KR100208954B1 - The manufacture method for the polyester conjugated fiber - Google Patents

Abstract

In the present invention, in the production of polyester fibers, one component (A) uses a polyether-ester block copolymer and the other component (B) uses a conventional polyester to prepare a conjugate fiber in a conjugated form. Cotton is bonded with irregularities, and is a method for producing a polyester composite fiber characterized by adding inorganic fine particles having a particle size distribution having different values to A component, manufactured by a conventional polyester melt spinning equipment, and bonded. As the surface is irregular, fairness, physical property uniformity and elasticity are good.

Description

Method for producing polyester composite fiber.

The present invention relates to a method for producing a polyester composite fiber excellent in elasticity, one component (A) is a polyether-ester block copolymer to which fine particles having two different particle size distributions are added, and another component (B ) Relates to a method for producing a polyester composite fiber having excellent workability and elasticity, in which a bonding surface of two components (A, B) is formed uneven using a conventional fiber-forming polyester.

Polyether-ester block copolymers produced by the polycondensation of phthalate esters with low molecular weight diols and poly (ether) glycols exhibit a polymorphic structure in their form, while the phase is a hard phase capable of crystallization The Han phase is composed of the soft phase which is in the amorphous state, and exhibits excellent elastic properties by physical crosslinking thereof, plasticizes at high temperature, chemical resistance, ozone resistance, heat aging resistance, tensile strength, tear resistance, impact strength, etc. It has excellent mechanical rigidity, and is used for automation parts, industrial hoses, packings, gaskets, cables, etc. by using molding technology such as extrusion and injection molding. It is also manufactured for textiles (Japanese Patent Publication No. 3-174043). Particularly, when fiberizing this block copolymer, elastic recovery ability similar to spandex is exhibited at low elongation compared with spandex, which is a polyurethane elastomer. It has good alkali resistance, heat setting resistance and high temperature and high pressure resistance, so that it can be interwoven with general polyester to produce a comfortable fabric (Japanese Patent Publication No. 3-8868, Hyeongpyeong 4-73241). .

However, in the preparation of such a block copolymer, by introducing the fourth component into the diacid and the diol and the polyether glycol having a long molecular chain, the polymer property stability is significantly decreased as the reaction mechanism is complexed (Japanese Patent Publication No. 2-117918, Pyeong 2-272055, pyeong 2-231959, pyeong 4-33919). In addition, in order to improve elasticity, when polyether glycol having a long molecular chain is added, crystallization is slowed down and viscosity becomes large. When extruding the polymer by spinning, a cooling zone is formed using a water quench bath. The manufacturing facilities are complicated and the fiber quality becomes unstable, such as multistage heat treatment (US Pat. No. 5,153,065).

Accordingly, the present invention is to solve the conventional problems, and as a result of thorough examination of the elasticity, processability, and facilities of the conventional polyether-ester block copolymer fibers, a conventional melt spinning equipment capable of air cooling can be used. By using it as it is, in order to simplify the process and to improve the resolution of the uncoated yarn of the block copolymer unwound during winding, fine particles having different particle size distributions are added during the polymerization to act as a crystal nucleating agent It is characterized in that to obtain a polyester fiber excellent in elasticity and processability, quality stability by controlling the.

That is, in the present invention, in the production of polyester fibers, one component (A) uses a polyether-ester block copolymer and the other component (B) uses conventional polyester to prepare a conjugate fiber in a conjugated form. Bonding surface is bonded to the unevenness, it is to provide a method for producing a polyester composite fiber, characterized in that the A component is added to the inorganic fine particles having a particle size distribution different from each other.

The present invention will be described in more detail as follows.

The polyester component constituting the hard segment of the polyether-ester block copolymer which is the basis of the elastic fiber of the present invention has a polybutylene terephthalate composed of terephthalic acid component and butylene glycol component as a main component. . Nevertheless, some of the components may be substituted for some of the other components.

That is, terephthalic acid may be substituted with dicarboxylic acid or oxydicarbon of 10 m0.1% or less, or may be substituted with 10 mlo% of dioxy component in the butylene glycol component.

Moreover, the polyether component which comprises a soft segment contains polyoxybutylene glycol as a main component.

However, polyether glycol substituted with a dioxy component other than butylene glycol component of 10 mol% or less may be sufficient. The polyether component is preferably 60-70wt% of the total copolymer.

The average molecular weight of the polyether portion is preferably 650 to 2500, the OH value is 40 to 190 (mgKOH / g), the polydispersion ratio (Mw / Mn) is 1.3 to 2.5, and the specific gravity is preferably 0.97 to 0.98.

If the average molecular weight is more than 2500, the OH value is less than 40mgKOH / g, the Mw / Mn is less than 1.3, or the specific gravity is less than 0.97, the polymerizability and polymer degradation occurs, away from the intention of the present invention.

In addition, when the average molecular weight is less than 650 or the OH value exceeds 190mgKOH / g, Mw / Mn exceeds 2.5, or the specific gravity exceeds 0.98, the elastic recovery is lowered, away from the intention of the present invention.

In addition, fine particles having different particle size distributions were used as crystal nucleating agents during polymerization in order to suppress the stickiness of the undrawn copolymer and to improve the dissolution properties of the undrawn copolymer. ) To (4) should be satisfied at the same time.

(S _A is the size of the fine particles A, S _B is the size of the fine particles B, W (A + B) is the amount of (A + B) added to the entire block copolymer.)

