KR20040061344A - A Process for preparing multi-functional polyester and the Polyester produced by the process - Google Patents

Abstract

PURPOSE: A manufacturing method of multi-functional polyester fiber which is characterized by having excellent antibacterial property, deodorization, moisture-absorbing property and quick dry function, being light and having thermo-keeping property is characterized by using zeolite containing metallic ions and having excellent spinning workability. CONSTITUTION: Multi-functional polyester fiber is obtained by the step of: preparing polyester master batch chip containing zeolite type inorganic particles having metallic ions; mixing the polyester master batch chip with common polyester chip and melting a mixture; and then spinning the melted mixture through a spinning base having a parenthesis type cross-section to manufacture the fiber having a hollow type section. The zeolite type inorganic particles are characterized by having 0.01-5.0μm of particle size and 0.1-3.0μm of average particle size and containing at least 50wt.% of particles being below the average particle size.

Description

A process for preparing multi-functional polyester and the polyester produced by the process}

The present invention relates to a multi-functional polyester fiber having excellent antibacterial and deodorant properties, sweat absorption quick-drying, light weight and heat retention, and more specifically, the particle size is in the range of 0.01 to 5.0 ㎛, the average particle size is 0.1 to 3.0 ㎛ And a polyester master batch chip containing zeolite-based inorganic particles with metal ions having a particle size of less than 50% by weight of the total particle size or less and mixed with a general polyester chip in a proportion to melt, which has a specific cross section. The present invention relates to a method for producing a multifunctional polyester fiber spinning through spinneret.

As many people nowadays have a lot of indoor life that lacks sunshine such as high-rise buildings and underground spaces, opportunities for exposure to various microorganisms such as bacteria and fungi have become frequent, but sufficient measures are insufficient. In particular, synthetic fibers have less absorption capacity than natural fibers, so synthetic fiber products are attached to sweat and various organic substances secreted by the human body to provide an environment suitable for microbial habitats such as bacteria and fungi. It can cause discoloration and contamination of textile products and even diseases caused by infection of the human body. As a conventional technique for solving this problem, there are largely a method of antibacterial and deodorant processing in a post-processing step, and a method of modifying a polymer or mixing and spinning a substance excellent in antibacterial properties.

For example, Japanese Patent Laid-Open Nos. 59-134418 and 61-17567 disclose a method of applying a metal compound or a zirconia-containing liquid to the general-purpose polyester fiber by the spray method, which has a problem of poor durability of washing. . Korean Patent Application No. 193-0009061, which improves the above disadvantages, discloses a method of heat treatment after attaching an inorganic antimicrobial composition to a fiber, but this method also has a limitation in washing durability. Meanwhile, a method of mixing an inorganic antimicrobial agent with a liquid polyester type dispersant and introducing it into a spinning process (Korean Patent Application No. 1992-0008832), an inorganic zeolite, an oxide ceramic, a porous alumina silicate, and silica / alumina subjected to high temperature baking After preparing a master batch chip using a method for producing antimicrobial polyester fiber through mixed spinning (Japanese Patent Laid-Open No. 61-234390, 62-101643 and Korean Patent Application No. 1991-0014960, 1990-0022031) and the like are known. These methods are difficult to secure radioactivity during melt spinning due to the strong water absorption characteristics of inorganic antimicrobial agents, and problems such as deterioration of the physical properties of fibers due to viscosity decrease of spinning spinning solution, pressure rise by inorganic fine particles, and control of color defects and dispersibility are still maintained. Remains. On the other hand, Korean Patent Application No. 1998-012949 discloses a method using elvan which is excellent in adsorption power of harmful substances such as metal oxides and bacteria and effective minerals emit far infrared rays. Due to the strong attraction, it is difficult to control the particle dispersibility, it is difficult to secure the radioactivity when spinning the filament of less than 2 denier, and there is a fatal disadvantage that causes the wear of the machine during the spinning and stretching operation due to the nature of natural minerals.

Therefore, there is a need in the art for the development of a method for stably spinning polyester fibers exhibiting excellent antibacterial and deodorant properties.

Meanwhile, in the case of polyester, the development of a multifunctional fiber having various functions, for example, light weight, warmth, sweat drying and antimicrobial deodorization, attracts attention. There is a need for a manufacturing method that can produce fibers that exhibit the best performance and at the same time do not degrade the properties of polyester, such as excellent strength and elongation, and maintain a stable state during spinning. come. In particular, it has a high hollow ratio and shows excellent light weight, warmth and sweat absorption, and can express antibacterial and deodorizing function. Maintaining the castle was a problem not solved by the prior art.

