KR20080062809A - Polyester fiber and method of manufacturing the same - Google Patents

Abstract

A polyester fiber and a manufacturing method thereof are provided to prevent the lowering of light shield performance from generating by adding inorganic particles with the shield property. A polyester resin compound is supplied to a spinning nozzle. The spinning nozzle changes the polyester resin compound into the spinning yarns and discharges. The polyester resin compound consists of polyester polymer, phosphorous group flame retardant, UV(Ultraviolet) stabilizer and shield inorganic particles. The resin compound is passed through an injection nozzle and changed into the spun yarns with the predetermined cross-section. The flat cross-section spinning yarn is defined by long shaft(a)/short shaft(b). The polyester spinning yarn(300) includes at least two or more curved portions(310) protruded convexly. The spinning yarn includes six curved portions on a surface thereof, preferably. The curved portions are also formed at front and back sides of the spinning yarn. Further, the UV(Ultraviolet) stabilizer is manganese phosphate and the shield inorganic particle is titanium dioxide.

Description

Polyester fiber and method of manufacturing the same

1 is a conceptual diagram of a fiber manufacturing apparatus shown to show a manufacturing process of a polymer fiber according to an embodiment of the present invention.

2 is a cross-sectional view showing a cross section of a general discharge yarn.

3 is a cross-sectional view showing a cross-section of the emitting yarn according to an embodiment of the present invention.

<Explanation of symbols for the main parts of the drawings>

110: spinning nozzle 120: emulsion supply device

132: first high roller 134: second high roller

140: winder 310: bend

The present invention relates to a polyester fiber and a method for producing the same, and more particularly, to a flame retardant polyester fiber and a method for producing the same excellent in the scratch resistance without deteriorating light transmission performance.

The method of imparting flame retardancy to fibers may be performed by post-treatment after fiber products are made, by adding a flame retardant in a spinning step of fiberizing, and preparing a polymer for fiber (mainly a polymerization step) ) And copolymerization with a monomer containing a flame retardant component.

In the case of synthetic fibers, the flame retardancy of the fiber product by the additive material mainly used is the method of filling the inorganic material and the method of adding the flame retardant which is an organic material. It is coming true.

In addition, in order to add shielding property to polyester fiber, the method of adding in-vehicle inorganic fine particles is used. Car-shielding means the function of not seeing the inside from the outside at the boundary of the fabric.

In particular, when the inorganic fine particles are contained in a small amount, the on-vehicle performance is lowered, so an appropriate amount should be added. However, when the inorganic fine particles are used in an excessive amount to impart the on-board property, the on-board performance is excellent, but light transmission is difficult, resulting in a problem in that the mining performance is poor.

The present invention has been made in view of the above problems, and an object of the present invention is to provide a polyester fiber which is excellent in light performance and does not reduce light blocking property.

The present invention also aims to provide a method for producing the polyester fiber.

Polyester fiber according to an aspect of the present invention is a cross-section that is produced by a resin composition comprising a polyester polymer, a phosphorus-based flame retardant, a UV stabilizer, and an interstitial inorganic fine particles, comprising at least two bent portions It consists of a plurality of emitting yarns having a shape.

As said phosphorus flame retardant, the compound represented by following formula (1) can be used.

In the above formula, R1 is hydrogen or a hydroxy alkyl group having 1 to 10 carbon atoms,

R <2> is hydrogen, a C1-C10 alkyl group, or a C6-C24 aryl group, R <3> is hydrogen, a C1-C10 alkyl group, or a hydroxy alkyl group.

Manganese phosphate may be used as the UV stabilizer. The manganese phosphate concentration in the resin composition is preferably 0.1 to 500 ppm on the basis of manganese atoms.

It is preferable that the said on-vehicle inorganic fine particles contain 0.3 weight% or less in the said polyester resin composition. In addition, titanium dioxide can be used as said on-vehicle inorganic fine particles.

The emitter comprises three to six bends on one side of the cross section.

Method for producing a polyester fiber according to an aspect of the present invention comprises the steps of preparing a resin composition comprising a polyester polymer, a phosphorus-based flame retardant, a UV stabilizer and an interstitial inorganic fine particles, a plurality of cross-sections of the emitter released Releasing the resin composition to form a plurality of discharge yarns, and combining the plurality of discharge yarns to provide a polyester fiber yarn so that a bent portion of the resin can be formed.

Manganese phosphate may be used as the UV stabilizer, and the manganese phosphate is prepared by adding the manganese acetate and phosphoric acid to the reactor, respectively, during the polymerization reaction for the production of the polyester polymer without being directly added to the polyester polymer.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

1 is a conceptual diagram of a fiber manufacturing apparatus shown to show a manufacturing process of a polymer fiber according to an embodiment of the present invention.

