KR101856139B1 - The Method Of Manufacturing High Strength Phenoxy Fiber And High Strength Phenoxy Fiber By The Same - Google Patents

Abstract

(B) spinning the chip using a spinning nozzle at a spinning temperature of 250 to 300 ° C and a spinning nozzle of 0.4 to 1.0Φ; (c) ; (C) passing through the post-spinning cooling zone and solidifying by blowing at 15-25 ° C; (D) winding the solidified yarn at a winding speed of 500 to 1500 m / min; (E) multi-step stretching the wound yarn at a stretching temperature of 80 to 100 DEG C and a stretching ratio of 1.5 to 3.0; And (f) an interlacing step of 5 to 150 times / m of interlaced number by double interlacing after the multi-step stretching.

Description

 TECHNICAL FIELD The present invention relates to a high strength phenoxy fiber and a high strength phenoxy fiber,

The present invention relates to a high strength phenoxy fiber for composite stitching and a method for producing the same. More particularly, the present invention relates to a high strength phenoxy fiber for stitching a composite material using multi-stage stretching to prevent warping or distortion of prepreg sheets during the production of a composite material, And a manufacturing method thereof.

Fiber-reinforced composites are widely used in the fields of aerospace materials, civil engineering and construction materials due to their excellent properties such as light weight, high rigidity and abrasion resistance.

In recent years, the development of new functional fibers and new materials has provided new opportunities for material development by complementing the weaknesses of existing materials, as well as possessing properties that approach the limitations that materials can have. Fiber-reinforced composites using high-performance fibers are widely used in today's industries because of their strength and strength.

Most conventional fiber-reinforced composites have a two-dimensional structure, and the double-layer composite material has a disadvantage that it can not withstand a large impact strength or fatigue strength because it has weak interlayer coupling force because there is no reinforcing fiber in the thickness direction.

Composites made of two-dimensional preforms may exhibit interlayer separation due to external load. There are brading, weaving, knitting, and stitching as a method of manufacturing a three-dimensional preform, which is a method to overcome this disadvantage.

Among these, the stitching process directly reinforces the fiber directly in the thickness direction to the two-dimensional preform, so that the three-dimensionally reinforced structure can be easily obtained compared with other methods.

Therefore, researches to prevent fracture toughness and to prevent non-resistance breakdown of laminated composites by preventing interlayer separation are being actively carried out. The method of double stitching is the easiest method of manufacturing composite materials by reinforcement in the thickness direction And can be said to be a manufacturing method of a three-axis reinforced composite material capable of being carried out.

The method of manufacturing a composite material by stitching can form a loop at the same time by using a plurality of needles in a short time, so that the manufacturing cost is small and the stitch type or pattern can be variously changed.

Therefore, a process of binding the sheet of the composite material made of a fabric through the needle in the thickness direction to improve the strength plays an important role in the manufacturing process of the composite material.

If the strength of the reinforcing fibers used for stitching is too low, a gap may be formed between the prepreg sheets to deteriorate physical properties, and a crimping phenomenon may occur during impregnation of the resin, resulting in warping or twisting between the sheets.

Korean Patent Laid-Open Publication No. 2015-0135378 discloses an improvement to a fiber-reinforced composite material comprising a layer of fibrous material and a curable resin on one side or more of an inventive curable resin matrix, and a resin-impregnated or pre- There is no description about the use of phenoxy fibers as reinforcing fibers in the thickness direction in which the composites are vertically bound by the legs.

Korean Patent Laid-Open Publication No. 2013-0009887 discloses a thermoplastic resin multi-layer reinforcing sheet material comprising a plurality of reinforcing fibers arranged in a predetermined direction so that a reinforcing fiber sheet material formed in a sheet shape and a thermoplastic resin reinforcement There is no description about the use of the phenoxy fiber as the reinforcing fiber in the thickness direction in which the composite material is vertically bound.

Korean Patent Laid-Open Publication No. 2005-0020411 discloses a high-strength polyethylene-2,6-naphthalate fiber and a method for producing the same, and has proposed a multi-stage drawing process for the fiber. However, There has been no description of a method for increasing the number of interstitials after the multi-step stretching.

Therefore, it is difficult to expect a high strength effect by a general multi-step stretching method for stitching for vertical binding of a multilayer fiber composite material.

The present invention provides a production method capable of improving the strength of phenoxy fiber.

Another object of the present invention is to provide a method of producing a fiber having a high strength such that the phenoxy fiber can be used as a reinforcing fiber in the stitching method through the double interlacing step after the multi-step drawing in the manufacturing process.

The present invention provides a method for producing high strength phenoxy fiber, comprising the steps of: (a) preparing a phenoxychip; (b) heating the chip at a spinning temperature of 250 to 300 占 폚 to a thickness of 0.4 to 1.0 mm? Radiating using a spinning nozzle; (C) passing through the post-spinning cooling zone and solidifying by blowing at 15-25 ° C; (D) winding the solidified yarn at a winding speed of 500 to 1500 m / min; (E) multi-step stretching the wound yarn at a stretching temperature of 80 to 100 DEG C and a stretching ratio of 1.5 to 3.0; And (f) a step of interlacing the double-interlaced material at a stretch ratio of 5 to 150 times / m after the multi-step stretching.

