KR102122151B1 - polyester composite fiber, non-woven fabric containing the same, and manufacturing method thereof - Google Patents

Abstract

The present invention relates to a polyester composite fiber, a non-woven fabric comprising the same, and a manufacturing method thereof and, more specifically, to a polyester composite fiber which is easy to process at a low temperature (below 200°C), and has excellent shape stability at a high temperature (100 to 150°C), to a non-woven fabric comprising the same, and to a manufacturing method thereof.

Description

A polyester composite fiber, a nonwoven fabric containing the same, and a manufacturing method therefor{polyester composite fiber, non-woven fabric containing the same, and manufacturing method thereof}

The present invention relates to a polyester composite fiber, a nonwoven fabric comprising the same, and a method for manufacturing the same, more specifically, it is easy to process at a low temperature (= 200° C. or less), and has morphological stability at a high temperature (= 100 to 150° C.). Excellent polyester composite fiber, and relates to a non-woven fabric comprising the same and a method for manufacturing the same.

In general, the low melting point (softening point: 110 ~ 180 ℃) because the heat-adhesive processing temperature of polyester fiber is 200 ℃ or less, it should have a lower melting point than ordinary polyethylene terephthalate (PET) fibers. To do this, remove the crystal structure in the polymer and remove the polymer The structure should be made into an amorphous form. In general, in synthesizing the polyester resin for this purpose, the molecular structure of the polyester resin is amorphous by using isophthalic acid instead of terephthalic acid as the acid component or 2-methyl-1,3-propanediol instead of ethylene glycol as the diol component. Form. However, these low-melting polyester fibers have lower glass transition temperature than ordinary polyethylene terephthalate fibers and are used as crystalline polyester-based binder fibers that do not melt at temperatures below 160°C due to poor form stability under high temperature environments. However, it is not suitable for use in interior and exterior materials for automobiles and interior and exterior materials for construction.

In Korean Patent Publication No. 2011-0059368, a polyol containing 1,4-butanediol was condensed to prepare a crystalline low melting point polyethylene terephthalate, and in Korean Patent Publication No. 10-1427793, terephthalic acid and Adi Heat-resistant low-melting polyethylene terephthalate was prepared by copolymerizing an acid component composed of finic acid and a diol component composed of ethylene glycol, neopentyl glycol and 1,4-butanediol. However, when manufacturing the heat-resistant low-melting binder fiber by such a polymerization method, there is a problem in that a facility for storing and inputting 1,4-butanediol, a facility for recovering by-products such as tetrahydrofuran, and the like are required. In particular, tetrahydrofuran is a high-risk material with toxic and explosive properties, making it difficult to manage safety.

In addition, since the heat-resistant low-melting binder fiber has a relatively small market size, there is a disadvantage in that a fixed ratio increases during polymer production by a polymerization method, leading to an increase in cost.

The present invention has been devised to solve the above problems, and the present invention is compounded using a crystalline mixed resin prepared by melt-kneading polybutylene terephthalate (PBT) resin in amorphous polyethylene terephthalate (PET). By manufacturing the fiber, by-products are not generated, process management is easy, and the process is simplified, which not only increases productivity, but also increases production costs in small quantities. It has an object to provide a method for manufacturing it.

In order to solve the above-mentioned problems, the polyester composite fiber of the present invention is a bicomponent fiber comprising a first component resin and a second component resin, the first component resin comprises a polyester resin, and the second component resin is The polybutylene terephthalate (PBT) resin and the amorphous polyethylene terephthalate (PET) resin may include a crystalline mixed resin melt-kneaded in a weight ratio of 35:65 to 65:35.

In a preferred embodiment of the present invention, the first component resin is polyethylene terephthalate (PET) resin, polybutylene terephthalene (PBT) resin, polytrimethylene tereline having an intrinsic viscosity of 0.50 to 1.00 dl/g and a melting point of 200°C or higher. It may include one or more selected from phthalate (PTT) resin and polyethylene naphthalate (PEN) resin.

In a preferred embodiment of the present invention, the amorphous polyethylene terephthalate (PET) resin is an acid component containing 60 to 90 mol% terephthalic acid and 10 to 40 mol% isophthalic acid and 2-methyl-1,3-propanediol 10 It may be prepared by polycondensation reaction of an ester compound and polyethylene glycol (PEG) prepared by esterifying a diol component containing ~ 45 mol% and ethylene glycol 55 to 90 mol%.

In one preferred embodiment of the present invention, the amorphous polyethylene terephthalate (PET) resin is an esterification reaction of an acid component containing 60 to 90 mol% of terephthalic acid and 10 to 40 mol% of isophthalic acid and a diol component comprising ethylene glycol. It may be prepared by a polycondensation reaction of the ester compound and polyethylene glycol (PEG) prepared by.

In one preferred embodiment of the present invention, the amorphous polyethylene terephthalate (PET) resin may have a softening point of 110 to 180°C and an intrinsic viscosity of 0.5 to 1.0 dl/g.

In a preferred embodiment of the present invention, the polybutylene terephthalate (PBT) resin may have a melting point of 213 to 253°C and an intrinsic viscosity of 0.9 to 1.5 dl/g.

In one preferred embodiment of the present invention, the crystalline mixed resin has an intrinsic viscosity of 0.50 dl/g or more, a melting point of 150 to 180°C, and an enthalpy (Enthalpy) required to melt the crystals in DSC (differential thermal analysis) analysis. The value may be 10 J/g or more.

