US3504078A - Melt spinning process - Google Patents

Melt spinning process Download PDF

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US3504078A
US3504078A US671832A US3504078DA US3504078A US 3504078 A US3504078 A US 3504078A US 671832 A US671832 A US 671832A US 3504078D A US3504078D A US 3504078DA US 3504078 A US3504078 A US 3504078A
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filaments
temperature
spinning
spinneret
spinning process
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US671832A
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Tin Yam Au
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EIDP Inc
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EI Du Pont de Nemours and Co
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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
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
    • 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
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D01D5/082—Melt spinning methods of mixed yarn

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  • This invention comprises a high speed, melt-spinning process for producing by co-spinning, from a polymer of PACM containing from 55 to 80% of the trans-trans isomer and dodecanedioic acid and a copolymer of the same composition wherein by weight of said acid is replaced by isophthalic acid, said polymers having a relative viscosity of 40 to 60, a mixed-shrinkage yarn.
  • the molten polymers are co-spun at a temperature of at least 300 C. through separate holes in a spinneret into a heated non-oxidizing gaseous atmosphere maintained at a temperature of at least 130 C.
  • the filaments are withdrawn from the spinneret at a speed of at least 1500 y.p.m. such that the tension on the filaments in the spinning and quenching zone is less than 0.20 gram per denier.
  • the filaments are quenched with air and then drawn at least 1.2x. Following draw, the filaments are annealed without further stretching at a temperature of 140 to 190 C.
  • the resulting yarns exhibit a higher differential shrinkage between the homopolymer and copolymer filaments after a boil-01f and heat setting treatment than yarns proluded under similar conditions but under a higher spinning tension.
  • FIG. 1 The drawings show a typical set-up for the high-speed process of the invention.
  • Homopolymer stream A and copolymer stream B are extruded through separate holes of spinneret C.
  • Chamber D represents a diffuser through which steam is passed to blanket the spinneret face.
  • Tail pipe E is a heated conduit that maintains the filaments at elevated temperatures whereby excessive tension build-up is prevented.
  • the filaments then pass over finish roll F to feed rolls G.
  • the filaments are drawn between feed rolls G and draw rolls H. Some additional draw may be applied between draw rolls H and annealing rolls I, the latter being enclosed by a heated chamber as indicated by broken lines.
  • the filaments are then led to a suitable windup means.
  • relative viscosity signifies the ratio of the flow time in a viscometer of a polymer solution relative to the flow time of the solvent by itself. Measurements of relative viscosities as referred to herein and as measured in the examples is determined from a solution of 3.7 grams of polyamide in 50 ml. of a 1:1 mixture by wt. of 98100% formic acid and phenol at 25 C., unless otherwise noted.
  • EXAMPLE A polymer of bis(4-aminocyclohexyl)methane and dodecanedioic acid (PACM12) containing 70% of the trans-trans isomer and having a relative viscosity of 52 and a copolymer of PACM having the same isomer composition with by weight of dodecanedioic acid and 10% isophthalic acid having a relative viscosity of 48 are cospun through a single spinneret containing 36 holes, 18 holes for each polymer.
  • the symmetrical Y-shaped spinneret holes consist of three intersecting slots, each of which is 6 mils wide and 15 mils long to produce filaments having a trilobal cross-section.
  • the spinneret block temperature (spinning temperature) is 330 C. and the polymer temperature going to the spinneret is 300 C.
  • the spinneret face is surrounded by a radial diffuser through which steam at 235 C. is fed to provide a hot nonoxidizing spinning atmosphere.
  • the steam is further confined below the ditfuser by a heated tail pipe about 12 cm. long which is heated maintaining a temperature of 235 C.
  • the filaments are then quenched with air, fed to a draw zone by feed rolls at a speed of 1930 y.p.m. in the spinning zone the filaments are under a tension of about 0.12 g.p.d.
  • the filaments are then drawn in two stages, 1.175X in each stage, by two pairs of draw rolls operating at 2267 and 2663 y.p.m. respectively.
  • the second pair of draw rolls are heated (thus termed annealing rolls) and enclosed in a heated chest at a temperature of C.
  • the filaments are annealed at substantially constant length on the heated rolls prior to being wound up at a speed of 2680 y.p.m.
  • the drawn yarn is about 60 denier and has a tenacity of 3.40 grams per denier, an elongation of 33.5%, an initial modulus of 28.0 and an average DFL on boil-off and heat-set as described herein of 4.9%.
  • the tension on the filaments in the spinning zone must be less than about 0.2 g.p.d. Highter tensions reduce to an undesirable level the amount of diiferential filament length which can be obtained in the yarn after boil-off and heat-setting treatment as herein described.
  • the ten sion may be reduced, for example, by increasing the spinnmg temperature, altering the spinneret orifice dimensions (smaller orifices reduce the tension) and by increasing the temperature of the non-oxidizing atmosphere in the spinning zone. As the spinning speed is increased, the spinning tension increases and adjustments must be made as described above to keep the tension below 0.20
  • Drawn yarn annealing temperatures (temperature of the annealing rolls) of-140 to 190 C. are used. When temperatures less than 140 C. are employed, it is found that the processed yarn possesses undesirably high shinkage. Above 190 C. the obtainable yarn DFL is substantially reduced.
  • a lubricant such as a silicone oil
  • a high-speed melt-spinning process for producing a mixed shrinkage yarn comprising co-spinning two molten polymer streams, one being a homopolymer of bis(4- aminocyclohexyl)methane of from 55 to 80% trans-trans isomer and dodecanedioic acid and the other being acopolymer of the same composition wherein about 10% by weight of said acid is replaced by isophthalic acid, said .4 polymers having a relatively viscosity of from to 60, at a temperature of at least 300 C, through separate holes in a spinneret into a non-oxidizing gaseous atmosphere maintained at a temperature of at least C.

