Classifications

• • D—TEXTILES; PAPER
  • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
  • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
  • D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
  • D02G1/18—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by combining fibres, filaments, or yarns, having different shrinkage characteristics
• • 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
  • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
  • D01D5/30—Conjugate filaments; Spinnerette packs therefor
  • D01D5/32—Side-by-side structure; Spinnerette packs therefor
• • 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
  • D01D5/42—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments
  • D01D5/423—Formation of filaments, threads, or the like by cutting films into narrow ribbons or filaments or by fibrillation of films or filaments by fibrillation of films or filaments
• • 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
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
• • 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
• • 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
  • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester 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
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
  • Y10S264/26—Composite fibers made of two or more materials

Definitions

• This invention relates to a process for producing composite filaments and more particularly to a process for producing splittable composite filaments.
• Composite filaments are well known in the art. Such filaments consist of at least two longitudinally extending components which are usually arranged in an eccentric manner with respect to one another so that the differing shrinkage propensities of the components results in the formation of a crimped fiber when the filament is appropriately treated, e.g., with hot water. Such filaments are produced by extruding the components in a side-by-side or sheath-core relationship. Recently it has been found that highly desirable fabrics may be prepared from sideby-side multicomponent filaments which split apart to give two or more filaments in place of each of the original filaments. Filaments of this type are disclosed and claimed in copending applications Serial No. 118,470, filed June 20, 1961, now US. Patent 3,117,362, and Serial No. 118,291, filed June 20, 1961, now US. Patent 3,117,906.
• the filament components remain adhered together during the steps of drawing and packaging of the yarn after extrusion. It is also desirable that the components remain adhered together until the yarn is woven into a fabric but that the components separate readily during the fabric finishing steps so that extraordinary measures do not have to be taken in order to achieve substantially complete splitting of the filaments. In addition, it is sometimes desirable that the filaments do not crimp clue to different retractive forces when removed from the package for fabric preparation.
• the components in the filament should, however, shrink to a substantially different extent when exposed to hot aqueous liquids in fabric finishing and also when subjected to higher temperatures in heat setting procedures.
• the above objects are accomplished by a process which comprises extruding at least one polyamide component having a relative viscosity measured after spinning of about 30 to 60 and at least one polyester component having a relative viscosity measured after spinning of about to 24 from a spinneret orifice in side-by-side relationship to form a composite filament, the ratio of the polyamide viscosity to the polyester viscosity being from 1.5 to 2.5, attenuating the composite filament by pulling it away from the orifice at a speed at least 40 times the speed at which it is extruded, quenching the extruded filament, and drawing the filament from 2 to 8 times its original length.
• the relative viscosity of the polyester component is from 18 to 22 when no polymeric additive is included and from 23 to 27 when from 2 to 15% of a polymeric additive is included.
• the filaments are drawn at a temperature above 100 C. but below their melting point and then heated at a temperature between about C. and 250 C. while being permitted to retract. By so treating the drawn filaments, substantially straight filamentary structures are provided. The period of heating should be sufiicient to cause a retraction in length of from 6 to 11%. Spinning speeds and attenuations within a broad range may be used.
• the filaments must be attenuated at least 40 times in order to prevent premature splitting; however, attenuations above about 1000 are usually unnecessary.
• 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 given in the examples were made with the following solutions:
• Extrusion viscosity refers to the relative viscosity of polymer samples which are taken before the spinneret assembly is put in place by collecting molten polymer as it is pumped in separate streams to the spinneret.
• the viscosities of the polyamide and polyester components in the yarn are determined as follows:
• the yarn sample has a finish on its surface, remove the finish by washing the sample with carbon tetrachloride or other suitable solvent.
• the sample remaining in the funnel is polyester. Rinse thoroughly with distilled water, and dry in a vacuum oven at 60 C.usually overnight. Determine the relative viscosity as described above.