In one preferred embodiment of the present invention, the bicomponent fiber is a sheath-core type fiber, a side-by-side type fiber, a sea-islands type fiber, or It may be a segmented-pie type fiber.

In a preferred embodiment of the present invention, the bicomponent fiber is a sheath-core type fiber, the core comprises a polyester resin, and the sheath may include a crystalline mixed resin.

In a preferred embodiment of the present invention, the average fineness of the polyester composite fiber is 1 to 10 denier (denier), the average fiber length may be 3 to 120mm.

On the other hand, the manufacturing method of the polyester composite fiber of the present invention is the first step of preparing the polyester resin chip and the crystalline mixed resin, respectively, the first component resin and the second component in which each of the polyester chip and the crystalline mixed resin is melted. The second step of manufacturing the unstretched sub-tow by cooling and cooling the resin after the resin is injected into the composite spinneret, and the third step of giving a crimp after stretching the unstretched sub-tow. And a fourth step of heat-setting and cutting and stretching and crimping the sub-tow, wherein the crystalline mixed resin comprises polybutylene terephthalate (PBT) resin and amorphous polyethylene terephthalate (PET) resin. 35: 65 ~ 65: 35 is prepared by melt-kneading and chipping in a weight ratio, the sub-tow may be a sheath-core monofilament, side-by-side monofilament, island-in-sea monofilament or split monofilament.

In a preferred embodiment of the present invention, melt kneading may be performed at a temperature of 260 ~ 290 ℃.

Furthermore, the fiber aggregate of the present invention includes the aforementioned composite fiber.

In addition, the nonwoven fabric of the present invention includes the aforementioned fiber aggregate.

In one preferred embodiment of the present invention, the nonwoven fabric of the present invention may be a dry-laid nonwoven fabric, a wet-laid nonwoven fabric, or an air-laid nonwoven fabric.

In a preferred embodiment of the present invention, the nonwoven fabric of the present invention may have a thickness of 5 to 35 mm and a surface density of 500 to 4000 g/m ² .

On the other hand, the manufacturing method of the nonwoven fabric of the present invention is a first step of manufacturing a nonwoven web by carding a mixed fiber obtained by mixing the polyester composite fiber and polyethylene terephthalate (PET) fiber of the present invention and heat-treating the nonwoven web. It may include a second step of manufacturing a non-woven fabric.

In a preferred embodiment of the present invention, the mixed fiber may be a mixture of the polyester composite fiber and polyethylene terephthalate (PET) fiber in a weight ratio of 40:60 to 60:40.

The polyester composite fiber of the present invention, a non-woven fabric comprising the same, and a method of manufacturing the composite fiber using a crystalline mixed resin, ensure high workability at a low process temperature (200° C. or lower) while high temperature (= 100 to 150) Excellent stability in form and adhesion strength at ℃).

In addition, the polyester composite fiber of the present invention, a nonwoven fabric comprising the same, and a method for manufacturing the same have less process trouble, high productivity, and low manufacturing cost.

In addition, the polyester composite fiber of the present invention, non-woven fabric comprising the same, and its manufacturing method are easy to be widely used as industrial material products such as interior and exterior materials for buildings and interior and exterior materials for automobiles that require shape stability at high temperatures.

1 is a cross-sectional view of a sheath-core composite fiber according to one preferred embodiment of the present invention.
2 is a cross-sectional view of the island-in-the-sea composite fiber according to one preferred embodiment of the present invention.
3 is a cross-sectional view of a side-by-side composite fiber according to one preferred embodiment of the present invention.
4 is a cross-sectional view of a divided pie-shaped composite fiber according to a preferred embodiment of the present invention.
5 is a cross-sectional view of a mosaic-type composite fiber according to a preferred embodiment of the present invention.
6 is a cross-sectional view of a matrix-dispersed composite fiber according to one preferred embodiment of the present invention.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art to which the present invention pertains can easily practice. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. In the drawings, parts not related to the description are omitted in order to clearly describe the present invention, and the same reference numerals are added to the same or similar elements throughout the specification.

The polyester composite fiber of the present invention is a bicomponent fiber comprising a first component resin and a second component resin.

First, the first component resin of the present invention may include a polyester resin, the polyester resin is polyethylene terephthalate (PET) resin, polybutylene terephthalene (PBT) resin, polytrimethylene terephthalate (PTT) It may include at least one selected from resins and polyethylene naphthalate (PEN) resins, preferably selected from polyethylene terephthalate (PET) resins, polybutylene terephthalene (PBT) resins, and polyethylene naphthalate (PEN) resins. It may include one or more, and more preferably may include a polyethylene terephthalate (PET) resin.

In addition, the first component resin of the present invention may have an intrinsic viscosity of 0.50 to 1.00 dl/g, preferably 0.55 to 0.90 dl/g, more preferably 0.65 to 0.75 dl/g, and if the intrinsic viscosity is 0.50 dl/g If it is less than g, there may be a problem that the strength of the polyester composite fiber is lowered, and if it exceeds 1.00 dl/g, there may be a problem of poor spinning and stretching workability.

In addition, the first component resin of the present invention may have a melting point of 200° C. or higher, preferably 230 to 280° C., more preferably 240 to 265° C., and if the melting point is less than 200° C., there is a problem that shape stability decreases. It can be.

In conclusion, it is best to use a polyethylene terephthalate (PET) resin having an intrinsic viscosity of 0.50 to 1.00 dl/g and a melting point of 200°C or higher as the first component resin of the present invention.

