US3257487A - Melt spinning of epsilon-polycaproamide filament - Google Patents

Melt spinning of epsilon-polycaproamide filament Download PDF

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Publication number
US3257487A
US3257487A US262546A US26254663A US3257487A US 3257487 A US3257487 A US 3257487A US 262546 A US262546 A US 262546A US 26254663 A US26254663 A US 26254663A US 3257487 A US3257487 A US 3257487A
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United States
Prior art keywords
zone
filaments
spinning
spinneret
plenum
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Expired - Lifetime
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US262546A
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English (en)
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Jr Grady N Dulin
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Allied Corp
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Allied Chemical Corp
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Priority to US262546A priority Critical patent/US3257487A/en
Priority to FR966094A priority patent/FR1385102A/fr
Priority to NL6402175A priority patent/NL6402175A/xx
Priority to BE644707A priority patent/BE644707A/xx
Priority to DE1435329A priority patent/DE1435329B2/de
Priority to GB9186/64A priority patent/GB1011644A/en
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Publication of US3257487A publication Critical patent/US3257487A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • D01D5/092Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D11/00Other features of manufacture
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S425/00Plastic article or earthenware shaping or treating: apparatus
    • Y10S425/815Chemically inert or reactive atmosphere

Definitions

  • expedients for solving this problem include the use of aspiration means for continuously removing volatilized monomer from the region neighboring the spinneret.
  • aspiration means for continuously removing volatilized monomer from the region neighboring the spinneret.
  • a satisfactory aspiration means must therefore be carefully devised and critically combined with the other elements of the spinning apparatus to coact in the general functions and requirements of the spinning process. Otherwise aspiration means would be ineffective and could cause undesired effects upon the freshly extruded yarn structure due to improper thermal or mechanical factors.
  • a fiber-producing apparatus comprising a vertical spinning chamber; a horizontal multiorifice spinneret forming the top of said spinning chamber, and aspiration means around the upper end of said spinning chamber and in communication with said chamber via channels piercing the walls therebetween.
  • Said aspiration means comprises a plenum and an exhaust port from which gas can be withdrawn.
  • a pressure drop is imposed between spinning chamber and plenum atmosphere to create gas flow from the chamber through the channels, into and through the plenum, and out the exhaust port or ports.
  • a vane which extends clear of the inner plenum wall and past said channels; preferably to points E where an angle of about 170 would be formed between the line drawn from E to the nearest point C of said channels, and the intersecting line from E to the point P which is on the axis of said spinning chamber'and is at the same horizontal level as said point C.
  • polycaproamide at a temperature in the range of 250 C. to 290 C. is extruded into contact with inert cooling gas or vapor in the spinning chamber at a jet velocity usually in the range between about 10 and about 40 yards per minute.
  • a lower pressure is maintained in said plenum than in said chamber with a variation of pressure of less than 0.5 inch of mercury throughout the volume of said plenum, the flow rate of gas from the spinning chamber into and through said plenum being maintained between 1 and 20 cubic feet per minute and being at substantially equal volumetric flow rates through the successive areas of wall separating the spinning chamber from the plenum.
  • the cooling gas enters the spinning chamber through inlets in the walls thereof having a highest level at I below the plenum, so positioned with respect to the outermost spinneret orifice thereabove O, and the point P on the axis of the chamber at the level of the channels, that the angle OPT is 45 to
  • a minor portion of the entering gas is drawn upward from the inlets, and the major portion of said entering gas flows downward in the spinning chamber below the inlets, cocurrently with the filaments, and exits below the inlets.
  • FIGURE 1 is a sectional elevation of a spinning apparatus utilized in the process of the present invention taken along the vertical axis of the spinning chamber.
  • FIGURE 2 is a similarly taken sectional elevation of another embodiment of the spinning apparatus utilized in the process of this invention.
  • a vertical spinning chamber is defined by cylindrical walls 1 and horizontal spinneret 2 having a multiplicity of orifices 3'.
  • Aspiration means at the upper end of said spinning chamber comprises a plenum 4 surrounding the chamber and provided with an exhaust port 8 which leads to a vacuum pump or other suitable means, not shown, for withdrawing gas.
  • several exhaust ports 18, 18 can be provided instead of one port.
  • Channels 5, forming a horizontal ring communicate through the inner wall of the plenum 4 with the gaseous atmosphere of the spinning chamber.
  • a vertical vane 6 within the spinning chamber is joined thereto along the full length of its upper edge by a horizontal lip 7, so that the vane covers but lies spaced inward from the channels 5.
  • the vane extends clear of the inner plenum wall, and downward past the inlet channels of the plenum, and is at greater distance from the chamber axis than that of the main sections of the chamber walls therebelow.
