiber is about 20-40 mu m under an optical microscope. Meanwhile, the liquid crystal polyester fiber has good mechanical properties by combining two-stage high-temperature heat treatment, the strength is 15-22 cN/dtex, the modulus is 75-105 GPa, and the elongation at break is 2-4%.
4. The equipment provided by the invention realizes continuous on-line treatment of the melt spinning process and the high-temperature heat treatment process. The melt-state liquid crystal polyester is extruded from a spinneret plate, fine fibers are prepared through three-stage slow cooling, and the fiber strength is improved through two-stage high-temperature treatment, so that two processes of melt spinning and high-temperature treatment are completed on one set of equipment, and continuous and efficient one-step preparation of the liquid crystal polyester fibers is realized.
Drawings
Fig. 1 is a construction view of the apparatus of the present invention.
The reference numerals are as follows:
1, a screw motor;
2-an outer screw sleeve;
3, a screw rod;
4, a flange;
5-a metering pump motor;
6-a metering pump;
7-a metering pump insulation cover;
8-a spinning unit;
9-slow cooling unit;
10-No. 1 godet;
11-first-level hot box;
12-a secondary hot box;
13—a heat roller;
14-No. 2 godet;
15-an oiling unit;
16-number 3 godet;
17-No. 4 godet;
18—a winding unit;
19—a melt plasticizing unit;
20-a metering unit;
21-a heat treatment unit.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
The filament linear density, strength, modulus and elongation at break of the liquid crystal polyester fibers obtained in all examples and comparative examples were measured by the method of high-strength fiber filament tensile property test GB/T19975-2005.
All examples were carried out in a one-step continuous process using the apparatus of FIG. 1 to produce liquid crystalline polyester fibers. As shown in fig. 1, the device comprises the following components:
melt plasticizing unit 19: the method comprises the steps of (1) carrying out melt extrusion on a liquid crystal polyester slice at a temperature above the melting point of the liquid crystal polyester slice to form molten liquid crystal polyester; the device comprises a screw motor 1, a screw outer sleeve 2, a screw 3 and a flange 4 which are sequentially connected according to the material conveying direction;
metering unit 20: the method is used for accurately calculating the discharge amount of the molten liquid crystal polyester so that the subsequent spinning is continuously and stably carried out; comprises a metering pump motor 5, a metering pump 6 and a metering pump heat-preserving cover 7; the metering pump motor 5 is connected with a metering pump 6, and the metering pump 6 is arranged in the metering pump heat-preserving cover 7;
spinning unit 8: the spinning device is used for spinning and spraying the molten liquid crystal polyester into tows; comprises a spinning component and a spinning component heat-insulating cover; wherein the spinning component is arranged in the spinning component heat-preserving cover;
slow cooling unit 9: the device is used for carrying out gradient cooling on the tows; comprises three slow coolers;
heat treatment unit 21: for high temperature treatment of the tow; the device comprises a first-stage heat box 11 and a second-stage heat box 12 which are sequentially connected according to the material conveying direction, wherein 2 to 6 heat rollers 13 are arranged in the first-stage heat box, and 4 to 8 heat rollers 13 are arranged in the second-stage heat box;
oiling unit 15: the method is used for oiling the tows subjected to high-temperature treatment on a tanker;
winding unit 18: the method comprises the steps of winding a silk bundle to form liquid crystal polyester fibers;
wherein, a number 1 godet 10 is arranged between the spinning unit 8 and the heat treatment unit 21;
a No. 2 godet 14 is arranged between the heat treatment unit 21 and the oiling unit 15;
a godet No. 3 16 and a godet No. 4 17 are arranged between the oiling unit 15 and the winding unit 18.
Example 1
Example 1 provides a method for continuously producing liquid crystal fibers, comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice at 120 ℃ for 6 hours;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 290 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 290 ℃ to spray out tows from a spinneret plate, wherein the number of holes of the spinneret plate is 10, the aperture is 0.1mm and the length-diameter ratio is 1.5;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 50mm are arranged from top to bottom, the temperatures of the three slow coolers are 280 ℃, 200 ℃ and 100 ℃ respectively, and the three slow coolers are simultaneously drafted by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 comprising three heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 180 ℃, and the tension is controlled to be 40cN; the second heat treatment is carried out in a second heat box 12 comprising five heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller 13 is 230 ℃, and the tension is 40cN;
and oiling the tows subjected to high-temperature treatment, and winding at the speed of 300m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in example 1 had a filament yarn density of 8dtex, a strength of 15cN/dtex, a modulus of 75GPa and an elongation at break of 2.0%.
