CN101225555A - Melt-spinning hot-stretch forming preparation method of polyetheretherketone fibre - Google Patents
Melt-spinning hot-stretch forming preparation method of polyetheretherketone fibre Download PDFInfo
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Abstract
The invention relates to a preparation method of polyetheretherketone fiber through melt spinning hot stretching and forming, belonging to technical field of macromolecular materials, which comprises the following steps: high temperature spinning in extruders, delayed heating and cooling through hot passages, solidification and forming using blowing devices, coiling, slow stretching through heating of drawing discs, and loosing/forming through heating of drawing discs. The temperature for high temperature spinning is 340 to 420 DEG C, the distance between the hot passages and spinnerets is 0.1 to 15cm, the delayed heating temperature is 200 to 330 DEG C; the blowing temperature for solidification and forming is 20 to 120 DEG C, the coiling speed is 80 to 200m/min; the hot stretching temperature is 190 to 260 DEG C, the stretching ratio is 2 to 3.5 to 1; the loosing/forming temperature is 250 to 320 DEG C, the ratio of loosing/forming through stretching is 0.8 to 0.98 to 1; the spun filament is multifilament with the number of the 4 to 30. The preparation method of polyetheretherketone fiber through melt spinning hot stretching and forming has the advantages of high breaking strength, high breaking elongation, and resistance to high temperature.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of polyetheretherketonefiber fiber and melt spinning thereof, hot-stretch heat setting method.
Background technology
Polyether-ether-ketone resin has characteristics such as temperature classification height, radiation hardness, impact strength height, ABRASION RESISTANCE and fatigue durability are good, fire-retardant, electrical property excellence.Since commercialization, obtained to use more widely in fields such as Aero-Space, automobile, electric, chemical industry, machinery and medical treatment.The polyether-ether-ketone goods that are applied to above-mentioned field generally are the structural type goods of making by injection molding method, but some Application Areas needs polyetheretherketonefiber fiber or monofilament goods, fuel filter filter screen, composite, high-performance rope and string, mesh grid and the medicine equipment etc. of conveyer belt, space shuttle and the automobile that uses as paper industry.Purpose of the present invention is exactly the polyether-ether-ketone special fibre that satisfies the different user needs in order to prepare.
Background technology related to the present invention is the synthetic method technology (Chinese patent: " preparation method of polyether ethersulfone and polyetheretherketoneterpolymer terpolymer " of polyether-ether-ketone resin, application number: 200610016723.6, not only can prepare polyether ethersulfone but also can prepare polyether-ether-ketone resin and their copolymer) and utilize the synthetic polyether-ether-ketone resin of above-mentioned patent to add processing aid or modifier, make special-purpose material for spinning-stage polyetheretherketoneresin resin (Chinese patent: " special-purpose material for spinning-stage polyetheretherketoneresin resin and preparation method thereof ", application number: 200810050213.X) by melt extruding process for granulating
Summary of the invention
The objective of the invention is to utilize special-purpose material for spinning-stage polyetheretherketoneresin resin, prepare the polyether-ether-ketone special fibre, thereby a kind of melt spinning, hot-stretch HEAT SETTING preparation method of polyetheretherketonefiber fiber are provided by melt spinning method.
The extruder that is used to prepare fiber is furnished with gear wheel metering pump, to guarantee can accurately measure the melten gel amount of the spinnerets of packing under the level pressure condition, measuring pump is the gear wheel metering pump of one-in-and-one-out, and operating temperature can reach 500 ℃, working speed is 3～180rpm, and the nominal output quantity is 0.6cc/r.Characteristics such as the polyetheretherketonefiber fiber with this method preparation has the fracture strength height, elongation at break is higher and high temperature resistant.
Special-purpose material for spinning-stage polyetheretherketoneresin resin is pressed each component and 100wt% and is calculated, and contains 90.0～100.0wt% polyether-ether-ketone resin, the high-temperature lubricant of 0～3.0wt% and the poly aromatic ether ketone liquid crystal copolymer of 0～10.0wt% structural formula shown in (II).
