AROMATIC POLYETHERKETONE FIBER PRODUCT AND PROCESS

Abstract: Filaments are produced from polymers having an inhe­ rent viscosity of at least 0.7 measured in concentrated sulfuric acid and containing in the polymer chain at least 50 per cent of the repeating units : by melting the polymer and heating the melt to a tempera­ ture of from about 20°C to about 80°C above the melting point of the polymer, passing the melt through a filter pack having a filtering area of at least about 8in² (51.5 cm²) and a total volume of at least about 1.2 in³ (19.5 cm³) per pound of polymer extruded per hour, and containing inert, irregularly shaped particles having a mesh size of about 25 to 140 to provide a pressure drop at least about 800 psig (57273 g/cm²), extruding the melt through spinning openings of desired shape to form filaments. A preferred embodiment also includes the step of passing the filaments immediately upon extrusion through a heating zone maintained at a temperature of about 200 to 320°C and having a length of about 3 to 12 inches (7.6 to 30.5 cm). The process is capable of producing fibers and yarns having a dpf of about 2.8 to 100, a tenacity of about 1 to 4.5 grams per denier, an elongation at break of about 15 to 200 percent and modulus of about 20 to 80 grams per denier.

Description: This invention relates to fibers and yarns of a certain class of aromatic polyetherketones and their production by a melt spinning process. BACKGROUND OF THE INVENTION The polymers contemplated by this invention are disclosed in the U.S. patents Nos.4,320,224; 4,360,630; and 4,446,294. These crystalline, linear polymers contain in the polymer chain at least 50 percent of the following repeating unit (hereinafter referred to as "repeating unit I"): The polymers may be composed solely of repeating units I or may contain other repeating units as hereinafter defined and they have inherent viscosities IV (measured at 25°C in a solution of the polymer in concentrated sulphuric acid of density 1.84 g cm⁻³, said solution containing 0.1 g of polymer per 100 cm³ of solution) of at least 0.7. These polymers are exceptionally useful in that they possess excellent mechanical and electrical properties, coupled with outstanding thermal and combustion characteristics. They also show resistance to a very wide range of solvents and proprietary fluids. They are thus very suitable in applications where the service conditions are too demanding for the more established, high performance polymers and in particular where the polymers are liable to high service temperatures. In view of the foregoing desirable properties of these particular aromatic polyetherketones, it would be advantageous if they could be easily formed into filaments, fibers and yarns since the latter products could then be made for example into knitted, woven, and non-woven fabrics, fiberfill and insulation products suitable for applications utilizing their excellent physical and chemical properties. However, the same combination of properties which would make filaments, fibers and yarns made from these polymers very desirable in various applications, e.g. heat and solvent resistance, also causes them to be very difficult to spin into such filaments, fibers and yarns. Thus, if it is attempted to melt spin these polymers into filaments in a conventional manner, the use of a relatively low spinning temperature results in a high melt viscosity which significantly reduces spinning stability due to high spinning pressures, clogging of the spinneret holes, uneven polymer coagulation and frequent filament rupture. On the other hand, unduly high spinning temperatures result in polymer degradation and cross-linking which cause void, gel and speck formation in the filaments and render them unsuitable for most uses. In view of these factors, successful spinning into filaments and yarns of the polymers contemplated by this invention is not easily accomplished. Although U.S. Patent Nos. 4,320,224, and 4,446,294 disclose broadly that polymers containing a major proportion of repeating unit I may be fabricated into any desired shape including fibers, they do not have any specific teaching of how such fibers may in fact be formed. Research Disclosure No. 21602 (April 1982) discloses that a sample of polyetheretherketone having the repeat unit -O-Ph-O-Ph-CO-Ph-, wherein Ph = p-phenylene, required an extrusion temperature of 420°C (nearly 80°C above the melting point of the polymer) in order to produce reasonably consistent and smooth spun yarn. US-A-4,359,501 discloses a fabric