Next, the second component resin of the present invention may include a crystalline mixed resin.

The crystalline mixed resin of the present invention may have an intrinsic viscosity of 0.50 dl/g or more, preferably 0.55 to 0.75 dl/g, more preferably 0.58 to 0.65 dl/g, and if the intrinsic viscosity is less than 0.5 dl/g There may be a problem of poor spinning workability.

In addition, the crystalline mixed resin of the present invention has a melting point of 150 to 180°C, preferably 155 to 170°C, and when performing differential thermal analysis (DSC) analysis, an enthalpy value required to melt the crystal is 10 J/g. Above, preferably may be 15 ~ 40 J / g, if the melting point exceeds 180 ℃ when manufacturing a conventional non-woven fabric using the composite fibers of the present invention, there may be a problem that it is difficult to obtain sufficient adhesion , If the melting point is less than 150 ℃, or the enthalpy value is less than 10 J / g, there may be a problem of insufficient heat resistance at a high temperature of 100 ~ 150 ℃.

Meanwhile, the crystalline mixed resin of the present invention may be a polybutylene terephthalate (PBT) resin and an amorphous polyethylene terephthalate (PET) resin melt-kneaded.

Specifically, the crystalline mixed resin of the present invention is polybutylene terephthalate (PBT) resin and amorphous polyethylene terephthalate (PET) resin 35: 65 ~ 65: 35 weight ratio, preferably 40: 60 ~ 60: 40 It may be melt-kneaded by weight ratio, if the weight ratio is less than 35: 65, there may be a problem that crystallinity is not sufficiently expressed, and if it exceeds 65: 35, there may be a problem that the melting point increases.

The polybutylene terephthalate (PBT) resin of the present invention may have a melting point of 213 to 253°C, preferably 223 to 243°C, more preferably 228 to 238°C. In addition, the polybutylene terephthalate (PBT) resin of the present invention may have an intrinsic viscosity of 0.9 to 1.5 dl/g, preferably 1.0 to 1.4 dl/g, and more preferably 1.1 to 1.3 dl/g.

The amorphous polyethylene terephthalate (PET) resin of the present invention may have a softening point of 110 to 180°C, preferably 110 to 170°C, and more preferably 110 to 150°C. Further, the amorphous polyethylene terephthalate (PET) resin of the present invention may have an intrinsic viscosity of 0.5 to 1.0 dl/g, preferably 0.55 to 0.9 dl/g, and more preferably 0.6 to 0.8 dl/g.

In addition, the amorphous polyethylene terephthalate (PET) resin of the present invention may be prepared by a polycondensation reaction of an ester compound and polyethylene glycol (PEG) prepared by esterifying an acid component and a diol component.

At this time, the amorphous polyethylene terephthalate (PET) resin of the present invention may contain 1 to 10 parts by weight of polyethylene glycol (PEG), preferably 3 to 6 parts by weight, with respect to 100 parts by weight of the ester compound, if polyethylene If it contains less than 1 part by weight of glycol (PEG), there is a problem that it is difficult to perform a subsequent weight loss process, and if it contains more than 10 parts by weight, polymerization reactivity decreases and the glass transition temperature of the amorphous polyethylene terephthalate (PET) resin becomes too low. There may be a problem that the thermal stability may be poor.

In addition, the polyethylene glycol (PEG) of the present invention may have a weight average molecular weight of 400 to 12,000, preferably 600 to 2,000.

In addition, the acid component and the diol component may have a molar ratio of 1: 1.0 to 2.0, preferably 1: 1.1 to 1.5, and if the molar ratio is less than 1: 1.0, the polymerization degree decreases due to a decrease in polymerization reactivity, and thus a targeted secret. Qualitative polyethylene terephthalate (PET) resin may be difficult to manufacture or the strength of the manufactured resin may be low, and when it exceeds 1: 2.0, side reaction products such as diethylene glycol used may occur, and trimming is performed during the spinning process. It may cause the workability to be remarkably lowered, and there may be a problem that may lead to an increase in manufacturing cost due to the use of an excess of diol components.

In addition, the acid component of the present invention may contain 60 to 90 mol% of terephthalic acid, preferably 60 to 80 mol%, more preferably 65 to 70 mol%, based on the total mol% of the acid component.

In addition, the acid component of the present invention may contain 10 to 40 mol%, preferably 20 to 40 mol%, more preferably 30 to 35 mol% of isophthalic acid, based on the total mole% of the acid component. If the content of isophthalic acid is less than 10 mol%, the crystallinity increases, but the melting point may be excessively increased. If it exceeds 40 mol%, the crystallinity of the amorphous polyethylene terephthalate (PET) resin may be impaired. Can be.

Further, the diol component of the present invention may include ethylene glycol, and may further include 2-methyl-1,3-propanediol.

In addition, when ethylene glycol and 2-methyl-1,3-propanediol are included as the diol component, 2-methyl-1,3-propanediol is preferably 10 to 45 mol% with respect to the total mole% of the diol component, preferably May include 15 to 40 mol%, more preferably 20 to 36 mol%, and 55 to 95 mol% of ethylene glycol, preferably 60 to 85 mol%, more preferably with respect to the total mol% of diol components It may contain 64 to 80 mol%. If 2-methyl-1,3-propanediol is included in an amount of less than 10 mol%, crystallinity increases, but a melting point may be excessively increased. If it exceeds 45 mol%, amorphous polyethylene terephthalate (PET) resin There may be a problem that the crystallinity of the.

