CN1155303A - Process of making polybenzazole staple and fibers - Google Patents
Process of making polybenzazole staple and fibers Download PDFInfo
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- CN1155303A CN1155303A CN 95194544 CN95194544A CN1155303A CN 1155303 A CN1155303 A CN 1155303A CN 95194544 CN95194544 CN 95194544 CN 95194544 A CN95194544 A CN 95194544A CN 1155303 A CN1155303 A CN 1155303A
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Abstract
A process for the preparation of polybenzazole filaments which includes extruding filaments from a spinneret (1) having at least 100 holes, which are arranged to form an annular pattern (2) around the center of the spinneret (1), the center and at least two radial sections (3) of the spinneret (1) having no holes and an average width which is at least 3 times the minimum pitch of the holes, and drawing the filaments through a quench chamber while providing a substantially radial gas flow therein across the spinneret (1) from at least two different directions.
Description
The present invention relates to a kind of method for preparing polybenzoxazole or polybenzothiozole long filament and fiber.
Fiber by polybenzoxazole (PBO) and polybenzothiozole (PBT) (hereinafter referred to as PBZ or polybenzoxazole base polymer) preparation prepares in order to following method: at first the solution (polymer " spinning solution ") of polybenzoxazole base polymer in inorganic acid is extruded by die head or spinnerets and made the spinning solution long filament.Then the spinning solution long filament is stretched by the air gap, in the bath of the mixture that contains water or water and inorganic acid, wash, dry then.If extrude a plurality of long filaments simultaneously, can be before washing step, in the step or after the step a plurality of long filaments are merged into multifilament fiber.
When the long filament of polybenzole kind spinning solution is extruded; because the tensile viscosity that spinning solution is high, the rapid cooling of long filament and long filament of extruding at the spinnerets edge and the long filament cooldown rate of extruding at the spinnerets center is different; when long filament stretches by the air gap, usually can cause filament breakage.Though by adopting slower spinning speed and/or lower hole density being arranged on spinnerets, can alleviate the problem of stability of spinning process to a certain extent, still from the viewpoint of productivity ratio or equipment design, these methods usually are undesirable.Because more wish the long filament than minor diameter, larger-diameter long filament makes with the spinnerets that big spinneret orifice is arranged usually, may need to significantly improve the recently abundant elongate filaments of spin-drawing, to produce the long filament than minor diameter, so also may make filament breakage.
In addition, though can improve the stability of spinning production line by the spinneret orifice number (hole density hereinafter referred to as) on each spinnerets of minimizing, but in order to spin multiplicity of filaments continuously from single spinneret, the essential size that improves the spinnerets number of each spinneret or improve spinnerets.But such device structure may be undesirable.
US5294 390 and 5385702 discloses by partially enclosed air gap and has extruded the method that polybenzazole staple improves spinning production line stability, has air communication to cross the air gap, so that cooling off long filament under the even temperature relatively.Though this method has improved the stability of spinning production line, still wish further to improve the method for stability of spinning process and further improve long filament number that each spinneret extrudes, the method for the spinning production line that keeps relative stability again simultaneously.
On the one hand, the present invention relates to a kind of method for preparing polybenzazole staple, this method comprises that (a) extrudes long filament from the spinnerets that has 100 spinneret orifices at least, spinneret orifice circularizes around the spinnerets central array, the central authorities of spinnerets and at least two radial portions do not have spinneret orifice, and their mean breadth is at least about 3 times of spinneret orifice minimum spacing; And, send into from two different directions at least simultaneously and cross spinnerets radially air-flow basically (b) by the quench chamber elongate filaments.
Second aspect, the present invention relates to a kind of method for preparing polybenzazole staple, this method comprises that (a) extrudes long filament from the spinnerets that has 100 spray line holes at least, spinneret orifice circularizes around the spinnerets central array, the no spinneret orifice of central authorities, its mean breadth is at least about 3 times of spinneret orifice minimum spacing; And, send into basically radially air-flow from two different directions at least simultaneously by long filament (b) by the quench chamber elongate filaments.