having machine direction and cross-machine direction threads interwoven with one another and finished into an endless belt, wherein certain of the threads are formed of a monofilament of a melt-extrudable polyetheretherketone having repeating units -Φ-O-Φ-CO-Φ-O- wherein Φ is p-phenylene. The monofilaments may be formed by extrusion through spinnerets having a 0.040 inch (1.02 mm) die hole. SUMMARY OF THE INVENTION In accordance with this invention, a linear aromatic polyetherketone comprising at least 50 percent of repeating unit I in the polymer chain and having an inherent viscosity (IV) of at least 0.7 as hereinbefore defined is melt spun at a temperature in the range of from 20°C above to 80°C above the melting point of the polymer, using a filter pack filtering area of at least 8 in² (51.6 cm²), preferably 15 to 25 in² (96.8 to 161.3 cm²) and a total volume of at least 1.2 in³ (19.7 cm³), preferably 1.6 to 2.3 in³ (26.2 to 37.7 cm³), per pound (0.45 kg) of polymer extruded per hour with a filtering medium of inert particles having numerous angles, indentations and/or irregularities and a mesh size of 25 to 140 (710 µm to 106 µm). The particles of filter medium may be for example "shattered metal", e.g. carbon steels and stainless steels, aluminium oxides and silicates, e.g. sold under the trademarks "Alundum" and "Bauxilite", ground ceramics and sand. The filter medium must be sufficient to provide a pressure drop of at least 800 psig (5516 kPa gauge), preferably 950 to 3000 psig (6550 to 20684 kPa gauge). Such a filter pack size and type of filter medium have been found to provide an adequate degree of shear necessary for stable spinning of the contemplated polymers to filaments of commercially acceptable deniers without an undesirably large increase in spinning pressure. In addition to the filter medium mentioned previously, it is in most instances desirable to employ a fine filter screen across the filtering area downstream of the filter for the purpose of separating specks and gels which get through the filter pack. Such a screen in general has openings of under 20 microns (µm), preferably in the range of 3 to 10 µm. In order to further maintain stable spinning in carrying out the process of the invention, it is preferable not to quench the extruded filaments, i.e. the filaments are cooled in non-circulating air at ambient temperatures and are not contacted with any forced draft of any gas cooler than the surroundings. Moreover, to maintain stable spinning, it is preferable to operate the process such that the extruded filaments converge within 15 to 50 inches (38.1 to 127 cm), preferably in the range of 20 to 30 inches (50.8 to 76.2 cm) of the spinneret. The process of this invention if carried out such that the filaments are extruded directly from the spinneret holes into non-circulating air at ambient temperatures is adequate for the formation of yarns of relatively higher dpf (denier per filament), e.g. up to 100. (1 denier = 1g per 9 km or about 0.1111 tex.) However, it may be difficult to use such a process for the production of yarns of relatively lower dpf,e.g. below about 15 dpf. The reason for this is that the polymer which is high melting rapidly solidifies as it is extruded into ambient conditions, and drawdown to relatively lower dpf's is severely limited. Thus, in accordance with another aspect of the invention, an improvement in the foregoing spinning process is provided whereby the extruded filaments are heated by passing them through a heating zone, e.g. a heated tube or shroud, immediately on being extruded through the spinneret holes. This prevents the filaments from solidifying too rapidly and allows for the drawdown of the filaments to deniers considerably lower than would otherwise be possible. If a heated tube is utilized to heat the filaments, it may be made of any material capable of withstanding the temperatures employed which will generally be in the range, for example, of about 200 to 320°C, preferably about 290 to 310°C. Such material may be, for example, metal, e.g. aluminium or steel, ceramic or glass. Any conventional heating means may be used, e.g. electrical heating elements, steam, hot liquid or gas etc. A specific heated tube assembly which may be used is an aluminium tube inclosed in a steel heater band. The diameter of the heating zone, e.g. the heated tube is generally the same as the spinneret, e.g. 1½ to 5 in. (3.8 to 12.7 cm), preferably about 3 to 4 ½ in. (7.6 to 11.4 cm) and the length is in the range,for example, of about 3 to 12 inches (7.6 to 30.5 cm), preferably about 5 to 8 inches (12.7 to 20.3 cm) and most preferably 6 inches (15.2 cm). The remaining conditions which may be utilized in the process are conventional for melt spinning and are not considered critical to the invention. Thus the polymer may be extruded through a spinneret plate containing, for example 10 to 100 holes each with a diameter in the range of about 0.009 to 0.013 inch (0.23 to 0.33 mm) to produce filaments which are taken up at a speed, for example of about 50 to over 1000 meters per minute, preferably about 70 to over 200 meters per minute if no heating zone is utilized downstream of the spinneret. The filaments produced may have a denier per filament, for example of about 2.8 to 100. If no heating zone is utilized on the downstream side of the spinneret, then the denier per filament is preferably about 15 to 100, more preferably about 15 to 40. If such a heating zone is utilized, the denier per filament is preferably about 2.8 to 40, more preferably about 2.8 to 15. The filaments may have a circular cross-section resulting from the use of circular spinneret holes, or may have any of various non-circular cross-sections resulting from the use of different non-circular spinneret hole shapes, e.g. multilobal cross-sections containing, for example, six lobes, produced by using star-shaped spinneret holes containing for example six protrusions. The fibers and yarns resulting from the process of this invention, and particularly when a heating zone is utilized on the downstream side of the spinneret, generally have a tenacity in the range of about 0.89 to 4.0 cN/dtex (1 to 4.5 grams per denier), an elongation at break of about 15 to 200 percent, a modulus of about 18 to 71 cN/dtex (20 to 80 grams per denier), and a birefringence in the range of about 0.025 to 0.220. The process of this invention when a heating zone is employed is particularly useful in the production of yarns having the foregoing mechanical properties and dpf's under 15, for example from about 2.8 to just under 15, e.g. from about 2.8 to 14.8. When no heating zone is employed on the downstream side of the spinneret, the fibers and yarns resulting from the process of this invention often have a tenacity in the range of about 0.89 to 1.78 cN/dtex (1 to 2 grams per denier), an elongation at break of about 50 to 160 percent and modulus of about 18 to 27 cN/dtex (20 to 30 grams per denier). The birefringence of such filaments may be in the range of about 0.025 to 0.150. The preferred polymers which may be formed into filaments in accordance with this invention consist solely of repeating unit I and have an IV of at least 0.7 measured in concentrated sulfuric acid as described previously. As disclosed in U.S. Patent No. 4,320,224 such polymers may be made by polycondensing hydroquinone and 4,4'-difluorobenzophenone with an alkali metal carbonate or bicarbonate (excluding the sole use of sodium carbonate or biocarbonate) in a solvent such as diphenyl sulfone. Part of the 4,4'-difluorobenzophenone e.g. up to 50 percent, may be replaced with 4,4'-dichlorobenzophenone or 4-chloro-4'fluorobenzophenone. These polymers consisting solely of repeating units I in the polymer chain generally have a melting point of about 335°C so that in carrying out the spinning process of the invention, the polymer melt is extruded at temperatures of about 355°C to about 415°C. Polymers containing up to 50 percent of repeating units other than repeating unit I are also contemplated and may be formed by replacing up to 50 mol percent of the hydroquinone in the monomer mixture with any of certain other dihydroxyphenols and up to 50 mol percent of the 4,4'-difluorobenzophenone with any or certain other aromatic dihalides. For example, up to 50 mol percent of the hydroquinone may be substituted with a dihydroxy phenol cocondensant of the formula: in which A is a direct link, oxygen, sulphur, -SO₂-, -CO-, or a divalent hydrocarbon radical. Examples of such bisphenols are: 4,4 -dihydroxybenzophene 4,4'-dihydroxydiphenylsulphone 2,2'-bis- (4-hydroxyphenyl) propane 4,4'-dihydroxybiphenyl. The substitution of part of the hydroquinone with any of the foregoing dihydroxy phenols causes the following repeating units (hereinafter referred to as "repeating unit II") to be present in the polymer chain interspersed with repeating unit I: Alternatively or in addition to the substitution of part of the hydroquinone with another dihydroxyphenol, up to 50 mol percent of the 4,4'-difluorbenzophenone may be replaced with one or more dihalide