Further preferred implementation comprises following four kinds of prescriptions,
Prescription a:
PEEK resin 100.0wt%
Prescription b:
PEEK resin 97.0～99.5wt%
High-temperature lubricant 0.5～3.0wt%
Prescription c:
PEEK resin 90.0～98.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2.0～10.0wt%
Prescription d:
PEEK resin 90.0～97.5wt%
High-temperature lubricant 0.5～3.0wt%
Poly aromatic ether ketone liquid crystal copolymer 2.0～9.5wt%
The logarithmic specific concentration viscosity of polyether-ether-ketone (PEEK) is 0.76～0.80, melt index is 12～30g/10min, and its structural formula is shown in (I), and n is 〉=1 integer, the expression degree of polymerization.
High-temperature lubricant is that graininess or the pulverulent GENIOPLASTPellet S that German Wacker company produces (is abbreviated as GPPS, the processing temperature of polyether-ether-ketone resin is very high, general lubricant can't satisfy instructions for use at all, has just decomposed before 360 ℃.This lubricant is that our seminar filters out for many years, and unique processing temperature that satisfies us is very effective again, has only this English name, does not have Chinese).
The structural formula of poly aromatic ether ketone liquid crystal copolymer is shown in (II):
R＝Cl，Ph，CH
3O，t-C
4H
9，
(II), y=0.2～0.8, n is a positive integer, the expression degree of polymerization.
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber of the present invention comprises the steps:
(1) with the fusion under 340～420 ℃ of temperature in extruder of the special-purpose material for spinning-stage polyetheretherketoneresin resin after the dried, the melt material bar of extruding through the porous spinnerets (radical depends on the hole count of spinnerets) flows out the cooling of delaying time through the hot path at distance spinnerets 0.1～15cm place again under 200～330 ℃ of temperature;
(2) the melt material bar that flows out through hot path leads the oiling device into bottom, hot path rapidly, leads in the annular blowing device again, and the blowing temperature is 20～120 ℃, cools off, and obtains the polyether-ether-ketone multifilament through beaming device;
(3) guide roller of polyether-ether-ketone multifilament through the beaming device bottom leads into the multifilament batching apparatus, and the multifilament speed of wrap is 80～200m/min, the polyether-ether-ketone precursor that is not stretched;
(4) the polyether-ether-ketone precursor that will not stretch places on the original silk rack, and precursor is imported the hot-stretch device, and the temperature that thermal potential is stretched is 190～260 ℃, and draw ratio is 2～3.5: 1;
(5) will import loose calibrator through the polyetheretherketonefiber fiber of hot-stretch again, the temperature of loose typing is 250～320 ℃, and loose typing ratio is 0.8～0.98: 1, then the polyetheretherketonefiber fiber that obtains is wrapped on the yarn wind-up device.
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, extruder adopts the heating of four districts, and one thermal treatment zone, back is higher 10～20 ℃ than the temperature of the last thermal treatment zone;
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, back at extruder is provided with measuring pump, below measuring pump and the front of porous spinnerets be provided with screen pack, the temperature of measuring pump casing is higher 10～20 ℃ than extruder final heating area temperature, and the polyether-ether-ketone resin melt is quantitatively extruded through filter screen and porous spinnerets under the effect of measuring pump;
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, spinnerets is 4～30 holes, thereby makes spun silk be multifilament, radical is 4～30;
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, in the annular blowing device that install bottom, hot path, blowing direction becomes 45～135 degree angles with spray silk direction, and the blowing temperature is 60～120 ℃;
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, special-purpose material for spinning-stage polyetheretherketoneresin resin carries out pre-dried before melt extruding spinning, and baking temperature is 130～150 ℃, and the time is 3～12 hours.
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, the multifilament batching apparatus is made up of guide roller, coiling core pipe and speed governing up-coiler, through being wrapped in behind the guide roller on the coiling core pipe, winding speed is realized by speed governing up-coiler control coiling core pipe through the polyether-ether-ketone multifilament behind annular blowing device, the beaming device.
Operations such as among the melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, the polyether-ether-ketone multifilament process after the process annular blowing solidifying and setting oils, boundling, coiling.In temperature is 20～30 ℃, and humidity is 70～80% the interior quiet weighing apparatus 8～12h that sets level of air-conditioned room, to eliminate internal stress and the top layer of winding bobbin and the difference between the internal layer that exists between the undrawn yarn interior molecules.These all are the processes known and the technology of spinning industry, carry out the hot-stretch typing again.