Example 2
Example 2 provides a method for continuously producing a liquid crystal fiber, comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice for 8 hours at 150 ℃;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 310 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 310 ℃ to spray filament bundles from a spinneret plate, wherein the number of holes of the spinneret plate is 40, the aperture is 0.2mm and the length-diameter ratio is 3;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 70mm are arranged from top to bottom, the temperatures of the three slow coolers are 300 ℃, 220 ℃ and 120 ℃ respectively, and the three slow coolers are simultaneously drafted by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 containing five heat rolls, the heat box being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 230 ℃, and the tension is 40cNThe second heat treatment was performed in a second heat box 12 containing seven heat rolls, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 270 ℃, the tension is 60cN,
and oiling the high-temperature treated tows, and winding at the speed of 150m/min to obtain the liquid crystal polyester fiber.
The liquid-crystalline polyester fiber obtained in example 2 had a filament yarn density of 10dtex, a strength of 19cN/dtex, a modulus of 90GPa and an elongation at break of 2.8%.
Example 3
Example 3 provides a method for continuously producing a liquid crystal fiber, comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice for 8 hours at 150 ℃;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 315 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 315 ℃ to spray filament bundles from a spinneret plate, wherein the number of holes of the spinneret plate is 20, the aperture is 0.1mm and the length-diameter ratio is 2;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 50mm are arranged from top to bottom, the temperatures of the three slow coolers are 305 ℃, 230 ℃, 130 ℃ respectively, and the tows are simultaneously drawn by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 containing five heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 230 ℃, and the tension is 40cN; the second heat treatment is carried out in a second heat box 12 comprising seven heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 275 ℃, and the tension is 40cN;
and oiling the tows subjected to high-temperature treatment, and winding at the speed of 300m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in example 3 had a filament yarn density of 5dtex, a strength of 20cN/dtex, a modulus of 95GPa and an elongation at break of 4.0%.
Example 4
Example 4 provides a method for continuously producing liquid crystal fibers comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice at 130 ℃ for 7h;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 320 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 320 ℃ to spray filament bundles from a spinneret plate, wherein the number of holes of the spinneret plate is 20, the aperture is 0.3mm and the length-diameter ratio is 6;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 100mm are arranged from top to bottom, the temperatures of the three slow coolers are 310 ℃, 210 ℃ and 110 ℃ respectively, and the tows are simultaneously drawn by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 comprising three heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 200 ℃, and the tension is 300cN; the second heat treatment is carried out in a second heat box 12 comprising five heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 260 ℃, and the tension is 300cN;
and oiling the tows subjected to high-temperature treatment, and winding at a speed of 50m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in example 4 had a filament yarn density of 12dtex, a strength of 17cN/dtex, a modulus of 85GPa and an elongation at break of 2.6%.
Example 5
Example 5 provides a method for continuously producing liquid crystal fibers comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice at 130 ℃ for 6 hours;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 360 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 360 ℃ to spray filament bundles from a spinneret plate, wherein the number of holes of the spinneret plate is 20, the aperture is 0.2mm and the length-diameter ratio is 4;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 50mm are arranged from top to bottom, the temperatures of the three slow coolers are respectively 350 ℃, 260 ℃ and 150 ℃, and the three slow coolers are simultaneously drafted by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 containing five heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 230 ℃, and the tension is controlled to be 100cN; the second heat treatment is carried out in a second heat box 12 comprising seven heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller 13 is 330 ℃, and the tension is 100cN;
and oiling the tows subjected to high-temperature treatment, and winding at the speed of 300m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in example 5 had a filament yarn density of 8dtex, a strength of 20cN/dtex, a modulus of 100GPa and an elongation at break of 3.2%.
Example 6
Example 6 provides a method for continuously producing a liquid crystal fiber, comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice for 8 hours at 150 ℃;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 350 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 350 ℃ to spray filament bundles from a spinneret plate, wherein the number of holes of the spinneret plate is 20, the aperture is 0.1mm and the length-diameter ratio is 1.5;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 60mm are arranged from top to bottom, the temperatures of the three slow coolers are 340 ℃, 240 ℃, 130 ℃ respectively, and the three slow coolers are simultaneously drafted by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 containing five heat rolls 13, the first stageThe hot box 11 is provided with N 2 Import and export, N 2 The flow rate was 10L/min, the heat roller temperature was 220℃and the tension was 80cN, the second heat treatment was carried out in a second heat box 12 containing seven heat rollers 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 320 ℃, and the tension is 80cN;
and oiling the tows subjected to high-temperature treatment, and winding at a speed of 200m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in example 6 had a filament yarn density of 6dtex, a strength of 22cN/dtex, a modulus of 105GPa and an elongation at break of 3.8%.