Meanwhile, the second component resin of the present invention may further include functional additives (for example, catalysts, antioxidants, chain extenders, etc.) in addition to the crystalline mixed resin, thereby improving reaction extrusion efficiency or/and improving physical properties. .

Specifically, when the catalyst is included, the catalyst may contain 0.01 to 0.1 parts by weight, preferably 0.02 to 0.05 parts by weight, based on 100 parts by weight of the crystalline mixed resin.

In addition, when containing an antioxidant, the antioxidant may contain 0.1 to 2.0 parts by weight, preferably 0.5 to 1.0 parts by weight based on 100 parts by weight of the crystalline mixed resin.

In addition, when the chain extender is included, the antioxidant may contain 0.5 to 5.0 parts by weight, preferably 1.0 to 2.0 parts by weight, based on 100 parts by weight of the crystalline mixed resin.

Furthermore, the polyester composite fiber of the present invention is a bicomponent fiber comprising a first component resin and a second component resin, sheath-core type fiber, side-byside type It may be a fiber, a sea-islands type fiber or a segmented-pie type fiber, preferably a sheath-core type fiber or a side-by-side type fiber, and more preferably a sheath-core type. It can be a mold fiber.

Specifically, Figure 1 is a cross-sectional view of a sheath-core (Sheath-Core) type composite fiber according to an exemplary embodiment of the present invention, as shown in Figure 1 sheath-core (Sheath-Core) type composite fiber , Preferably, the first component resin may be the core 21, and the second component resin may be the sheath 20. At this time, more preferably, the core 21 includes a polyester resin that is a first component resin, and the sheath 20 may include a crystalline mixed resin that is a second component resin.

In addition, Figure 2 is a cross-sectional view of the island (Island in the Sea) type composite fiber according to a preferred embodiment of the present invention, in the case of island (Island in the Sea) type fiber, more preferably dissolve the second component resin It may be an island-in-the-sea type fiber made of powder 30 and a first component resin as an island component 31.

In addition, Figure 3 is a cross-section of a side by side (Side by side) type composite fiber according to a preferred embodiment of the present invention, Figure 4 is a segmented pie (segmented pie) type composite fiber cross-section, Figure 5 is a mosaic type Cross-sectional view of the composite fiber, Figure 6 is a matrix-dispersed cross-sectional view. In the case of the composite fiber form shown in Figs. 3 to 6, since the positions formed separately are the same, the second component resin (40 in Fig. 4) and the first component resin (41 in Fig. 4) of the present invention are preferable. If the weight ratio is satisfied, the position in which the first component resin and the second component resin are included may not be particularly limited.

On the other hand, the average fineness of the polyester composite fiber of the present invention may be 1 to 10 denier, preferably 1 to 5 denier, and if the average fineness is less than 1 denier, there is a problem that the radioactivity and productivity are lowered. When it is more than 10 denier, the adhesive strength may be non-uniform and deteriorated when manufacturing a nonwoven fabric.

In addition, the average fiber length of the polyester composite fiber of the present invention may be 3 to 120 mm, preferably 3 to 50 mm, and more preferably 3 to 35 mm, and if the average fiber length is less than 3 mm, sufficient composition is exhibited when manufacturing the nonwoven fabric. There may be a problem that is not, and if it exceeds 120mm, there may be a problem in dispersibility.

Furthermore, the present invention may include a fiber aggregate such as a nonwoven fabric containing the polyester composite fiber of the present invention mentioned above.

At this time, the nonwoven fabric of the present invention may be a dry-laid non-woven fabric, a wetaid non-woven fabric, or an air-laid non-woven fabric, preferably a thermal bonding non-woven fabric, needle-punching. punching) may be a dry non-woven fabric such as a non-woven fabric.

In addition, the nonwoven fabric of the present invention may have a thickness of 5 ~ 35mm, preferably a thickness of 10 ~ 30mm, 500 ~ area density of 4000g / m ^2, preferably the area density of 1000 ~ 3000g / m ^2, and, if this If it is less than the range, there may be a problem that the strength decreases, and if it exceeds this range, there may be a problem that the productivity and workability decrease.

Furthermore, the method for producing the polyester composite fiber of the present invention includes the first to fourth steps.

First, in the first step of the method for producing a polyester composite fiber of the present invention, a polyester resin chip and a crystalline mixed resin can be prepared, respectively.

At this time, the characteristics, types, etc. of the polyester chip are the same as those of the first component resin described above, and chipped, and the characteristics, types, etc. of the crystalline mixed resin are the same as those of the second component resin described above. .

Specifically, the crystalline mixed resin melts the polybutylene terephthalate (PBT) resin and the amorphous polyethylene terephthalate (PET) resin in a weight ratio of 35:65 to 65:35, preferably 40:60 to 60:40. It can be prepared by kneading.

The melt kneading may be performed using a stationary kneader or an extrusion kneader, and when a stationary kneader is used, the higher the number of divisions, and when using an extrusion kneader, using a twin-screw extrusion kneader is an ester by reaction extrusion. The efficiency of the exchange reaction can be increased.

In addition, melt kneading may be performed at a temperature of 260 to 290°C, preferably 270 to 285°C, and if the temperature is less than 260°C, the reaction extrusion efficiency may be lowered and productivity may be a problem, and if it exceeds 290°C Due to deterioration by thermal decomposition, there may be a problem in that physical properties are deteriorated and/or discoloration occurs.