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, the oiling device of multifilament is that two-sided oil tanker oils, oil agent is a complex high temperature resistant, the corrosion resistant type dimethicone; The effect of beaming device is exactly to make the monofilament after oiling be gathered into tow, reels by multifilament guide roller, up-coiler again.
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, stretching is to carry out on stretching device, and promptly the original silk rack back is provided with 3 temperature and all controlled drawing-off dish of speed, and the drawing-off dish claims hot-rolling again, it is longer than general spinning thread-guiding dish, is the roller shape.Each hot-rolling all has branch roll dies (active or passive branch silk rotor).Load coil is equipped with in heat dish inside, and temperature is controlled automatically, surperficial spraying plating pottery.Regulate and control the loose typing speed of output speed, draw speed and fiber of precursor by the drawing-off dish, realize the different paces of polyether-ether-ketone multifilament between the drawing-off dish, thus control stretching than and loose typing ratio.Wherein No. 1 drawing-off dish and No. 2 drawing-off dishes are formed fiber draw unit, and the temperature of No. 1, No. 2 drawing-off dish is 190～260 ℃; No. 2 drawing-off dishes and No. 3 drawing-off dishes are formed the loose calibrator of fiber, and the temperature of No. 3 drawing-off dishes is 250～320 ℃.
The melt spinning hot-stretch typing preparation method of polyetheretherketonefiber fiber recited above, No. 1 drawing-off dish control precursor output speed is 50～500m/min, No. 2 drawing-off dish control stretching speed is 50～500m/min, No. 3 the loose typing speed of drawing-off dish controlling fiber is 50～500m/min, the precursor output speed, draw speed, the loose typing speed of fiber is adjustable continuously, and satisfy the precursor output speed simultaneously less than draw speed, the loose typing speed of fiber is less than the requirement of draw speed, draw ratio is a draw speed and the ratio of precursor output speed, and loose typing is than being the ratio of loose typing speed with draw speed.
In the present invention, be solidified in the fiber condition process at PEEK melt strand, adopt polyetheretherketonefiber fiber high temperature spinning time-delay heating cooling curing molding technology, hot path both had been set below spinnerets, make the melt strand pass through this zone with melt state, by the further slenderizing of batching apparatus, avoid making filament to cool off too fast and the generation waste material, guarantee to become noncrystalline attitude after fiber leaves mould by the blowing type of cooling simultaneously, be convenient to next step stretch orientation typing, thereby improve the spinning properties of polyetheretherketonefiber fiber and the mechanical performance of fiber; Polyetheretherketonefiber fiber is taked under the condition that is higher than the polyether-ether-ketone resin glass transition temperature in the stretching aftertreatment technology, and the PEEK fiber heats stretching technique at a slow speed, makes the PEEK molecular chain orientation perfect; Take to heat the degree of crystallinity that loose/tensioning heat setting method improves polyetheretherketonefiber fiber, adopt the polyetheretherketonefiber fiber of this technology preparation to have the fracture strength height, elongation at break is higher and characteristics such as high temperature resistant.
Description of drawings
Fig. 1: polyether-ether-ketone melt-spinning technology general flow chart;
Fig. 2: polyetheretherketonefiber fiber hot-stretch setting process general flow chart;
In Fig. 1 to Fig. 2, symbol 1 is represented the extruder drive motors, and symbol 2 is represented deceleration device, and symbol 3 is represented hopper, symbol 4 is represented electric heater, symbol 5 is represented the high temperature single screw extrusion machine, and symbol 6 measuring pumps, symbol 7 are represented the screen pack below the measuring pump 6, symbol 8 is represented spinnerets, the hot path of symbol 9 representatives, symbol 10 is represented oiling device, the annular blowing device of symbol 11 representatives, the wind speed of annular blowing device is adjustable, by air cleaner, formations such as air channel and blowing window, its effect is that the tow of extruding is carried out cooling and shaping, symbol 12 is represented blower fan, symbol 13 is represented the multifilament beaming device, symbol 14 is represented guide roller, and symbol 15 is represented the PEEK multifilament, and symbol 16 is represented multifilament coiling core pipe, symbol 17 is represented polyether-ether-ketone multifilament coiler device, symbol 18 is represented original silk rack, the PEEK multifilament that 19 representatives do not stretch, and symbol 20 is represented the drawing-off dish No. 1, symbol 21 is represented the drawing-off dish No. 2, symbol 22 is represented the drawing-off dish No. 3, and symbol 23 represents fiber roll around the core pipe, and symbol 24 is represented yarn wind-up device.