Example 7
Example 7 provides a method for continuously producing a liquid crystal fiber, comprising the steps of:
step (1): vacuum drying the liquid crystal polyester slice for 8 hours at 120 ℃;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 355 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 355 ℃ to spray filament bundles from a spinneret plate, wherein the number of holes of the spinneret plate is 10, the aperture is 0.22mm and the length-diameter ratio is 2;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 100mm are arranged from top to bottom, the temperatures of the three slow coolers are 340 ℃, 240 ℃, 130 ℃ respectively, and the three slow coolers are simultaneously drafted by air cooling,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 containing five heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 210 ℃, and the tension is 50cN; the second heat treatment is carried out in a second heat box 12 comprising seven heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 310 ℃, and the tension is 50cN;
and oiling the tows subjected to high-temperature treatment, and winding at the speed of 300m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in example 7 had a filament yarn density of 12dtex, a strength of 16cN/dtex, a modulus of 80GPa and an elongation at break of 3.6%.
Comparative example 1
Step (1): vacuum drying the liquid crystal polyester slice at 120 ℃ for 6 hours;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 290 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 290 ℃ to spray out tows from a spinneret plate, wherein the number of holes of the spinneret plate is 10, the aperture is 0.1mm and the length-diameter ratio is 1.5;
step (3): the sprayed silk bundle is cooled in a gradient way, a section of slow cooler with the length of 50mm and the temperature of 280 ℃ is adopted, and then the silk bundle is cooled by air and simultaneously drafted,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 comprising three heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 180 ℃, and the tension is controlled to be 40cN; the second heat treatment is carried out in a second heat box 12 comprising five heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller 13 is 230 ℃, and the tension is 40cN;
and oiling the tows subjected to high-temperature treatment, and winding at the speed of 300m/min to obtain the liquid crystal polyester fibers.
The liquid-crystalline polyester fiber obtained in comparative example 1 had a filament yarn density of 8dtex, a strength of 13cN/dtex, a modulus of 68GPa and an elongation at break of 1.8%.
Comparative example 2
Step (1): vacuum drying the liquid crystal polyester slice at 120 ℃ for 6 hours;
step (2): melting and plasticizing the dried liquid crystal polyester slice at 290 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit 20 and a spinning unit 8 at 290 ℃ to spray out tows from a spinneret plate, wherein the number of holes of the spinneret plate is 10, the aperture is 0.1mm and the length-diameter ratio is 1.5;
step (3): the sprayed tows are cooled in a gradient way, three slow coolers with the length of 50mm are arranged from top to bottom, the temperatures of the three slow coolers are 200 ℃ and 100 ℃ and 50 ℃, the three slow coolers are respectively cooled by air and simultaneously drafted,
the drawn filament bundle is then subjected to a high temperature treatment, the first stage heat treatment being carried out in a first stage heat box 11 comprising three heat rolls 13, the first stage heat box 11 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller is 180 ℃, and the tension is controlled to be 40cN; the second heat treatment is carried out in a second heat box 12 comprising five heat rolls 13, the second heat box 12 being provided with N 2 Import and export, N 2 The flow is 10L/min, the temperature of the hot roller 13 is 230 ℃, and the tension is 40cN;
and oiling the tows subjected to high-temperature treatment, and winding at the speed of 300m/min to obtain the liquid crystal polyester fibers.
The liquid crystal polyester fiber obtained in comparative example 2 had a filament yarn density of 10dtex, a strength of 12cN/dtex, a modulus of 65GPa and an elongation at break of 1.8%.
Therefore, the method of the invention adopts 3 slow coolers for gradient cooling, and the tows sprayed by melt spinning are subjected to three temperature ranges of 280-350 ℃, 200-260 ℃ and 100-150 ℃ in sequence for slow cooling, and finally air cooling is carried out, so that the fiber sheath-core structure can be weakened, the draft ratio can be increased, the filament linear density range of the finally prepared liquid crystal polyester fiber is about 5-15 dtex, and simultaneously, the liquid crystal polyester fiber has good mechanical properties, the strength is 15-22 cN/dtex, the modulus is 75-105 GPa, and the elongation at break is 2-4% which is far greater than that of the product obtained by the comparative example.