• Precipitate the nylon by adding distilled water to the formic acid solution and stirring well. Let this precipitate stand one-half hour to be sure that precipitation is complete. Filter this preparationthrough a fine fritted glass funnel and then rinse the precipitate several times with distilled Water. Dry the precipitated nylon in a vacuum This is accomplished by flexing the end of the filament until it begins to splitand then pulling the individual components apart. Next, a suflicient number of the individual component filaments are collected to provide: a total denier for the filament bundle of about 85 (9.3 tex); The filament bundle is cut to a length of about 20 centimeters, the exact length being carefully observed.
• filament bundle is heated at 205 C. for 3 minutes in an m-cresol vapor bath under the same tension as used previously and the reduction in lengthof the filament bundle noted.
• the percentage reduction in length in the m-cresol vapor relative to the length of the bundle after the boil-off shrinkage measurement is referred :to as thermal shrinkage.
• the splittability of the filaments of this invention' is determined by the procedure given below. Samples for determination of premature splitting in drawn yarns are taken after reeling off to yards of yarn to remove any damaged yarn. If a single package is used to represent a yarn lot two samples at least 100 yards apart are taken. When using two or more packages to represent a yarn lot,'one sampling from each package is suflicient.
• the yarn of this invention is woven as a filling in a conventional 7 O-denier nylon warp to form a 100 x 64 plain weave fabric.
• the fabric is then scoured by boiling for 60 minutes in an aqueous solution containing 10 grams per liter of Varsol (trademark for Esso Standard Oil Comp-anys petroleum distillate), 0.5 gram per, liter of Triton X-100 (trademark for Roh'm'& Haas Companys alkyl-aryl polyether alcohol emulsifying agent) and 0.5
• spinning speed refers to the. a
• the expression attenuation refers to the ratio of: spinning speed to the linear velocity of the filaments as they pass through the spinneret orifices, both speeds being in yards per minute.
• normal fa'bric finishing refers to procedures used in the trade to finish polyester fabrics and includes the fabric. Less than 40% splitting in the test gives poor splittability in fabric finishing.
• the degree of yarn splitting is determined on samples taken as described above, according to the following procedure:
• Example I Polyhexamethylene. adipamide. and polyethylene terephthalate flake are prepared in the conventionel manner.
• the cross-sectional area of each spinneret orifice is 0.145
• neretand are .air quenched in the conventional manner.
• the filaments are subsequently drawn on a drawtwister uring a 100 C. draw pin and wound into a package in the conventional manner.
• the draw ratio is shown in Table 1 below.
• the fiinal drawn yarn consists of 26 filaments of 2.7 denier (0.3 tex) each, the polyamide component being 1.0 denier (0.11 tex) and the polyester component 1.7 denier (0.2 tex).
• the filaments are examined for premature splitting and splittability after weaving into fabric as described previously. Results are shown in Table 1 for three yarns, designated A, B, and C, in which the relative viscosity (RV) of the polyamide component at extrusion is progressively increased while the viscosity of the polyester component is held substantially constant. As can be seen, varying the polyamide viscosity within the limits previously specified has no appreciable effect on filament splittability.
• Table 2 shows the results obtained when the extrusion viscosity of the polyamide component is held substantially constant while the viscosity of the polyester component is lowered. As can be seen, the splittability of the filaments in fabric form is unsatisfactory for yarn D, yarn E is satisfactory in this respect, while yarn F exhibits excellent splittability.
• Example II Undrawn yarns I through P are prepared as described in Example I, except that an antistatic agent is added during polymerization to the 6-6 polymer.
• the antistatic agent employed is polyethylene oxide capped with nonylphenol and containing about 30 ethoxy units. This compound is added as a 30% aqueous solution to the stirred autoclave in sufficient amount to give 2.5 percent based on a weight of the final polymer.
• the undrawn yarn is attenuated by winding at a speed of 1500 y.p.m., which is about times the extrusion speed. The undrawn yarn is then drawn over a hot pin at the pin temperature and draw ratio given in Table 4.
• the yarn After drawing, the yarn is passed through a tube about 3 inches in length and 0.25 inch in diameter where high pressure steam is jetted onto the yarn at the tube entrance to give the temperatures shown in Table 4.
• the yarn is then wound into a package in the conventional manner at a speed of 750 y.p.m.
• Y-arn is removed from the package after winding to determine whether it develops a slight crimp due to differential retraction of the components or remains straight as desired.
• Table 4 also shows the boil-off shrinkage values for the two components and the difference in shrinkage between the two.
• the thermal shrinkage values and differences are given.
• straight filaments can be obtained under a number of different conditions.
• the combination of straight filaments, together with an appreciable difference in both boil-off shrinkage and thermal shrink-age is obtained only under carefully selected conditions.
• Yarns N and O are the only ones having straight filaments and a satisfactory level of boil-off shrinkage.
• Example III Yarns Q and R are prepared following the general procedure of Example II, except that the antistatic agent is omitted. Yarn is removed from the package after 8 4
