KR920007108B1 - Producing process of polyester fiber - Google Patents

Abstract

The preparing method of polyester fiber with good heat retaining property by distributing evenly of far-infrared radiating ceramic particles into the fiber is characterized; incorporating and dispersing of transitional metal oxides belonged to IV family in periodic table, or carbide whose addition amount against polyester polymer is 0.1-60 wt.% into the polyester polymer, while affinity imparting additive polymer whose adding amount against that of metal oxide or carbide is 0.1-30 wt.% and which is expressed as formulas of A(Y)m(OCOR)n [m = n = 1-3; A= transitional metal belonged to IV family in periodic table; Y= C1-5 roxyl gp.; R= C1-5 methyl or methoxy gp. being added to the ceramic particles, that is, transitional metal oxidesor carbides.

Description

Manufacturing method of polyester fiber excellent in heat retention

The present invention relates to a method for producing polyester fibers having excellent thermal insulation properties such that ceramic fine particles radiating far-infrared rays are uniformly distributed in the polyester fibers using a polymer affinity aid in the process of producing the polyester fibers.

In general, ceramics, in terms of their function, absorb energy of visible rays and near infrared rays of relatively short wavelength, which are highly energy efficient in sunlight, and replace and radiate them with far-infrared rays which are hot rays. By re-reflecting even the heat, it is effective for health promotion by promoting blood flow along with excellent warmth.

As a conventional method for producing a polyester fiber having such excellent thermal insulation, firstly, according to Japanese Patent Laid-Open No. 63-35810, a far-infrared radiation ceramic particle is coated on a fiber structure, or a ceramic particle is coated on a film or the like. And then laminating with other fiber structures.

This method has the advantage of easy handling and technical application, but the problem of dropping ceramic particles due to friction or washing, and the touch is also not good.

Further, according to Japanese Patent Laid-Open No. 63-203873, a method of coating a ceramic filament with a thermoplastic polymer material, wherein the filament formed by melting the ceramic material at a temperature above the melting point, extruding and solidifying the coating is passed through a melting tank of the thermoplastic polymer material. Way.

This method requires a high temperature treatment apparatus to melt the ceramic and is not suitable for use in clothing because the fibers are inflexible and feel bad even after the fiberization.

On the other hand, according to Japanese Patent Application Laid-Open No. 63-196710, a ceramic particle is granulated, uniformly dispersed in a thermoplastic polymer material, spun and stretched to form a fiber. This method is advantageous to industrialization, is durable against friction and washing, and has no problem with touch. However, this method has a relation that agglomeration between ceramic particles occurs in the polymer material, and the spinning pressure is increased during spinning.

The problem in introducing the ceramic fine particles in the yarn production is closely related to the content of the ceramic fine particles in the fiber.

When the content is relatively small, the process yield such as spinning workability and stretching is good, but it is insufficient to obtain effects such as thermal insulation.

On the other hand, in the case of distributing excess ceramic fine particles, agglomeration occurs between ceramic particles in the polymer, resulting in poor spin workability and weakening of various physical properties of the fiber.

As a method of distributing the ceramic fine particles in a polymer material, there are a method of introducing into a polymer polymerization process, a method of mixing with a basic polymer material after master pelletizing, and a method of feeding into a spinning material.

In this way, when ceramic fine particles are distributed in ceramic material, ceramic fine particles do not have affinity with polymer and aggregate due to interaction between particles, thus forming coarse particles in polymer material. It causes the deterioration.

In view of this, the present inventors used transition metal oxides or carbides belonging to group IV of the periodic table as ceramic fine particles, and the polymer affinity aid of the general formula (I) shown below was uniformly distributed in polyester. Agglomeration of the ceramic fine particles in the polyester is prevented and uniformly distributed, thereby producing far-infrared radiation polyester fibers having excellent operability and good physical properties.

Where m and n are integers from 1 to 3, A is a Group IV transition metal on the periodic table, Y is a hydroxyl group or a hydroxyl group containing 1-5 carbon atoms, and R is a methyl group or 1-5 carbon atoms It is a methoxy group.

The ceramic fine particles used in the present invention are group IV transition metal oxides or carbides on the periodic table, and specific examples include zirconium oxide, titanium dioxide, zirconium carbide, and titanium carbide, and the amount of the polymer added is 0.1 to 60% by weight, preferably 0.5-50 weight%, More preferably, it is 1-30 weight%.

However, if less than 0.1% by weight can not be expected thermal effect, if it exceeds 60% by weight spinning workability worsens.

Specific examples of the polymer affinity aid used in the present invention include hydroxy zirconium methyl carbonate, hydroxy zirconium methoxy carbonate, hydroxy titanium lithium carbonate, hydroxy titanium methyl carbonate, and the addition amount is added to the added ceramic fine particles. 0.1 to 30% by weight, preferably 1 to 20% by weight, more preferably 2 to 10% by weight.

When the affinity aid is added less than 0.1% by weight, the ceramic fine particles are not uniformly dispersed in the polyester, forming coarse particles, resulting in poor spin workability, and when the affinity aid is added in excess of 30% by weight, the ceramic particles are uniform in the polyester. It is dispersed, but the physical properties of the polyester is lowered, spinning workability is worse.