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  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)

Description

Mal-d1 31, 1970 TIN Y AM AU MELT SPINNING PROCESS Filed Sent. 29, 1967 mvsmox TIN YAH AU ATTORNEY United States Patent 3,504,078 MELT SPINNING PROCESS Tin Yam Au, Wilmington, Del., assignor to E. I. du Pont de Nemours and Company, Wilmington, Del., a corporation of Delaware Filed Sept. 29, 1967, Ser. No. 671,832 Int. Cl. D01d /12 U.S. Cl. 264-210 1 Claim ABSTRACT OF THE DISCLOSURE This invention provides a high speed, melt-spinning process for producing mixed shrinkage yarn of enhanced differential filament length.
Summary of the invention This invention comprises a high speed, melt-spinning process for producing by co-spinning, from a polymer of PACM containing from 55 to 80% of the trans-trans isomer and dodecanedioic acid and a copolymer of the same composition wherein by weight of said acid is replaced by isophthalic acid, said polymers having a relative viscosity of 40 to 60, a mixed-shrinkage yarn. The molten polymers are co-spun at a temperature of at least 300 C. through separate holes in a spinneret into a heated non-oxidizing gaseous atmosphere maintained at a temperature of at least 130 C. and the filaments are withdrawn from the spinneret at a speed of at least 1500 y.p.m. such that the tension on the filaments in the spinning and quenching zone is less than 0.20 gram per denier. The filaments are quenched with air and then drawn at least 1.2x. Following draw, the filaments are annealed without further stretching at a temperature of 140 to 190 C.
The resulting yarns exhibit a higher differential shrinkage between the homopolymer and copolymer filaments after a boil-01f and heat setting treatment than yarns pro duced under similar conditions but under a higher spinning tension.
Description of drawings The drawings show a typical set-up for the high-speed process of the invention. Homopolymer stream A and copolymer stream B are extruded through separate holes of spinneret C. Chamber D represents a diffuser through which steam is passed to blanket the spinneret face. Tail pipe E is a heated conduit that maintains the filaments at elevated temperatures whereby excessive tension build-up is prevented. The filaments then pass over finish roll F to feed rolls G. The filaments are drawn between feed rolls G and draw rolls H. Some additional draw may be applied between draw rolls H and annealing rolls I, the latter being enclosed by a heated chamber as indicated by broken lines. The filaments are then led to a suitable windup means.
Standards and calculations The percent difference in filament length (DFL) between the high and low shrinkage filaments in the mixed shrinkage yarn is determined as follows: A water bath is heated to boiling over a /2 hour period. When the temperature reaches 50 C. a skein of the yarn with a suspended weight amounting to 4 mg. per denier (mg.d.) is placed in the bath and remains there for 10 minutes after the boiling point is reached. It is then removed and air dried with the weights attached. The DFL after exposure to heat setting temperature is measured by hanging the skein in an oven at 177 C. for 2 minutes under a load of 16 mg.d. A 40-centimeter strand, containing both high and low shrinkage filaments is cut from the boiled and heat-set skein. The average lengths of the filaments in Patented Mar. 31, 1970 Percent DFL=W where L is the average length of the longer filaments and L is the average length of the shorter filaments.
The expression relative viscosity as used herein signifies the ratio of the flow time in a viscometer of a polymer solution relative to the flow time of the solvent by itself. Measurements of relative viscosities as referred to herein and as measured in the examples is determined from a solution of 3.7 grams of polyamide in 50 ml. of a 1:1 mixture by wt. of 98100% formic acid and phenol at 25 C., unless otherwise noted.
