KR900004912B1 - Manufacturing process of electric conductive polyester fiber - Google Patents

Abstract

An electric conductive polyester fiber is manufactured by conjugated- spinning a polyester resin (I) contg. al least 95 mol.% ethyleneterephthalate gp., as a first component, and a low m.p. polyester resin (II) contg. 15-55 wt.% carbon black, as a second component. The carbon black has esp. 10-30 micro-m of particle dia. and 10-2 ohm.cm of natural specific resistance. The composition ratio of (I) and (II) is pref. 70:30-90:10.

Description

Manufacturing method of conductive polyester fiber

1 to 4 are enlarged cross-sectional cross-sectional views of the conductive polyester fibers produced by the present invention.

* Explanation of symbols for main parts of the drawings

a: conductive portion containing carbon black b: non-conductive polyester fiber portion

The present invention relates to a method for producing a conductive polyester fiber excellent in operability, physical properties and conductivity by using a carbon black master batch containing a low melting point polyester resin as a binder component.

U.S. Patent No. 3,803,453 of the method for producing conductive fibers containing carbon black is a method of complex spinning such that the conductive component is located in the core portion of the fiber. At least 1/15 had to be occupied, but the conductive part was completely sealed in the fiber, so the conductivity was not excellent.

In addition, Japanese Patent Application Laid-Open No. 51-143723 is a method in which the conductive portion is eccentrically positioned on the cross section of the fiber to solve the above problem, but this method is compatible with polyester fibers because the binder of the carbon black masterbatch is polyamide. There is a problem that the trimming phenomenon is frequent and the conductivity is poor because the conductive part is easily detached when stretching because there is no property.

The present invention solves the problems as described above, the characteristics of the present invention by using a highly concentrated carbon black masterbatch can exhibit sufficient conductivity even if the area of the conductive portion is reduced, and the low melting point polyester resin is a binder of the masterbatch By using it to improve the compatibility and affinity with the polyester fiber to improve the operation and physical properties at the same time bar to describe the present invention in detail as follows.

Low-melting polyester resins (melting point = 100 ° C. to 230 ° C.) used in the present invention usually have a polyester structure copolymerized with a component that lowers crystallinity and melting point.

At this time, the acid component mainly used is terephthalic acid, isophthalic acid, or a mixture thereof, and an aliphatic acid component such as adipic acid, sebacic acid, or the like may be used in combination.

As the glycol component, ethylene glycol, 1,4-butadiol, 1,6-hexanediol, 1,2-butanediol, 1,3-butanediol, or a mixture thereof is used, and polyethylene glycol and polypropylene glycol are used here. And polyether components such as polytetramethylene glycol may be used in combination.

The carbon black has a particle diameter of 10 to 30 μm and a specific resistivity of 10 ⁻² Ω · cm, which is a superconductive carbon black, and can be produced in a master batch by a conventional method such as compounding with a low melting polyester resin.

At this time, it is preferable to add after milling process to minimize the secondary particle formation between the carbon black fine particles, and to improve the stability of the master batch during the compounding process, conventional antioxidants, weathering agents, coupling agents (COUPLING) Additives such as these may be added.

The carbon black masterbatch thus prepared is used as the second component, the polyester resin having an ethylene terephthalate group of 95 mol% or more is used as the first component, and each of the cationic components is melted in an extruder, and then, Two-component composite conductive polyester fibers were prepared.

In this case, the cross-sectional shape of the two-component composite conductive fiber is a) a concentric cross-sectional structure in which the first component is a SHEATH phase of the fiber and the second component is a Core phase of the fiber (FIG. 2) or (b) One component is in the core of the fiber, the second component is a concentric cross-sectional structure (figure 4) in which the second phase is the fiber phase, and the second component is eccentrically positioned with respect to the first component, and the second component is the fiber. It may have an eccentric cross-sectional structure that is 10-50% exposed on the surface (FIGS. 1 and 3).

Such a change in the cross-sectional structure can be freely formed by a conventional method of changing the connection position of the holding plate of the holding device, the hole and the distribution plate discharge space directly above the holding plate. The component composition ratio of the two-component composite conductive polyester fiber can be 1st component: 2nd component = 97: 3 ~ 5: 95, but considering the functionality, operation and economic efficiency, 1st component: 2nd component = 70: 30 90 to 10 is most suitable, and the carbon black content ratio in the total fiber is preferably 1.5 to 16.5 parts by weight.

This is a test result of the present inventors, if the carbon black content ratio in the fiber is less than 1.5 parts by weight, the conductivity is extremely poor, and at a level of 16.5 parts by weight or more, it is inappropriate in terms of function and economics.