Have now found that method of the present invention provides such method for preparing polybenzazole staple and fiber: polybenzazole staple and fiber can spin from the spinning die head that quite high spinneret orifice density is arranged, the spinning that can keep quite stable again simultaneously.The stability of spinning is reduced to minimum thereby efficient is higher by making the broken string number, guarantees the uniformity of elongate filaments, and it makes people can optimize the cooling condition of long filament, can improve the tensile strength and the tensile modulus of long filament.Improving through the air flow penetrability between the long filament behind the spinnerets, the cooling of single thread and drawing-down process become more even, and the method for the application of the invention makes spinning process stable.From the following description, these advantages and some other advantage will become clearer.
Fig. 1 illustrates an example of the spinnerets spinneret orifice arrangement pattern of the method that is used for first aspect present invention.Refer now to Fig. 1, it shows spinnerets (1), and spinnerets top is spinneret orifice (2), and three groups of spinneret orifices are separated from each other by the radial portion on the spinnerets (3), and radial portion (3) does not have spinneret orifice, and its width is (W).Fig. 2 illustrates an example of the spinnerets spinneret orifice arrangement pattern of the method that is used for second aspect present invention.
The polybenzazole staple that is used for the inventive method can make by the spinning solution spinning that contains the polybenzoxazole base polymer." polybenzole kind " used herein refers to polybenzoxazole (PBO) homopolymers, polybenzothiozole (PBT) homopolymers, and random, the gradual change (sequential) of PBO and PBT or block copolymer.Random, the gradual change or the block copolymer of polybenzoxazole, polybenzothiozole and they are for example open in following patent: US4703103 (on October 27th, 1987, Wolfe etc.), " liquid-crystalline polymer composition, method and product "; US 4533692 (on August 6th, 1985), " liquid-crystalline polymer composition, method and product "; US 4533724 (on August 6th, 1985), " poly-(2, the 6-benzothiazole) liquid-crystal composition, method and product "; US4533693 (on August 6th, 1985), " liquid-crystalline polymer composition, method and product "; US4539567 (November 16 nineteen eighty-two, Evers), " hinge that thermal oxide is stable to benzene and two oxazoles with to benzo dithiazole polymer "; And US4578432 (on March 25th, 1986, Tsai), " method for preparing the heterocycle block copolymer ".
The preferred construction unit of selecting like this in the PBZ polymer is so that polymer is a lyotropic liquid crystal.Preferred monomeric unit is represented with following formula I～VIII.Polymer more preferably is made up of the monomeric unit that is selected from following explanation basically, most preferably is made up of suitable-polybenzoxazole, anti--polybenzoxazole or anti--polybenzothiozole basically.
Suitable-polybenzoxazole gathers (benzo (1,2-d:5,4-d ') Er oxazole-2,6-two bases-1,4-phenylene)
Instead-poly-(benzo (1,2-d:5,4-d ') Er oxazole-2,6-two bases-1,4-phenylene) of polybenzoxazole
Instead-polybenzothiozole
Along polybenzothiozole
AB-PBO
Poly-(2, the 5-benzoxazole)
Poly-(2, the 5-benzothiazole)
AB-PBO
Poly-(2, the 6-benzoxazole) and
Poly-(2, the 6-benzothiazole)
Available known method synthetic polybenzoxazole base polymer or copolymer or the spinning solution that is fit to, for example following patent disclosure: US4533693 (on August 6th, 1985, Wolfe etc.); US4772678 (on September 20th, 1988, Sybert etc.); (on July 11st, 1989 is Harris) with US 5089591 (on February 18th, 1992, Gregory etc.) for US 4847350.Put it briefly, these methods comprise, with the monomer that is fit in non-oxide and acid (sour solvent) dehydration, under nonoxidizing atmosphere, react under violent mixing and high shear and under suitable temperature, described temperature rises at least about 190 ℃ from being not more than about 120 ℃ of stepwises or orthoscopic.For preparation PBZ polymer spun silk stock solution, suitable solvent comprises cresols and non-oxide acid.The sour solvent that is fit to comprises polyphosphoric acid, methanesulfonic acid and high-concentration sulfuric acid or its mixture.Preferably, solvent acid is polyphosphoric acid or methanesulfonic acid, and polyphosphoric acid most preferably.
The concentration of polymer in solvent is preferably at least about 7% (weight), more preferably at least about 10% (weight), most preferably at least about 14% (weight).Maximum concentration is limited by some actual operation factors, as the dissolubility of polymer and the viscosity of spinning solution etc.The concentration of polymer is no more than 30% (weight) usually, preferably is not more than about 20% (weight).Also can add oxidation retarder, the agent of frosting, colouring agent and antistatic agent in the spinning solution.