The fiber manufacturing apparatus includes a spinning nozzle 110, an emulsion supply device 120, a first roller roller 132, a second roller roller 134, and a winder 140.

The spinning nozzle 110 is supplied with a polyester resin composition according to the present invention, and the spinning nozzle 110 converts the polyester resin composition into a discharge yarn and discharges it.

The polyester resin composition includes a polyester polymer, a phosphorus flame retardant, a UV stabilizer, and an interstitial inorganic fine particle.

Flame retardants currently industrially used to impart flame retardancy are largely divided into halogen-based and phosphorus-based flame retardants. Halogen-based flame retardants are expanding their use due to the generation of toxic gases during combustion.

Therefore, in this invention, it is preferable to use a phosphorus flame retardant, and especially the phosphorus flame retardant represented by following formula (1). The following flame retardants have the advantage of good purity and reactivity with ethylene glycol (EG).

[Formula 1]

In the above formula, R1 is hydrogen or a hydroxy alkyl group having 1 to 10 carbon atoms,

R2 is hydrogen, an alkyl group having 1 to 10 carbon atoms, or an aryl group having 6 to 24 carbon atoms, and R3 is hydrogen, an alkyl group having 1 to 10 carbon atoms, a hydroxy alkyl group, or an ester-forming functional group.

The flame retardant polyester polymer of the present invention preferably contains 500 to 50,000 ppm of the phosphorus-based flame retardant represented by Chemical Formula 1 relative to the polyester polymer on the basis of phosphorus atoms.

In addition, a manganese salt or a phosphorus compound may be used as the UV stabilizer, and in particular, manganese phosphate may be used in the present invention.

The content of the manganese salt and phosphorus compound is preferably 0.1 ~ 500ppm based on the manganese and phosphorus atoms.

In this embodiment, titanium dioxide is used as the onboard inorganic fine particles. The content of titanium dioxide is preferably 0.3% by weight or less in the resin composition. Therefore, the polyester fiber produced according to the present invention does not cause a decrease in mining performance. On the other hand, due to the predetermined cross-sectional structure of the emitting yarns constituting the fiber, the excellent shielding property can be maintained.

The content of phosphorus flame retardant introduced into the polymer is preferably 500 to 50,000 ppm based on phosphorus atoms relative to the polymer regardless of the structure of the phosphorus flame retardant, especially from the viewpoint of polymerization process and yarn production from 1,000 to 1,000 phosphorus atoms relative to the polymer. 10,000 ppm is more preferable. If the phosphorus atom content is less than 500ppm compared with the polymer, excellent flame retardant effect cannot be expected, and if it reaches a certain content, it is difficult to expect further flame retardancy.In particular, if it exceeds 50,000ppm, it is difficult to increase the degree of polymerization of the produced polyester and crystallinity. It is too low to produce a problem that is difficult to produce into fibers, which is undesirable.

In addition, in the case of interior products that require flame retardancy, since the purpose of mining and car (遮 狀), the stability of the polymer is important when exposed to sunlight, especially UV, and therefore the addition of UV stabilizer is important.

As mentioned above, it is preferable to use manganese phosphate as a UV stabilizer. In the case of the manganese phosphate was not dissolved in ethylene glycol as a solvent it was difficult to add into the polymer. Therefore, the present invention uses a method of synthesizing manganese phosphate in the reaction system by adding manganese acetate and phosphoric acid separately in the reaction tank, rather than adding manganese phosphate to the reaction tank.

The content of manganese acetate used for the synthesis of manganese phosphate is preferably 0.1 to 500ppm, more preferably 0.2 to 200ppm based on the manganese atoms in the polymer. If it is less than 0.1ppm, it is difficult to obtain the desired UV stability, and if it exceeds 500ppm, there is a problem in dispersibility, which results in poor spinning processability.

In addition, the content of phosphoric acid is preferably in the range of 0.1 to 500ppm content of the number of people in the polymer. More preferably, the range of 0.2-200 ppm is good. The content of the phosphorus-based material may be added as long as the reaction with manganese salt is not a problem, but if it exceeds 500 ppm, the activity of the catalyst is lowered, making it difficult to prepare a desired flame retardant polyester.

The content of titanium dioxide is preferably in the range of 0.3% by weight or less and more preferably in the range of 0.1% by weight or less for excellent light performance. If the content of the inorganic fine particles is more than 0.3% by weight, the object of the present invention cannot exhibit the light properties.