The above description is only of the preferred embodiment of the present invention, and is not intended to limit the present invention in any other way, but is intended to cover any modifications or equivalent variations according to the technical spirit of the present invention, which fall within the scope of the present invention as defined by the appended claims.
Claims (5)
1. A process for continuously producing liquid crystal polyester fibers, characterized in that the process comprises the steps of:
step (1): vacuum drying is carried out on the liquid crystal polyester chip for 6-8 hours at the temperature of 120-150 ℃;
step (2): melting and plasticizing the dried liquid crystal polyester slices at the temperature of 290-360 ℃, and sequentially passing the obtained molten liquid crystal polyester through a metering unit (20), a spinning unit (8) at the temperature of 290-360 ℃ and a spinning plate to spray tows;
step (3): the sprayed tows are subjected to gradient cooling and drafting at the same time, and the drafted tows are subjected to high-temperature treatment, oiling by an oil tanker and winding to obtain liquid crystal polyester fibers;
3 slow coolers are arranged from top to bottom in a gradient cooling mode, and the temperature interval is sequentially set to 280-350 ℃, 200-260 ℃ and 100-150 ℃;
the high-temperature treatment comprises two-stage heat treatment, wherein the temperature of the first-stage heat treatment is set to be 180-230 ℃, and the tension of the filament bundles is controlled to be 40-300 cN; setting the second-stage heat treatment temperature to be 230-330 ℃, and controlling the tension of the filament bundles to be 40-300 cN;
the method is implemented by using the following equipment, wherein the equipment sequentially comprises the following units according to the material processing direction:
melt plasticizing unit (19): the method comprises the steps of (1) carrying out melt extrusion on a liquid crystal polyester slice at a temperature above the melting point of the liquid crystal polyester slice to form molten liquid crystal polyester;
metering unit (20): the method is used for accurately calculating the discharge amount of the molten liquid crystal polyester so that the subsequent spinning is continuously and stably carried out;
spinning unit (8): spinning the molten liquid crystal polyester and spraying out a silk bundle;
slow cooling unit (9): the device is used for carrying out gradient cooling on the tows;
a heat treatment unit (21): for subjecting the tow to a high temperature treatment;
oiling unit (15): the method comprises the steps of (1) carrying out oil tanker oiling on the tows subjected to high-temperature treatment;
a winding unit (18): the yarn bundles are wound to form liquid crystal polyester fibers;
the spinning unit (8) comprises a spinning component and a spinning component heat-insulating cover, and a spinneret plate is arranged at the tail end of the spinning component;
the heat treatment unit (21) comprises two heat boxes, wherein the primary heat box (11) is provided with 2 to 6 heat rollers (13), and the secondary heat box (12) is provided with 4 to 8 heat rollers (13).
2. The method according to claim 1, wherein in the step (1), the monomers constituting the liquid crystal polyester chips are any one of the following combinations a to f: a, p-hydroxybenzoic acid and 2-hydroxy-6-naphthoic acid; b, p-hydroxybenzoic acid, terephthalic acid, isophthalic acid and biphenol; c, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid and hydroquinone; d, p-hydroxybenzoic acid, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid and biphenol; e, p-hydroxybenzoic acid, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid and hydroquinone; f, p-hydroxybenzoic acid, 2-hydroxy-6-naphthoic acid, terephthalic acid, isophthalic acid, biphenol and hydroquinone.
3. The method according to claim 1 or 2, wherein in the step (2), the liquid crystal polyester chips are melted and plasticized in a single screw extruder, the rotation speed of the single screw extruder is 10-40r/min, the diameter is 25-35 mm, and the length-diameter ratio is 24-28:1.
4. The method according to claim 1 or 2, wherein in step (2), the internal spinneret of the spinning unit (8) has a specification of 10 to 40 holes, a pore diameter of 0.1 to 0.3mm, and an aspect ratio of 1.5 to 6.
5. The method according to claim 1 or 2, characterized in that in step (2), the temperature of the spinning unit (8) is set to 295-355 ℃.
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Inventor after: Zhao Zhongzheng Inventor after: Gao Jianwei Inventor before: Zhao Zhongzheng Inventor before: Gao Jianwei Inventor before: Sun Jianwu Inventor before: Guan Zhenhong Inventor before: Jiang Ming Inventor before: Wang Zhonghua Inventor before: Wang Zhongwei Inventor before: Li Jingjin |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |