US3901989A - Composite filament - Google Patents

Composite filament Download PDF

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Publication number
US3901989A
US3901989A US381320A US38132073A US3901989A US 3901989 A US3901989 A US 3901989A US 381320 A US381320 A US 381320A US 38132073 A US38132073 A US 38132073A US 3901989 A US3901989 A US 3901989A
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Prior art keywords
nylon
filament
percent
crimp
copolyamide
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Hisao Hokonoki
Tatsuo Ishikawa
Masahira Sakashita
Tetsuhiro Kusunose
Noboru Fukuma
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Asahi Kasei Corp
Asahi Chemical Industry Co Ltd
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Asahi Chemical Industry Co Ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2922—Nonlinear [e.g., crimped, coiled, etc.]
    • Y10T428/2924—Composite
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2929—Bicomponent, conjugate, composite or collateral fibers or filaments [i.e., coextruded sheath-core or side-by-side type]

Definitions

  • COMPOSITE FILAMENT Inventors: Hisao Hokonoki; Tatsuo lshikawa;
  • the obtained filament is superior in crimp developing ability and the knit from the filament is especially suitable for. among oth' ers, stretch hosiery 9 Claims, 7 Drawing Figures PATENTED M182 5 I975 SHEET 3 BF 90 a0 70 so so 40 3o 20 I0 6M weight PATENTED msz ms 3. 901 ,989
  • shrinkage in boiling water of these known fiber was low.
  • Preferred shrinkage properties were especially required for panty stocking yarn, which is one of the predominant uses for this kind of fibers.
  • Filaments with shrinkage in boiling water more than percent necessitate a longer knitted fabric with course structure, due to taking into consideration heat shrinkage in boiling water and crimping shrinkage when knitted product is heat relaxed. Accordingly, for these known fibers, the conventional knitting machine can not be used and alteration of the machine such as modification of fabric tube is required.
  • large knit structure causes disadvantage in later processes such as crimp producing process and tends easily to induce defect in knitted fabric.
  • Japanese Patent Publication No. 25507/1967 was proposed.
  • the gist of this Japanese Patent Publication was:
  • composition as the one component substantially comprising crystallizable homogeneous polyamide, and the composition substantially comprising random non-isomorphic copolyamide containing at least percent of each two of contained polymer unit (preferably, one of the polymer units being same with homogeneous polyamide),
  • This invention relates to crimpable composite filament obtained by i. eccentrically forming into fiber, homogeneous polyamide and random copolyamide, ii. drawing thus obtained fiber,
  • Preferable shrinking percentage in boiling water of thus produced filament is less than 15 percent. most preferably around 10 percent. And number of crimps of thus produced crimpable filament is less than 25, preferably less than 20/25 mm.
  • Knitted fabric from thus obtained composite fiber develops crimp upon sufficient heat relax treatment by boiling water or steam and crystallization of copolymer occurs.
  • the obtained fiber is superior product with high crimp developing ability.
  • FIG. 1 shows the spinneret assembly for composite spinning used for the present invention.
  • FIG. 2 shows sheet of processing the yarn according to the invention.
  • FIG. 3 shows triangle co-ordinate diagram for copolyamide 6/66/6T.
  • FIG. 4 shows triangle coordinate diagram for copolyamide 6/66/6l0.
  • FIG. 5 shows triangle coordinate diagram for copolyamide 6/66/612.
  • FIG. 6 shows triangle coordinate diagram for copolyamide 66/6T/6l0.
  • FIG. 7 shows triangle coordinate diagram for copolyamide 66/6T/6l 2.
  • Homogeneous polyamide used for the present invention includes polycapramide (nylon 6), polyhexamethylene adiamide (nylon 66), polyundecamide (nylon ll), polydodecamide (nylon 12), polyhexamethylene decamide (nylon 6 l 0) and polyhexamethylene dodecamide (nylon 612).
  • Random copolyamide used for the present invention includes:
  • bicomponent copolymer of 6/66 prepared from scaprolactam (hereinafter referred to as 6M) and hexamethylene diammonium adipate (hereinafter referred to as 66 salt) with the amount of 6M in the range of 30-60 weight percent;
  • 6T salt hexamethylene diammonium terephthalate
  • tricomponent copolymer of 6/66/610 prepared from 6M, 66 salt and hexamethylene diammonium sebacate (610 salt), wherein its composition is represented by the area covered by a,b and c in FIG. 4, with the amount of 6M, 66 salt and 610 salt at each point of a,b and c being respectively represented by weight as 60z40z0, 30:70:0 and 30:40:30.
  • tricomponent copolymer of 66/6T/610 prepared from 66 salt, 6T salt and 610 salt, wherein its composition is represented by the area covered by a,b,c,d,e, and fin FIG. 6 with the amount of 66 salt, 6T salt and 610 salt at each point of a,b,c,d,e, and f being respectively represented by weight as 6252225115, 55:30:15, 45:35:20, :35:65, 0:20:80 and 17.5:22.5:60;
  • tricomponent copolymer of 6/66/6T having copolymerization ratio by weight of /70/25 or 5/60/35
  • tricomponent copolymer of 66/6T/6 l 0 having copolymerization ratio by weight of 60/30/10.