As shown in Figure 1, the polyether-ether-ketone PP Pipe Compound is in hopper 3 adds extruder 5 to, at electric heater 4 And melting under the shear action of screw rod; Drive motors 1 is interior molten with extruder 5 through deceleration device 2 drive screws The polyether-ether-ketone PP Pipe Compound of melting is squeezed in the measuring pump 6, and measuring pump 6 makes polyether-ether-ketone melt quantitative ground process Filter screen 7, spinneret 8 rear formation polyether-ether-ketone monofilament, the polyether-ether-ketone monofilament enters hot path 9, in hot path The cooling of delaying time in 9; (oil agent can be adjusted fiber to many polyether-ether-ketone monofilament behind oiling device 10 And the friction between the fiber, between fiber and the metal reduces coefficient of friction, reduces the static that produces because of friction, Make fiber have good convergence, flatness and fiber separation, satisfy the needs of processing concerned process steps behind the fiber, This technical process is the process that the spinning industry is known) enter blowing device 11 and cool off rear importing beaming device 13, boundling becomes polyether-ether-ketone multifilament 15 by guide roller 14, at the work of polyether-ether-ketone multifilament coiler device 17 With lower, be wrapped on the multifilament winding core pipe 16, be 20～30 ℃ in temperature then, humidity is 70～80% left sides The quiet weighing apparatus 8～12h that sets level in the right air-conditioned room;
As shown in Figure 2, the polyether-ether-ketone multifilament 19 that is placed on the original silk rack 18 is carried out hot-stretch typing and pine Speed the typing, drawing-off dish 20,21,22 has different rotating speeds and temperature, be used for precursor output speed, The loose typing speed of draw speed and fiber realizes different stretch ratio and loose typing ratio, carries out hot-stretch and pine Speed to finalize the design, polyether-ether-ketone multifilament 19 is wrapped in the fiber winding core under the effect of yarn wind-up device 24 then On the pipe 23.
In the present invention, if not refer in particular to, all equipment and auxiliary material etc. all can be buied or spinning from market Industry is commonly used, and equipment component uses through transforming at high temperature.
The specific embodiment
Further specify the present invention below by specific embodiment, but embodiment only is used for explanation, does not limit the scope of the invention.
Embodiment 1:
Adopt as depicted in figs. 1 and 2 equipment and process to prepare polyether-ether-ketone (PEEK) fiber.The screw diameter of employed single screw extrusion machine is 20mm, L/D=25, and heating system is the electrical heating of 4 districts; Measuring pump is the gear wheel metering pump of one-in-and-one-out, spin manifold temperature can reach 500 ℃, the nominal output quantity is 0.6cc/r, spinnerets is 0.2mm * 12 holes, spinnerets is 0.5mm apart from hot path distance, blowing device and hot path distance are 1000mm, screen pack is 80～1000 purpose multilayer stainless (steel) wires, and the material in hot path is heat-resisting, wear-resisting, corrosion resistant stainless steel, mode of heating adopt the heating of electrical heating cover, coiler device is a JRT10A-4BD920/16 type up-coiler, maximum winding speed is 1000m/min, and drawing-off dish specification is 98, L=100, speed is 50～700m/min, and is adjustable continuously.
A kind of special-purpose material for spinning-stage polyetheretherketoneresin resin is added extruder hopper (Chinese patent: " special-purpose material for spinning-stage polyetheretherketoneresin resin and preparation method thereof ", application number: 200810050213.X), prescription is as described in the following table, and the logarithmic specific concentration viscosity of PEEK resin is 0.80:
PEEK resin 99wt%
High-temperature lubricant 1wt%
The extrusion temperature of screw extruder is: a district is 300 ℃, and two districts are 360 ℃, and three districts are 380 ℃, four districts are 380 ℃, and the measuring pump temperature is 390 ℃, and hot path temperature is 260 ℃, annular blowing temperature is 80 ℃, multifilament speed of wrap (spinning speed) is 100m/min, and draw ratio is 2.0: 1, and draft temperature is 200 ℃, loose setting temperature is 280 ℃, loose typing ratio is 0.94: 1, and the synnema fiber number that makes fiber is 57.7Tex, and fibre strength is 35cN/tex.
