US3758658A - Ecular weight linear polymers process for the production of technical endless filaments of high mol - Google Patents

Ecular weight linear polymers process for the production of technical endless filaments of high mol Download PDF

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Publication number
US3758658A
US3758658A US00058054A US3758658DA US3758658A US 3758658 A US3758658 A US 3758658A US 00058054 A US00058054 A US 00058054A US 3758658D A US3758658D A US 3758658DA US 3758658 A US3758658 A US 3758658A
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melt
spinning
pressure drop
temperature
filaments
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US00058054A
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English (en)
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K Riggert
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Vickers Zimmer AG
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Vickers Zimmer AG
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/06—Feeding liquid to the spinning head
    • D01D1/09—Control of pressure, temperature or feeding rate

Definitions

  • ABSTRACT Process for production of endless filaments fromhigh molecular weight polymers having improved properties of lown loss, and few capillary breaks per '10 Km, in a melt spinning process wherein the polymer melt is supplied to a spinning beam at high pressure, the melt is thereafter passed through a flow path constriction which effects apressure drop of from 150 to 1200 atmospheres and a melt enthalpy increase sufficient to internally heat each of the melt particles uniformly and independently of their position in the melt flow cross section, and thereafter maintaining the increased temperature of the melt by heating all the surfaces thereafter contacted by the melt.
  • the invention relates to a process for the production of so-called technical filaments and threads (yarns) of high-molecular weight linear polymers, in particular polyesters, according to an improved melt-spinning process.
  • Polyethylene terephthalate has come into strong prominence in the last few years for use in tire cord production. Polyethylene terephthalate unfortunately undergoes a considerable thermal decomposition between the conclusion of the production of the spinning raw material (raw polymer melt) and its subsequent shaping into threads. This thermal decomposition increases appreciably as the molar weight of the spinning raw material rises, and in the case of filament formation from polymer chips -5 cannot be prevented even by an intensive drying of the spinning raw material. Be-
  • the melt is not uniformly heated to the spinning temperature over the flow cross section.
  • the undesirable conse quence is inhomogeneity of the filaments over the cross section of the spinning nozzle plate, especially where the/nozzle plate has a relatively large number'of holes. It is among the objects of the present invention to avoid these disadvantages, and in particular, to attain a rapid, uniform heating of the melt over the flow cross section before the spinning.
  • The-process of theinvention solves the above problems by heatingthe melt prior to spinning by pressure decrease by means of a flow path construction, and then maintaining the melt temperature level by corresponding heating of all the surfaces touched by the melt before the final spinning.
  • the process of this invention results in an ideally uniform temperature'increase over the full flow cross section by energy transformation at the choke point during the pressure decrease, in which each melt particle undergoes an equally great enthalpy increase, or tempering independently of its position in the flow cross section.
  • this .tempering', state cannot be lost through heat lead-off byproviding a simultaneous, corresponding heating' of apparatus is unfortunately prescribed by the dimensions of the apparatus, and the lower limit of the spinning temperature is determined by the highly undesirable eondition of melt fracture.
  • melt fracture occurs, the spun, unstretched filaments do not have a smooth or even surface, and exhibit fluctuations in diameter which are unacceptable for use as technical yarn, like tire cord.
  • the threads of yarns produced according to the invention consist of filaments which are distinguished by a low scatter of both the diameter and the double refraction as measured over the thread cross section, i.e., low variation in these values from filament to filament. As a result, further processing propertires are excellent.
  • yarns or threads of high tensile strength having a low filament capillary breakage number.
  • the filaments show only a relatively slight decrease in the molecular weight as compared to the spinning raw material.
  • the high molecular weight melt is supplied at a temperature T between 280 and 330 C., and 2) is exposed to a pressure drop or pressure gradient, Ap, between I50 and 1200 atmospheres, at the earliest after 50 percent of its residence time between melt generation and spinning, and 3) the surface temperature, T of all the surfaces contacted by the melt after the pressure drop is maintained within the following limits:
  • T depends on the height of the pressure gradient (drop) and the temperature T of the melt before the pressure drop.
  • the polyethylene terephthalate melt is supplied at a temperature T, between 285 and 310 C., and is exposed to a pressure drop (gradient) Ap between 200 and 800 atmospheres.
  • the pressure decrease is carried out in the flow path between spinning pump and spinning nozzle plate. Good results are achieved in the finished filaments or threads especially when the pressure drop is located in the vicinity of the spinning nozzle plate.
  • An especially simple and effective manner of carrying out the process of this invention is in providiilg that the pressure drop takes place substantially at the spinning filter, which in spinning devices in general is placed in the upper part of the so-called spinning nozzle pack.
  • Metal sieves having l0,000 to 50,000 meshes/cm are well suited as spinning filter'material for this purpose. Such sieves can be stratified in several layers one over another and are suitably supported against the high spinning pump pressure. Sintered metal filters have also proved usable for this purpose.
  • the pressure decrease can be carried out according to three methods or combinations thereof in the spinning apparatus.
  • spinning filter as the main choke zone for achieving the pressure drop
  • the supporting plate and/or nozzle bores bores with a large length/diameter ratio, l/d, are required to achieve the pressure drop required in this invention.
  • unlimited l/d ratios are not possible, at least for the nozzle bores, principally for reasons of manufacturing technology. For example, diameters of less than 1mm, very common for this spinning technology, cannot be manufactured with adequate precision where the l/d ratio is above 20.
  • the pressure is brought down preferably and largely at the spinning filter. Letting pressure down at the spinning filter is also preferable because there the temperature distribution in the melt is more uniform.
  • the process of the invention it is possible to proceed both from polymer chips, which, in a known manner, are melted up on grids or by means of extruder devices, and also directly from a polymer melt obtained directly after the conclusion of the polymerization or polycondensation. In either case, short feed paths between melt discharge and spinning device are recommended.
  • the process of the invention is particularly adapted to the processing of polymers having spinning melt solution viscosities, m equal or greater than 0.85, and preferably equal to or greater than 0.92.
  • FIG. 1 represents a section througha spinning position of a spinning beam.
  • FIG. 2 shows a six-position-beam in a rear view.
  • a high-pressure spinning pump 2 normally a gear wheel type metering pump, having product inlet line 3 and product outlet line 4, as well as a spinning head,generally designated as 5.
  • the spinning head 5 in the present examp le,.being substantially rotationally symmetrical, consists of a feed plate 6 and a spinning nozzle pack holder 7 screwed together with it from above (not shown);
  • the feedplate 6 has a radially-outward directed product inlet line 8 aligned with the product out-' let line 4, which product inlet line 8 expands conically downward to about the diameter of the spinning nozzle pack.
  • the spinningnozzle pack comprises: a.
  • the spinning nozzle plate 9 provided with a-large number of nozzle bores, which plate is seated on an inwardly-directed ring shoulder 10 of theholder 7, b. a filter support plate 11 resting on the plate 9, and c. the filter 12 sandwiched between supporting plate 11 and feed plate 6.
  • the filter in this embodiment consists of a plurality of edge-framed wire gauze layers.
  • the filter 12 has a double function: On the one hand it filtersthe spinning melt in a known manner, and on the other hand, with respect to its ,fl ow resistance, it is dimensioned in such a way that it brings about the main-proportion of the desired pressure drop.