  • the position of E with respect to the nearest point C, of the channels and with respect to the point P, on the axis of the chamber and at the same level as the channels, is critical for optimum spinning characteristics of the apparatus.
  • Inlet means 9 in the walls of the spinning chamber are provided for the entrance of cooling gas into the spinning chamber. Best results are generally obtained when the topmost of these inlets, which can be designated I, are in a critical area below the plenum, where the line IP drawn from I to P (designating, as before, the point on the axis of the chamber and at the same level as the inlet channels of the plenum) meets the line from P to O (designating the outermost of the spinneret orifices directly above I) at an angle of 45 to 120. Again when the channels lie at more than one level, there will be corresponding additional values of the angle OPI as indicated at O'PI', O'P"I' of FIG. 2.
  • Contact sealing means 10 of FIG. 1 are provided close below the plenum, comprising a lip 14 depending below the plenum and accommodated in horizontal groove 11, containing non-volatile inert liquid 15, such as molten Woods metal.
  • An alternative as shown in FIG. 2 is to use a gasket 25, e.g. of the O-ring type or of soft or resilient material, in a groove 21 to make sealing contact between the w'alls of chamber 1(a) and plenum 4(a).
  • an outlet is shown for cooling gas descending from inlets 9 toward the bottom of chamber 1.
  • the form and position of this outlet is not critical provided it is at a point where the filaments 13 have solidified and cooled.
  • the plenum which surrounds the spinning chamber may be a single chamber or several separate chambers; each separate chamber requiring an individual exhaust port.
  • the inner wall of the plenum constitutes the topmost wall of the spinning chamber. It is generally preferred. that the plenum be maintained at a sufficiently elevated temperature to further minimize the accumulation of condensable material therein.
  • the baffle or vane preferably of non-porous, rigid construction, is adjacent to and spaced away from the channels in the plenum wall so as to block direct flow of gas from the immediately adjacent chamber atmosphere into said channels.
  • the vane is supported along the full length of one edge or the other, as in the drawings; or alternately along first one edge, then the other. It can also be held just at a few points as a shield in front of the plenum channels.
  • the sectional shape of the vane is not critical and may be angular or curved in various configurations provided however, it does not interfere with the yarn.
  • the edges of the vane should preferably be continuous and uniform and lie in a single plane horizontal to the chamber and at distances from the channels to form angles CEP, as above defined, of 90--170.
  • the inlet channels to the plenum are preferably numerous holes of relatively small diameter roughly approximating their length. Usually they are circular, but narrow slits can be used. These channels are preferably dimensioned to create a pressure drop in the gas flowing therethrough, and maintain pressure differential of about 0.05 to about 10 inches of mercury between spinning chamber atmosphere and plenum.
  • the plenum is so sized and the channels leading thereto and exhaust ports leading therefrom are so sized and spaced as to maintain this pressure differential substantially uniformly within about 0.5 inch mercury throughout the plenum volume, and maintain volumetric rates of gas flow which are substantially equal through all successive areas of the wall separating the spinning chamber and the plenum.
  • the plenum cross-sectional area suitably will exceed by several fold the total cross-sectional area of the inlet channels whereby the linear rates of flow of gas throughout the plenum will be a fraction of that through the channels.
  • the channels can then be all of the same size and spaced uniformly and at a single level around the plenum and will then provide a uniform pressure throughout the plenum volume and equal volumetric rates and flow of gas into all areas around the plenum.
  • the exhaust port or ports will usually be sized with a view to avoiding pressure gradients in the plenum; accordingly they will have relatively large cross-sectional area.
  • the channels are evenly sized and spaced and all at the same level, they can be of different sizes and spacings and at different levels as long as equal volumetric gas fiow rates through each sizable area of the plenum are obtained.
  • the freshly extruded filaments .13 emanating from orifices 3 undergo solidification starting in the region of the aspirator under the influence of a countercurrent flow of essentially inert gas or vapor entering through inlet means 9, said flow eing aminor part of the total flow of gas entering the chamber through the inlets 9.
  • This flow of gas carries withit through channels 5 volatilized monomer given off by the molten freshly extruded filament in the upper regions of the spinning chamber.
  • the filaments further solidify and cool in the lower part of the spinning chamber, below the inlets 9.
  • the major portion of the entering inert gas fiows downwardly, cocurrent with the filaments, from inlets 9, and exits at a level where the filaments are cool, e.g. at outlet 12 at the bottom of the spinning chamber.
  • inert gas is drawn into the inlets 9 and upwardly .at a rate of 1 to 20 cubic feet per minute, the rates used being greater for greater diameters of the spinning chamber; and thence through the channels 5; through the plenum 4; and out through exhaust port 8 to a vacuum pump, water aspirator or analogous means for propelling or transporting gas.