The present inventors have made a thorough effort to solve the above problems in developing a multifunctional having antibacterial, deodorant and light weight, sweat-absorbent quick-drying and thermal insulation, newly recognized that the dispersibility of the inorganic has a great influence on the production of the multifunctional fiber As a result, a master batch chip was prepared using a zeolite containing metal ions, and then mixed with a general-purpose polyester, and then melted, and the resultant was formed in parentheses (ie, (()): see FIG. 3) through spinneret. When spinning, the present invention was confirmed that it is possible to reliably spin with a high production efficiency a fiber assembly that is excellent in the required function, while maintaining the excellent physical properties of polyester.

In conclusion, the present invention is to provide a method for stably spinning a multifunctional polyester fiber having excellent antibacterial, deodorant and light weight, quick drying and heat insulation.

1 is a schematic view showing an extrusion apparatus of a polyester fiber according to the present invention.

2 is a cross-sectional view showing a cross section of the fiber according to the present invention.

3 is a cross-sectional view showing a section of parenthesis-shaped spinnerets used in the present invention.

(Explanation of symbols for the main parts of the drawing)

1: Polyester Silo 2: MB Chip Silo

3: Auto blender 4, 4 ': motor

5: Extruder 6: Polymer Melting Pump

7: spin block 8: pack

10: polyester fiber 11; Hollow part

The present invention relates to a multi-functional polyester fiber aggregate having excellent antibacterial and deodorant properties, sweat absorption and quick drying, light weight and heat retention, and more specifically, the particle size is in the range of 0.01 to 5.0 ㎛, the average particle size is 0.1 to 3.0 A polyester master batch chip containing zeolite-based inorganic particles with metal ions having a diameter of less than 50% by weight and having a particle size below the average particle size is mixed with a general polyester chip and melted, and a specific cross section is formed. The present invention relates to a method for producing a multifunctional polyester fiber which is spun through a spun spinneret.

Hereinafter, the present invention will be described in more detail.

In the present invention, a polyester masterbatch chip containing one quantitative amount of zeolite-based inorganic particles having metal ions as an antimicrobial component is used.

The zeolitic inorganic particles used in the present invention are solid inorganic particles represented by the following Chemical Formula 1 prepared by exchanging a metal having antibacterial properties of silver, copper, zinc, and sodium with synthetic ions and sodium ions:

M (x / n) [(AlO ₂ ) _x . (SiO ₂ ) _y ] zH ₂ O

Wherein M is a metal selected from the group consisting of 1 to 3 valent metals, preferably Ag, Cu, Zn, Ca, Ni, and Fe, n is the valence of the cation M, and x + y is the unit cell ( Number of tetrahedrals per unit cell, z is the number of moles of water molecules).

The zeolite-based inorganic particles should have a size in the range of 0.01 to 5.0㎛, the average particle size should be 0.1 to 3.0㎛. According to the research of the present inventors, during spinning, the problem of lowering the radioactivity and the pressure increase due to the aggregation of the added particles is mainly due to the particle size, shape, surface area, charge, chemical properties and scatter of particle size.

In particular, the scattering degree of particle size directly affects the dispersibility of particles in the spinning melt. When the particle size is less than 50% of the average particle size, agglomeration phenomenon occurs very rapidly due to intermolecular attraction. Greatly decreases. Therefore, in order to prevent aggregation, inorganic particles having 50% or more of particles having an average particle size or less should be used. For example, when the average particle size is 0.5㎛, inorganic particles having a particle size of 0.5㎛ or less should be at least 50% by weight.

The zeolite inorganic particles having the above formulas contain at least 5% water and at least 30% water in their structure, regardless of whether they are natural zeolites or synthetic zeolites, and have the ability to adsorb moisture. Hydrolysis by water causes property deterioration. It is difficult to completely remove the moisture in the zeolite structure and to prevent the degradation of the physical properties of the polyester fiber due to the property of rapidly adsorbing the moisture of the atmosphere during the storage or master batch and the fiber manufacturing process even if the moisture is removed to a satisfactory level. The water content in the process should be 40 ppm or less, preferably 30 ppm or less.

According to the research of the present inventors, the decrease in viscosity of the melt when the zeolite inorganic particles are mixed and spun in the spinning melt is due to the aggregation of fine particles and strong water absorption characteristics and hydrolysis in the process by the water absorption. Therefore, in the present invention, a master batch chip of polyester containing inorganic particles was first prepared and mixed melt spun to solve the above problem.