  • 40/40/20, 20/40/40 and 10/40/50, tricomponent copolymer of 66/6T/612 having copolymerization ratio by weight of 70/25/5, 60/30/10, 35/45/20, 20/50/30 or 10/50/40', etc can satisfy the crystallization condition for the present invention, but cannot produce enough crimp for crimp yarn, due to small shrinkage in boiling water which eventually causes only less than 10 percent of difference of shrinkage in boiling water between that of homogeneous polyamide.
  • tricomponent copolymer of 6/66/6T having copolymerization ratio by weight of 25/72.5/2.5 or 80/10/10; tricomponent copolymer of 6/66/610 with copolymerization ratio by weight of 20/70/10, 20/60/20, 20/50/30 or /45/40; tricomponent copolymer of 6/66/612 with copolymerization ratio by weight of /50/30, 20/60/20 or 20/70/10', tricomponent copolymer of 66/6T/6l0 with copolymerization ratio by weight of 20/20/60, 30/20/50, 40/20/40, 50/20/30, 70/10/20, 50/10/40, 30/10/60 or 20/ 10/70: tricomponent copolymer of 66/6T/612 with copolymerization ratio by weight of 20/30/50, 35/30/35, 65/20/15, 40/20/40, 10/20/70 or 30/10/60; etc can satisfy the requirement of shrinkage in boiling water as
  • tricomponent copolymer of 6/66/6T with copolymerization ratio by weight of 10/85/5, 10/80/10, 5/85/10, 5/90/5, 90/5/5, 85/10/5, or 85/5/10 can not satisfy both of crystallization condition and shrinkage in boiling water for copolymer specified according to the present invention.
  • tricomponent copolymer of 6/66/6T with copolymerization ratio of 20/20/60 or /20/65 which satisfy the condition of crystallization condition and shrinkage in boiling water, extremely lowers spinning ability and drawing ability, and therefore excluded from the present invention.
  • Random copolymer used for the present invention should be the copolymer, fiber from which shows more than 10 percent of the difference in thermal shrinkage between the fiber from homopolyamide and cannot be turned into crystalline structure as described in Japanese Patent Publication 25507/1967 upon exposure of steam at 200C for 10* 0.5 second in relaxed status, does not show by densitomer X-ray reflection characteristics along equatorial direction in the plane of 100), and (010, and accordingly shows only one peak instead showing inherently distinct two peaks and, upon relax treatment by boiling water or steam forms crystaline or pseudo-crystalline structure.
  • Composite filament having these properties can be obtained by introducing the yarn to heat-relax treatment zone under steam or heated gaseous fluid, which zone is provided after draw step.
  • Drawn filament was passed through chamber or tube under steam or fluid heated at l00-200C, for less than 0.5 second.
  • filament is fed to the chamber to obtain relax percentage of the filament being more than 15 percent, preferably 20-25 percent.
  • shrinking percentage in boiling water of the filament can be lowered to around 10 percent, while substantially avoiding crystallization of random copolymer component of the fiber.
  • FIG. 2 shows preferable example of heat relax treatment zone.
  • Undrawn filaments are fed from drawing zone (including delivery roll 3) to heat treatment chamber 5.
  • This chamber is equipped with a inlet for filament. Steam or other heated fluid is blown from a nozzle part in an arrow direction. Heat-relax condition of the filament can be kept excellent by blowing simultaneously from both of the inlet and the outlet. Filaments passed through this heat treatment zone are wound on a bobbin by a spindle.
  • copolymerization component is not crystallized during heat relax treatment step and there is no need to completely develop crimp at this step. Accordingly, stretching step to remove crimp is not necessitated and treating speed is remarkably enhanced up to i200 m/min, due to mild heat relax treatment.
  • shrinking percentage is calculated according to the following equation:
  • m is the length of the skein by removing the weight of 0.0012 g/d, allowing to stand for l minute and then suspending a weight of 0.33 g/d for one minute.
  • the number of crimps means number of crimps in 25mm wherein the crimp filament is suspended with a weight of 2 mg/d, by counting from the one peak to the other peak as one crimp or from the one trough to the other trough as one crimp.
  • V is the speed of the drawing roll. and V, is the speed of the delivery roll.
  • Relative viscosity (nreL) of the polymer is viscosity of the solution whereby lg of polymer is dissolved into ml. of 95.5 percent of sulfuric acid.
  • EXAMPLE I To I20 kg of 50 percent aqueous solution of hexamethylene diammonium adipate (hereinafter referred to as 66 salt) in an 400-! autoclave was added and dissolved 40 kg of e-caprolactam (hereinafter, referred to as 6M) to obtain the weight ratio of 66 salt to 6M being 60/40. Then the inside of the autoclave was purged with nitrogen for the polymerization. The autoclave was heated at 230C for 1 hour, while gradually removing steam and keeping the inside pressure at l7.5 kglcm Then the inside pressure was brought from 17.5 Kg/cm" to an atmospheric pressure over a period of l hour and heating was continued for l hour while flowing nitrogen at an atmospheric pressure.
  • 66 salt hexamethylene diammonium adipate
  • 6M e-caprolactam
  • the random copolyamide 66/6 component is supplied from groove (2), and the homopolyamide from grooves (b) and (c).