EXAMPLE A polymer of bis(4-aminocyclohexyl)methane and dodecanedioic acid (PACM12) containing 70% of the trans-trans isomer and having a relative viscosity of 52 and a copolymer of PACM having the same isomer composition with by weight of dodecanedioic acid and 10% isophthalic acid having a relative viscosity of 48 are cospun through a single spinneret containing 36 holes, 18 holes for each polymer. The symmetrical Y-shaped spinneret holes consist of three intersecting slots, each of which is 6 mils wide and 15 mils long to produce filaments having a trilobal cross-section. The spinneret block temperature (spinning temperature) is 330 C. and the polymer temperature going to the spinneret is 300 C. The spinneret face is surrounded by a radial diffuser through which steam at 235 C. is fed to provide a hot nonoxidizing spinning atmosphere. The steam is further confined below the ditfuser by a heated tail pipe about 12 cm. long which is heated maintaining a temperature of 235 C. The filaments are then quenched with air, fed to a draw zone by feed rolls at a speed of 1930 y.p.m. in the spinning zone the filaments are under a tension of about 0.12 g.p.d. The filaments are then drawn in two stages, 1.175X in each stage, by two pairs of draw rolls operating at 2267 and 2663 y.p.m. respectively. The second pair of draw rolls are heated (thus termed annealing rolls) and enclosed in a heated chest at a temperature of C. The filaments are annealed at substantially constant length on the heated rolls prior to being wound up at a speed of 2680 y.p.m.
The drawn yarn is about 60 denier and has a tenacity of 3.40 grams per denier, an elongation of 33.5%, an initial modulus of 28.0 and an average DFL on boil-off and heat-set as described herein of 4.9%.
The tension on the filaments in the spinning zone must be less than about 0.2 g.p.d. Highter tensions reduce to an undesirable level the amount of diiferential filament length which can be obtained in the yarn after boil-off and heat-setting treatment as herein described. The ten sion may be reduced, for example, by increasing the spinnmg temperature, altering the spinneret orifice dimensions (smaller orifices reduce the tension) and by increasing the temperature of the non-oxidizing atmosphere in the spinning zone. As the spinning speed is increased, the spinning tension increases and adjustments must be made as described above to keep the tension below 0.20
mit higher DFL up to a total draw ratio of about 1.4 to 1.7. Draw ratios of 1.2 to 2.0x are preferred.
Drawn yarn annealing temperatures (temperature of the annealing rolls) of-140 to 190 C. are used. When temperatures less than 140 C. are employed, it is found that the processed yarn possesses undesirably high shinkage. Above 190 C. the obtainable yarn DFL is substantially reduced.
Spinning tension on the filaments is measured on the quenched filaments prior to contact with any surfaces such as guide pins or finish roll applicators. It is measured in a conventional manner using a yarn tensiometer such as a Type R-1092 of Rothschild =Instruments,'Zu- 7 rich, Switzerland. Since the filaments at the point of measurement contain no surface lubricant (finish), frictional problems due to filament contact with the tensiometer can be avoided by spraying a lubricant, such as a silicone oil, onto the moving filaments immediately prior to contact with the tensiometer measuring surfaces.
What is claimed is:
-1. A high-speed melt-spinning process for producing a mixed shrinkage yarn comprising co-spinning two molten polymer streams, one being a homopolymer of bis(4- aminocyclohexyl)methane of from 55 to 80% trans-trans isomer and dodecanedioic acid and the other being acopolymer of the same composition wherein about 10% by weight of said acid is replaced by isophthalic acid, said .4 polymers having a relatively viscosity of from to 60, at a temperature of at least 300 C, through separate holes in a spinneret into a non-oxidizing gaseous atmosphere maintained at a temperature of at least C. and withdrawing the filaments from the spinneret at a speed of at least 1500 yards per minute and at a tension less than 0.2 gram per denier, quenching the filaments, drawing the filaments at least 1.2 and annealing the filaments without stretching at a temperature of between C. and C.
References Cited UNITED STATES PATENTS 3,017,686 1/1962 Breen et a1. 264l7l X 3,161,914 12/1964 Bloomfield et a1.
3,361,859 1/1968 Cenzato.
3,381,074 4/1968 Bryan et al. 264-l71 3,397,107 8/1968 Kimara et a1. 161-173 3,399,108 8/1968 Olson 264171 X 3,418,200 12/1968 Tanner 264171 X JULIUS FROME, Primary Examiner J. H. WOO, Assistant Examiner US. Cl. X.R. 264-176, 234
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3846532A (en) * 1969-01-29 1974-11-05 Bayer Ag Continuous spinning and stretching process of the production of polyamide-6 filaments