Embodiment 2:
As described in embodiment 1, just the extrusion temperature with screw extruder changes into: a district is 300 ℃, and two districts are 365 ℃, three districts are 385 ℃, and four districts are 385 ℃, and the measuring pump temperature changes 395 ℃ into, hot path temperature changes 265 ℃ into, and annular blowing temperature changes 70 ℃ into, and spinning speed changes 120m/min into, draw ratio is 2.2:1, draft temperature is 210 ℃, and loose setting temperature is 285 ℃, and loose typing ratio is 0.95: 1, the synnema fiber number that makes fiber is 56.5Tex, and fibre strength is 38cN/tex.
Embodiment 3:
As described in embodiment 1, just the extrusion temperature with screw extruder changes into: a district is 300 ℃, and two districts are 370 ℃, three districts are 390 ℃, and four districts are 390 ℃, and the measuring pump temperature is 395 ℃, hot path temperature changes 270 ℃ into, and annular blowing temperature changes 90 ℃ into, and spinning speed changes 130m/min into, draw ratio is 2.3: 1, draft temperature is 220 ℃, and loose setting temperature is 290 ℃, and loose typing ratio is 0.96: 1, the synnema fiber number that makes fiber is 58.9Tex, and fibre strength is 40cN/tex.
Embodiment 4:
As described in embodiment 1, just the extrusion temperature with screw extruder changes into: a district is 300 ℃, and two districts are 375 ℃, three districts are 395 ℃, and four districts are 400 ℃, and the measuring pump temperature is 395 ℃, hot path temperature changes 275 ℃ into, and annular blowing temperature changes 100 ℃ into, and spinning speed is 130m/min, draw ratio is 2.8: 1, draft temperature is 225 ℃, and loose setting temperature is 295 ℃, and loose typing ratio is 0.97: 1, the synnema fiber number that makes fiber is 59.9Tex, and fibre strength is 48cN/tex.
Embodiment 5:
As described in embodiment 1, just the extrusion temperature with screw extruder changes into: a district is 300 ℃, and two districts are 370 ℃, three districts are 390 ℃, and four districts are 390 ℃, and the measuring pump temperature changes 400 ℃ into, hot path temperature changes 280 ℃ into, and annular blowing temperature changes 60 ℃ into, and spinning speed changes 100m/min into, draw ratio is 3.0: 1, draft temperature is 220 ℃, and loose setting temperature is 290 ℃, and loose typing ratio is 0.96: 1, the synnema fiber number that makes fiber is 59.5Tex, and fibre strength is 51cN/tex.
Embodiment 6:
As described in embodiment 1, just changing the extrusion temperature of screw extruder into a district is 300 ℃, and two districts are 380 ℃, three districts are 400 ℃, and four districts are 405 ℃, and the measuring pump temperature is 400 ℃, hot path temperature changes 280 ℃ into, and annular blowing temperature changes 110 ℃ into, and spinning speed changes 120m/min into, draw ratio is 2.4, draft temperature is 230 ℃, and loose setting temperature is 300 ℃, and loose typing ratio is 0.98: 1, the synnema fiber number that makes fiber is 56.5Tex, and fibre strength is 55cN/tex.
Embodiment 7:
As described in embodiment 1, just the extrusion temperature with screw extruder changes into: a district is 300 ℃, and two districts are 390 ℃, three districts are 400 ℃, and four districts are 410 ℃, and the measuring pump temperature changes 410 ℃ into, hot path temperature changes 285 ℃ into, and annular blowing temperature changes 95 ℃ into, and spinning speed changes 100m/min into, draw ratio is 2.5, draft temperature is 235 ℃, and loose setting temperature is 300 ℃, and loose typing ratio is 0.95: 1, the synnema fiber number that makes fiber is 57.5Tex, and fibre strength is 58cN/tex.