  • non-spun filaments are spun to 3.5 times through feed roll 1 and draw roll 3 and then heat relaxed by introducing the filament yarn to 30 cm longheating chamber 5 under steam kept at C, wherein steam was introduced from ejector 4 at the top of heating chamber 5 and the supply speed of the yarn was 800 m/min. and the yarn was heat-relaxed at a rate of 21 percent of relax in the heating chamber 5 by adjusting the speeds of draw roll 3 and delivery roll 6 to give 2ld/5f composite filament developping 20 percent of latent crimp (number of crimps being ll/25mm).
  • the fabric was subjected to heat relax treatment for 5 minutes in boiling water at l00C, followed by the steps of allow ing to dry in air elevating the heating temperature from normal temperature to 100C over 40 minutes, continuing heating treatment at 100C for 30 minutes, reducing the temperature to 60C over 15 minutes, and then dried in air for 24 hours. Stretch-back was measured in term of tension (g). when stretched to 50 per cent.
  • non-spun filament composite filaments yarn of 2ld/5f was obtained by following the same procedure for sample (I) of Example 1, except by employing heat-relax treatment in an atmosphere of hot air at 175C. Testing result was 22 percent for crimp developping ability and l 1 percent for shrinking percentage in boiling water. Evaluation of knitted fabric and X-ray measurement gave substantially same result as that for sample (I) of Example 1.
  • the copolyamide component is supplied from groove (a), and nylon 66 from grooves (b) and (c).
  • undrawn filaments are spun to 3.3 times through feed roll 1 and draw roll 3 and then heat relaxed by introducing the drawn yarn to 30 em long-heating chamber 5 under steam at I60C supplied from ejector 4 at the top of heating chamber 5 wherein the yarn was supplied at a speed of 700 m/min and was heat-relaxed at a rate of 23 percent in the heating chamber 5 by adjusting the ...-...---m.- .t M H. H. 4.0.... U H...
  • EXAMPLE 5 From the tricomponent random copolyamide 6/66/6T prepared as in Example 4 with a copolymerization ratio of e-caprolactam, hexamethylene diammonium adipate and hexamethylene diarnmonium terephthalate being 20/50/30 by weight and having relative viscosity of 2.47 as the one component and nylon 66 having relative viscosity of 2.47 as the other component, composite spinning as in Example 4 was conducted. Thus obtained undrawn filaments were drawn to 3.4 times on a drawing pin heated at 110C (2 in FIG.
  • Example EXAMPLE 6 From the tricomponent random copolyamide 6/66/6T prepared as in Example 4 with a copolymerization ratio of e-caprolactam, hexamethylene diammonium adipate and hexamethlene diarnmonium terephthalate being 30/65/5 by weight and having relative viscosity of 2.48 as the one component and nylon 66 having relative viscosity of 2.47 as the other component.
  • composite filament (III) of 22d/5f with number of crimps being I5/2Smm was obtained in the manner as described in Example 4.
  • EXAMPLE 7 The same procedure for preparing composite yarn as in Example 4 was followed except that the copolyamide with a copolymerization ratio of e-caprolactam, hexamethylene diammonium adipate and hexamethylene diammonium terephthalate being 40/10/50 by weight and having relative viscosity of 2.50 was employed.
  • the copolyamide with a copolymerization ratio of e-caprolactam, hexamethylene diammonium adipate and hexamethylene diammonium terephthalate being 40/10/50 by weight and having relative viscosity of 2.50 was employed.
  • undrawn composite filament was drawn to 3.3 times by a drawing pin (2 in FIG. 2) heated at ll0C, introduced to a 30 cm long-heating chamber under steam at l60C wherein steam was supplied from objector 4 at the top of heating chamber 5, and then heat-relaxed, wherein the yarn was supplied to the heating chamber 5 with a speed of
  • the composite fiber of 2ld/5f was prepared in the same manner as in Example 4 except that undrawn filaments yarn obtained in Example 4 was heat-relaxed in an hot-air atmosphere at 180C. Crimp developping ability and shrinking percentage in boiling water of the filment were 23 and 8 percent, respectively. Evaluation of knit and X-ray measurement gave substantially same result as that of Example 4.
  • EXAMPLE 10 To ISO Kg of percent aqueous solution of hexamethylene diammonium adipate (66 salt) in an 400-1 autoclave, was added anddissolved 5 Kg of hexamethylene diammonium sebacate and subsequently was added dissolved 35 Kg of e-caprolactam (6M) to obtain the weight ratio of 6M 66 salt 6l0 salt 35 5. Then the inside of the autoclave was purged with nitrogen for polymerization. The autoclave was heated at 230C for 1 hour, while gradually removing steam and keeping the inside pressure at 17.5 Kg/cm?
  • the copolyamide component is supplied from groove (a), and nylon 66 from grooves (b) and (c).
  • undrawn filaments are drawn to 3.5 times through feed roll 1 and draw roll 3 and then heat relaxed by introducing to 25 cm long-heating chamber under steam kept at 155C wherein steam was supplied from ejector 4 at the top of heating chamber 5 and whereby the yarn was supplied at a speed of 800 m/min. and the yarn was heat-relaxed at a rate of 22 percent in the heating chamber 4 by adjusting the speeds of draw roll 3 and delivery roll 6 to give composite fiber (V) of 22d/5f with number of crimps being /25 mm.