Next, in the second step of the method for manufacturing the polyester composite fiber of the present invention, the first component resin and the second component resin, each of which melted the polyester chip and the crystalline mixed resin, are put into the composite spinning pad and compound spinning is performed. , Cooled to produce an unstretched sub-tow.

In the second step of melting, the polyester resin chip and the crystalline mixed resin can be performed under 260 to 330°C, preferably 270 to 300°C.

In addition, the composite spinning in the second step can be performed under conditions of a spinning temperature of 260 to 300°C and a winding speed of 500 to 1800 m/min, preferably 275 to 290°C and a winding speed of 1000 to 1600 m/min. At this time, if the spinning temperature is less than 260 °C (pack) there may be a problem that the pressure rise and the workability is lowered, if the spinning temperature exceeds 300 °C there may be a problem that the physical properties of the composite fiber is lowered. In addition, if the winding speed is less than 500 m/min, the elongation increases and there may be a problem that the properties of the composite fiber and/or the application product using the same decrease, and if the winding speed exceeds 1800 m/min, the unstretched sub-tow There may be a problem in that the form stacked on the can is non-uniform and thus the drawability is deteriorated.

The complex spinning in the second step can be performed through various types of detention, and the sub-tow produced according to the form of detention is a sheath-core type monofilament, side-by-side type monofilament, sea-island monofilament or split It may be a type monofilament, preferably a sheath-core type monofilament through a sheath-core type detention.

Next, in the third step of the method for producing the polyester composite fiber of the present invention, after stretching the unstretched sub-tow, crimp may be applied.

At this time, stretching may be performed by stretching the unstretched sub-tow at 2.5 to 5 times under 70°C to 100°C, preferably at 3.0 to 4.5 times. At this time, if the draw ratio is less than 2.5 times, the elongation increases, the physical properties of the application product using the composite fiber may decrease, and if the draw ratio exceeds 5.0 times, there may be a problem of trimming, so that the draw is performed within the above range. It is good.

In addition, the crimping may be performed through a general crimping method used in the art.

Finally, the fourth step of the method for producing the polyester composite fiber of the present invention can heat-fix and cut the stretched and crimped sub-tow.

At this time, the drawn and crimped sub-tow can be performed for 10 to 20 minutes under 140°C to 180°C, preferably after 140°C to 170°C, after being introduced into the oven. At this time, if the heat setting temperature is less than 140 ℃, there may be a problem that the shrinkage rate of the final composite fiber is produced, if it exceeds 180 ℃, the dispersibility of the composite fiber is lowered, the composite fiber density of the fiber aggregate falls, workability Since there may be a problem of falling, it is preferable to perform heat setting under the above temperature range.

In addition, the cutting of the fourth step is a process of cutting a subtow that is heat-set so that the composite fiber has an appropriate fiber length according to the processed product to use the composite fiber, and can be performed by a general cutting method used in the art. , It is preferable to cut the average fiber length of the composite fiber within a range of 3 mm to 120 mm.

On the other hand, the manufacturing method of the nonwoven fabric of the present invention is the first step of preparing the nonwoven web by carding the mixed fiber obtained by mixing the polyester composite fiber and polyethylene terephthalate (PET) fiber of the present invention mentioned above and the nonwoven fabric. And a second step of manufacturing a nonwoven fabric by heat-treating the web.

At this time, the polyethylene terephthalate (PET) fiber mixed with the mixed fiber has an average fineness of 2 to 12 denier (de), preferably 2 to 5 denier, and an average fiber length of 3 to 120 mm, preferably 20 to 70 mm, crimp The number may be 9 to 15/inches, preferably 10 to 14/inches.

In addition, the heat treatment may be performed through a tenter process, in the tenter process, the temperature of the tenter inlet is 150 to 190°C, preferably 160 to 180°C, and the temperature of the tenter outlet is 180 to 220°C, Preferably it may be 190 ~ 210 ℃.

In addition, the mixed fiber of the present invention may be a mixture of the polyester composite fiber and the polyethylene terephthalate (PET) fiber of the present invention in a weight ratio of 40:60 to 60:40, preferably 45:55 to 55:45. .

In the above, the present invention has been mainly described with reference to embodiments, but this is merely an example and does not limit the embodiments of the present invention, and those having ordinary knowledge in the field to which the embodiments of the present invention pertain will provide essential characteristics of the present invention. It will be appreciated that various modifications and applications not illustrated above are possible without departing from the scope. For example, each component specifically shown in the embodiments of the present invention can be implemented by modification. And differences related to these modifications and applications should be construed as being included in the scope of the invention defined in the appended claims.

Preliminary Preparation Example 1: Preparation of amorphous polyethylene terephthalate (PET) resin

(1) The acid component and the diol component were added at a molar ratio of 1:1.2, and mixed and esterified under a temperature of 250° C. and a pressure of 1140 torr to prepare an ester compound, and the production rate was 97.5%.

At this time, as the acid component, 33 mol% of isophthalic acid and 67 mol% of terephthalic acid were used relative to the total mol% of the acid component. Moreover, 100 mol% of ethylene glycol was used with respect to the total mol% of diol components as a diol component.

(2) Into the prepared ester compound, polyethylene glycol (PEG) and antimony trioxide (polycondensation catalyst) having a weight average molecular weight of 1,000 are added, and the pressure is gradually reduced to a final pressure of 0.5 torr. An amorphous PET resin having a softening point of 120°C and an intrinsic viscosity of 0.65 dl/g was produced by condensation reaction.

At this time, 5 parts by weight of polyethylene glycol (PEG) with respect to 100 parts by weight of the ester compound was used.

Preparative Example 2: Preparation of amorphous polyethylene terephthalate (PET) resin

(1) The acid component and the diol component were added at a molar ratio of 1:1.2, and mixed and esterified under a temperature of 250° C. and a pressure of 1140 torr to prepare an ester compound, and the production rate was 97.5%.

At this time, as the acid component, 33 mol% of isophthalic acid and 67 mol% of terephthalic acid were used relative to the total mol% of the acid component. Further, as the diol component, 67 mol% of ethylene glycol and 33 mol% of 2-methyl-1,3-propanediol were used based on the total mol% of the diol component.

(2) Into the prepared ester compound, polyethylene glycol (PEG) and antimony trioxide (polycondensation catalyst) having a weight average molecular weight of 1,000 are added, and the pressure is gradually reduced to a final pressure of 0.5 torr. An amorphous PET resin having a softening point of 118°C and an intrinsic viscosity of 0.63 dl/g was prepared by condensation reaction.

At this time, 5 parts by weight of polyethylene glycol (PEG) with respect to 100 parts by weight of the ester compound was used.

Preparation Example 1: Preparation of crystalline mixed resin

PBT resin having a melting point of 233°C and an intrinsic viscosity of 1.21 dl/g, amorphous PET resin prepared in Preparative Example 1, and functional additives (catalyst, antioxidant, chain extender) were mixed with a mixer, and twin-screw extrusion kneading was performed. It is melt-kneaded at a temperature of 280°C, and in DSC (differential thermal analysis) analysis, the enthalpy value required to melt the crystal is 27 J/g, the melting point is 161°C, and the intrinsic viscosity is 0.62 dl/g. A crystalline mixed resin was prepared.

At this time, the crystalline mixed resin contains PBT resin and the amorphous PET resin prepared in Preparative Example 1 in a weight ratio of 50:50, and PBT resin and 100 parts by weight of the amorphous PET resin prepared in Preparative Example 1 , 0.03 parts by weight of catalyst, 0.5 parts by weight of antioxidant, and 1.0 parts by weight of chain extender.

Preparation Example 2: Preparation of crystalline mixed resin

A crystalline mixed resin was prepared in the same manner as in Preparation Example 1. However, instead of the amorphous PET resin prepared in Preparative Example 1, a crystalline mixed resin was prepared using the amorphous PET resin prepared in Preparative Example 2, thereby dissolving the crystal during DSC (differential thermal analysis) analysis. A crystalline mixed resin having an enthalpy value of 25 J/g, a melting point of 159°C, and an intrinsic viscosity of 0.62 dl/g was prepared.

Preparation Example 3: Preparation of crystalline mixed resin

A crystalline mixed resin was prepared in the same manner as in Preparation Example 1. However, in the case of melt kneading, it was prepared by performing at a temperature of 300°C rather than a temperature of 280°C. Through this, in DSC (differential thermal analysis) analysis, the enthalpy value required to melt the crystal is 6 J/g, A crystalline mixed resin having a melting point of 148°C and an intrinsic viscosity of 0.54 dl/g was prepared.

Preparation Example 4: Preparation of crystalline mixed resin

A crystalline mixed resin was prepared in the same manner as in Preparation Example 1. However, in the case of melt kneading, it was manufactured by performing at a temperature of 250°C rather than a temperature of 280°C. Through this, in DSC (differential thermal analysis) analysis, the enthalpy value required to melt the crystal is 32 J/g, A crystalline mixed resin having a melting point of 212°C and an intrinsic viscosity of 0.73 dl/g was prepared.

Preparation Example 5: Preparation of crystalline mixed resin

A crystalline mixed resin was prepared in the same manner as in Preparation Example 1. However, the crystalline mixed resin was prepared by including the PBT resin and the amorphous PET resin prepared in Preparative Example 1 in a weight ratio of 30:70, and through this, when analyzing differential thermal analysis (DSC), the enthalpy required to dissolve the crystal ( Enthalpy) A crystalline mixed resin having a value of 5 J/g, a melting point of 179°C, and an intrinsic viscosity of 0.59 dl/g was prepared.

Preparation Example 6: Preparation of crystalline mixed resin

A crystalline mixed resin was prepared in the same manner as in Preparation Example 1. However, the crystalline mixed resin was prepared by including the PBT resin and the amorphous PET resin prepared in Preparative Example 1 in a weight ratio of 70:30, and through this, when analyzing DSC (differential thermal analysis), the enthalpy required to melt the crystal ( Enthalpy) A crystalline mixed resin having a value of 35 J/g, a melting point of 215°C, and an intrinsic viscosity of 0.85 dl/g was prepared.

Example 1: Preparation of sheath-core type polyester composite fiber

(1) A PET chip obtained by chipping a PET resin having an intrinsic viscosity of 0.65 dl/g and a melting point of 252°C was prepared.

(2) The prepared PET chips are melted at 290° C., the crystalline mixed resin prepared in Preparation Example 1 is transferred, and they are introduced and spun into a sheath-core composite spinneret, and then cooled to cool the sheath-core type unstretched. -A subtow was prepared.

At this time, the composite spinning was combined spinning under a spinning temperature of 285°C and a winding speed of 1000 m/min, and then loaded into a can through a take-up process.