The present invention also provides a process for producing a high-strength phenoxy fiber characterized by having a weight average molecular weight (mw) of 30,000 to 60,000 and a transition temperature (Tg) of 90 to 95 ° C, to provide.

           [Chemical Formula 1]

In the present invention, the step of preparing the phenoxy chip includes a step of drying the chip, wherein the chip is dried at 65 to 85 ° C under reduced pressure for 12 to 15 hours to maintain the moisture content at 0.01% or less And a method for producing the high strength phenoxy fiber.

The present invention also provides a high strength phenoxy fiber produced by the above method.

The present invention also provides a high strength phenoxy fiber characterized in that the fiber has a strength of 2.0 to 5.0 g / d.

The present invention also provides a high strength phenoxy fiber characterized by being able to use the high strength phenoxy fiber as a reinforcing fiber for a stitching method of a composite material. .

The present invention has the effect of improving the strength of the fiber through the double interlacing step after the multi-step stretching in the fiber production process.

Further, the present invention is characterized in that phenoxy fiber having improved strength can be used as a reinforcing fiber for a stitching method of a composite material.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view of a process for producing phenoxy fiber according to an embodiment of the present invention. FIG.

Hereinafter, preferred embodiments of the present invention will be described in detail. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

As used herein, the terms " about, " " substantially, " " etc. ", when used to refer to a manufacturing or material tolerance inherent in the stated sense, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view of a process for producing phenoxy fiber according to an embodiment of the present invention. FIG.

(B) spinning the chip using a spinning nozzle at a spinning temperature of 250 to 300 캜 and a spinning nozzle of 0.4 to 1.0 mm Φ; (c) ; (C) passing through the post-spinning cooling zone and solidifying by blowing at 15-25 ° C; (D) winding the solidified yarn at a winding speed of 500 to 1500 m / min; (E) multi-step stretching the wound yarn at a stretching temperature of 80 to 100 DEG C and a stretching ratio of 1.5 to 3.0; And (f) an interlacing step of 5 to 150 times / m of interlaced number by double interlacing after the multi-step stretching.

The preparation step of (a) phenoxychip is a step of preparing a phenoxychip as a component of the phenoxychip, and includes the atomic group C ₆ H ₅ O ^- derived from phenol.

Generally, it is contained in phenoxide and phenol ether, and the structure of the compound can be represented by the following formula (1).

[Chemical Formula 1]

The phenox chip of the present invention has a viscosity of 100-800 cps at 25 ° C, a weight average molecular weight (MW) of 30,000-60,000, and a glass transition temperature (Tg) of 90-95 ° C . In addition, the phenoxychip is prepared to have a dry moisture content of 0.01% or less for at least 12 hours under reduced pressure at 80 캜.

Next, (B) the spinning step is carried out by spinning the chip at a spinning temperature of 250 to 300 캜 using a spinning nozzle of 0.4 to 1.0 mmΦ while maintaining a pressure of 50 to 150 bar and a spinning speed of 1000 to 2000 m / min.

Further, in the present invention, it is preferable to set the L / D (length / diameter) of the extruder screw to 20 to 50. If the L / D of the screw is less than 20, uniform melting is difficult. If it exceeds 50, This is because the lowering of the molecular weight is severe and the physical properties are lowered

Further, in the present invention, adjusting the filtration retention time in the pack to 3 to 30 seconds is an important factor. If the filtration retention time in the pack is less than 3 seconds, the filtering effect of the foreign substance is insufficient, and if it is more than 30 seconds, the increase in the packing pressure is excessive,

(C) In the solidification step, the molten discharge yarn 4 generated in the (b) spinning step is solidified by passing through the cooling zone 3, and if necessary, from right below the nozzle 2 to the starting point of the cooling zone 3 That is, the hood length (L). This zone is referred to as delayed cooling zone or heating zone, which may have a length of 200 to 700 mm and a temperature of 300 to 400 ° C.

In the cooling zone 3, an open quenching method, a circular closed quenching method, and a radial outflow quenching method can be applied according to a method of blowing cooling air, . The solidified discharged yarn 4 can then be oiled to 0.5 to 1.0% by the emulsion applying device 5 while passing through the cooling zone 3.

(D) In the winding step, the spinning speed of the non-drawn yarn is set to 500 to 1,500 m / min in the feed roller 6.

(E) In the multi-step stretching step, the yarn passed through the feed roller 6 is once wound, and then a separate stretching process is used, or preferably a series of stretching rollers 7, 8, 9 and 10) to obtain a final drawn filament yarn 11, wherein the temperature of the second-stage filament winding is adjusted to 150 to 180 ° C. More specifically, first free drawing is performed at 0.5 to 3%, first stretching is performed at 150 to 180 占 폚 at 5 to 7 times, second stretching is performed at 160 to 200 占 폚 at 1.2 to 2.0 times, And the steam jet method may be applied to increase the uniformity of the high-ratio stretching during the first-stage stretching. Then, the stretched yarn can be heat-set at a temperature of 220 to 250 ° C and relaxed to 0 to 3% according to a conventional method.