cocondensants of the formula: in which X and X', which may be the same or different, are halogen atoms and are ortho or para - preferably the latter - to the groups Q and Q'; and Q and Q', which may be the same or different, are -CO- or -SO₂-; Ar' is a divalent aromatic radical; and n is 0,1,2 or 3. The aromatic radical Ar' is preferably a divalent aromatic radical selected from phenylene, biphenylylene or terphenylylene. Particularly preferred dihalides have the formula: where m is 1,2 or 3. Examples of such dihalides include: 4,4-dichlorodiphenylsulphone 4,4-difluorodiphenylsulphone 4,4'-dichlorobenzophenone bis-4,4' -(4-chlorophenylsulphonyl) biphenyl bis-1,4- (4-chlorobenzoyl) benzene bis-1,4- (4-fluorobenzoyl) benzene 4-chloro-4' -fluorobenzophenone 4,4'-bis-(4-fluorobenzoyl)biphenyl 4,4'-bis-(4-chlorobenzoyl) biphenyl Although substitution of the 4,4-difluorobenzophenone with 4,4' -dichlorobenzophenone and/or 4-chloro-4' - fluorobenzophenone does not change the units of the polymer chain, it has been found that up to 50 mol percent of the difluoro compound may be so replaced without adverse effects and with consequent cost advantage. Substitution of part of the 4,4-difluorobenzophenone with any of the other specified dihalides causes the following units (hereinafter referred as "repeating unit III") to be present in the polymer chain. in which the oxygen atoms in the sub-units: are ortho or para to the groups Q and Q'. Where both dihydroxy phenol and dihalide (other than the dichloro- or chlorofluoro- benzophenone) cocondensants are employed, the polymer will contain, in addition to repeating units I, II and III, the following repeating units (hereinafter referred to as "repeating unit IV"): In the following examples tenacity and modulus are given in grams/denier. The corresponding S.I. unit is cN/dtex. 0.89 cN/dtex = 1 gram/denier. Example 1 Examples 1 and 2 illustrate the process of the invention without the employment of a heating zone on the downstream side of the spinneret. Filaments were produced in accordance with the process of this invention using spinning apparatus as depicted schematically in the Figure I. Polymer chip in an amount of 1.3 lb/hr (0.59 kg/hr.) with polymer chains consisting solely of repeating unit I having an inherent viscosity in concentrated sulfuric acid of 0.9 and prepared as described in Example 1 of U.S. Patent No. 4,320,224, was fed to closed hopper 1 under nitrogen or vacuum. From there, it passed into screw extruder 2 which was heated by electrical heater bands divided into three zones. The polymer which followed the path indicated by line 3 was heated to 246°C in the near section of the extruder, and melted and heated to 346°C and 363°C in the centre and front sections respectively. The melted polymer was then passed into the top of "block" i.e. spinning chamber, 4 from which it was passed to pump 5 (a standard Zenith gear pump) and back into block 4 which was surrounded by electrical heater bands. The polymer melt, heated in block 4 to about 382°C, was passed into filter pack 6 which contained shattered metal filtering medium 7 in which the particles had a mesh size of about 25 to 50 (710 µm to 300 µm). The filter pack had a filtering area of slightly over 20 in² (129 cm²) and a total filter volume of about 2.75 in³ (45.1 cm³) or 2.12 in³ (34.7 cm³) per pound of polymer extruded. The pressure drop of the polymer melt developed in the filter pack was about 1000 psig (6894 kPa gauge). At the start of spinning from filter pack 7, the polymer melt passed through screen 8 having openings less than 20 microns in size and thence through the 33 holes of spinneret 9 arranged in a circle in the spinneret plate. The holes each had a diameter of 0.0127 inch (0.32 mm) and a length of 0.019 inch (0.48 mm). Filaments 10 extruded from the spinneret were collected into a yarn at yarn guide 11 located about 24 inches (61 cm) below the spinneret. The yarn was taken up without quenching in 5 to 10 wraps around speed controlled take up roll 12 at a speed of about 165 meters per minute and was forwarded to a tension control winder (not shown). The resulting yarn had a dpf of 18.1, a tenacity of 1.64 grams/denier, an elongation at break of 86 percent, a modulus of 25.97 grams/denier, and a birefringence of 0.086. Example 2 The process of Example 1 was followed except that the yarn was taken up on roll 12 at a speed of about 195 meters per minute. The resulting yarn had a dpf of 15.0, a tenacity of 1.42 grams per denier, and elongation at break of 66 percent, a modulus of 