• Example" VII Arnixture of p-xylylenediarnine and m-xylylenediamine containing 10% of the latter ,diarnine is combined with azelaic acid and polymerized. This copolyamide and Winding to determine whether it crimps or remains polyethylene terephthalate are extruded to form a comstraight. As shown in Table 5 below, yarn'Q which posite filament containing 50% of each componentfolis given 9% relaxation, remains straight while y-arn.R,i lowing the procedure of Example I.
• the filaments are which is' given only 6% relaxation, crimps.
• the split attenuated, drawn and wound up as described in Example tability of the filament is satisfactory.
• the copolymer. component in the filament has a rela- TABLE 5 I tive viscosity of 43.8, while the. polyethylene terephthalate has a relative viscosity of 19.7.
• the yarn istested Q R as'previously described/thefilaments are found to split satisfactorily .in fabric form: but exhibit no premature -1 s littin 1 assets/ pines???1; 221252313 was P Example VH1. Viscosity Ratio, (Hi/polyester. 2. 25 2.
• a modified polyethylene terephthalate polymer is pre- Relaxation: Temp $6. ..j 200 200 pared as described in US. Patent 3,018,272, Example I. Yam Ofi Package Straight Crimped This polymer, having a relative viscosity of 20, is ex-' truded in side-by-sidef relation with polyhexamethylene ple IV adipamide having a relative viscosity of 40 following .the Example IIIis repeated except that the filament cross-- Procedure Example The filam,ents are attenuamd section is round.
• Example I as found for the trilobal filament yarns Q and R of polyemldfi component'm yam 18 found to have Example In relative viscosity of 45.l while the polyester component Example V has a relative vlscosity of 19.2.
• the diamine consists Sphttmg .Poor yam propemlis' of trans-trans, 25% cistrans, and 5% cis-cis iso- T Vlscoslty of the Polyamld?
• Componeni be mers ad usted to-the proper level relative to the viscosity of As a viscosity stabilizer, 17.5 millimols of acetic acid the polyester. .component' Fallilre to do thls leads to i are added for every mol of the polyamide Salt. T118760 poor spinnability of the composite filament due to bendsalt solution is heated under 350 lbs/sq. in.
• The, filaments are attenuated, areusuany unnecessary and may l d t difficulties in drawn and wound up as descr bed in Example I.
• the attenuation, drawing tested yk Procedures prevlhusly deserlhed, filaments temperature,'and polyester viscosity levels should be addo not xh y Premature p g, hut split Sails. justed relative to one another as illustrated in the exfactorily in the fabric.
• the composite filaments are preferably heated to a temperature of at least about 80 C. before or during drawing or, while held at constant length, subsequent to drawing to achieve the desired splittability and also to obtain the desired shrinkage differences between the components. Heating the filaments in this manner leads to a higher shrinkage for the polyamide component when the fabric is subjected to hot aqueous treatments in finishing while the polyester component exhibits the higher shrinkage in subsequent heat-setting procedures.
• the shrinkage differences lead to optimum bulk and aesthetics in the fabric and also act as a driving force to promote splitting.
• the filament In order to produce a filament which does not spontaneously crimp when removed from the package for fabric preparation, the filament must be subjected to a hot relaxation or length stabilization treatment under carefully selected conditions of drawing and relaxation. To obtain uncrimped filaments,'while retaining a satisfactory level of boil-off and thermal shrinkage, the filaments must be drawn at a temperature above 100 C., preferably 115-130" C., and must subsequently be permitted to relax, sufiicient heat being applied during the relaxation step to cause a retraction in length of 6 to 11%. Where a steam treatment is employed, temperatures in the range of 150200 C. are preferred. Other heating means may be used, however, and if dry heat is employed a somewhat different temperature level may be required.
• Suitable fiber-forming polyamides and polyesters suit able for use in the present invention are those described in US. Patents 2,071,250, 2,071,253, 2,130,523, 2,130,- 948, 2,190,770 and 2,465,319.
• the preferred group of polyamides comprises polyhexamethylene adipamide, polyhexamethylene sebacamide, poly(epsilon-caproamide).
• Suitable polyesters besides polyethylene terephthalate include those containing recurring units derived from glycols with more than two carbons in the chain, e.g., diethylene glycol, butylene glycol, decamethylene glycol, and trans-bis-1,4-(hydroxymethyl)-cyclohexane.
• the yarns and fabrics prepared by the process of this invention are useful for many purposes.
• the very fine deniers and various cross-sectional shapes which can be obtained make the woven fabrics particularly desirable substitutes for silks and fine cottons.
• a process for preparing a splittable composite filament which comprises (1) extruding a polyamide component having a relative viscosity, measured after extrusion, of about 30 to and a polyester component having a relative viscosity, measured after extrusion, of about 22 to 30, the ratio of the viscosities of said polyamide and polyester components being from 1.5 to 2.5, and

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Mechanical Engineering (AREA)
• Manufacturing & Machinery (AREA)
• Multicomponent Fibers (AREA)
• Artificial Filaments (AREA)

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Cited By (13)

Citations (7)

• 0
  • NL NL279868D patent/NL279868A/xx unknown
• 1963
  • 1963-07-15 US US295242A patent/US3264390A/en not_active Expired - Lifetime
• 1964
  • 1964-07-14 BE BE650539D patent/BE650539A/xx unknown
  • 1964-07-15 GB GB29161/64A patent/GB1063286A/en not_active Expired

Patent Citations (7)

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