(3) The prepared cis-core type unstretched-subtoe was stretched at an area ratio of 1:1 and 3.5 times at a temperature of 85°C, and then subjected to heat treatment at a temperature of 130°C for 10 seconds.

(4) The stretched sub-tow was crimped using a spuffing box.

(5) Next, the drawn and crimped sub-tow was put in an oven, and then heat-set at 165° C. for 15 minutes to give an average fineness of 3 denier, an average fiber length of 6 mm, and a sheath-core poly having an average number of crimps of 12/inch. Ester composite fibers were prepared. At this time, the cross-sectional area ratio of the sheath and the core was 5:5, the sheath was composed of a crystalline mixed resin resin, and the core was composed of a PET resin.

Example 2: Preparation of sheath-core polyester composite fiber

In the same manner as in Example 1, sheath-core polyester composite fibers were prepared. However, the sheath-core type polyester composite fiber was prepared by using the crystalline mixed resin prepared in Preparation Example 2 rather than the crystalline mixed resin prepared in Preparation Example 1.

Comparative Example 1: Preparation of sheath-core type polyester composite fiber

In the same manner as in Example 1, sheath-core polyester composite fibers were prepared. However, the sheath-core type polyester composite fiber was prepared by using the crystalline mixed resin prepared in Preparation Example 3 rather than the crystalline mixed resin prepared in Preparation Example 1.

Comparative Example 2: Preparation of sheath-core type polyester composite fiber

In the same manner as in Example 1, sheath-core polyester composite fibers were prepared. However, the sheath-core type polyester composite fiber was prepared using the crystalline mixed resin prepared in Preparation Example 4 rather than the crystalline mixed resin prepared in Preparation Example 1.

Comparative Example 3: Preparation of sheath-core type polyester composite fiber

In the same manner as in Example 1, sheath-core polyester composite fibers were prepared. However, the sheath-core type polyester composite fiber was prepared using the crystalline mixed resin prepared in Preparation Example 5 rather than the crystalline mixed resin prepared in Preparation Example 1.

Comparative Example 4: Preparation of sheath-core type polyester composite fiber

In the same manner as in Example 1, sheath-core polyester composite fibers were prepared. However, the sheath-core type polyester composite fiber was prepared using the crystalline mixed resin prepared in Preparation Example 6 rather than the crystalline mixed resin prepared in Preparation Example 1.

Comparative Example 5: Preparation of sheath-core type polyester composite fiber

In the same manner as in Example 1, sheath-core polyester composite fibers were prepared. However, a sheath-core type polyester composite fiber was prepared using the amorphous PET resin prepared in Preparative Example 1 rather than the crystalline mixed resin prepared in Preparation Example 1.

Experimental Example 1: radioactivity measurement

The spinning properties of the cis-core type polyester composite fibers prepared in Examples 1 to 2 and Comparative Examples 1 to 5 were respectively measured and are shown in Table 1 below. The radioactivity was evaluated by the average number of trimmings when 1 ton was emitted. The number of times of trimming is less than 1 is indicated by ○, the number of times of trimming is 2-3, △, and X is greater than 4 times.

division Example
One Example
2 Comparative example
One Comparative example
2 Comparative example
3 Comparative example
4 Comparative example
5 Radioactive ○ ○ △ ○ ○ △ ○

As can be seen in Table 1, it was confirmed that the sheath-core polyester composite fibers prepared in Comparative Examples 1 and 4 had poor spinning properties.

Production Example 1: Preparation of non-woven fabric

(1) The cis-core type polyester composite fiber and polyethylene terephthalate (PET) fiber prepared in Example 1 were carded with a mixed fiber mixed in a weight ratio of 50:50 to prepare a nonwoven web.

At this time, the polyethylene terephthalate (PET) fibers used were those having an average fineness of 3 denier (de), an average fiber length of 51 mm, and a crimp number of 12/inch.

(2) The prepared nonwoven web was heat treated in a tenter to produce a nonwoven fabric having a thickness of 10 mm and a surface density of 800 g/m ² . In the tenter process, the temperature of the tenter inlet was 170°C and the temperature of the tenter outlet was 200°C.

Production Example 2: Preparation of non-woven fabric

A nonwoven fabric was prepared in the same manner as in Production Example 1. However, a non-woven fabric was prepared using the sheath-core type polyester composite fiber prepared in Example 2, not the sheath-core type polyester composite fiber prepared in Example 1.

Manufacturing Comparative Example 1: Preparation of non-woven fabric

A nonwoven fabric was prepared in the same manner as in Production Example 1. However, a non-woven fabric was prepared using the sheath-core type polyester composite fiber prepared in Comparative Example 1, not the sheath-core type polyester composite fiber prepared in Example 1.

Manufacturing Comparative Example 2: Preparation of non-woven fabric

A nonwoven fabric was prepared in the same manner as in Production Example 1. However, a non-woven fabric was prepared using the sheath-core type polyester composite fiber prepared in Comparative Example 2, not the sheath-core type polyester composite fiber prepared in Example 1.

Manufacturing Comparative Example 3: Preparation of non-woven fabric

A nonwoven fabric was prepared in the same manner as in Production Example 1. However, a non-woven fabric was prepared using the sheath-core type polyester composite fiber prepared in Comparative Example 3, not the sheath-core type polyester composite fiber prepared in Example 1.