25.01 grams per denier, and birefringence of 0.110. Examples 3 to 20 illustrate the process of this invention employing a heating zone in the form of a heated tube on the downstream side of the spinneret. Example 3 Filaments were produced in accordance with the process of this invention using spinning apparatus as depicted schematically in Figure II. Polymer chip in an amount of 3.05 lb/hr. (1.38 kg/hr.) with polymer chains consisting solely of repeating unit I having an IV in concentrated sulfuric acid of 0.9 and prepared as described in Example I of U.S. Patent No. 4,320,224, was fed to closed hopper I under nitrogen or vacuum. From there, it passed into screw extruder 2 which was heated by electrical heater bands divided into three zones. The polymer which followed the path indicated by line 3 was heated to 246°C in the near section of the extruder, and melted and heated to 346°C and 363°C in the centre and front sections respectively. The melted polymer was then passed into the top of "block" i.e. spinning chamber, 4 from which it was passed to pump 5 (a standard Zenith gear pump) and back into block 4 which was surrounded by electrical band heaters. The polymer melt, heated in block 4 to about 382°C, was passed into filter pack 6 which contained shattered metal filtering medium 7 in which the particles had a mesh size of about 25 to 50. The filter pack had a filtering area of over 20 in² (129 cm²) and a total filter volume of about 2.75 in³ (45.1 cm³). The pressure drop of the polymer melt developed in the filter pack was about 1000 psig (6894 kPa gauge). At the start of spinning from filter pack 7, the polymer melt passed through screen 8 having openings less than 20 µm in size and thence through the 33 holes of spinneret 9 arranged in a circle in the spinneret plate. The holes each had a diameter of 0.0127 inch (0.32 mm) and a length of 0.019 inch (0.48 mm). Filaments 10 extruded from the spinneret passed immediately through heated tube 11 which had the same diameter as the outside of the spinneret, i.e. 4 in (10.2 cm), a length of 6 in (15.2 cm). and was at a temperature of 200°C. After passing through heated tube 11, the filaments were collected into a yarn at yarn guide 12 located about 24 inches (61 cm) below the spinneret. The yarn was taken up without quenching in 5 to 10 wraps around take up rolls 12 at a speed of about 225 meters per minute and was forwarded to a winder (not shown). The resulting yarn and a dpf of 12.6 a tenacity of 1.66 grams/denier, an elongation at break of 72 percent and modulus of 27.86 grams/denier. Example 4 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 217°C and the yarn was taken up at a speed of 300 meters/min. The yarn had a dpf of 9.6, a tenacity of 1.59 grams/denier, an elongation at break of 65 percent and a modulus of 29.06 grams/denier. Example 5 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 212°C and the take-up speed of the yarn was 200 meters/min. The yarn had dpf of 13.9,a tenacity of 1.76 grams/denier, an elongation at break of 96 percent and a modulus of 25.69 grams/denier. Example 6 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 218°C and the yarn was taken up at a speed of 350 meters/min. The yarn had a dpf of 7.9, tenacity of 1.95 grams/denier, and elongation at break of 71 percent, and a modulus of 30.13 grams/denier. Example 7 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 218° and the yarn was taken up at a speed of 325 meters/min. The yarn had a dpf of 8.9, a tenacity of 1.97 grams/denier, an elongation at break of 78 percent,and a modulus of 29.86 grams/denier. Example 8 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 205°C and the yarn take-up speed was 400 meters/min. The yarn had a dpf of 5.0, a tenacity of 2.07 grams/denier, an elongation at break of 65 percent and a modulus of 34.62 grams/denier Example 9 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 300°C and the yarn was taken up at a speed of 510 meters/min. The yarn had a dpf of 5.7, a tenacity of 2.00 grams/denier, an elongation at break of 65 percent and a modulus of 30.95 grams/denier. Example 10 The procedure of Example 9 was followed except that the yarn taken-up speed was 550 meters/min. The yarn had a dpf of 4.8, a tenacity of 2.21 grams/denier, an elongation at break of 61 percent and a modulus of 33.97 grams/denier. Example 11 The procedure of Example 9 was followed except that the take-up speed was 606 meters/min. The yarn had a dpf of 4.5, a tenacity of 2.15 grams/denier, an elongation at break of 5.7 percent and modulus