  • the spinning ,pump 2 isv surrounded by a heating jacket 13, which is heated by any convenient heat transfer medium, for example the mixture of diphenyl ing tube 15 is closed by an insulating plug 17.
  • a heating jacket 13 which is heated by any convenient heat transfer medium, for example the mixture of diphenyl ing tube 15 is closed by an insulating plug 17.
  • FIG. 2 shows that the product lines 19 are adapted to have equal length between a central supply place 18 and the individual spinning pumps 2, so that the melt has a uniform residence time for all thespinning positions.
  • the reference number 20 designates the spinning pump drive shafts.
  • Example 1 describes a conventional technique not according to this invention, operating without appreciable pressure drop and without temperature rise before the spinning.
  • Examples 2, 5 and 7 relate to the process of this invention and clearly show its advantages.
  • Examples 3, 4 and 6 relate to processes in which not all the features of this invention are present simultaneously, or the work is done according to the state of technology.
  • the solution viscosity is given in the examples as the measure for the mean molecular weight, which was determined as the m value by standard procedures.
  • the concentration of the measuring solution amounted to 0.5 g/l0.0 ml.
  • the solvent is a phenoltetrachloroethane mixture (60 40) and the measuring temperature was C.
  • the diameter fluctuations along an unstretched thread filament serve as the measure of the melt fracture.
  • the diameter fluctuations are recorded as the variation coefficient (CV value) in percentages.
  • the variation coefficient of the double refraction (CV, value) is given in percentages.
  • EXAMPLE I (Conventional Technique) A; A melt of polyethylene terephthalate having a solution viscosity of m 1.04 was supplied at a temperature'T of 310 C. to a six-position spinning beam. All the product lines, including spinning pump and spinning nozzle pack, were heated to T 310 C. The
  • Example 2 The Invention
  • the initial procedure as in Example 1 was fillowed, but with the modification that the polymer was supplied to the spinning beam, at T 292 C. instead of at 310 C.
  • the spinning beam, including spinning pump, was likewise heated to T, 292 C.
  • the melt residence time during its conveyance from the place of generation to the spinning beam was the same as in Example 1.
  • the spinning nozzle pack was heated to a-temperature of T 310 C.
  • the pressure drop, Ap was 320 at- I mospheres.
  • the temperature of the spinning nozzle pack was therefore within the temperature range according to the invention.
  • a thread having spinning titerof 5900 denier was spun, again at 400 m/min.
  • the mean CV value of the thread filaments was 4.6 percent.
  • the thread had 25 breaks per 10,000 m, which is within the measurement error limits.
  • the molecular decomposition of the polymer was significantly improved, being considerably less under the process parameters of the invention, the thread having a solution viscosity of m 0.94.
  • CV value was 10 percent, as a result of the temperature inhomogeneity of the melt emerging from the spinviscosity of the thread, which was found to be m thread material obtained was no longer faultlessly' spinnable and stretchable because of setting in of melt ning nozzle plate. For the'same reason, the CV, value amounted to 15 percent, and as a consequence the capillary break frequency was considerable. With respect to a thread tensile strength of 9.0 g/den. I00 capillary breaks per l0,000 m were counted.
  • the improve ment whicfh comprises: T [(l7+l0 3) (M7)] T [1O( a. supplying said melt at a temperature T between 100 280 and 330 C and at high pressure to a spinning unit comprising a spinning pump, a nozzle plate and construction means disposed between said pump and said nozzle plate,
  • a process as i claim 1 i temperature is uniform and independent of the id bl comprises a i i pump and a melt position in the flow cross section under condii i nozzle l t d tions which provide low loss of intrinsic viscosity 5 b id pressure d i eff ct d i h fl w h and (1085 not change the laminarity Of melt flOW, tween aid spinning pump and spinning nozzle c.
  • said filaments a. said polymer is polyethylene terephthalate,
  • said pressure drop is effected at the earliest after low diameter and double refraction variation coef- 50 percent of the total melt residence time between ficients, and few filament breaks per 10 Km. spun generation and spinning, and