  • the single-component filament prepared only from random copolyamide components of the composite fiber (V) was, in the same condition as described above, drawn and subjected to heat-relax treatment, and then X-ray measurement according to Japanese Patent Publication No. 25507/1967 was conducted.
  • Table 9 Each of the testing results after drawing filament, subjecting to the heat-relax treatment and treating by boiling water were summarized in Table 9. The result shows no crystallization of said copolyamide during heat-relax treatment.
  • Table 9 6/66/6210 prepared as in Example l0 with a copolymerization ratio of e-caprolactam. hexamethylene diamm onium adipate and hexamethylene diammonium sebacate being 35/50/15 by weight and having relative viscosity of 2.45 as the one component and nylon 66 having relative viscosity of 2.47 as the other component. composite filament (VII) of 22d/5f with number of crimps being l4/2Smm was obtained in the manner as described for sample (V) in Example I0.
  • Example ID hexamethylene diammonium adipate and hexamethylene diammonium sebacate being /45/5 by weight and having relative viscosity of 2.53 as the one component and nylon 66 having relative viscosity of 2.47 as the other component, composite spinning as in Example ID was conducted.
  • EXAMPLE 13 The same procedure for preparing composite yarn as in Example 10 was followed except that random tricomponent copolyamide 6/66/610 with a copolymerization ratio of /50/20 by weight and having relative viscosity of 2.49 was used and that nylon 6 having relative viscosity of 2.45 was used as homogeneous polyamide, to obtain undrawn filament. From thus obtained undrawn filament, the composite filaments of 22d/5f with number of crimps 14/25 mm was prepared by following the same manner for sample (V) as described in Example 10, except that the non-spun yarn was drawn and subjected to heat relax treatment in hot air atmosphere at 175C. Crimp developping ability and shrinking percentage in boiling water of the fiber were 23 and 12 percent, respectively. Evaluation of knit and X-ray measurement gave substantially same result as that of the sample (V) of the Example 10.
  • EXAMPLE 14 To 150 Kg of percent aqueous solution of hexamethylene diammonium adipate (66 salt) in an 4004 aqutoclave, was added and dissolved 10 Kg of the salt of hexamethylene diamine and dodecane dicarboxylic acid (612 salt) and subsequently was added and dis solved 30 Kg of e-caprolactam (6M), to obtain the weight ratio of 6M 66 salt 612 salt 30 10. Then the inside of the autoclave was purged with nitrogen for polymerization.
  • the autoclave was heated at 230C for 1 hour, while gradually removing steam and keeping the inside pressure at 17.5 Kg/cm Then the inside pressure was brought from 17.5 Kg/cm to an atmospheric pressure over a period of 1 hour and heating was continued for 1 hour while flowing nitrogen at an atmospheric pressure for about 1 hour.
  • random tricomponent copolyamide having relative viscosity of 2.45 as the one component and nylon LII Incomplete in crystalline structure.
  • No peak separation was observed by densit-o-mctcr trace (one peak) Possesscs crystalline structure. Separation of two peaks in plane and 010.110 plane was clearly observed by densit-o-meter trace Possesscs crystalline structure. Separation of two peaks in 100 plane and (111),] It) plane was clearly observed by dcnsit-o-metcr trace.
  • the copolyamide component is supplied from groove (a), and nylon 66 from grooves (b) and (c).
  • FIG. 2 thus obtained non-spun filaments were spun to 3.5 times through feed roll 1 and draw roll 3 and then beat relaxed by introducing to 30 cm long'heating chamber 5 under steam at C wherein steam was supplied from ejector 4 at the top of heating chamber 5 and the yarn was supplied at a speed of 800 m/min.. and the yarn was heat-relaxed at a rate of 23 percent in the heating chamber 5 by adjusting the speeds of draw roll 3 and delivery roll 6 to give 22d/5f composite filament developing 25 percent of crimp with number of crimps being l7/25mm.
  • Crimp developping ability and shrinking percentage in boiling water of the fiber were 25 and 9 percent, respectively. Evaluation of knitted fabric, crimpability and stretch-back ability were good. The X-ray measurement gave substantially same result as that of the sample (V) of the Example 10.
  • EXAMPLE 15 From the random tricomponent copolyamide prepared as in Example 14 with a copolymerization ratio of e-caprolactam, hexamethylene diammonium adipate and salt of hexamethylene diamine and dodecane di carboxylic acid being 35/60/5 by weight and having relative viscosity of 246 as the one component and nylon 66 having relative viscosity of 2.47 as the other component, composite spinning as in Example 14 was conducted. Thus obtained undrawn filaments were drawn to 3.5 times and then introduced to 30 cm long-heat chamber 5 under steam atmosphere at 168C, wherein the yarn was supplied with a speed of l 100 m/min. and heat relaxed at 21 percent of relax to obtain 2ld/5f composite filament developing 10 percent of crimp with number of crimps being 7/25 mm.