These PBZ with the form that is dissolved in the spinning solution in the polyphosphoric acid directly or separately use the dry-jet wet spinning spinning.The PBZ spinning solution preferably filters by the porous plate that 1～5 millimeter hole of many diameters is arranged.Its preferred space by the so-called melt pool (meltpool) that constitutes by the porous plate and the spinning nozzle back side subsequently, and textile material or bondedfibre fabric by the metal fibre that wherein contains.Spinning solution is then by there being the spinnerets spinning in many holes of arranging by circular, grid shape or trilobal cross.The density of the arrangement of spinneret orifice and spinneret orifice can influence gas and flows through the long filament of more close source of the gas and reach ability away from the long filament of source of the gas on spinnerets.
Fig. 1 explanation can be used for an example of the spinnerets of first aspect present invention method.As shown in the drawing, the hole of spinning nozzle is divided into several groups, and they are not had several districts of spinneret orifice to be separated from each other on the spinnerets.In two methods of the present invention, the spinneret orifice density on the spinnerets preferably surpass at least 2.0 holes/centimetre
2, more preferably at least about 4.0 holes/centimetre
2, most preferably at least about 6.0 holes/centimetre
2, but preferably less than about 10.0 holes/centimetre
2(press the planimeter of hole area on the spinnerets, it is also referred to as " effective area ").Usually, from the viewpoint of productivity ratio, higher spinneret orifice density is preferred, though when spinneret orifice density increases, more be difficult to make the long filament of extruding to contact with even velocity with refrigerating gas and fully cool off long filament.
In the method for a first aspect of the present invention, spinnerets constitutes like this, so that spinneret orifice is divided at least two groups, and more preferably at least three groups.The group number is preferably less than 10, because there is not the space on the required spinnerets in the district of spinneret orifice can reduce the available space of spinneret orifice on the spinnerets.Pattern to the spinneret orifice group of separating has no particular limits, but the preferred center of spinnerets relatively is radial symmetric.Preferably, in the method aspect two of the present invention, do not have the width of the radial portion of spinneret orifice and central area to be at least about 5 millimeters and on the spinnerets, be more preferably less than about 10 millimeters less than about 50 millimeters; Perhaps preferably at least about 3 times to the minimum spacing of spinneret orifice with less than the minimum spacing of about 30 times of spinneret orifices.
Fig. 2 explanation is used for the spinnerets of the method for second aspect present invention.In a second aspect of the present invention, be the zone that does not have spinneret orifice in the central authorities of spinnerets, and spinneret orifice need not be divided into several districts.An advantage of this one side method of the present invention is, in case spinning condition is under given pitch of holes, (outside of effective area is to the distance of effective area inboard to given long filament radial width, part is determined by the width of spinnerets middle section) optimised, just can under substantially the same spinning condition, design and the spinnerets that utilizes the different sizes that different number spinneret orifices are arranged, as long as the spinneret orifice on the spinnerets keeps this given radial width.Term used herein " annular " instigates spinneret orifice to be arranged on spinnerets, reserves the space of atresia in the central authorities of arranging.Fig. 2 illustrates annular grid pattern.
The spinning solution long filament of extruding by spinnerets makes them be cooled to be lower than the solidification temperature of spinning solution by the air gap, and sends in the washing bath that contains suitable cleaning solution.When the long filament of extruding from spinnerets when going out spinnerets, preferred at first by quench chamber around long filament.Though the length of quench chamber is chosen wantonly, preferably can be enough to provide the length of relative stationary temperature atmosphere for initial stretching from spinnerets, for example cross flowing of long filament by inert gas, make the temperature in the quench chamber remain on 0～100 ℃.One denier filament leaves quench chamber, and it just can be exposed under the atmospheric conditions, until it solidifies.The length of quench chamber is preferably 2～120 centimetres, but also can be longer.
