KR20130078550A - Process for preparing lyocell filament fiber, lyocell filament fiber and tire cord - Google Patents

Process for preparing lyocell filament fiber, lyocell filament fiber and tire cord Download PDF

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Publication number
KR20130078550A
KR20130078550A KR1020110147559A KR20110147559A KR20130078550A KR 20130078550 A KR20130078550 A KR 20130078550A KR 1020110147559 A KR1020110147559 A KR 1020110147559A KR 20110147559 A KR20110147559 A KR 20110147559A KR 20130078550 A KR20130078550 A KR 20130078550A
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South Korea
Prior art keywords
filament
lyocell
fiber
spinning
lyocell filament
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KR1020110147559A
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Korean (ko)
Inventor
정종철
김우철
진상우
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코오롱인더스트리 주식회사
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Priority to KR1020110147559A priority Critical patent/KR20130078550A/en
Publication of KR20130078550A publication Critical patent/KR20130078550A/en

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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06Washing or drying
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D4/00Spinnerette packs; Cleaning thereof
    • D01D4/02Spinnerettes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44Yarns or threads characterised by the purpose for which they are designed
    • D02G3/48Tyre cords
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • DTEXTILES; PAPER
    • D07ROPES; CABLES OTHER THAN ELECTRIC
    • D07BROPES OR CABLES IN GENERAL
    • D07B2501/00Application field
    • D07B2501/20Application field related to ropes or cables
    • D07B2501/2046Tire cords
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20Cellulose-derived artificial fibres
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/06Load-responsive characteristics
    • D10B2401/063Load-responsive characteristics high strength
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2505/00Industrial
    • D10B2505/02Reinforcing materials; Prepregs
    • D10B2505/022Reinforcing materials; Prepregs for tyres
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S57/00Textiles: spinning, twisting, and twining
    • Y10S57/902Reinforcing or tire cords

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The present invention comprises the steps of spinning the lyocell manufacturing dope through a spinneret; Solidifying the spun dope to produce a filament; Passing the filament through a traction; Washing the filament passing through the towing unit in a water washing unit; And drying the washed filaments; and a method of manufacturing a lyocell filament fiber, a lyocell filament fiber, and a tire cord having a spinning draft ratio of the filament of 5.10 to 6.0.
The present invention by effectively controlling the spinning draft ratio of the discharge line speed and the filament running speed in the traction unit during the spinning process of lyocell filament fiber, to improve the stretching characteristics and processability of the fiber and to produce a lyocell filament fiber having excellent physical properties To help.

Description

Process for producing lyocell filament fiber, lyocell filament fiber, and tire cord {PROCESS FOR PREPARING LYOCELL FILAMENT FIBER, LYOCELL FILAMENT FIBER AND TIRE CORD}

The present invention relates to a method for producing a high-strength lyocell filament fiber for tire cords, and more particularly, by optimizing the spinning draft ratio of the discharge line speed and the filament running speed in the traction part during the spinning process of the lyocell filament fiber, excellent tensile strength In particular, it relates to a method for producing lyocell filament fibers having high strength and high modulus.

The tire is a composite of fiber / steel / rubber and generally has a structure as shown in FIG. 1. In other words, steel and fiber cords serve to reinforce rubber and form a basic skeletal structure in the tire. In other words, compared to the human body is a bone-like role.

The performance required for the cord as a tire reinforcement is fatigue resistance, shear strength, durability, resilience and adhesion to rubber. Therefore, a cord of appropriate material is used according to the performance required for the tire.

Commonly used materials for the cord are rayon, nylon, polyester, steel, and aramid, and rayon and polyester are used for body ply (or also called carcass, 6 in FIG. 1), and nylon is mainly capply. In Fig. 1 4, steel and aramid are mainly used for the tire belt portion (5 in Fig. 1).

The following briefly illustrates the tire structure and its characteristics shown in FIG. 1.

Tread (1): This part is to be in contact with the road surface to provide the necessary frictional force for braking and driving, to have good abrasion resistance, to withstand external shocks, and to generate little heat.

Body Ply or Carcass (6): A layer of cord inside the tire, which must support loads, withstand impacts and have strong fatigue resistance to flexing movements while driving.

Belt (5): Located between the body plies, consisting of steel wires in most cases to mitigate external shocks and maintain a wide tread ground to provide excellent driving stability.

Side Wall (3): refers to the rubber layer between the lower part of the shoulder (2) from the bead (9) and serves to protect the body ply (6) inside.