The resin composition is converted into a discharge yarn having a predetermined cross-sectional shape while passing through the spinning nozzle 110. In order to have a predetermined cross-sectional shape, the inside of the spinning nozzle 110 is provided with a shape corresponding to the cross-sectional shape so that a cross-section of a desired shape can be output.

2 is a cross-sectional view showing a cross section of a general discharge yarn.

Referring to FIG. 2, in the case of a general flat cross-section emitting yarn 200, the flatness is defined by a long axis a and a short axis b, that is, a / b.

3 is a cross-sectional view showing a cross-section of the emitting yarn according to an embodiment of the present invention.

However, unlike the flat cross-section yarns of FIG. 2, the polyester yarns 300 according to an embodiment of the present invention include at least two bent portions 310 that protrude convexly. Preferably, the discharge yarn 300 preferably includes three to six bent portions 310 on one surface. Of course, the bent portion 310 may be formed on both the front and rear of the discharge yarn (300).

Unlike the general flatness, in order to more accurately define the bent portion 310 of the present invention, the "deformation degree" property is newly defined. In other words, the degree of release is defined as b / c by the thickest part (b) and the thinnest part (c) of the bending in FIG. 3.

The preferred range of release degree is preferably 1.0 to 3.0, more preferably 1.05 to 2.0. If the degree of release is 1.0, it has the same cross section as the existing plain flat yarn, and if it is larger than 3.0, the connection between the filaments is difficult and the appearance quality is poor.

The polyester fiber yarn of the present invention can be either a 1-Step radial direct drawing method for simultaneously spinning and drawing, or a 2-Step method for drawing after drawing a non-drawn yarn, but for convenience of description, the following is based on the radial direct drawing method. To explain.

Melting the dried polyester polymer at 280 ~ 300 ℃ to discharge so that the discharge amount per minute from the spinning nozzle 110 0.4 ~ 0.6g / min.hole, the temperature of the cooling air to 0.25 ~ 0.5m / s and then The emulsion is impregnated directly under the spinning nozzle 110, and the quenched polymer is heated to a stretching temperature of 70 to 100 ° C. in the first gourd roller (132) and 110 to 150 ° C. in the second gourd roller (134). A polyester fiber is manufactured by setting the speed difference between the roller roller 132 and the second roller roller 134, that is, the soft mystery to 1.5 to 3.0.

The plurality of discharge yarns are combined into one unit fiber while passing through the emulsion supply device 120.

In addition, the manufactured unit fibers are wound by the winding machine 140.

Before describing the present invention in detail through the following examples, a method for evaluating the performance of the fibers provided in the test will be described.

(Example)

Prior to the description of the examples, methods for evaluating the performance of polymers and fibers provided in the test will be described.

(1) Strength and elongation: It was measured according to KS K 0412.

(2) Deformation degree: The ratio between the thickest part and the thinnest part of the bend, that is, the degree of curvature is calculated as the degree of release (see FIG. 3).

(3) Spinning workability: The polymer prepared according to the test method was dried in a vacuum dryer to have a moisture content of 30 ppm or less, and then spun using an extruder having an inner diameter of 95 mm. If the number of rounds is less than 5 times in a week, ◎, 5 ~ 10 times, △, and X are above.

(4) Flame retardant: The fabric was tested according to KS M ISO 4589-2: 2001 of Korea to evaluate the LOI (Limited Oxyden Index).

(5) Sunlight yellowing: In order to determine the effect of sunrays by inorganic particles, the prepared polymer was stretched on a glass plate and exposed to UV for 48 hours in QUV of Q-Panel Co. Judgment was judged as yellowing when the change of b value was greater than 1.5 among L, a, and b values by a color difference meter.

(6) Lightability: Calculate the light transmittance obtained by subtracting the measured shading rate (%) from 100% after evaluating the shading rate (%) of the manufactured textile products according to KS K 0819 standard of Korea.

(7) Carborneness: First, a black standard plate is applied to the back side of the fiber and white light is measured to measure its reflectance (Lb), and then the white standard plate is irradiated instead of a black standard plate to measure its reflectance (Lw), and then the two reflectances are measured. Is defined as the opacity index (Lt). It was judged to be excellent when the degree of delamination of the woven fabric was 12 or less.