If it is out of the range of the above formulas (10 to (4)), the radioactivity is remarkably lowered due to the agglomeration of the fine particles, or the maritime properties are extremely poor.

The fine particles are selected from TiO ₂ , BaSO ₄ , CaCO ₃ , Al (OH) ₃ and polymerized in size and content satisfying the above formula.

The polyester fiber intended by the present invention is composite spun in the form of a side by side of the polyether-ester block copolymer and a conventional polyester, but has irregularities on the joint surface to increase elasticity and processability. It is characterized by the improved.

The concave-convex feature of the joining surface satisfies Eq.

(Where r is the radius of short fibers and T is the uneven length between both ends of the joint)

At this time If the value is greater than or equal to 1, the elastic recovery falls off, thereby leaving the intention of the present invention.

In addition, the composite fiber of the present invention is preferably 45 to 55:55 to 45 in the content ratio of the block copolymer and polyester, if it is out of the elastic recovery rate is lowered.

In the polyester composite fiber of the present invention, one component (A) uses a polyether-ester block copolymer and the other component (B) uses an ordinary fiber-forming polyester to provide unevenness on the joint surface of the two components. It was prepared, but the fine particles having two different particle size distributions were added to the component A to prepare a conventional polyester melt spinning equipment, and as a result, the processability, physical property uniformity and elasticity were good.

Example 1

To remove the water produced by direct esterification by adding 2.0 times mole% of 1,4-butanediol to the terephthalic acid and the acid component and the polytetramethylene ether glycol shown in Table 1 and raising the temperature from 160 ° C to 220 ° C for 4 hours. After synthesizing oligomer BHBT with n = 4 ~ 5 levels, TiO ₂ (size S _A ) with an average particle size of 0.03 μm was 0.5Wt% of the total block copolymer and CaCO ₃ (size of 0.3 μm with an average particle size). S _B ) is added to 0.5Wt% of the total block copolymer, and then transferred to a polycondensation reactor and reacted at 250 ° C. for 3 hours and 30 minutes under reduced pressure to thereby transesterify the polyether. -Ester block copolymer was obtained. At the beginning of the reaction, conventional polybutylene terephthalate catalyst and stabilizer were appropriately added.

After chipping the obtained polyether-ester block copolymer, this copolymer and polyethylene terephthalate were melt-bonded and spun-type normal air cooling system (Air Quenching System) of 50:50 content ratio. The spinning temperature was 260 ° C., and the take-up speed was 800 m / min.

The conditions, processability, physical property uniformity, and elastic recovery (at 200% elongation) of the fibers thus obtained are shown in Tables 1 and 2.

Example 2

The same procedure as in Example 1 was conducted except that the polydispersion ratio (Mw / Mn) of the polyether portion of the block copolymer was 1.6 and the OH value was 59. Together.

Example 3

Example 1 was carried out in the same manner as in Example 1, but polytetramethylene glycol 60Wt% PET: block copolymer 55:45 was carried out as shown in Table 1 to prepare a composite fiber and its properties are shown in Table 2.

Comparative Examples 1 to 6

A composite fiber is prepared similarly to Example 1, but it is out of the range of polydispersion ratio (Mw / Mn) (Comparative Example 1), or the particle size ratio S _A / S _B is out of 0.06 to 0.15 (Comparative Example 2, 3) Do not exceed the content ratio of block polymer and polyester of 45 to 55:55 to 45 (Comparative Examples 4 and 6) or to produce irregularities on the cross section of the composite fiber (Comparative Example 5). The properties are shown in Table 2 together.

In Table 1, MW is the weight average molecular weight, Mw / Mn is the weight average molecular weight / number average molecular weight S is the average particle size of the A particles (㎛), S is the average particle size of the B particles (㎛), W (A + B) is Ratio of A and B particle addition to weight of polymer, Where r is the fiber cross section radius and T is the length between the two ends ) FA (%) is (full Bobbin-Short Bobbim) / Full Bobbin x 100, FT (%) is (Short Bobbin-seed Short Bobbin) / Short bobbin x 100, elongation x (%) is average, The standard deviation and elastic recovery rate (%) represent the elastic recovery rate at 200% elongation according to JIS L 1073 (1977).

As shown in Table 2, it can be seen that Examples 1 to 3 have higher elongation and higher elastic recovery than Comparative Examples 1 to 6.

Claims (4)

In the production of polyester fibers, one component (A) uses polyether-ester block copolymer and the other component (B) uses conventional polyester to prepare a conjugate fiber in conjugated form, but the joint surface is uneven. Bonding to the left, and a method for producing a polyester composite fiber, characterized in that the A component is added to the inorganic fine particles having a particle size distribution different from each other. According to claim 1, wherein the average molecular weight of the polyether portion is 650 to 2500, the OH value is 40 to 190 (mgK OH / g), polydispersion ratio (Mw / Mn) is 1.3 to 2.5, specific gravity is 0.97 to 0.98 Method for producing a polyester composite fiber characterized in that. According to claim 1, wherein the different particle size and content of the A component (The fine particles S _A , S _B are each selected from TiO ₂ , BaSO ₄ , SiO ₂ , CaCO ₃ , Al (OH) ₃ , and W (A + B) is the amount of S _A + S _B for the whole block copolymer. A method of producing a polyester composite fiber, characterized in that the amount of addition (Wt%)) is satisfied at the same time. The cross-sectional shape of the composite fiber according to claim 1, wherein 1 (wherein r is the radius of the short fiber and T is the uneven length between both ends of the joining surface).