Manufacturing Comparative Example 4: Preparation of non-woven fabric

A nonwoven fabric was prepared in the same manner as in Production Example 1. However, a non-woven fabric was prepared using the sheath-core type polyester composite fiber prepared in Comparative Example 4, not the sheath-core type polyester composite fiber prepared in Example 1.

Production Comparative Example 5: Preparation of non-woven fabric

A nonwoven fabric was prepared in the same manner as in Production Example 1. However, a non-woven fabric was prepared using the sheath-core type polyester composite fiber prepared in Comparative Example 5, not the sheath-core type polyester composite fiber prepared in Example 1.

Experimental Example 2: Evaluation of adhesive strength

After cutting the nonwoven fabrics prepared in Production Examples 1 and 2 and Comparative Examples 1 to 5 to a length of 100 mm and a width of 20 mm, the tensile strength was measured in a tensile strength measuring machine to evaluate the adhesive strength, and the results are shown in Table 2. Did. The adhesive strength passing criterion was set to 300 N or more, and 300 N or more was indicated by ○, and in other cases, x.

Experimental Example 3: Heat resistance evaluation

After cutting the nonwoven fabrics prepared in Production Examples 1, 2 and Comparative Examples 1, 3, and 5 to a length of 150 mm and a width of 25 mm, respectively, after standing at a temperature of 90° C. for 8 hours, the degree of drooping of the cut nonwoven fabric was measured. Measured by length, heat resistance was evaluated, and the results are shown in Table 2. The sagging length of the non-woven fabric cut by the heat resistance passing criteria was set to 10 mm or less.

The non-woven fabrics prepared in Comparative Examples 2 and 4 had low adhesive strength and could not be evaluated for heat resistance.

Experimental Example 4: Acceptance judgment

In accordance with the adhesive strength and heat resistance evaluation results of the non-woven fabrics prepared in Manufacturing Examples 1 to 2 and Comparative Examples 1 to 5, joint determination was performed. ○, in other cases, x was used.

division Produce
Example
One Produce
Example
2 Produce
Comparative example
One Produce
Comparative example
2 Produce
Comparative example
3 Produce
Comparative example
4 Produce
Comparative example
5 Adhesive strength ○ ○ ○ × ○ × ○ Heat resistance Specimen sag height
(mm)
5
13
16
-
18
-
25 Judgment ○ ○ × × × × ×

As can be seen in Table 2, it was confirmed that the nonwoven fabrics prepared in Production Examples 1 and 2 had excellent adhesive strength and heat resistance.

Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be considered to be included in the scope of the present invention.

Claims (13)

A bicomponent fiber comprising a first component resin and a second component resin,
The first component resin includes a polyester resin,
The second component resin includes a crystalline mixed resin in which polybutylene terephthalate (PBT) resin and amorphous polyethylene terephthalate (PET) resin are melt-kneaded in a weight ratio of 35:65 to 65:35,
The crystalline mixed resin has an intrinsic viscosity of 0.58 to 0.65 dl/g, a melting point of 150 to 180°C, and when analyzing differential thermal analysis (DSC), an enthalpy value required to melt the crystal is 15 to 40 J/g. Polyester composite fiber, characterized in that.
According to claim 1,
The first component resin is polyethylene terephthalate (PET) resin, polybutylene terephthalene (PBT) resin, polytrimethylene terephthalate (PTT) resin and polyethylene naphthalate having an intrinsic viscosity of 0.50 to 1.00 dl/g and a melting point of 200°C or higher. (PEN) A polyester composite fiber comprising at least one selected from resins.
According to claim 1,
The amorphous polyethylene terephthalate (PET) resin
Esterification of diol components containing 60-90 mol% terephthalic acid and 10-40 mol% isophthalic acid and 10-45 mol% 2-methyl-1,3-propanediol and 55-90 mol% ethylene glycol Ester compounds prepared by reaction; And
Polyethylene glycol (PEG); polyester composite fiber, characterized in that produced by the polycondensation reaction.
According to claim 1,
The amorphous polyethylene terephthalate (PET) resin
An ester compound prepared by esterification reaction of an acid component containing 60 to 90 mol% of terephthalic acid and 10 to 40 mol% of isophthalic acid with a diol component containing ethylene glycol; And
Polyethylene glycol (PEG); polyester composite fiber, characterized in that produced by the polycondensation reaction.
According to claim 1,
The amorphous polyethylene terephthalate (PET) resin is a polyester composite fiber characterized in that the softening point is 110 ~ 180 ℃, intrinsic viscosity of 0.5 ~ 1.0dl / g.
According to claim 1,
The polybutylene terephthalate (PBT) resin is a polyester composite fiber, characterized in that the melting point is 213 ~ 253 ℃, intrinsic viscosity 0.9 ~ 1.5dl / g.
delete According to claim 1,
The bicomponent fiber is a sheath-core fiber, a side-by-side fiber, a sea-islands fiber, or a segmented-pie fiber. Polyester composite fiber, characterized in that.
The method of claim 8,
The bicomponent fiber is a sheath-core type fiber,
The core includes a polyester resin, and the sheath comprises a crystalline mixed resin.
According to claim 1,
The polyester composite fiber has an average fineness of 1 to 10 denier, and an average fiber length of 3 to 120 mm.
A fiber aggregate comprising the composite fiber of claim 1.
Non-woven fabric comprising the fiber assembly of claim 11.
The method of claim 12,
The non-woven fabric is a non-woven fabric, characterized in that it has a thickness of 5 ~ 35mm, a surface density of 500 ~ 4000g / m ² .

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