BEAD (9): A square or hexagonal wire bundle with rubber coating on the wire that rests and secures the tire to the rim.

Inner Liner (7): Located on the inside of the tire instead of the tube, this prevents air leakage and enables pneumatic tires.

CAP PLY (4): A special cord paper placed on the belt of some passenger radial tires that minimizes belt movement when driving.

APEX (8): A triangular rubber filler used to minimize the dispersion of beads, to mitigate external impacts, to protect the beads, and to prevent the ingress of air during molding.

Generally used tire cord material is nylon, polyester, rayon and the like. These materials are limited in size and use, etc. of the tires used due to their advantages and disadvantages.

Nylon fiber has high tensile elongation and high strength, and is mainly used for tires used on curved roads such as heavy trucks and unpaved roads. However, the nylon fiber is not suitable for a tire for a passenger car in which concentrated heat accumulation occurs inside the tire, and a low modulus is used to travel at high speed or require a ride comfort.

Polyester fiber has better shape stability and price competitiveness than nylon, and strength and adhesion are improved due to continuous research, and its usage is increasing in the tire cord field. However, it is not suitable for high-speed running tires because of limitations in heat resistance and adhesive strength.

Rayon fiber, a regenerated cellulose fiber, exhibits excellent strength retention and shape stability at high temperatures. Therefore, rayon fiber is known as an optimal tire cord material. However, due to the strong deterioration due to moisture, thorough moisture management is required during tire manufacturing, and due to the nonuniformity in yarn manufacturing, the rate of defective products is high. Above all, its price / performance ratio is very low compared to other materials, and it is mainly applied only to high speed or expensive tires.

In addition, general cellulose-based tire cords, such as rayon, have a rigid molecular structure and low elongation, and thus, it is difficult to withstand repeated high temperature expansion and contraction in a tire, and technology development for improving them is required.

Therefore, in the manufacture of tire cords having excellent high-speed driving properties and shape stability in the related art, research on improving the rigidity and strength reduction and low elongation of the structure of lyocell filament fibers is required.

The present invention is to provide a method for producing a lyocell filament fiber to improve the stretching properties and processability of the lyocell filament fiber.

The present invention also provides a lyocell filament fiber having excellent durability and stability and a tire cord comprising the same.

The present invention comprises the steps of spinning the lyocell manufacturing dope through a spinneret; Solidifying the spun dope to produce a filament; Passing the filament through a traction; Washing the filament passing through the towing unit in a water washing unit; And it comprises a step of drying the washed filament, and provides a method for producing a lyocell filament fiber of the spinning draft ratio of the filament represented by the following formula 1 is 5.10 to 6.0.

[Equation 1]

Radiation Draft Ratio = V 1 / V 0

Where V 0 is the linear velocity at which the dope is discharged in the spinning step, and V 1 is the traveling velocity of the filament coming out of the towing portion.

The present invention also provides lyocell filament fibers produced according to the above method.

The present invention also provides a tire cord comprising the lyocell filament fibers.

Hereinafter, a method of manufacturing a lyocell filament fiber, a lyocell filament fiber prepared therefrom, and a tire cord including the same according to a specific embodiment of the present invention will be described in detail. It will be apparent to those skilled in the art, however, that this is not intended to limit the scope of the invention, which is set forth as an example of the invention, and that various modifications may be made to the embodiments within the scope of the invention.

In addition, unless otherwise indicated throughout the specification, "comprise" or "contains" refers to the inclusion of any component (or component) without particular limitation, and the addition of other components (or components) It cannot be interpreted as excluding.

In the present invention, a filament bundle including a plurality of filament fibers is referred to as a 'multi filament', and a raw cord manufactured by upper and lower edges (or lower and upper edges) of the multifilament is referred to as 'ply twisted yarn', The deep cord treated with the adhesive for the tire cord in the twisted yarn is referred to as 'tire cord' or 'code'.

The lyocell filament fibers to be developed in the present invention have optimal properties for use in the use of tire cords, and in particular, have improved characteristics in elongation and strength.

The present inventors effectively control the spinning draft ratio of the linear speed at which the dope is discharged and the filament running speed passing through the traction part during the spinning process of the lyocell filament, thereby securing the excellent spinning stability and providing the lyocell filament fiber having excellent elongation and modulus. The fact that it can manufacture is revealed, and this invention was completed.