Air-flow passes long filament from two different directions at least.Preferably, use a plurality of gas nozzles to make air-flow pass the radial component of long filament from a plurality of directions on demand.On the other hand, can use a series of dividing plates to change wherein airflow direction in quench chamber, perhaps also can use the pressurized equipment that screen cloth or filter be arranged around long filament, it makes homodisperse air communication cross the radial portion of long filament.Gas can produce from the outside that long filament is arranged, and also can arrange middle source of the gas generation from being installed in long filament.Though do not plan to be subjected to any restriction, but just cool off all long filaments, make the easier stability that all long filaments are optimized and improved spinning production line of chilling temperature with uniform speed, can think gas from many directions around the long filament make long filament radially chilling wish most.When gas passed through the radial component of long filament arrangement, it constantly passed the gap of long filament.The temperature of gas more preferably at least about 40 ℃, most preferably at least about 50 ℃, but preferably is not more than about 100 ℃ preferably at least about 30 ℃, more preferably no more than about 90 ℃, most preferably is not more than about 80 ℃.
In the multistep washing method, be that curing groove, the multistep water that makes long filament pass through flared type is inhaled silk device or other vertical groove as the method that makes things convenient for of the washing long filament of initial washing step.After this, long filament can further wash in the groove that uses the washing roller.Long filament is by behind first sink, and they stride across a live-roller at least.Along with the dawn number of long filament attenuates, can guarantee that in the air gap the maximum spin-draw ratio of continous-stable spinning descends.Can under greater than 200 meters/minute speed, make 1.5 denier filaments stablize spinning with method of the present invention.The average dawn number (dpf) of every threads preferably at least about 1.5 less than about 3.5.
Long filament washs being enough to preferably to remove under the condition of the solvent acid that exists in long filament at least about 98.0% (weight) subsequently, more preferably at least about 99% (weight), most preferably at least about 99.5% (weight).The cleaning solution that is fit to comprises that any is not the liquid of solvent to polymer, and it can dilute the sour solvent in the spinning solution long filament.The example of cleaning solution comprises the mixture of the solvent that water, methyl alcohol, acetone and water and PBZ spinning solution contain, and they can be liquid form, also can be vapor form.Preferably, spinning solution prepares with polyphosphoric acid, and cleaning solution is the mixture of water and polyphosphoric acid.In addition, the washing of long filament can be undertaken by multistep processes.
The available subsequently suitable drying means drying of long filament through washing.In addition, also can before or after drying, carry out the spinning arrangement, so that prevent the long filament mechanical damage to long filament.In order to improve the tensile modulus of long filament, can under greater than 300 ℃ temperature, heat-treat, more preferably greater than 450 ℃, but less than 650 ℃.
Method of the present invention preferably is at least about under 200 meters/minute in terminal velocity carries out, more preferably at least about 400 meters/minute, most preferably at least about 600 meters/minute.
In the methods of the invention the long filament of Shi Yonging can be in the methods of the invention any one and other long filament combination, make multifilament fiber.But, preferably before first sink a bit or in groove, make the long filament combination.In addition, when while spinning multiplicity of filaments, can behind initial washing step, they be divided into several groups, as the method for preparing by same spinnerets more than one multifilament fiber with thread guide.
The tensile strength of the long filament of producing with the inventive method is preferably at least about (600000 pounds/inch of 600Ksi
2), more preferably at least about (800000 pounds/inch of 800Ksi
2).The tensile modulus of the long filament of producing with the inventive method is preferably at least about 20Msi (30 * 10
6Pound/inch
2), more preferably at least about 30Msi.
Embodiment
Following examples are used for illustrating the present invention, but should not think limitation of the present invention by any way.Obtain the listed data of Table I with the physical property of following measurement long filament and fiber and the method for stability of spinning process.
The method of intrinsic viscosity
Be dissolved in methanesulfonic acid by the PBZ with variable concentrations, the method that is extrapolated to zero-dose then obtains the reduced viscosity under 30 ℃.
Filament denier
Fiber sample was kept 18 hours for 65 ± 2% times in 20 ± 2 ℃ of temperature, relative humidity, get 90 meters samples, measure its weight, the weight that records is converted into 9000 meters weight, obtain the dawn number of fiber.Filament denier can be calculated divided by intrafascicular monofilament number by fibre bundle dawn number.
Measure the method for maximum spinning/draw ratio
Get silvalin with carry-over pinch rolls, make it not contact cleaning solution, by increasing the peripheral speed that given pace improves described roller, spray the ratio of linear speed (Vo) in maximum spinning speed (Vw) when maximum spinning/draw ratio is defined as fiber and fracture occurs and the hole that obtains by single hole spray volume and bore dia, i.e. Vw/Vo.