  • EXAMPLE 16 From the randon tricomponent copolyamide 6/66/612 prepared as in Example 14 with a copolymerization ratio of e-caprolactam, hexamethylene diammonium adipate and the salt of hexamethylene diamine and dodecane dicarboxylic acid being 30/55/15 by weight and having relative viscosity of 2.48 as the one component and nylon 66 having relative viscosity of 2.47 as the other component, composite filaments (IX) 17 of 22d/5f with number of crimps being l7/25mm was obtained in the manner as described in Example l4.
  • Kg of percent aqueous solution of hexapositc filament (X) of 22d/5f with number of crimps methylene diammonium sebacate (6l0 salt) in an being l6/25mm was obtained by treating in the same 400-l autoclave, was added and dissolved Kg of manner as above-mentioned.
  • Crimp developping abil hexamethylene diammonium terephthalate (6T salt) ity and evaluation of knit prepared and treated by boiland subsequently was added and dissolved 25 Kg of ing water as in Example l of(lX) and (X) were shown 10 percent aqueous solution of hexamethylene diammoin Table 12.
  • X-ray measurement was made nium adipate (66 salt), to obtain the weight ratio of 66 for the single-component filament of copolyamide insalt: 6T salt: 6l0 salt 10 30 60.
  • Crimpability ponent copolyamide of 66/6T/6l0 having relative visand stretching back ability of the knitted fabric were cosity of 2.45 as the one component and nylon 66 havgood.
  • Crimp developing ability and shrinking percenting relative viscosity of 2.47 as the other component age in boiling water of the filaments were 24 and 7 percomposite spinning as in Example l was conducted. cent, respectively.
  • undrawn filaments were drawn to 3.3 From the above results, in view of crimp developping times on a drawing pin heated at l 10C (2 in FIG.
  • the composite fiber of 22d/5f with number of 66/6T/6l0 prepared as in Example 18 with a copolycrimps being l8/25mm was prepared by following the merization ratio of hexamethylene diammonium adisame manner as described in Example 14, except that pate, hexamethylene diammonium terephthalate and undrawn yarn was subjected to heat-relax treatment in hexamethylene diammonium sebacate being 15/25/60 hot air atmosphere at lC. Crimp developing ability and shrinking percentage in boiling water of the yarn were 24 and 10 percent. respectively.
  • the composite filament of 22d/5f (XII) with number of crimps being l4/25mm was obtained by treating in the same manner as above-mentioned.
  • EXAMPLE 21 To 220 Kg of 25 percent aqueous solution of the salt of hexamethylene diamine and dodecane dicarboxylic acid (612 salt) in an 400-1 autoclave, was added and dissolved 35 Kg of hexamethylenee diammonium terephthalate (6T salt) and subsequently was added and dissolved 25 Kg or 40 percent aqueous solution of hcxamethylene diammonium adipatc (66 salt), to ob tain the weight ratio of 66salt 6T salt 6l2 salt 10 35 55.
  • 6T salt hexamethylenee diammonium terephthalate
  • 66 salt hcxamethylene diammonium adipatc
  • the yarn having the same composition of (XII) was heat-relaxed-stretched as in the man ner of Example 1 of Japanese Patent Publication No. 25507/1967 to obtain composite fiber of 22d/5f.
  • the knitted fabric from thus obtained composite yarn was treated as above mentioned. Crimpability and stretching back ability of the knitted fabric were good. Crimp developing ability and shrinking percentage in boiling water were 24 and 9 percent, respectively.
  • EXAMPLE The same procedure for preparing composite yarn as in Example 18 was followed except that bicomponent copolyamide 6T/6l0 with a copolymerization ratio of 20/80 by weight and having relative viscosity of 2.5L From thus obtained undrawn composite filament, the composite fiber of 20d/5f with number of crimps being l3/25mm was prepared by following the same manner as described in Example l8, except that undrawn yarn was drawn and subjected heat-relax treatment in hot air atmosphere at I80C. Crimp developing ability and shrinkking percentage in boiling water of filament yarn were 25 and 10 percent, respectively. Evaluation of relative viscosity of 2.43 as the one component and nylon 66 having relative viscosity of 2.47 as the other component, composite spinning as in Example I was conducted.
  • EXAMPLE 22 From the random tricomponent copolyamide 66/6T/6l2 prepared as in Example 21 with a copolymerization ratio of 25/35/40 by weight having relative viscosity of 2.46 as the one component and nylon 66 having relative viscosity of 2.47 as the other component, composite filament (XIII) of 20d/5f with number of crimps being l3/25mrn was obtained in the manner as described in Example I8. On the other hand, using copolyamide 66/6T/6l2 with a copolymerization ratio being 35/25/40 by weight and having relative viscosity of 2.47. the composite filament (XIV) of 20d/5f with number of crimps being l4/2Smm was obtained by treating in the same manner as above mentioned.
  • the yarn having the same composition of(Xl ⁇ was heat-relaxed-stretched as in the manner of Example I of Japanese Patent Publication No. 25507/l967 to obtain composite fiber of 20d/5f.
  • the knitted fabric from thus obtained composite fibers was treated as above mentioned. Crimpability and stretching back ability were good. Crimp developing ability and shrinking percentage in boiling water were 24 and 8 percent, respectively.