Hereinafter, a method for manufacturing a lyocell filament fiber according to an embodiment of the present invention will be described in detail with reference to the accompanying drawings so that a person skilled in the art can easily carry out the present invention.

Figure 2 is a schematic diagram showing an example of a spinning device for producing a lyocell filament fiber according to an embodiment of the present invention. Referring to the configuration of Figure 2, the general type lyocell multifilament manufacturing apparatus is a gear pump 11 for supplying a spinning spinning stock solution at a constant pressure, spinning spinning spinning spinning stock solution supplied from the extruder in the form of fibers A first coagulation bath 14 for solidifying the mold 12 and the uncoagulated fiber 13 discharged from the spinneret may be provided, and a second coagulation bath 15 may be further provided if necessary. The filament having passed through the coagulation baths 14 and 15 moves to the water washing part by driving the traction part 16, and removes the solvent from the water washing part 17. Subsequently, the filament washed with the washing part may be dried in the drying part 18 and then wound to obtain a final lyocell filament.

At this time, the spinning method of the lyocell filament fiber of the present invention is not particularly limited to the method shown in FIG.

According to the present invention, the radial draft ratio represented by the following formula ( 1 ) between the linear velocity (V 0 ) of the dope discharged from the spinneret (12) and the filament traveling speed (V 1 ) at the towing portion (16) is 5.10 to 6.0. It is characterized by optimizing and adjusting, and improving the stiffness and modulus of the resulting lyocell filament fibers can be given:

[Equation 1]

Radiation Draft Ratio = V 1 / V 0

Where V 0 is the linear velocity at which the dope is discharged in the spinning step, and V 1 is the traveling velocity of the filament coming out of the towing portion.

The spinning draft ratio of the present invention can be adjusted to 5.10 to 6.0, preferably 5.15 to 5.8, more preferably 5.12 to 5.6. The radiation draft ratio should be 5.10 or more in terms of high strength physical properties, and 6.0 or less in terms of securing radiation stability.

In the present invention, the linear velocity V 0 at which the dope is discharged in the spinning step is more specifically, a traveling speed at which the dope is discharged from the spinning nozzle of the spinneret 12. The discharge linear velocity V 0 of the spinning dope may be determined by the fineness of the final multifilament, the dope concentration, the spinning nozzle diameter, and the spinning nozzle odd number. Further, the traveling speed (V 1 ) of the filament coming out of the towing unit 16 is more specifically, the traveling speed of the filament at the last last pulling roll of the towing unit 16 before applying the solidified filament to the washing process . The present invention maintains the filament running speed, that is, the pulling roller speed at a higher value than the standard spinning speed in the towing unit, and the general spinning draft determined by the fineness, dope concentration, spinning nozzle diameter, spinning nozzle odd number, etc. of the multifilament ( Drafts can be given additional draw ratios.

In the present invention, the linear velocity V 0 at which the dope is discharged in the spinning step may be 18 to 41 m / min, more preferably 18.5 to 38 m / min, and more preferably 19.89 to 36.83 m / min. . However, the discharge linear velocity (V 0 ) of the spinning dope may exceed 41 m / min when the dope concentration is lowered or may be less than 18 m / min when the dope concentration is increased.

The dope thus solidified can be solidified to carry out a sufficient stretching process in producing the filament. The present invention can be carried out by adjusting the filament running speed to the optimum range when passing through the traction in terms of such stretching process. In particular, in the present invention, the filament running speed, ie, the reference spinning speed, entering the traction part may be 100 to 250 m / min, preferably 130 to 200 m / min, more preferably 150 to 180 m / min. have. In addition, the traveling speed (V 1 ) of the filament coming out of the towing portion may be 102 to 253 m / min, preferably 132 to 203 m / min, more preferably 152 to 183 m / min. The passage speed of the filament when passing through the traction unit can be increased by lowering the dope concentration or lowered by increasing the dope concentration.

In the present invention, the filament advancing speed at the time of entering and discharging the towing unit may be 100 m / min or more and 102 m / min or more, respectively, in terms of productivity improvement, and 250 m / min and 253 m / min, respectively, in terms of securing the radiation stability. It may be as follows. However, in the present invention, the traveling speed (V 1 ) of the filament coming out of the traction part, that is, the traveling speed of the filament in the final last traction roll of the traction part 16 is a standard spinning so that the high-strength high modulus characteristics can be expressed in the final fiber It can be kept high for speed.