Estimate the method for stability of spinning process
Under 200 meters/minute, carry out spinning,, then it is converted into 8 hours fracture number until obtain reliable rate of fiber breakage on the statistics.
Measure the method for lousiness (long filament breaks)
Make the winding up roller loose winding of the fiber of washing and drying with 100 meters/minute speed, and,, then it is converted into the long filament rupture rate of every ten thousand metres up to obtaining statistically number reliably with photoelectric tube type spilt filament detection instrument counting lousiness.
Measure the method for tensile strength, tensile modulus and elongation at break
With test method No.JIS L1013 (1981), 5 centimetres of grip separation, draw speed 100%/minute and n=30 under, the Tensilon that produces with Orientech (Inc.) company
TMThe measured value of machine obtains average tensile strength, tensile modulus and elongation at break.
Embodiment 1
With a part of two hydrochloric acid 4,6-diaminostilbene, 3-Benzenediol (50.0 grams, 0.235 mole) and 200 gram polyphosphoric acid (P
2O
5Content is 83.3% (weight)) in nitrogen current, 40 ℃ stirred 12 hours.The temperature of mixture is raised to 60 ℃, and under the decompression of about 50 millimetress of mercury, removes hydrochloric acid.Terephthalic acid (TPA) (39.0 gram, 0.236 mole) and phosphorus pentoxide (103 restrain) are added in the said mixture, and in nitrogen current, 60 ℃ of polymerizations 8 hours, 120 ℃ of polymerizations 9 hours, 150 ℃ of polymerizations 15 hours with 180 ℃ of polymerizations 24 hours.The spinning solution that the PBZ polymer solution that so makes is used as spinning.In blender and mixing, obtain polymer beads sample by liquor sample and water, measure the inherent viscosity of polymer through washing.Polymer beads is dissolved in the methanesulfonic acid, measures viscosity down at 215 ℃, inherent viscosity (11) is 30.5dl/g.
The concentration of polymer is 14.0% (weight) in the spinning solution, use phosphorus pentoxide as the situation of polyphosphoric acid under the concentration of solvent be 86.0% (weight).With Bitruder make spinning solution mediate and the degassing after, with gear pump it is sent in the spinneret.It is by particles filled layer of 50 millimeters of the bed thickness is made up of inorganic substances (average particulate diameter and average aspect ratio change) at the spinneret place, by the distribution plate of 2 millimeters holes of many diameters (by frame form punching) is arranged, then by make by the metal fibre interlacement of 10 millimeters of diameters, be 2.5% superimposed layer greater than the transmitance of 15 mm granules.
Under 160 ℃ of temperature, ejection speed 64.2 gram/minute, with spinning solution by such spinnerets spinning: spinneret orifice density be 4.8 holes/centimetre
2, the thin spinneret orifice that 284 diameters are 0.20 millimeter, hole length is 0.20 meter, and inlet angle is 20 degree, and using width (W) as shown in Figure 1 is 8.6 millimeters be distinguished into several groups.It is about 500 that the number of spinneret orifice preferably is at least, more preferably at least about 1000, most preferably at least about 2500.
Then, make spun long filament by send into and pass the quench chamber of the air flow of long filament at least from both direction, importing is installed in the flared type coagulation devices of spinning-nozzle lower face 35 centimeters, wherein has temperature to remain on 22 ± 2 ℃ 20% polyphosphoric acid aqueous solution circulation.In addition, spun fiber is rolled being installed on the roller that exports below the described extraction tank, the direction of motion that changes filamental thread is carried out the extraction and the washing of the polyphosphoric acid in the filamental thread, roll on roller by filamental thread, reduce spinning tension with being installed on the filamental thread that near the described roller spray appliance is sprayed on water motion simultaneously.Make fiber pass through the hot air circulate drier then, its water content is dropped to below 2.0% (weight), twine with 200 meters/minute speed again.The result lists down Table I in.
Embodiment 2-11
The method of describing with example I prepares fiber, and difference is: for embodiment 2 and 3, the orifice diameter on the spinnerets is 0.20 millimeter, and hole length is 0.20 millimeter, and the inlet angle of spinneret orifice is 20 degree, hole density be respectively 3.4 and 4.0 holes/centimetre
2For embodiment profit and 5, divide in groups interval wide (W) to become 6.5 millimeters (embodiment 4) and 9.9 millimeters (embodiment 5) spinneret orifice.In embodiment 6～8, spinnerets has 2,6 and 8 groups of spinneret orifices respectively.In embodiment 9～11, the single hole spray volume is 0.69 Grams Per Minute, and the spinning solution long filament of ejection cools off in mean air flow speed is the air gap of air-flow of 55～95 ℃ of 0.7 meter per seconds, temperature.The result lists Table I and Table II in.