  • Flow rates in excess of 20 cubic feet per minute are found to cause turbulence in the flow path of the freshly formed filaments in spinning chambers of usual commercial sizes, thereby causing the filaments to entangle or interadhere during their downward travel.
  • Flow rates less than 1 cubic foot per minute are found inadequate in commercial size apparatus to prevent the accumulation of volatilized material in the upper regions of the spinning chamber.
  • the major portion of the entering inert gas descends in the spinning chamber cocurrent with the filaments and is withdrawn at the bottom of the spinning chamber.
  • my vane The function of my vane is apparently to create a relatively quiescent region of relatively dead air from which the exhaust is smoothly withdrawn; and to prevent cross currents of air being drawn from the immediate vicinity into the channels 5 of the plenum and creating turbulence. It should be appreciated that when an outlet for a major portion of the cooling air is provided below the inlets as in my preferred operations, it will require appreciable pressure differential between my plenum atmosphere and my spinning chamber atmosphere to draw a portion of the entering gas upward; and accordingly there will be a tendency to create local currents of air near the plenum. My vane contributes importantly to smoothing out operation under these conditions whereby uniformly high quality filaments are obtained in accordance with my invention.
  • angle CEP made at the edges of the vane relates several geometrical factors: (a) the vertical position of the channels with respect to the edge of the vane, (b) the spacing of the vane with respect to the entrance to the channels, and (c) the diameter of the spinning chamber. It has been found that when this angle exceeds or is below about 90 the yarn quality is adversely affected.
  • angle 0P1 relates the geometrical factors of: (a) vertical spacing of the outermost spinneret orifices and the uppermost gas inlet with respect to the avoided by the spinning apparatus of the present invention.
  • coupling means associated with the chamber wall may preferably be located below the aspirator means, although in some embodiments the coupling means may desirably be positioned above the aspirator means.
  • the coupling means must provide an efiective airtight .seal so as to prevent extraneous air from entering the spinning chamber.
  • Preferred coupling means should thus include a deformable, resilient member which can conform to the geometrical requirements of the two coupling entities, thereby providing a rapid-acting, tight seal which will retain its efiectiveness even after many coupling cycles.
  • Specific resilient members include elastorneric O-rings, impregnated gaskets, and troughs of non-volatile liquids or molten metal into which one of the coupling members becomes immersed to form an airtight seal.
  • the orifice of the spinneret may be circular or polygonal, having symmetrical or asymmetrical configuration, or may consist of separate groups of closely spaced orifices whose combined extrudate merges partially or entirely to form a single integral filament. Filaments produced from said orifices will generally have a crosssectional configuration determined by the orifice and may be round, angular, multilobal, multibranched, crenulated, dog-boned or the like.
  • Example Employing a spinning apparatus essentially as represented by FIG. 1, a polycaproamide polymer having a formic acid relative viscosity of 45 (as determined by ASTM procedure D78953T) and volatiles content of about 1%3% by weight, was extruded at a temperature of 262 C. and at a jet velocity of about yards per minute through a stainless steel spinneret containing 136 orifices each of 0.018 inch diameter, radially arranged. The spinneret face had been wiped with a liquid polyorganosiloxane before spinning commenced.
  • the spinning chamber into which the filaments were extruded was about 22 feet long and 9 inches in diameter. It was supplied with 41 cubic feet per minute of air at 82 F.
  • the angle OPI was 83.
  • the inner plenum wall as shown in FIG. 1 was pierced by circular channels each about li inch in diameter and inch long, uniformly set in a ring around the axis of the chamber. The diameter across this ring was about 1 foot.
  • the vertical, downwardly extending vane 6 was at a distance of about /41 inch from the inner plenum wall and the channels therein. It was positioned so that angle CEP was 129.
  • a pressure differential as against the atmosphere of the spinning chamber of 0.6 inch of mercury was maintained throughout the volume of plenum 4 by means of a vacuum pump acting through a condenser for recovery of monomer and communicating with the plenum through a single exhaust port.
  • the volumetric flow rate through the plenum to the exhaust pump was 8 cubic feet per minute, the remainder of the air exiting at the bottom of the chamber where the filament emerged.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
US262546A 1963-03-04 1963-03-04 Melt spinning of epsilon-polycaproamide filament Expired - Lifetime US3257487A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US262546A US3257487A (en) 1963-03-04 1963-03-04 Melt spinning of epsilon-polycaproamide filament
FR966094A FR1385102A (fr) 1963-03-04 1964-03-04 Appareil et procédé pour le filage à l'état fondu de filaments de polycaproamide permettant d'éliminer les impuretés volatiles de la zone de la filière
NL6402175A NL6402175A (xx) 1963-03-04 1964-03-04
BE644707A BE644707A (xx) 1963-03-04 1964-03-04
DE1435329A DE1435329B2 (de) 1963-03-04 1964-03-04 Vorrichtung zur Herstellung von epsilon-Caproamidfäden
GB9186/64A GB1011644A (en) 1963-03-04 1964-03-04 Apparatus for and a method of melt-spinning poly-caproamide filaments