In addition, in the present invention, the flow rate of the filament in the water washing step by step immediately after being discharged from the towing unit in step, and the traveling speed of the filament entering the towing unit and the traveling speed of the filament from the water washing unit can be performed the same. have.

The spinning draft ratio (draft, stretching ratio) of the multi-filament to be emitted in the present invention can be increased by adjusting the speed of the traction unit, that is, the traction roller. The purpose of this tow roller is to pull the solidified filament with a uniform and stable force, which is located between the radiating part and the water washing part, and to control the pulling roller speed to impart elongation at the radiating part. Called the spin draft ratio, the cellulose fibers are stretched once in the spinneret and are not stretched in subsequent processes.

The general spinning draft is determined by the desired fineness of the multifilament, the dope concentration, the spinning nozzle diameter, and the spinning nozzle odd number. have. That is, the discharge linear speed (V 0) at said conditions are determined when the spinning nozzle from the reference radiation rate is determined the ratio (V 1 / V 0) of the draw roller speed (V 1) and the discharge linear speed (V 0) It will be a draft draft. In addition, by lowering the speed after the traction roller in steps as much as the elongation ratio given by the traction roller to give a shrinkage ratio equal to the elongation ratio, it is possible to manufacture a high strength multifilament that does not lower the desired fineness and elongation properties.

For the lyocell manufacturing dope in the present invention, any spinning stock solution commonly used in the lyocell filament fiber manufacturing process may be used, such as cellulose, N-methylmorpholine-N-oxide (N-methylmorpholine-N-oxide; NMMO) and spinning stock containing water may be used.

The spinning stock solution may be prepared according to a conventional method, but is not particularly limited. Cellulose may be added to an NMMO aqueous solution containing N-methylmorpholine-N-oxide (NMMO) and water in a weight ratio of 93: 7 to 85:15. It is preferably prepared by dissolving at 7 to 18% by weight. In addition, the viscosity of the spinning stock solution is preferably maintained at 8,000 to 25,000 Poise.

The spinning process using the spinning stock solution can be carried out according to a generally known method, except for the step of spraying the coagulating solution of the lower part of the coagulation bath, preferably spinning dope at a temperature in the range of 80 ℃ to 130 ℃ Spinning, cooling the non-coagulated fiber through the air gap section, a coagulating solution section for solidifying the cooled uncoagulated fiber, and a washing section for removing residual N-methylmorpholine-N-oxide (NMMO) from the coagulated fiber. And, after passing the drying section, it is preferable to include the step of winding up.

Solidification of the filament spun through the spinneret in the present invention is carried out by passing through the air gap section through the coagulation liquid, in terms of controlling the coagulation rate of the filament, the temperature of the coagulation liquid is -20 ℃ to 30 ℃, preferably May be performed at 0 ° C to 30 ° C.

In addition, the coagulating solution in the present invention is not particularly limited because it can be prepared and used in the conventional composition in the art, preferably N-methylmorpholine-N-oxide (NMMO) NMMO aqueous solution containing water and water can be used, the concentration of NMMO in the coagulation solution to be 5% by weight or more in terms of optimization of the coagulation draft ratio in the pre-washing step, it can be used NMMO aqueous solution of 5 to 30% by weight.

In addition, in the present invention, after passing the filament through the coagulation solution, the process may be carried out without additional coagulation bath, and if necessary, after passing the filament through the first coagulation solution as shown in FIG. It may further comprise the step of further passing through the coagulating solution.

Subsequently, the prepared lyocell filament is passed through a towing unit, followed by washing and drying.

The filament passed through the coagulation bath has a state in which the internal structure is not fixed yet, and the elongation of the fiber can be adjusted to the optimum range by controlling the speed of the filament. The traveling speed of the filament in the coagulation bath is the same as described above in the filament running speed entering the traction.

According to the present invention, in consideration of the ease of recovery and reuse of the solvent after washing, NMMO can be removed with a washing solution. At this time, water may be used as the washing liquid, and other additives may be further included if necessary.

The filament fibers thus obtained can be carried out by adjusting to a temperature of 80 to 200 ℃, 90 to 180 ℃, or 100 to 150 ℃ in the drying step. The drying step may be carried out in a one-step drying process, it may also be carried out in a multi-stage drying process by varying the drying process conditions by dividing the interval.