Table I
| Experiment # | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Spinneret orifice group number | ????- | ????3 | ????3 | ????3 | ????3 | ????3 |
| The width of subregion | Millimeter | ????8.6 | ????8.6 | ????8.6 | ????6.5 | ????9.9 |
| The effective diameter of spinnerets | Millimeter | ????95 | ????95 | ????95 | ????95 | ????95 |
| Spinneret orifice density | The hole/centimetre 2 | ????4.8 | ????3.4 | ????4.0 | ????4.6 | ????4.9 |
| The spinneret orifice number | ????- | ????284 | ????200 | ????234 | ????284 | ????284 |
| Every hole extrusion capacity | Grams Per Minute | ????0.23 | ????0.23 | ????0.23 | ????0.23 | ????0.23 |
| Maximum spinning speed | Rice/minute | ????246 | ????246 | ????246 | ????247 | ????246 |
| Spinning one draw ratio under maximum spinning speed | ????- | ????67 | ????67 | ????67 | ????67 | ????67 |
| The dawn number of each long filament under maximum spinning speed | ????- | ????1.16 | ????1.16 | ????1.16 | ????1.15 | ????1.16 |
| 8 hours broken fiber number under maximum spinning speed | ????1 | ????0 | ????1 | ????0 | ????2 | |
| Lousiness under maximum spinning speed | / ten thousand metres | ????1.3 | ????0.8 | ????1.3 | ????1.1 | ????1.1 |
| Fiber Denier | Dawn | ????403 | ????284 | ????332 | ????403 | ????403 |
| Each filament denier | ????- | ????1.42 | ????1.42 | ????1.42 | ????1.42 | ????1.42 |
| Tensile strength | ????GPa | ????6.2 | ????6.1 | ????6.3 | ????6.2 | ????6.1 |
| Elongation at break | ????％ | ????3.6 | ????3.6 | ????3.6 | ????3.6 | ????3.6 |
| Tensile modulus | ????GPa | ????217 | ????215 | ????219 | ????214 | ????212 |
Table II
| Experiment # | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | |
| Spinneret orifice group number | ????- | ????2 | ????6 | ????8 | ????3 | ????3 | ????3 |
| The width of subregion | Millimeter | ????8.6 | ????8.6 | ????8.6 | ????8.6 | ????8.6 | ????8.6 |
| The effective diameter of spinnerets | Millimeter | ????95 | ????106 | ????112 | ????95 | ????95 | ????95 |
| Spinneret orifice density | The hole/centimetre 2 | ????4.5 | ????4.5 | ????4.5 | ????4.8 | ????4.8 | ????4.8 |
| The spinneret orifice number | ????- | ????284 | ????284 | ????284 | ????284 | ????284 | ????284 |
| Every hole extrusion capacity | Grams Per Minute | ????0.23 | ????0.23 | ????0.23 | ????0.68 | ????0.68 | ????0.68 |
| Maximum spinning speed | Rice/minute | ????246 | ????245 | ????246 | ????731 | ????738 | ????730 |
| Spinning one draw ratio under maximum spinning speed | ????- | ????67 | ????66 | ????67 | ????66 | ????67 | ????66 |
| The dawn number of each long filament under maximum spinning speed | ????- | ????1.16 | ????1.16 | ????1.16 | ????1.17 | ????1.16 | ????1.17 |
| 8 hours broken fiber number under maximum spinning speed | ????1.1 | ????1.2 | ????2.5 | ????1 | ????0 | ????1 | |
| Lousiness under maximum spinning speed | / ten thousand metres | ????1.7 | ????1.8 | ????3.8 | ????1.3 | ????1.0 | ????1.2 |
| Fiber Denier | Dawn | ????403 | ????403 | ????403 | ????403 | ????403 | ????403 |
| Each filament denier | ????- | ????1.42 | ????1.42 | ????1.42 | ????1.42 | ????1.42 | ????1.42 |
| Tensile strength | ????GPa | ????6.2 | ????6.2 | ????6.0 | ????6.2 | ????6.2 | ????6.1 |
| Elongation at break | ????％ | ????3.6 | ????3.6 | ????3.6 | ????3.6 | ????3.7 | ????3.6 |
| Tensile modulus | ????GPa | ????217 | ????214 | ????212 | ????219 | ????220 | ????215 |
Claims (11)
1. method for preparing polybenzazole staple, this method comprises that (a) extrudes long filament from the spinnerets that has 100 spinneret orifices at least, spinneret orifice around the spinnerets central array circlewise, the central authorities of spinnerets and at least two radial portions do not have spinneret orifice, and their mean breadth is at least about 3 times of spinneret orifice minimum spacing; And, send into from two different directions at least simultaneously and cross spinnerets radially air-flow basically (b) by the quench chamber elongate filaments.