The master batch chip to be manufactured should use a high viscosity, for example, polyester with an intrinsic viscosity (IV) of 0.70 to 0.95 in order to prevent radioactivity and property deterioration due to viscosity decrease, and the inorganic material in the manufactured master batch chip The particulate content should be 1 to 20% by weight.

The prepared master batch chip is melted by mixing with a general polyester chip, and spun through a spinneret having a bracket-shaped cross section as shown in Figure 3 to obtain a fiber having a hollow cross section.

When having a hollow cross section as in the present invention, it is possible to produce a polyester fiber excellent in the sweat-absorbing quick-drying function by the capillary effect and light weight and heat retention by the hollow. More specifically, the fiber according to the present invention is a hollow cross section. Moisture is freed by the capillary effect due to hollow, absorbs sweat and discharges faster than natural fiber, and maintains dry and comfortable feeling at all times by increasing the lightness and warmth according to air layer content. . The hollow ratio of the hollow cross section is preferably 5% to 30%. If the hollow ratio is less than 5%, there is no effect, if the hollow ratio is more than 30% will cause problems in radioactivity and physical properties.

Mixing with the general polyester chip should adjust the concentration of fine particles in the final obtained fiber to be 0.1 to 5% by weight. If it is out of the above range, the antibacterial and deodorant improvement is not great, while the radioactivity and physical property decrease are remarkable, which is not preferable.

Hereinafter, the structure and effect of the present invention will be described in more detail with specific examples and comparative examples, but these examples are only intended to more clearly understand the present invention, and are not intended to limit the scope of the present invention.

EXAMPLE

A measuring method for measuring the performance of a multifunctional polyester fiber having antibacterial, deodorizing, light weight, quick drying and heat insulating properties according to the present invention will be described first.

1) particle size distribution:

In order to measure the particle size distribution of the injected particles, an electron microscope (SEM) equipped with an image analyzer was used.

2) Tensile strength, elongation and uniformity of fiber:

Tensile strength / elongation and uniformity of the fibers were tested according to the methods set forth in KS K 0412 and KS K 0467, respectively.

3) Penetration rate:

This is a factor for testing the superiority of the radioactivity of the manufacturing method according to the present invention, which was operated for 48 hours to make the basis weight of 4kg, the ratio of full tube to total output was the full rate.

4) Antibacterial, Deodorant, Lightweight and Warmth:

Fabrics and / or knits were made from the fibers obtained according to examples or comparative examples. The antimicrobial, deodorant, light weight and thermal insulation of the obtained fabrics were tested according to the methods defined in KS K 0693, KICM-FIR-1004, KS K 0514 and KS K 0466, respectively.

5) Absorbent Quick Drying:

It was tested according to JIS L 1096 method.

Example 1

The particle size distribution is 0.01-5.0 μm, the average size is 2.0 μm, and the zeolite inorganic fine particles having 50% or more of the particles having a size of 2.0 μm or less are mixed with a melt of high viscosity polyester (IV 0.79) and mastered. Master Batch Chip (hereinafter referred to as MB chip) was made. MB chips are mixed with general polyester (IV 0.64) to achieve a concentration of 1.0% by weight of the fine particles in the final fiber, and the POY process is carried out through nozzles in brackets (see Fig. 3) at a speed of 3000 m / min at 285 ° C. After spinning to draw ratio of 1.7, stretching temperature 80/120 ℃ (1st / 2nd roller) to prepare a 75d / 36f. The MB chip was supplied using a separate improved auto blender 3 located before the melt extruder as shown in FIG. In the drawings, reference numeral 1 denotes a polyester silo, 2 denotes an MB chip silo, 4, 4 'denotes a motor, 5 denotes an extruder, and 6 denotes a polymer melt pump. 7 represents a spin block, 8 represents a pack. 2 is a cross-sectional view of a polyester fiber, and reference numeral 11 in the drawing denotes a hollow part.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Example 2

MB chips were mixed with general polyester (IV 0.64) so that the concentration of the fine particles in the final fiber was 0.5% by weight, and spun using SDY method at 4000m / min at 286 ° C. Except for the spinning in the same manner as in Example 1 to prepare a polyester fiber of 75d / 36f.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Comparative Example 1

As a general semi-dull chip, 75d / 36f of polyester fiber was prepared by spinning and stretching in the same manner as in Example 1 except that the fiber cross section was rounded using a circular nozzle.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Comparative Example 2