At this time, the relaxation rate may be imparted to the filament fibers in the drying process. The relaxation rate may be 1.01% to 1.20%, preferably 1.01% to 1.15% relaxation rate, and more preferably 1.03% to 1.18% relaxation rate. By providing a relaxation rate in the drying process, it is possible to prevent damage to the fiber and to express excellent physical properties in the cord. The relaxation rate may be 1.01% or more in terms of expression of high elongation properties, and may be 1.20% or less in terms of securing stability of the washing process.

The relaxation rate can be imparted by lowering the flushing roller speed than the roller speed to withstand. That is, immediately after being discharged from the towing unit, the running speed of the filament is gradually reduced in the water washing unit, and the traveling speed of the filament entering the towing unit and the traveling speed of the filament coming out of the washing unit may be equally performed. Thus, the traveling speed of the filament coming out of the water washing section can be said to correspond to the speed in the final take-up roll, that is, take-up speed through the dryer.

Specific drying conditions of each step in the multi-stage drying process can be arbitrarily selected as necessary within the temperature range.

In addition, after-spinning and post-treatment techniques of lyocell filament fibers can be prepared using general wet spinning. In addition, the spinning method used for the production of rayon filament yarn, which is a cellulose fiber, may be used by modifying the lyocell process, and other conditions may be used in the technical field to which the present invention pertains.

On the other hand, according to another embodiment of the invention, there is provided a lyocell filament fiber produced according to the method described above. The lyocell filament fibers have excellent elongation and initial modulus.

As described above, by effectively adjusting the spinning draft ratio of the linear speed at which the dope is discharged and the filament traveling speed passing through the towing part during the spinning process of the lyocell filament, the lyocell filament fiber having excellent elongation and modulus can be provided. The points were confirmed through experiments. Such lyocell fibers can be used as industrial fibers, such as materials for tire cords.

The lyocell filament fibers of the present invention may have a tensile strength of at least 7 g / d or 7 to 10 g / d, preferably at least 7.1 g / d, more preferably at least 7.2 g / d. The tensile elongation of the fibers may be at least 4% or at least 4% to 15%, preferably at least 5%, more preferably at least 6%. In addition, the modulus of the fiber, that is, the initial modulus of the fiber may be 235 g / d or more or 235 to 400 g / d, preferably 240 g / d or more, more preferably 245 g / d or more.

In addition, the lyocell filament fibers of the present invention may have a fineness of 1,000 to 3,000, preferably 1,500 to 2,500, more preferably 1,650 to 2,200. The degree of crystallinity of the fibers may be 40 to 52, preferably 42 to 48, more preferably 44 to 46.

The lyocell filament fibers of the present invention have a fineness variation of single yarn of 2% or less, cutting strength and elongation variation (CV%) of 8% or less, and evenness (U%) of 3% or less, more preferably 2.5% or less. Can be

On the other hand, according to another embodiment of the invention, there is provided a tire cord comprising the lyocell filament fiber.

The tire cords of the present invention may comprise 2-3 ply twisted yarns with a total number of filaments of 400 to 6,000, a total fineness of 400 to 9,000 deniers and a twist of 200 to 600 TPM.

The lyocell tire cord of the present invention is excellent in shape stability and durability and can be applied to applications such as body plies or cap plies of pneumatic tires.

Tire cord of the present invention by twisting the lyocell filament fibers to produce a ply twisted yarn of 2 to 3 ply (ply), the twisted yarn is treated with an adhesive solution for tire cord according to a conventional dipping method, and dried and It can be produced by heat treatment.

In addition, the adhesive solution may be a conventional tire cord impregnation solution, preferably a resorcinol-formaldehyde-latex (RFL) adhesive solution may be used.

The cord passing through the adhesive solution is manufactured as a tire cord through a drying process and a heat treatment process. The drying process is carried out with a tension of 20 to 2,000 g / cord for 1 minute to 10 minutes at 105 to 160 ℃, the heat treatment process is carried out with a tension of 20 to 2,000 g / cord for 1 minute to 10 minutes at 105 to 220 ℃ can do.

In the drying step, moisture existing in the lyocell is dried, and in the heat treatment step, the impregnation solution is reacted to impart adhesion to the tire cord.

In the present invention, matters other than those described above can be added or subtracted as required, and therefore, the present invention is not particularly limited thereto.

The lyocell filament manufacturing process of the present invention can secure excellent spinning stability and improve spinning performance by adjusting the spinning draft ratio of the filament running speed in the discharge line speed and the towing portion during the spinning process, the lyocell filament fiber of the present invention And tire cords exhibit excellent elongation and strength properties.