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
US00058054A 1969-12-22 1970-07-24 Ecular weight linear polymers process for the production of technical endless filaments of high mol Expired - Lifetime US3758658A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19691964051 DE1964051B2 (de) 1969-12-22 1969-12-22 Verfahren zur herstellung hochmolekularer technischer filamente aus linearen plymeren

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US (1) US3758658A (enrdf_load_stackoverflow)
JP (1) JPS497091B1 (enrdf_load_stackoverflow)
CA (1) CA979169A (enrdf_load_stackoverflow)
DE (1) DE1964051B2 (enrdf_load_stackoverflow)
GB (1) GB1311024A (enrdf_load_stackoverflow)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3846377A (en) * 1971-11-12 1974-11-05 Allied Chem Method of producing polyethylene terephthalate fibers
US3963678A (en) * 1974-06-17 1976-06-15 E. I. Du Pont De Nemours And Company Large denier polyethylene terephthalate monofilaments having good transverse properties
US4072663A (en) * 1977-02-22 1978-02-07 Allied Chemical Corporation Transfer system for conveying polyester polymer
US4089917A (en) * 1974-05-16 1978-05-16 Ikegai Tekko Kabushiki Kaisha Process of cross-linking and extrusion molding thermoplastic polymers
US4195161A (en) * 1973-09-26 1980-03-25 Celanese Corporation Polyester fiber
US4380570A (en) * 1980-04-08 1983-04-19 Schwarz Eckhard C A Apparatus and process for melt-blowing a fiberforming thermoplastic polymer and product produced thereby
US6364647B1 (en) 1998-10-08 2002-04-02 David M. Sanborn Thermostatic melt blowing apparatus
US20030035855A1 (en) * 2001-08-18 2003-02-20 Holger Brandt Spinning apparatus
US20040201127A1 (en) * 2003-04-08 2004-10-14 The Procter & Gamble Company Apparatus and method for forming fibers
US20110037194A1 (en) * 2009-08-14 2011-02-17 Michael David James Die assembly and method of using same

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59150279U (ja) * 1983-03-29 1984-10-08 篠田　国雄 釣糸巻装具
EP0289531B1 (de) * 1986-09-29 1992-06-03 Rita Diekwisch Verfahren und vorrichtung zur kunststoffbeschichtung von dreidimensionalen körpern
TW311945B (enrdf_load_stackoverflow) * 1994-11-23 1997-08-01 Barmag Barmer Maschf
DE19924838A1 (de) * 1999-05-29 2000-11-30 Lurgi Zimmer Ag Spinnvorrichtung zum Verspinnen schmelzflüssiger Polymere und Verfahren zum Beheizen der Spinnvorrichtung

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3104419A (en) * 1962-08-24 1963-09-24 Du Pont Spinneret pack
DE1660209A1 (de) * 1965-07-15 1970-02-05 Barmag Barmer Maschf Schmelzespinnkopf fuer das Spinnen unter hohem Druck

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3846377A (en) * 1971-11-12 1974-11-05 Allied Chem Method of producing polyethylene terephthalate fibers
US4195161A (en) * 1973-09-26 1980-03-25 Celanese Corporation Polyester fiber
US4089917A (en) * 1974-05-16 1978-05-16 Ikegai Tekko Kabushiki Kaisha Process of cross-linking and extrusion molding thermoplastic polymers
US3963678A (en) * 1974-06-17 1976-06-15 E. I. Du Pont De Nemours And Company Large denier polyethylene terephthalate monofilaments having good transverse properties
US4072663A (en) * 1977-02-22 1978-02-07 Allied Chemical Corporation Transfer system for conveying polyester polymer
US4380570A (en) * 1980-04-08 1983-04-19 Schwarz Eckhard C A Apparatus and process for melt-blowing a fiberforming thermoplastic polymer and product produced thereby
US6364647B1 (en) 1998-10-08 2002-04-02 David M. Sanborn Thermostatic melt blowing apparatus
US20030035855A1 (en) * 2001-08-18 2003-02-20 Holger Brandt Spinning apparatus
US20040201127A1 (en) * 2003-04-08 2004-10-14 The Procter & Gamble Company Apparatus and method for forming fibers
US7018188B2 (en) 2003-04-08 2006-03-28 The Procter & Gamble Company Apparatus for forming fibers
US7939010B2 (en) 2003-04-08 2011-05-10 The Procter & Gamble Company Method for forming fibers
US20110037194A1 (en) * 2009-08-14 2011-02-17 Michael David James Die assembly and method of using same
US10704166B2 (en) 2009-08-14 2020-07-07 The Procter & Gamble Company Die assembly and method of using same
US11414787B2 (en) 2009-08-14 2022-08-16 The Procter & Gamble Company Die assembly and methods of using same
US11739444B2 (en) 2009-08-14 2023-08-29 The Procter & Gamble Company Die assembly and methods of using same

Also Published As

Publication number Publication date
DE1964051A1 (de) 1971-09-23
CA979169A (en) 1975-12-09
JPS497091B1 (enrdf_load_stackoverflow) 1974-02-18
DE1964051B2 (de) 1976-09-23
GB1311024A (en) 1973-03-21

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