of 32.90 grams/denier. Example 12 The procedure of Example 9 was followed except that spinneret 9 contained 72 holes arranged in a circle to produce 72 filaments and the yarn was taken up at a speed of 188 meters/min. The yarn had a dpf of 7.0, a tenacity of 2.11 grams/denier, an elongation at break of 90 percent, and a modulus of 24.47 grams/denier. Example 13 The procedure of Example 3 was followed except that spinneret 9 contained 100 holes each having a diameter of 0.008 inch (0.2 mm) and a length of 0.012 inch (0.3 mm) to produce 100 filaments, the temperature of heated tube 11 was 290°C, and the yarn take-up speed was 50 meters/min. The yarn had a dpf of 18.3, a tenacity of 1.53 grams/denier, an elongation at break of 160 percent and a modulus of 22.58 grams/denier. Example 14 The procedure of Example 13 was followed except that heated tube 11 was at a temperature of 300°C and the yarn was taken up at a speed of 75 meters/min. The yarn had a dpf of 12.6, a tenacity of 1.41 grams/denier, an elongation at break of 112 percent and a modulus of 23.80 grams/denier. Example 15 The procedure of Example 13 was followed except that the temperature of heated tube 11 was then 320° C and the yarn take-up speed was 100 meters/min. The yarn had a dpf of 9.1, a tenacity of 1.55 grams/denier, an elongation at break of 94 percent, and a modulus of 25.25 grams/denier. Example 16 The procedure of Example 3 was followed except that the temperature of heated tube 11 was 313°C, the yarn was initially wound on take-up roll 12 at a speed of 355 meters/min. and was forwarded to a second roll capable of acting as a draw roll but in this case rotating at the same speed as take-up roll 12 i.e. 355 meters/min. From the draw roll which was at ambient temperature, the yarn was forwarded to the tension control winder. The yarn had a dpf of 7.5, an elongation at break of 91 percent and a modulus of 29.70 grams/denier. Example 17 The procedure of Example 16 was repeated except that the draw roll was operating at a speed of 400 meters/minute providing for a drawing of the yarn of 12.7 percent at ambient temperature. The yarn had a dpf of 7.2, a tenacity of 2.13 grams/denier, an elongation at break of 78 percent and a modulus of 28.84 grams/denier. Example 18 The procedure of Example 17 was followed except that the draw roll was at a temperature of 200°C. The yarn had a dpf of 6.6, a tenacity of 2.37 grams/denier,an elongation at break of 66 percent and a modulus of 31.75 grams/denier. Example 19 The procedure of Example 18 was followed except that the take-up roll was operating a speed of 350 meters/min. and the draw roll at a speed of 425 meters/min.resulting in the yarn being drawn 21.4 percent. The yarn had a dpf of 6.9, a tenacity of 2.48 grams/denier, an elongation at break of 49 percent and a modulus of 37.29 grams/denier. Example 20 The procedure of Example 19 was followed except that the take-up roll operated at 300 meters/min. providing for a drawing of the yarn of 41.7 percent. The yarn had a dpf of 6.7, a tenacity of 3.19 grams/denier, an elongation at break of 32 percent and a modulus of 49.05 grams/denier. Example 21 The procedure of Example 20 was repeated except that the take-up roll operated at a speed of 278 meters/min. resulting in the yarn being drawn 45.7 percent. The yarn had a dpf of 6.4, a tenacity of 3.64 grams/denier, an elongation at break of 32 percent and a modulus of 57.84 grams/denier. The yarn produced by the process of this invention may be subjected to a drawing treatment using techiques well-known in the art to increase its tenacity. Furthermore, the filaments and yarns produced by the disclosed process may be converted to other fiber products such as tow, staple fiber, staple spun yarn etc. by means of conventional methods. The various fiber products which may be produced in accordance with the invention are suitable for a variety of end-uses requiring good high temperature performance. For example, they may be used in the preparation of high performance structural components, e.g. by blending with carbon fiber in the form of filament or staple spun yarns, knitting or weaving the blend into a fabric and heat pressing the fabric into the desires shape. The fiber of the invention may also be used as a component of filter bags used in hostile environments and, in the form of knitted or woven fabrics, in the manufacture of various textile products requiring resistance to high temperatures such as specialized clothing, draperies and upholstery fabrics,e.g., those employed in airline seats.