1 is a partial cutaway perspective view showing a configuration of a general tire.
Figure 2 is a schematic diagram showing an example of a spinning device for producing a lyocell filament fiber according to an embodiment of the present invention.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples.

Example  One

A pulp with a degree of polymerization (DPw) of 1,200 and 97% of α-cellulose is mixed with an NMMO / H 2 0 mixed solvent (weight ratio 90/10) having a propylgallate content of 0.01% by weight, to prepare a lyocell dope having a concentration of 11% by weight. Prepared.

The lyocell dope was spun, coagulated, washed with water and dried using a spinning apparatus based on the configuration as shown in FIG. 2 to prepare lyocell filament fibers.

The production dope was maintained at a spinning temperature of 110 ℃ in the spinneret of the spinneret, and was controlled by spinning the discharge amount and spinning speed so that the final filament fineness is 1,650 denier. At this time, the linear velocity (V 0 ) at which the dope was discharged from the spinneret was 28.93 m / min, and was calculated based on the discharge amount, the number of the prisoners in the hole, and the diameter size.

The uncoagulated fiber discharged from the spinning nozzle of the spinneret was spun into a first coagulation bath and a second coagulation bath, and the coagulation solution was used at a temperature of 25 ° C., at a concentration of 85% by weight of water and 15% by weight of NMMO. The filament running speed, that is, the reference spinning speed, was maintained at 150 m / min as it passed through the coagulation bath. In addition, the coagulant concentration of the coagulation bath was continuously monitored using a sensor and a refractometer.

After passing through the coagulating solution, the filament enters the towing unit at a reference spinning speed of 150 m / min, and then raises the final towing roller speed (V 1 ) to 155 m / min in the towing unit to increase the final draft ratio by 5.2 times. It gave and extended | stretched.

The filament stretched through the traction roller was removed by the washing liquid sprayed in the water washing apparatus, dried on a drying roll and wound up to prepare a lyocell filament fiber. In this case, the traveling speed of the filament in the water washing part in the traction roller is gradually reduced, that is, immediately after being discharged from the traction part, the traveling speed of the filament is gradually decreased in the water washing part, and the traction rate is finally 1.03%. The running speed of the filament entering the part and the filament coming out of the flush portion was performed to be the same. In other words, the final winding speed was set to 150 m / min equal to the standard spinning speed. In addition, the drying temperature was given to 120 ℃ to 140 ℃ to maintain the moisture content of the filament at a level of 8% to 10%, dried for 60 seconds and then wound up.

Example  2

In the drawing step, when the infiltrating part enters the filament, the pulling speed of the roller is increased to 160 m / min from the standard spinning speed of 150 m / min, and the final radial drawing ratio (Draft) is 5.36 times, and the relaxation rate is finally 1.07%. Except for the adjustment, the same procedure as in Example 1 was repeated to prepare lyocell filament fibers.

Example  3

In the drawing step, when the infiltrating part enters the filament, the pulling speed of the roller is raised to 165 m / min from the standard spinning speed of 150 m / min, and the final radial drawing ratio (Draft) is 5.53 times, and the relaxation rate is finally 1.1%. Except for the adjustment, the same procedure as in Example 1 was repeated to prepare lyocell filament fibers.

Comparative example  One

In the drawing step, when the infiltrating part enters the filament, the traction roller speed is increased to 150 m / min from the standard spinning speed of 150 m / min, and the final radial drawing ratio is 5.03 times, and the relaxation rate is 1.0%. Except for the adjustment, the same procedure as in Example 1 was repeated to prepare lyocell filament fibers.

Comparative example  2

In the drawing step, when the infiltrating part enters the filament running speed, the traction roller speed is raised to 185 m / min from the standard spinning speed of 150 m / min, giving 6.2 times the final draft elongation ratio (Draft), and finally the relaxation rate is 1.23%. Except for the adjustment, the same procedure as in Example 1 was repeated to prepare lyocell filament fibers.

The physical properties of the lyocell filament fibers prepared according to Examples 1 to 3 and Comparative Examples 1 to 2 were evaluated by the following method.