  • yarns to be crystallized in heat relax step do not show good result by the treatment of the present invention but show good result by heat-relaxed-stretching treatment as described in Japanese Patent Publication No. 25507/1967. Good result can be obtained only by using the material of the present invention satisfying the condition described in the present specification.
  • EXAMPLE 23 The same procedure for preparing composite yarn as in Example I was followed except that copolyamide tricomponent copolyamide 66/6T/6l 2 with a copolymerization ratio of /35/60 by weight and having relative viscosity of 2.48. From thus obtained non-spun filament, the composite fiber of 22d/5f with number of crimps being 13/2Smm was prepared by following the same manner as described in Example 18, except that undrawn yarn was drawn and subjected to heat-relax treatment in hot air atmosphere at 180C.
  • Crimp developping ability and shrinking percentage in boiling water of the filaments yarn were 24 and ll percent, respectively. Crimpability and stretching back ability of the knitted fabric were good. Evaluation of knit and X-ray measurement gave substantially same result as that for sample (I) of Example l.
  • EXAMPLE 24 From the tricomponent random copolyamide 6/66/6T as in Example 4 with a copolymerization ratio of 30/30/40 by weight and having relative viscosity of 2.53 as the one component and nylon 6 having relative viscosity 2.45 as the other component, composite spinning as in Example 4 was conducted. Thus obtained un drawn filaments were drawn to 3.3 time on a drawing pin heated at l C (2 in FIG. 2) and then by introducing to 30cm long-heating chamber under steam at l73C. wherein the steam was supplied from heat ejector at the top of heating chamber 5 and the yarn was supplied with a speed of 800m/min.. and heat-relaxed at 24 percent of relax.
  • EXAMPLE 25 The same procedure as in Example 4 was followed except that random tricomponent copolyamide 6/66/6T with a copolymerization ratio of 50/4/45 by weight and having relative viscosity of 2.45 was used as the one component, and the composite fiber of 2ld/5f with number of crimps being l7/25mm was obtained. Crimp developping ability and shrinking percentage in boiling water of the yarn were 27 and I0 percent, respectively. Evaluation of knitted fabric in terms of crimpability and stretch-back ability were good. X-ray measurement gave substantially same result as that of Example 4.
  • EXAMPLE 26 From the tricomponent random copolyamide of 6/66/6T prepared as in Example 4 with a copolymerization ratio of 15/65/20 by weight and having relative viscosity of 2.53 as the one component and nylon 66 having relative viscosity of 2.47 as the other component. composite spinning was conducted through a kidneytype composite spinneret as shown in FIG. 1 having l5 orifices, each with a diameter of O.5mmd
  • the copolyamide component is supplied from groove (a), and nylon 66 from grooves (b) and (c).
  • FIG. 2 thus obtained undrawn filaments were spun to 3.3 times through feed roll I and draw roll 3 and then heat relaxed by introducing to 30cm long-heating chamber 5 under steam at C wherein the steam was supplied from ejector 4 at the top of heating chamber 5 and the yarn was supplied at a speed of 900m/min and the yarn was heat-relaxed at a rate of I9 percent of relax to give l600d/60f composite filament with number of crimps being 5/25mm.
  • Crimp developping ability and shrinking percentage in boiling water of the fiber were l5 and 8 percent, respectively.
  • EXAMPLE 27 The same procedure as in Example 26 was followed except that tricomponent random copolyamide 6/66/6T with a copolymerization ratio of /50/40 by weight and having relative viscosity of 2.5 l was used as the one component to obtain undrawn filament. After drawing 3.3 times on a drawing pin heated at [C (2 in FIG. 2), the yarn was then heat relaxed to obtain composite fiber of l600d/60f with number of crimps being 3/25mm. Crimp developping ability and shrink ing percentage in boiling water of the fiber were l3 and 7 percent. respectively. The carpet prepared as in Example 26 from thus obtained composite yarns was rich in bulkiness with superior quality. It was confirmed that the yarn was extremely excellent in tufting properties.
  • EXAMPLE 28 From the random tricomponent copolyamide 66/6T/6l0 as in Example l8 with copolymerization ratio of 50/30/20 by weight and having relative viscos ity of 2.54 as the one component and nylon 66 having relative viscosity of 2.47 as the other component. composite spinning as in Example 26 was conducted. Thus obtained undrawn filament were drawn to 3.3 times on a drawing pin heated at l20C (2 in FIG. 2) and then by introducing to 30cm long-heating chamber under steam at [70C, wherein the steam was supplied from ejector 4 at the top of heating chamber 5 and the yarn was supplied with a speed of 900m/min., and heatrelaxed at 18 percent of relax.
  • EXAMPLE 29 The same procedure as in Example 28 was followed except that random tricomponent copolyamide 66/6T/610 with a copolymerization ratio of 40/30/30 by weight and having relative viscosity of 2.45 was used as the one component, and the composite filaments yarn of l600d/60f with number of crimps being 4/25mm was obtained. Crimp developing ability and shrinking percentage in boiling water of the; fiber were l4 and 9 percent, respectively. Carpet prepared as in Example 26 from thus obtained yarns was rich in bulkiness and highly rcsilent with superior quality. The yarn was also extremely excellent in tufting properties.