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3017686A (en) * 1957-08-01 1962-01-23 Du Pont Two component convoluted filaments
US3161914A (en) * 1961-07-28 1964-12-22 British Nylon Spinners Ltd Spinnerets for producing heterofilaments
US3361859A (en) * 1960-04-29 1968-01-02 Du Pont Melt-spinning process
US3381074A (en) * 1962-12-17 1968-04-30 Du Pont Process for spinning bicomponent filaments
US3397107A (en) * 1965-07-22 1968-08-13 Kanegafuchi Spinning Co Ltd Composite polyamide filaments with improved potential crimpability and method of making the same
US3399108A (en) * 1965-06-18 1968-08-27 Du Pont Crimpable, composite nylon filament and fabric knitted therefrom
US3418200A (en) * 1964-11-27 1968-12-24 Du Pont Splittable composite filament

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3017686A (en) * 1957-08-01 1962-01-23 Du Pont Two component convoluted filaments
US3361859A (en) * 1960-04-29 1968-01-02 Du Pont Melt-spinning process
US3161914A (en) * 1961-07-28 1964-12-22 British Nylon Spinners Ltd Spinnerets for producing heterofilaments
US3381074A (en) * 1962-12-17 1968-04-30 Du Pont Process for spinning bicomponent filaments
US3418200A (en) * 1964-11-27 1968-12-24 Du Pont Splittable composite filament
US3399108A (en) * 1965-06-18 1968-08-27 Du Pont Crimpable, composite nylon filament and fabric knitted therefrom
US3397107A (en) * 1965-07-22 1968-08-13 Kanegafuchi Spinning Co Ltd Composite polyamide filaments with improved potential crimpability and method of making the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3846532A (en) * 1969-01-29 1974-11-05 Bayer Ag Continuous spinning and stretching process of the production of polyamide-6 filaments

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