The tensile strength , Elongation , And initial modulus

The strength and elongation of lyocell filament fibers obtained in Examples 1 to 3 and Comparative Examples 1 to 2 were measured using a universal testing machine (Model 5566, Instron) according to the American Society for Testing and Materials Standard (ASTM) D-885. Measured at room temperature. For this measurement, the lyocell filament fibers obtained in Examples 1 to 3 and Comparative Examples 1 and 2 were dried in an oven at 105 ° C. for 2 hours.

In addition, the initial modulus of elasticity of each lyocell filament fiber was measured under the conditions described below.

The specific measurement conditions were as follows, and the measurement results were expressed by the average value of 10 repeated experiments.

(1) Tensile strength and elongation

    1) Crosshead Speed: 300 mm / min

    2) Experiment error: ± 1 MPa

(2) Initial modulus

    1) Head Speed: 300 mm / min

    2) Grip Distance: 250 mm

3) 25 ° C. and 60 RH% atmosphere

Fiber properties measured according to the above method are summarized in Table 1 below.

division Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Radiation discharge line velocity (m / min, V 0 ) 29.83 29.83 29.83 29.83 29.83 When entering the penetration
Filament running speed (m / min)
150 150 150 150 150
When discharging traction
Filament Running Speed (m / min, V 1 )
155 160 165 150 185
When discharging water
Filament running speed (m / min)
150 150 150 150 150
Final spinning draft ratio 5.20 5.36 5.53 5.03 6.20 % Relaxation 1.03 1.07 1.1 1.0 1.23 Tensile strength (g / d) 7.3 8.1 7.2 6.8 6.0 Tensile Elongation (%) 7.3 7.6 7.1 7.0 5.4 Initial modulus (g / d) 245 250 240 230 260

As shown in Table 1, the lyocell filament fibers of Examples 1 to 3 exhibited excellent tensile strength and tensile elongation compared to Comparative Examples 1 to 2, it was confirmed that the initial modulus can also be expressed with a high value.

1: Tread
2: shoulder
3: sidewall
4: cap fly
5: belt
6: body fly
7: inner liner
8: Apex
9: bead
11: Gear pump
12: spinneret (12)
13: Unclotting fiber
14: First coagulation bath
15: Second coagulation bath
16: towing unit
17: Flushing device
18: Drying device

Claims (9)

Spinning dope for lyocell manufacturing through spinneret;
Solidifying the spun dope to produce a filament;
Passing the filament through a traction;
Washing the filament passing through the towing unit in a water washing unit; And
Drying the washed filaments
Including;
Method for producing a lyocell filament fiber having a spinning draft ratio of the filament represented by the following formula 1 is 5.10 to 6.0:
[Equation 1]
Radiation Draft Ratio = V 1 / V 0
Where V 0 is the linear velocity at which the dope is discharged in the spinning step and V 1 is the traveling velocity of the filament from the towing section.
The method of claim 1,
The drying step is a method for producing a lyocell filament fiber is carried out at a temperature of 80 to 200 ℃.
The method of claim 1,
Method of producing a lyocell filament fiber to give a relaxation rate of 1.01% to 1.20% to the filament in the drying step.
The method of claim 3,
A method for producing a lyocell filament fiber which gradually lowers the traveling speed of the filament in the water washing part immediately after being discharged from the traction part.
The method of claim 1,
Method for producing a lyocell filament fiber to perform the same traveling speed of the filament entering the tow portion and the traveling speed of the filament from the water washing unit.
A lyocell filament fiber prepared according to any one of claims 1 to 5. The method according to claim 6,
A lyocell filament fiber having a tensile strength of 7 g / d or more, a tensile elongation of 4% to 15%, and an initial elastic modulus of 235 to 400 g / d.
The method according to claim 6,
Lyocell filament fibers having a fineness of 1,000 to 3,000.
A tire cord comprising lyocell filament fibers according to claim 6.
KR1020110147559A 2011-12-30 2011-12-30 Process for preparing lyocell filament fiber, lyocell filament fiber and tire cord KR20130078550A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108486668A (en) * 2018-03-16 2018-09-04 常熟市翔鹰特纤有限公司 A kind of staged water washing device
CN110578179A (en) * 2018-06-08 2019-12-17 郑州中远氨纶工程技术有限公司 Production method and production device of cellulose fiber filaments

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108486668A (en) * 2018-03-16 2018-09-04 常熟市翔鹰特纤有限公司 A kind of staged water washing device
CN110578179A (en) * 2018-06-08 2019-12-17 郑州中远氨纶工程技术有限公司 Production method and production device of cellulose fiber filaments

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