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US262546A US3257487A (en) 1963-03-04 1963-03-04 Melt spinning of epsilon-polycaproamide filament

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US3257487A true US3257487A (en) 1966-06-21

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US (1) US3257487A (xx)
BE (1) BE644707A (xx)
DE (1) DE1435329B2 (xx)
GB (1) GB1011644A (xx)
NL (1) NL6402175A (xx)

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3308221A (en) * 1963-05-14 1967-03-07 Allied Chem Melt spinning of modified cross section yarn
US3389429A (en) * 1966-09-13 1968-06-25 Allied Chem Spinning apparatus
US3466357A (en) * 1965-12-18 1969-09-09 Glanzstoff Ag Method and apparatus for spinning organic high polymers
US3487144A (en) * 1968-01-04 1969-12-30 Fmc Corp Apparatus and method for cooling extruded molten filaments
US3489832A (en) * 1967-04-28 1970-01-13 Allied Chem Continuous spinning and drawing of polycaproamide yarn
US3659980A (en) * 1970-05-11 1972-05-02 Phillips Fibers Corp Apparatus for melt spinning of synthetic filaments
US3679786A (en) * 1970-05-21 1972-07-25 Phillips Fibers Corp Method and apparatus for melt spinning of synthetic filaments
US4212606A (en) * 1978-05-25 1980-07-15 Allied Chemical Corporation Quench stack reel assembly and clamping device
US4504085A (en) * 1978-05-25 1985-03-12 Allied Corporation Reel assembly and clamping device
US4732720A (en) * 1981-02-26 1988-03-22 Asahi Kasei Kogyo Kabushiki Kaisha Process for the production of uniformly dyeable nylon 66 fiber
US5034182A (en) * 1986-04-30 1991-07-23 E. I. Du Pont De Nemours And Company Melt spinning process for polymeric filaments
US5141700A (en) * 1986-04-30 1992-08-25 E. I. Du Pont De Nemours And Company Melt spinning process for polyamide industrial filaments
US5935512A (en) * 1996-12-30 1999-08-10 Kimberly-Clark Worldwide, Inc. Nonwoven process and apparatus
EP1505180A1 (en) * 2003-07-24 2005-02-09 TMT Machinery, Inc. Melt spinning apparatus
US20080012170A1 (en) * 2006-07-14 2008-01-17 General Electric Company Process for making a high heat polymer fiber
CN109868511A (zh) * 2017-12-01 2019-06-11 日本Tmt机械株式会社 熔融纺丝装置
CN111676534A (zh) * 2020-06-02 2020-09-18 安徽东锦环保科技有限公司 一种功能性聚酯纤维的制备方法
CN111809255A (zh) * 2019-04-10 2020-10-23 欧瑞康纺织有限及两合公司 用于熔融纺丝以及冷却多个合成长丝的装置
CN114182366A (zh) * 2022-01-14 2022-03-15 福建永荣锦江股份有限公司 一种超细聚酰胺纤维风冷装置

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2217743A (en) * 1939-03-28 1940-10-15 Du Pont Apparatus
US2252684A (en) * 1938-08-09 1941-08-19 Du Pont Apparatus for the production of artificial structures
GB714330A (en) * 1949-10-29 1954-08-25 Perfolan Holding Trust Improvements in or relating to apparatus for melt-spinning artificial fibres
US2719776A (en) * 1949-11-23 1955-10-04 Inventa Ag Elimination of monomers from lactampolymerization products
US2847704A (en) * 1952-11-27 1958-08-19 American Enka Corp Method and apparatus for cooling melt spun threads
US2957747A (en) * 1958-07-22 1960-10-25 Du Pont Process for producing crimpable polyamide filaments
US3015480A (en) * 1956-09-20 1962-01-02 Bayer Ag Apparatus for melting polyamide shreds
US3079219A (en) * 1960-12-06 1963-02-26 Du Pont Process for wet spinning aromatic polyamides