  • EXAMPLE 30 The same procedure as in Example 28 was followed except that random tricomponent copolyamide 66/6T/6l0 with a copolymerization ratio of /30/45 by weight and having relative viscosity of 2.5] was used as the one component, and the composite filaments of l600d/60f with number of crimps being 6/25mm was obtained. Crimp developing ability and shrinking per- 24 centage in boiling water of the yarn were 15 and 7 percent, respectively. Carpet prepared as in Example 26 from thus obtained yarns was rich in bulkiness and highly resilient with superior quality. The yarn was also extremely excellent in tuft properties.
  • Example 3 The same procedure as in Example 26 was followed except that random tricomponent copolyamide 66/6T/6l2 with a copolymerization ratio of /30/20 by weight and having relative viscosity of 2.42 was used as the one component, to obtain undrawn composite yarn. Then, the yarn was drawn and subjected to heatrelax treatment as in Example 28, to obtain composite filaments yarn of l600d/f with number of crimps being 5/25mm. Crimp developing ability and shrinking percentage in boiling water of the yarn were l4 and 8 percent, respectively. Carpet prepared as in Example 26 from thus obtained yarns was rich in bulkiness and highly reesilient with superior quality. The yarn was also extremely excellent in tufting properties.
  • EXAMPLE 32 The same procedure as in Example 3! was followed except that tricomponent copolyamide 66/6T/6I 2 with a copolymerization ratio of 35/35/30 by weight and having relative viscosity of 2.52 was used the one component, and the composite fiber of l600d/60f with number of crimps being 8/25mm was obtained. Crimp developping ability and shrinking percentage in boiling water of the fiber were l5 and 9 percent, respectively. Carpet prepared as in Example 26 from thus obtained yarns was rich in bulkiness and highly resilient with superior quality. It was confirmed that the yarn was also extremely excellent in tufting properties.
  • EXAMPLE 33 Undrawn yarn was prepared as in Example 4 from random tricomponent copolyamide of 6/66/6T with a copolymerization ratio by weight of 20/30/50 and having relative viscosity of 2.55 as the one component and nylon 66 having relative viscosity of 2.47 as the other component.
  • undrawn composite filament was drawn to 3.3 times by a drawing pin (2 in FIG. 2) heated at l l0C, introduced to a 30cm longheating chamber 5 under steam atmosphere at C, supplied from ejector 4 at the top of heating chamber 5 and then heat-relaxed, wherein the yarn was supplied to the heating chamber 5 with a speed of 800m/min.
  • a crimpable partially heat relaxed composite nylon filament comprising eccentrically arranged homopolyamide and random copolyamide components, the homopolyamide component being selected from the group consisting of nylon 6, nylon 1], nylon 12, nylon 66, nylon 6 l 0 and nylon 61 2, the random copolyamide component being non-crystalline and being made up of monomeric units of a. nylon 6 and nylon 66 containing 30 to 60 weight percent of nylon 6,
  • nylon 6, nylon 66 and nylon 6T of a composition falling within the shaded area of FIG. 3 b. nylon 6, nylon 66 and nylon 6T of a composition falling within the shaded area of FIG. 3, c. nylon 6, nylon 66 and nylon 6l0 ofa composition falling within the shaded area of FIG. 4, d. nylon 6, nylon 66 and nylon 6
  • nylon 66 e. nylon 66, nylon 6T and nylon 610 ofa composition falling within the shaded area of FIG. 6, or
  • a filament according to claim 1, wherein the random copolyamide component comprises monomeric units of nylon 6 and nylon 66 containing to 60 weight percent of nylon 6.
  • a filament according to claim 1, wherein the random copolyamide component comprises monomeric units of nylon 6, nylon 66 and nylon 6T of a composition falling within the shaded area of FIG. 3.
  • a filament according to claim I, wherein the random copolyamide component comprises monomeric units of nylon 6, nylon 66 and nylon 610 of a composition falling within the shaded area of FIG. 4.
  • a filament according to claim I, wherein the random copolyamide component comprises monomeric units of nylon 6, nylon 66 and nylon 6l2 ofa composition falling within the shaded area of FIG. 5.
  • a filament according to claim I, wherein the random copolyamide component comprises monomeric units of nylon 66, nylon 6T and nylon 610 of a composition falling within the shaded area of FIG. 6.
  • a filament according to claim I, wherein the random copolyamide component comprises monomeric units of nylon 66. nylon 6T and nylon 6 I 2 of a composition falling within the shaded area of FIG. 7.
  • a filament according to claim I wherein the filament has 5 to 30 percent of crimp developing ability, less than I5 percent shrinkage in boiling water and a difference of at least 10 percent in the boiling water shrinkages of the homopolyamide and copolyamide components.