Claims: A process for producing filaments of a polymer having an inherent viscosity of at least 0.7 (measured at 25°C in a solution of the polymer in concentrated sulfuric acid of density 1.84 g cm⁻³, said solution containing 0.1 g of polymer per 100 cm³ of solution) and containing in the polymer chain at least 50 percent of the repeating units: which comprises melting the polymer and heating the melt to a temperature in the range of from 20°C above its melting point to 80°C above its melting point, and extruding the melt through spinning openings of desired shape to form filaments, characterised in that, prior to extrusion through said spinning openings the melt is passed through a filter pack having a filtering area of at least 8 in ² (51.6 cm²) and a total filter volume of at least 1.2 in³ (19.7 cm³) per pound (0.45 kg) of polymer extruded per hour, the filter pack containing inert irregularly shaped particles having a mesh size of 25 to 140 (710 µm to 106 µm) to provide a pressure drop of at least 800 psig (5516 kPa gauge). The process of claim 1 wherein the polymer consists solely of the said repeating units in the polymer chain and the melt is heated to a temperature of 355°C to 415°C. The process of claim 1 or 2 wherein the filter particles are shattered metal. The process of any of claims 1-3 wherein the filter pack as a filtering area of 15 to 25 in² (96.8 to 161.3 cm²), a total volume of 1.6 to 2.3 in³ (26.2 to 37.7 cm³) per pound (0.45 kg) of polymer extruded per hour and a pressure drop of 950 to 3000 psig (6550 to 20684 kPa gauge). The process of any of claims 1-4 wherein the melt from the filter pack is further filtered by being passed through openings less than 20 microns (µm) in size prior to being passed through the spinning openings to form filaments. The process of any of claims 1-5 wherein the filaments are collected at a point within 15 to 50 inches (38.1 to 127 cm) from spinning openings to form a yarn. The process of any of claims 1-6 including the step of passing the filaments immediately upon extrusion through a heating zone maintained at a temperature of 200 to 320°C and having a length of 3 to 12 inches (7.6 to 30.5 cm). Fibers and yarns of a polymer having an inherent viscosity of at least 0.7 (measured at 25°C in a solution of the polymer in concentrated sulfuric acid of density 1.84 g cm⁻³, said solution containing 0.1 g of polymer per 100 cm³ of solution) and containing in the polymer chain at least 50 percent of the repeating units: the fibers and yarns having a denier per filament (dpf) of 2.8 to 100 (3.1 to 111 dtex), a tenacity of 0.89 to 4.0 cN/dtex (1 to 4.5 grams per denier), an elongation at break of 15 to 200 percent, and a modulus of 18 to 71 cN/dtex (20 to 80 grams per denier). The fibers and yarns of claim 8 wherein the polymer consists solely of the said repeating units in the polymer chain. The fibers and yarns of claim 8 or 9 wherein the individual fibers have a birefringence of 0.025 to 0.220. The fibers and yarns of any of claims 8-10 having a denier per filament of 15 to 100 (16.7 to 111 dtex), a tenacity of 0.89 to 1.78 dtex (1 to 2 grams per denier), an elongation at break of 50 to 160 percent, and a modulus of 18 to 27 cN/dtex (20 to 30 grams per denier). The fibers and yarns of any of claims 8-11 wherein the individual fibers having a birefringence of 0.025 to 0.150. The fibers and yarns of any of claims 8-12 having a denier per filament of 2.8 to 15 (3.1 to 16.7 dtex).

Inventors: DEEG, MARTIN H.G.
Applicants: CELANESE CORPORATION
Application year: 1986
Main classification: D01F6
IPC codes: D01D1, D01F6