In addition, in the production of the conductive polyester fiber as the carbon black masterbatch using the low melting point polyester resin as described above, the first component: second component = 75: 25 to 90: 10 Suitable carbon black content in the polyester-based carbon black masterbatch is 15 to 55 parts by weight.

If the carbon black content in the carbon black master batch is 15 parts by weight or less, it is difficult for the carbon black to be present in a uniform continuous phase in the matrix, and in the case of 55 parts by weight or more, it is economically unsuitable.

In addition, when the size of the carbon black is 30mμ or more, the dispersibility is good, but the content ratio should be increased. When the carbon black size is 10mμ or less, it is difficult to crush and difficult to disperse.

The two-component composite conductive polyester non-drawn yarn prepared as described above can be used as a filament by stretching by a general drawing method or by forming a non-drawn yarn into a tow shape to prepare short fiber staples after tow stretching. Two-component composite conductive polyester partially drawn yarns may be prepared, and then stretch processed to produce stretch yarns, or ultra high-speed spinning to produce fully drawn yarns.

Compared with the conventional method, the present invention has excellent conductivity and excellent radioactivity, and does not cause dropping of the conductive portion due to high concentration of carbon black at the time of stretching.

This is because low-melting polyester resin has excellent flowability and bonding strength with carbon black, so that it is possible to easily manufacture a highly concentrated carbon black master batch with conventional compounding. In this case, even if the ratio of the entire conductive region is reduced, the decrease in conductivity does not occur, and the synergistic effect of the fiber properties can be obtained by shrinking the conductive portion.

Example 1

A polyester having an intrinsic viscosity of 0.65 TiO ₂ content of 3,000 ppm is used as the first component, and carbon black having a particle size of 15 mμ is uniformly dispersed in a low melting polyester resin, and carbon is contained in 100 parts by weight of the total low melting polyester fiber. Low melting point poly with 45 parts by weight of black, 0.15 parts by weight of IRGANOX-1010 (CIBA-GEIGY), and 0.15 parts by weight of Leica (LICA) -09 (KENRICH) as carbon coupling agent with respect to carbon black. With the ester-based carbon black master batch as the second component, the first component: second component = 6: 1, the cross-sectional shape of the fiber, the second component is located eccentrically with respect to the first component as shown in FIG. The composite was spun to expose the front side of the two components to the side of the fiber. At this time, the carbon black content of the entire filament is 6.43 parts by weight, and the fiber surface exposure rate is about 15% on the outer periphery of the fiber section.

The spinning speed was 1,350 m / min, and 180 deniers of undrawn yarn were obtained.

At this time, the two extruder temperatures of the spinning machine were 280-290 ° C. for the first component extruded part, 145-180 ° C. for the second component extruded part, and the temperature of the spin block was 290 ° C.

The stretched yarn of 60 denier 6 filaments was obtained by drawing this magnification 3.0 at hot roll 85 degreeC, and hotplate 135 degreeC.

The bicomponent conductive polyester fiber thus prepared had almost no difference in specific resistance after washing 3 times and 30 times, and thus had excellent washing resistance and satisfactory chemical resistance.

Properties and test results are shown in Table 1.

TABLE 1

Example 2

In the production of the non-drawn yarn under the same spinning conditions as in Example 1, the cross-sectional shape was as shown in FIG. 2, FIG. 3 and FIG.

The prepared non-drawn yarn was drawn in the same manner as in Example 1 to observe the physical properties of the conductive polyester fiber.

Physical properties are shown in Table 2 and it can be seen that the conductivity is slightly different depending on the fiber cross-sectional shape.

TABLE 2

Comparative Example 1

In preparing the second component of Example 1, carbon black having a particle size of 15 mμ was uniformly dispersed in a polyester having an intrinsic viscosity of 0.65 and a TiO ₂ content of 700 ppm, and thus carbon black with respect to 100 parts by weight of the total low melting polyester fiber. 45 parts by weight of a polyester-based carbon black masterbatch having a heat-resistant agent Iganox-1010 0.1 parts by weight and Leica-09 as a coupling agent 0.15 parts by weight of carbon black as a second component, The composite was spun as the second component = 6: 1.

At this time, the two extruder temperature was the same as the first component and the second component, and the fiber cross-sectional shape was prepared as shown in FIG.

Properties and test results are shown in Table 3.

TABLE 3

Claims (1)

The first component is a polyester resin having an ethylene terephthalate group of 95 mol% or more as a first component, and a low melting polyester resin containing 15 to 55 parts by weight of carbon black having a particle size of 10 to 30 mμ as a second component. Component: Second component = 70: 30-90: 10 A method for producing conductive polyester fibers which are composite spun with a conventional spun spinning device.

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