Yarn produced by the present invention was prepared using a conventional spinneret, the cross-sectional shape can be produced in any existing shape, such as circular, triangular, oval. The present invention can be used in applications requiring heat retention, such as winter clothes, ski suits, winter uniforms, work clothes and curtains by combining the polyester fibers produced alone or in combination with ordinary fibers in the desired fabric, knitted fabric in the same way as conventional It is the most suitable for use in a cold area because the human body generates heat by causing the heat-molecule movement by the far-infrared emission effect.

Prior to describing specific examples of the present invention, the average particle diameter of the additives in the examples was measured as follows.

Ten milligrams of the polymer sample was placed between 18 × 18 mm sized microscopy covers and thermally bonded on a hotplate at 280 to 300 ° C. to prepare a film, and then the size of 100 additives was measured by a phase contrast microscope to obtain an average value.

In addition, the thermal insulation evaluation was performed for 3 minutes with a high-efficiency reflecting lamp having a center wavelength of 1 micron and a capacity of 500 watts on a fabric woven from the yarn manufactured according to the present invention in a constant temperature chamber maintained at 36 ° C. and a conventional fabric having the same structure. Then, the temperature distribution of each fabric surface is measured by an infrared thermograph (Thermograph, manufactured by NEC-San ei, Model 6T62).

The temperature values in Examples and Comparative Examples represent the surface temperature of each sample fabric as an average value per unit area.

Parts in the examples represent weight percent.

Example 1

100 parts of ethylene glycol and 20 parts of zirconia having a primary average particle diameter of 40 microns are charged into a stirrer, followed by stirring for 1 hour to obtain an ethylene glycol slurry (a).

Zirconia fine particles (c) are uniformly added by adding the above slur to a wet mill with a large number of disks on a rotating spindle, adding 6 parts of trihydroxy zirconium methyl carbonate to the amount of zirconia, and then stirring for 8 hours or more. Prepare the dispersed slurry (b).

Separately, 100 parts of terephthalic acid, 180 parts of ethylene glycol, 0.18 parts of sodium acetate, and 0.02 parts of zinc acetate were added to the glass flask to which the rectification column was attached to perform a transesterification reaction, and after removing the theoretical amount of water, the reaction product was attached to the rectification column. The zirconia fine particle slurry (b) prepared above was introduced into the above-mentioned polycondensation flask three times so that the zirconia fine particle (c) was 0.01-60 parts with respect to the polyester polymer, and 0.001 part of phosphoric acid and antimony trioxide as a polycondensation catalyst were added. 0.1 part was added.

The mixture was subjected to a polycondensation operation under normal pressure for 20 minutes at 280 ° C. for 15 minutes under a reduced pressure of 30 mmHg, and for 120 minutes under high vacuum, and the final pressure was 0.25 mmHg.

The polymer thus produced is pelletized in a conventional manner and dried in a conventional manner, and then the pellet is used as the central portion of the yarn and the ordinary polyester pellet is used as the outer portion at a content ratio of 50:50, with a spinning speed of 1.500 m. Melt-combined spinning at / min produced 225 d / 36 f of undrawn yarn, and then stretched at a computation ratio of 3.0 to obtain 75 d / 36 f of drawn yarn.

The stretched yarn was woven under the same conditions as in a conventional polyester fabric containing no zirconium compound, and thermal insulation was evaluated according to Japanese Industrial Standard, JIS L 1413.

Table 1 shows the overall physical properties of the yarn and the warmth of the fabric according to the addition amount of the zirconia fine particles (c).

In Table 1, the amount of zirconia fine particles (c) added is based on the weight of the polymer.

TABLE 1

(Legend: ◎; Very good, ○; Good, △; Normal)

Comparative Example 1

Except that the ordinary pellets prepared in Example 1 without the addition of the zirconia microparticles and the polymer affinity aid were spun as a single component, all the same experiments, and the results are shown in Table 2.

TABLE 2

(Legend: ◎; Very good, ×; Poor)

Comparative Example 2

Except not adding the polymer affinity aid used in Example 1 and all the same experiments, the results are shown in Table 3.

The addition amount of c in Table 3 is addition amount with respect to a polymer weight.

TABLE 3

(Legend: ○; Good, △; Normal, ×; Poor)

Example 2

20 parts of the zirconia fine particles (c) used in Example 1 were added to the polyester polymer, and trihydroxy zirconium methyl carbonate, a polymer affinity aid, was added to the zirconia fine particles, respectively, 0.01, 0.1, 1, 5, 10, All experiments were the same except that 20, 30, 40 parts were added and spun, and the results are shown in Table 4.

The addition amount of the polymer affinity aid in Table 4 is based on the zirconia addition weight.

TABLE 4

(Legend: ◎; Very good, ○; Good, △; Normal, ×; Poor)

Claims (3)

In preparing polyester fibers by dispersing transition metal oxides or carbides belonging to group IV of the periodic table, the polymer affinity aid represented by the following general formula (I) is used. Method for producing polyester fiber. next

Provided that m and n are integers from 1 to 3, A is a transition metal belonging to group IV of the periodic table, Y is a hydroxyl group, or a hydroxyl group containing 1-5 carbons, R is a methyl group, or 1-5 carbons Methoxy group containing. The method for producing a polyester fiber having excellent thermal insulation according to claim 1, wherein the amount of transition metal oxide or carbide of Group IV on the periodic table is 0.1 to 60% by weight relative to the polymer. The method according to claim 1, wherein the amount of the polymer affinity aid added is 0.1 to 30% by weight based on the amount of the transition metal compound or carbide of the group IV on the periodic table.