Embodiment 8:
As described in embodiment 1, just the extrusion temperature with screw extruder changes into: a district is 300 ℃, and two districts are 400 ℃, three districts are 410 ℃, and four districts are 420 ℃, and the measuring pump temperature changes 420 ℃ into, hot path temperature changes 275 ℃ into, and annular blowing temperature changes 85 ℃ into, and spinning speed changes 140m/min into, draw ratio is 2.6, draft temperature is 245 ℃, and loose setting temperature is 290 ℃, and loose typing ratio is 0.95: 1, the synnema fiber number that makes fiber is 58.5Tex, and fibre strength is 50cN/tex.
Claims (10)
1. the melt spinning hot-stretch of polyetheretherketonefiber fiber typing preparation method comprises the steps:
A) with the fusion under 340～420 ℃ of temperature in extruder (5) of the special-purpose material for spinning-stage polyetheretherketoneresin resin after the dried, the melt material bar of extruding through porous spinnerets (8) flows out the cooling of delaying time through the hot path (9) at distance spinnerets 0.1～15cm place again under 200～330 ℃ of temperature;
B) the melt material bar that flows out through hot path leads the oiling device (10) into bottom, hot path rapidly, leads (11) in the annular blowing device again, and the blowing temperature is 20～120 ℃, cools off, and obtains polyether-ether-ketone multifilament (15) through beaming device (13);
C) polyether-ether-ketone multifilament (15) leads into the multifilament batching apparatus through the guide roller (14) of beaming device (13) bottom, and the multifilament speed of wrap is 80～200m/min, the polyether-ether-ketone precursor that is not stretched;
D) the polyether-ether-ketone precursor (19) that will not stretch places (18) on the original silk rack, and precursor is imported the hot-stretch device, and the temperature that thermal potential is stretched is 190～260 ℃, and draw ratio is 2～3.5: 1;
E) will import loose calibrator through the polyetheretherketonefiber fiber of hot-stretch again, the temperature of loose typing is 250～320 ℃, and loose typing ratio is 0.8～0.98: 1, then the polyetheretherketonefiber fiber that obtains is wrapped in (23) on the yarn wind-up device.
2. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: extruder (5) adopts four districts heating (4), and afterwards a thermal treatment zone is higher 10～20 ℃ than the temperature of the last thermal treatment zone.
3. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: be provided with measuring pump (6) in the back of extruder (5), below measuring pump (6), the front of porous spinnerets (8) is provided with screen pack (7), the temperature of measuring pump (6) casing is higher 10～20 ℃ than extruder final heating area temperature, and the polyether-ether-ketone resin melt is quantitatively extruded through filter screen (7) and porous spinnerets (8) under the effect of measuring pump (6).
4. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: spinnerets (8) is 4～30 holes, thereby makes spun silk be multifilament, radical is 4～30.
5. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: in the annular blowing device (11) that install bottom, hot path (9), blowing direction becomes 45～135 degree angles with spray silk direction, and the blowing temperature is 60～120 ℃.
6. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: special-purpose material for spinning-stage polyetheretherketoneresin resin carries out pre-dried before the fusion drawn typing, baking temperature is 130～150 ℃, and the time is 3～12 hours.
7. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: the multifilament batching apparatus is made up of guide roller (14), coiling core pipe (16) and speed governing up-coiler (17), and winding speed is realized by speed governing up-coiler (17) control coiling core pipe (16).
8. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: the polyether-ether-ketone multifilament that is wrapped on the coiling core pipe (16) is 20～30 ℃ in temperature, humidity is 70～80% the interior quiet weighing apparatus 8～12h that sets level of air-conditioned room, carries out the hot-stretch typing again.
9. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: the drawing-off dish (20,21,22) that 3 Controllable Temperature are set in the original silk rack back, drawing-off dish (20,21) is formed fiber draw unit, and drawing-off dish (21,22) is formed the loose calibrator of fiber.
10. the melt spinning hot-stretch of polyetheretherketonefiber fiber as claimed in claim 1 typing preparation method, it is characterized in that: special-purpose material for spinning-stage polyetheretherketoneresin resin presses each component and 100wt% calculates, contain 90.0～100.0wt% polyether-ether-ketone resin, 0～3.0wt% high-temperature lubricant and 0～10.0wt% poly aromatic ether ketone liquid crystal copolymer.
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| US4992485A (en) * | 1988-10-11 | 1991-02-12 | The Dow Chemical Company | Microporous peek membranes and the preparation thereof |
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