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Multicomponent Fibers (AREA)
US381320A 1972-07-27 1973-07-20 Composite filament Expired - Lifetime US3901989A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4277433A (en) * 1977-01-10 1981-07-07 Inventa Ag Fur Forschung Und Patentverwertung Process for ternary polyamide filaments
US4302507A (en) * 1977-11-10 1981-11-24 Rhone-Poulenc Textile Two-constituent polyamide filament and the process for its production
US4424257A (en) 1981-11-12 1984-01-03 Monsanto Company Self-crimping multi-component polyamide filament wherein the components contain differing amounts of polyolefin
US4521484A (en) * 1984-06-07 1985-06-04 E. I. Du Pont De Nemours And Company Self-crimping polyamide filaments
US5352518A (en) * 1990-06-22 1994-10-04 Kanebo, Ltd. Composite elastic filament with rough surface, production thereof, and textile structure comprising the same
WO2002008503A2 (fr) * 2000-07-25 2002-01-31 Solutia Inc. Fils de nylon elastiques
US20030201568A1 (en) * 2002-04-30 2003-10-30 Miller Richard W. Tacky polymer melt spinning process
EP2531545A2 (fr) * 2010-02-01 2012-12-12 Invista Technologies S.A R.L. Terpolymères à base biologique et procédé de fabrication de ceux-ci
CN109970970A (zh) * 2019-04-18 2019-07-05 东华大学 一种高强高韧透明尼龙材料及其制备和应用

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JP6899453B2 (ja) * 2018-01-24 2021-07-07 旭化成株式会社 偏心鞘芯型複合繊維を少なくとも片方の面に用いた複合長繊維不織布

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US3399108A (en) * 1965-06-18 1968-08-27 Du Pont Crimpable, composite nylon filament and fabric knitted therefrom
US3551277A (en) * 1966-10-10 1970-12-29 Kanebo Ltd Highly crimpable polyamide composite filaments
US3607610A (en) * 1967-01-31 1971-09-21 Asahi Chemical Ind Crimped composite filaments of polycaprolactam or polyhexamethylene adipamide, and a terpolyamide of e-caprolactam, hexamethylenediammonium adipate, hexamethylene diammonium sebacate
US3620904A (en) * 1970-07-23 1971-11-16 Snia Viscosa Highly crimpable polyamide composite filaments
US3779853A (en) * 1972-01-05 1973-12-18 Du Pont Crimpable bicomponent filament

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US3720576A (en) * 1966-03-11 1973-03-13 Asahi Chemical Ind Crimped composite fibers and process for preparation thereof
FR1600920A (en) * 1968-11-21 1970-08-03 Composite polyamide threads

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Publication number Priority date Publication date Assignee Title
US3399108A (en) * 1965-06-18 1968-08-27 Du Pont Crimpable, composite nylon filament and fabric knitted therefrom
US3551277A (en) * 1966-10-10 1970-12-29 Kanebo Ltd Highly crimpable polyamide composite filaments
US3607610A (en) * 1967-01-31 1971-09-21 Asahi Chemical Ind Crimped composite filaments of polycaprolactam or polyhexamethylene adipamide, and a terpolyamide of e-caprolactam, hexamethylenediammonium adipate, hexamethylene diammonium sebacate
US3620904A (en) * 1970-07-23 1971-11-16 Snia Viscosa Highly crimpable polyamide composite filaments
US3779853A (en) * 1972-01-05 1973-12-18 Du Pont Crimpable bicomponent filament

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4277433A (en) * 1977-01-10 1981-07-07 Inventa Ag Fur Forschung Und Patentverwertung Process for ternary polyamide filaments
US4302507A (en) * 1977-11-10 1981-11-24 Rhone-Poulenc Textile Two-constituent polyamide filament and the process for its production
US4424257A (en) 1981-11-12 1984-01-03 Monsanto Company Self-crimping multi-component polyamide filament wherein the components contain differing amounts of polyolefin
US4521484A (en) * 1984-06-07 1985-06-04 E. I. Du Pont De Nemours And Company Self-crimping polyamide filaments
US5352518A (en) * 1990-06-22 1994-10-04 Kanebo, Ltd. Composite elastic filament with rough surface, production thereof, and textile structure comprising the same
WO2002008503A2 (fr) * 2000-07-25 2002-01-31 Solutia Inc. Fils de nylon elastiques
WO2002008503A3 (fr) * 2000-07-25 2002-04-11 Solutia Inc Fils de nylon elastiques
US6413635B1 (en) 2000-07-25 2002-07-02 Solutia Inc. Elastic nylon yarns
US20030201568A1 (en) * 2002-04-30 2003-10-30 Miller Richard W. Tacky polymer melt spinning process
US7261849B2 (en) 2002-04-30 2007-08-28 Solutia, Inc. Tacky polymer melt spinning process
EP2531545A2 (fr) * 2010-02-01 2012-12-12 Invista Technologies S.A R.L. Terpolymères à base biologique et procédé de fabrication de ceux-ci
EP2531545A4 (fr) * 2010-02-01 2013-10-02 Invista Tech Sarl Terpolymères à base biologique et procédé de fabrication de ceux-ci
AU2011210623B2 (en) * 2010-02-01 2015-06-25 Invista Technologies S.A R.L. Bio-based terpolymers and process of making the same
CN109970970A (zh) * 2019-04-18 2019-07-05 东华大学 一种高强高韧透明尼龙材料及其制备和应用

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JPS5119043B2 (fr) 1976-06-15
FR2194804A1 (fr) 1974-03-01
FR2194804B1 (fr) 1976-05-07
JPS4930623A (fr) 1974-03-19
IN139336B (fr) 1976-06-05
DE2338286A1 (de) 1974-02-14
GB1415943A (en) 1975-12-03

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