As a general semi-dull chip, 75d / 36f of polyester fibers were produced in the same manner by spinning in the same manner as in Example 2 except that the fiber cross section was rounded using a circular nozzle.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Comparative Example 3

75 d / 36f of polyester fibers were prepared by spinning and stretching in the same manner as in Example 1 except for using a circular spinneret.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Comparative Example 4

A 75d / 36f polyester fiber was prepared by spinning in the same manner as in Example 2 except for using a circular spinneret.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Comparative Example 5

Except for using a particle size distribution of 0.01 to 8㎛, using an average particle size of 4.0㎛, zeolite-based inorganic fine particles of 40% or more particles and a circular spinneret Spinning and stretching in the same manner as 1 to produce a polyester fiber of 75d / 36f.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

Comparative Example 6

Except for the use of zeolite-based inorganic fine particles having a particle size distribution of 0.01 to 8 μm, an average size of 4.0 μm, and particles having a size of 4.0 μm or less, and zeolite-based inorganic fine particles, and a circular spinneret. Spinning was performed in the same manner as 2 to prepare 75 d / 36f of polyester fiber.

Fabrics and / or knitted fabrics were prepared from the obtained fibers, and the physical properties such as antimicrobial and deodorant were evaluated according to the above-described method, and the results are shown in Table 1.

division Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Particle Average Size (㎛) 2.0 2.0 - - 2.0 2.0 4.0 4.0 Particle distribution (%) (less than average particle size) 50 50 - - 50 50 40 40 % Of particles in fiber 1.0 0.5 - - 1.0 0.5 1.0 0.5 MB Supply ○ ○ × × ○ ○ ○ ○ Strength (g / den) 3.9 4.0 4.4 4.6 4.1 4.2 4.0 4.1 10% strength (g / den) 3.2 3.2 3.1 3.1 3.2 3.3 3.2 3.2 Elongation (%) 23 25 32 34 24 26 23 27 Uniformity (%) 1.0 1.1 0.8 0.9 0.9 1.0 1.2 1.1 % Full rate 86 88 95 93 90 91 86 87 % Bacteriostatic bacterium (Staphylococcus aureus) 99 99 62 65 99 99 99 99 Infection rate (%) (pneumoniae) 99 99 28 23 99 98 99 98 Deodorization (%) (NH ₃ removal rate) 94 92 18 22 88 85 88 86 Sweat absorption ^* 1.78 1.80 1.0 0.99 0.94 0.96 1.02 1.03 Quick Dry ^* 1.48 1.52 1.0 1.0 0.94 0.94 0.92 0.94 Lightweight ^* 0.73 0.71 1.0 1.0 1.04 1.02 1.05 1.04 Warmth ^* 1.72 1.68 1.0 0.99 1.06 1.02 1.06 1.04 Shape of cross section Hollow Hollow circle circle circle circle circle circle Pack Pressure Rise radish radish radish radish radish radish U U

^* Absorbency, quick drying, light weight, and heat retention are relative values based on Comparative Example 1 as reference (1.0).

As can be seen from Table 1, in the case of the multifunctional polyester fiber produced by the method according to the present invention, while maintaining excellent polyester inherent physical properties, excellent antibacterial and deodorizing performance, quick drying, light weight and warmth It can be seen that. In particular, it can be seen that the antibacterial deodorant fiber of the hollow fiber cross-sectional cross-sectional shape according to the present invention exhibits superior characteristics compared to the fiber of the circular cross section, and has a synergistic effect between the sweat-absorbing quick-drying, the light weight, and the heat retention and the deodorization. You can expect

Using the method according to the present invention, using a zeolite containing a metal ion, it is possible to produce a polyester fiber having excellent antimicrobial, deodorant, sweat-absorbent quick-drying, lightweight and thermal insulation with a stable spinning workability.

Claims (4)

A polyester masterbatch chip containing zeolite-based inorganic particles having metal ions having a particle size in the range of 0.01 to 5.0 탆, an average particle size of 0.1 to 3.0 탆, and particles having an average particle size of less than 50 wt% or more. Is melted by mixing with a general polyester chip, it is spun into a fiber having a hollow cross-section through a spinneret having a cross-section parenthesis. The method of claim 1 wherein the concentration of inorganic particles in the final polyester fiber is 0.1 to 5% by weight. The method according to claim 1, wherein the hollow ratio of the fiber having a hollow cross section is 5 to 30%. Polyester fibers produced by the process according to claim 1.