Finally, (B) the step of entangling the double-interlaced fiber yarns causes the air fluid to vertically collide with the filaments, where turbulence parallel to the filament axis is created around the yarns and tangled or twisted together. At this time, the air is filament bundled according to the tension of the filament yarn, the speed and amount of the air, and at the same time, the yarn is completely randomly mixed and entangled. Such interfacing devices can be used with flammable devices.

As the air pressure increases, the fluid resistance of the seal generally increases, increasing almost linearly. However, it tends to decrease when the pressure is 4.5 to 5.0 kgf / cm 2 or 5.0 kgf / cm 2 or more.

In the interlacing process, the air pressure is preferably 3.0 to 5.0 kgf / cm 2. When the air pressure is less than 3 kgf / cm 2, the air pressure is insufficiently interrupted. When the air pressure is 5.0 kgf / cm 2 or more, The contact area may be irregular. Therefore, 3.0 to 6.0 kgf / cm 2 is suitable, and the double-interface device can increase the chirping probability with a relatively small air pressure.

Hereinafter, the present invention will be described in more detail with reference to examples. It is to be understood, however, that these examples are provided so as to understand the scope of the present invention, and are not to be construed as limiting the scope of the present invention.

Example

100 g of a phenoxyether component having a viscosity of 500 cps at 25 캜, a molecular weight of 4,500 and a Tg of 90 캜 was prepared and dried at 80 캜 for 12 hours to obtain a water content of 0.005%. Thereafter, the phenoxy chips are spinned at a spinning temperature of 250 ° C. using a spinning nozzle of 0.5 mmΦ, then passed through a cooling zone, solidified by blowing at 17 ° C., and immediately wound at a winding speed of 500 to 1500 m / min. Further, the wound yarn was subjected to multi-step stretching at a stretching temperature of 90 DEG C at a draw ratio of 2.5, and then entangled with an air pressure of 3.0 kgf / cm < 2 >

Comparative Example 1

Under the same conditions as those in the above examples, general drawing was conducted at a drawing ratio of 1.5 instead of multi-stage drawing.

Comparative Example 2

The same conditions as those of the above embodiment are obtained, and the interlocking step which is a double-ended refresh interface is omitted.

※ Robust

A sample length of 250 mm, a tensile speed of 300 mm / min and a tensile strength of 80 turns / min were measured under standard conditions (20 ° C, 65% relative humidity) according to the provisions of ASTM D 885 using Instron 5565 (Instron, USA) m < / RTI >

Item Example  Comparative Example 1 Comparative Example 2
effect
Fineness (d) 16.4 16.5 16.5 Strength (g / d) 2.2 1.3 1.8 Shinto (%) 92.3 93.6 93.5

As in the results of Table 1, the fineness and elongation are not different from those of Examples and Comparative Examples 1 and 2. However, Comparative Example 1 in which multistage stretching is omitted and Comparative Example 2 in which a double interfacing step is omitted, Is low.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the inventions. It will be clear to those who have knowledge of.

1: Pack 2: Nozzle
3: Cooling zone 4: Melting zone
L: Hood length 5: Emulsion dispensing device
6: feed rollers 7, 8, 9 and 10: stretching roller
11: final drawn yarn (yarn) 12: dual interface means

Claims (6)

In the method for producing a high strength phenoxy fiber,
(A) preparing a phenoxychip;
(B) spinning the chip at a spinning temperature of 250-300 占 폚 using a spinning nozzle of 0.4-1.0 mmΦ;
(C) passing through the post-spinning cooling zone and solidifying by blowing at 15-25 ° C;
(D) winding the solidified yarn at a winding speed of 500 to 1500 m / min;
(E) multi-step stretching the wound yarn at a stretching temperature of 80 to 100 DEG C and a stretching ratio of 1.5 to 3.0; And
(F) A method for producing a high-strength phenoxy fiber having a fiber strength of 2.0 to 5.0 g / d, which can include an interlacing step of 5 to 150 turns / m by double interlacing after the multi-step drawing.
The method according to claim 1,
Wherein the phenoxy polymer has a weight average molecular weight (mw) of 30,000 to 60,000, a transition temperature (Tg) of 90 to 95 ° C and a viscosity of 100 to 800 cps at 25 ° C (Method for manufacturing high strength phenoxy fiber).

[Chemical Formula 1]
The method according to claim 1,
The step of preparing the phenoxy chip includes a step of drying the chip,
Wherein the chip is dried at 65 to 85 ° C under reduced pressure for 12 to 15 hours to maintain the moisture content at 0.01% or less.
A high strength phenoxy fiber having a fiber strength of 2.0 to 5.0 g / d produced by any one of the manufacturing methods of claims 1 to 3.
delete 5. The method of claim 4,
Characterized in that the high-strength phenoxy fiber can be used as a reinforcing fiber for a stitching method of a composite material.

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