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2252684A (en) * 1938-08-09 1941-08-19 Du Pont Apparatus for the production of artificial structures
US2217743A (en) * 1939-03-28 1940-10-15 Du Pont Apparatus
GB714330A (en) * 1949-10-29 1954-08-25 Perfolan Holding Trust Improvements in or relating to apparatus for melt-spinning artificial fibres
US2719776A (en) * 1949-11-23 1955-10-04 Inventa Ag Elimination of monomers from lactampolymerization products
US2847704A (en) * 1952-11-27 1958-08-19 American Enka Corp Method and apparatus for cooling melt spun threads
US3015480A (en) * 1956-09-20 1962-01-02 Bayer Ag Apparatus for melting polyamide shreds
US2957747A (en) * 1958-07-22 1960-10-25 Du Pont Process for producing crimpable polyamide filaments
US3079219A (en) * 1960-12-06 1963-02-26 Du Pont Process for wet spinning aromatic polyamides

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3308221A (en) * 1963-05-14 1967-03-07 Allied Chem Melt spinning of modified cross section yarn
US3466357A (en) * 1965-12-18 1969-09-09 Glanzstoff Ag Method and apparatus for spinning organic high polymers
US3389429A (en) * 1966-09-13 1968-06-25 Allied Chem Spinning apparatus
US3489832A (en) * 1967-04-28 1970-01-13 Allied Chem Continuous spinning and drawing of polycaproamide yarn
US3487144A (en) * 1968-01-04 1969-12-30 Fmc Corp Apparatus and method for cooling extruded molten filaments
US3659980A (en) * 1970-05-11 1972-05-02 Phillips Fibers Corp Apparatus for melt spinning of synthetic filaments
US3679786A (en) * 1970-05-21 1972-07-25 Phillips Fibers Corp Method and apparatus for melt spinning of synthetic filaments
US4212606A (en) * 1978-05-25 1980-07-15 Allied Chemical Corporation Quench stack reel assembly and clamping device
US4504085A (en) * 1978-05-25 1985-03-12 Allied Corporation Reel assembly and clamping device
US4732720A (en) * 1981-02-26 1988-03-22 Asahi Kasei Kogyo Kabushiki Kaisha Process for the production of uniformly dyeable nylon 66 fiber
US5034182A (en) * 1986-04-30 1991-07-23 E. I. Du Pont De Nemours And Company Melt spinning process for polymeric filaments
US5141700A (en) * 1986-04-30 1992-08-25 E. I. Du Pont De Nemours And Company Melt spinning process for polyamide industrial filaments
US5935512A (en) * 1996-12-30 1999-08-10 Kimberly-Clark Worldwide, Inc. Nonwoven process and apparatus
EP1505180A1 (en) * 2003-07-24 2005-02-09 TMT Machinery, Inc. Melt spinning apparatus
US20080012170A1 (en) * 2006-07-14 2008-01-17 General Electric Company Process for making a high heat polymer fiber
US9416465B2 (en) * 2006-07-14 2016-08-16 Sabic Global Technologies B.V. Process for making a high heat polymer fiber
CN109868511A (zh) * 2017-12-01 2019-06-11 日本Tmt机械株式会社 熔融纺丝装置
CN111809255A (zh) * 2019-04-10 2020-10-23 欧瑞康纺织有限及两合公司 用于熔融纺丝以及冷却多个合成长丝的装置
CN111676534A (zh) * 2020-06-02 2020-09-18 安徽东锦环保科技有限公司 一种功能性聚酯纤维的制备方法
CN111676534B (zh) * 2020-06-02 2021-04-20 安徽东锦环保科技有限公司 一种功能性聚酯纤维的制备方法
CN114182366A (zh) * 2022-01-14 2022-03-15 福建永荣锦江股份有限公司 一种超细聚酰胺纤维风冷装置

Also Published As

Publication number Publication date
DE1435329C3 (xx) 1976-01-08
DE1435329A1 (de) 1969-01-30
DE1435329B2 (de) 1975-05-28
NL6402175A (xx) 1964-09-07
GB1011644A (en) 1965-12-01
BE644707A (xx) 1964-07-01

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