[Examples 1 and 2]

The slurry prepared with 1300 g of TPA and 560 g of EG was subjected to an esterification reaction by a semibatch method. In the esterification reactor, an oligomer prepared in the same composition as the slurry was stirred, and the temperature of the esterification reactor was maintained at 250 to 260 ° C. After the slurry addition was completed, the esterification reaction was further performed for 30 minutes, and the esterification reaction rate was 97%. 1.5 tons of the prepared oligomer was left in the DE-1 reactor and the remainder was transferred to the DE-2 reactor. As a flame retardant, 68 Kg of a flame retardant having R1 = H, R2 = phenyl group and R3 = H in Chemical Formula 1 was first reacted with EG 68 Kg, and then the reaction solution was added thereto, and 20 ppm of manganese acetate and phosphoric acid were used as UV stabilizers on an atomic basis. , 100ppm, titanium dioxide was added as shown in Table 1, followed by stirring at 260 ° C, and then the whole oligomer in the DE-2 tank was transferred to the polycondensation reactor, and then the antimony tree dissolved in EG as a catalyst at 2% by weight. 200 g of an oxide solution was added and vacuum was started. Polymerization was prepared by polycondensation in the same manner as in a conventional polyester polymerization reaction.

Flame-retardant polyester fiber yarn having a cross-section as shown in FIG. 3 was prepared by spinning using the flame-retardant polyester polymer prepared, and the fire-retardant polyester flammable yarn 75/72 produced by Hyosung Co., Ltd. After weaving, we evaluated the performance such as lightness and shielding property, and are shown in Table 1.

Comparative Example 1

The same process as in Example 1 was conducted except that the phosphorus content of the flame retardant polyester polymer was prepared to be 400 ppm.

Comparative Example 2

The same procedure as in Example 1 was carried out except that manganese acetate and phosphoric acid were not added during the flame retardant polyester polymerization.

Comparative Example 3

The same procedure as in Example 1 was carried out except that the titanium dioxide content of the inorganic fine particles in the flame retardant polyester polymer was prepared to be 3.0% by weight.

[Comparative Example 4]

As a manufacturing method of general polyester fiber, the stretched yarn which has a circular cross-sectional shape was manufactured using the flame-retardant polyester polymer used in Example 1. Table 1 shows the results of weaving and evaluating the yarn as a weft yarn and using flame retardant polyester flammable yarn 75/72 produced by Hyosung Co., Ltd. as a slope.

As described above, the polyester fibers produced according to the present invention have excellent flame retardancy, light properties and onboard performance. In particular, by adding a small amount of the on-vehicle inorganic fine particles by the cross-sectional structural characteristics of the fiber, the on-vehicle performance is maintained, while the lightness is not deteriorated.

As described above, although the present invention has been described with reference to limited embodiments and drawings, the present invention is not limited to the above embodiments, and those skilled in the art to which the present invention pertains various modifications and variations from such descriptions. This is possible. Therefore, the scope of the present invention should not be limited to the described embodiments, but should be determined not only by the claims below but also by the equivalents of the claims.

Claims (9)

It is manufactured by the resin composition containing a polyester polymer, a phosphorus flame retardant, a UV stabilizer, and a phase-breaking inorganic fine particle, A polyester fiber composed of a plurality of discharge yarns having a cross-sectional shape including at least two bends. The method of claim 1, The phosphorus-based flame retardant is a polyester fiber, characterized in that the compound represented by the following formula.

(In the above formula, R1 is hydrogen or a hydroxy alkyl group having 1 to 10 carbon atoms, R2 is hydrogen, an alkyl group having 1 to 10 carbon atoms, or an aryl group having 6 to 24 carbon atoms, and R3 is hydrogen, an alkyl group having 1 to 10 carbon atoms, or a hydroxy alkyl group.) The method of claim 1, The polyester stabilizer, characterized in that the UV stabilizer is manganese phosphate. The method of claim 3, Manganese phosphate concentration in the resin composition is a polyester fiber, characterized in that 0.1 to 500 ppm on the basis of the manganese atoms. The method of claim 1, The said on-vehicle inorganic fine particles are contained less than 0.3 weight% in the said polyester resin composition, The polyester fiber characterized by the above-mentioned. The method of claim 1, The said on-vehicle inorganic fine particles are polyester dioxide, It is characterized by the above-mentioned. The method of claim 1, Wherein said yarn comprises three to six bends on one side of said cross section. Preparing a resin composition comprising a polyester polymer, a phosphorus-based flame retardant, a UV stabilizer, and phase-set inorganic fine particles; Releasing the resin composition to form a plurality of discharge yarns so that a plurality of bends may be formed on a cross section of the discharge yarns emitted; And Combining the plurality of discharge yarns to provide polyester fiber yarns. The method of claim 8, The UV stabilizer is prepared by adding the manganese acetate and phosphoric acid to the reaction tank, respectively, during the polymerization reaction for the production of the polyester polymer.

Images