2. according to the process of claim 1 wherein that spinnerets has at least 500 spinneret orifices.
3. according to the process of claim 1 wherein that spinnerets has at least 1000 spinneret orifices.
According to the process of claim 1 wherein the hole density of spinnerets be at least about 4.0 holes/centimetre
2
According to the process of claim 1 wherein the hole density of spinnerets be at least about 6.0 holes/centimetre
2
6. method for preparing polybenzazole staple, this method comprises that (a) extrudes long filament from the spinnerets that has 100 spinneret orifices at least, spinneret orifice circularizes around the spinnerets central array, the no spinneret orifice of central authorities, and its mean breadth is at least about 3 times of spinneret orifice minimum spacing; And, send into basically radially air-flow from two different directions at least simultaneously by long filament (b) by the quench chamber elongate filaments.
7. according to the method for claim 6, wherein spinnerets has at least 500 spinneret orifices.
8. according to the method for claim 6, wherein spinnerets has at least 1000 spinneret orifices.
9. according to the method for claim 6, wherein the hole density of spinnerets be at least about 4.0 holes/centimetre
2
10. according to the method for claim 6, wherein the hole density of spinnerets be at least about 6.0 holes/centimetre
2
11. method for preparing polybenzazole staple, this method comprises, extrude long filament from the spinnerets that has 100 spinneret orifices at least, spinneret orifice circularizes around the central array of spinnerets, the central authorities of spinnerets and at least two radial portions do not have spinneret orifice, and its mean breadth is at least about 3 times of spinneret orifice minimum spacing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95194544 CN1155303A (en) | 1994-08-12 | 1995-08-10 | Process of making polybenzazole staple and fibers |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP190635/94 | 1994-08-12 | ||
| CN 95194544 CN1155303A (en) | 1994-08-12 | 1995-08-10 | Process of making polybenzazole staple and fibers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1155303A true CN1155303A (en) | 1997-07-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95194544 Pending CN1155303A (en) | 1994-08-12 | 1995-08-10 | Process of making polybenzazole staple and fibers |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1155303A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101238248B (en) * | 2005-03-28 | 2011-07-27 | 纳幕尔杜邦公司 | Process for the production of polyarenazole yarn |
| CN102628192A (en) * | 2012-04-06 | 2012-08-08 | 浙江恒逸高新材料有限公司 | Production method for porous fine denier polyester filament |
| CN115434021A (en) * | 2022-10-08 | 2022-12-06 | 无锡市兴盛新材料科技有限公司 | Short fiber direct spinning process for optimizing cooling forming |
-
1995
- 1995-08-10 CN CN 95194544 patent/CN1155303A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101238248B (en) * | 2005-03-28 | 2011-07-27 | 纳幕尔杜邦公司 | Process for the production of polyarenazole yarn |
| CN102628192A (en) * | 2012-04-06 | 2012-08-08 | 浙江恒逸高新材料有限公司 | Production method for porous fine denier polyester filament |
| CN102628192B (en) * | 2012-04-06 | 2015-02-25 | 浙江恒逸高新材料有限公司 | Production method for porous fine denier polyester filament |
| CN115434021A (en) * | 2022-10-08 | 2022-12-06 | 无锡市兴盛新材料科技有限公司 | Short fiber direct spinning process for optimizing cooling forming |
| CN115434021B (en) * | 2022-10-08 | 2024-01-05 | 无锡市兴盛新材料科技有限公司 | Short fiber direct spinning process for optimizing cooling forming |
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